(SANITIZED)SOVIET METALLURGICAL RESEARCH AND EXPERIMENTS(SANITIZED)

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• Document Number (FOIA) /ESDN (CREST): CIA-RDP80T00246A002700010001-0
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• Document Page Count: 238
• Document Creation Date: December 21, 2016
• Document Release Date: July 31, 2008
• Sequence Number: 1
• Publication Date: January 6, 1958
• Content Type: REPORT

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A New Method of Investigation of the Chemical
Composition in the Micro Volume. of An Alloy
By I. B. Borovskii and N. P. Ilyin
?
?
(From ACADEMY OF SCIENCES USSR REPORTS 106, (4+) 655-657 (1956))
The development of the theory of solids as well as practical prob-
lems for producing alloys with special properties require the de-
velopment of special investigation methods as well as analysis of
the atomic and electronic structure and of the micro composition of
metals, alloys, compounds. .The existing physical methods of investi-
gation were directed in the majority to the study of atomic and
electronic structures of solids.
In 1951, a new method was suggested by one of the authors (1) in the
USSR and simultaneously in France (2), consisting in an X-ray-
spectral quantitative analysis of the composition at a "point" which
permits to carry out quantitative determination of the majority of
elements of the Mendeleev periodic system in the region of the size
of a few microns.
In the following, we developed an apparatus and the method of in-
vestigation permitting determination of the chemical composition in
the micro volume of the sample based on the characteristic X-ray
radiation, excited by a focused electron beam in a volume of 10
with the sensitivity of .1%. The developed method gives a possi-
bility of determining the content of various elements at a given spot
of the sample, as well as the distribution of a given element in
various parts of the sample.
For analyzing the composition at the "point", one of the procedures
of the regular X-ray spectroscopy is used (3). A schematic presenta-
tion of the arrangement worked out by,us is shown in Figure 1. The
electron beam (3.T..= electronic "cannon" or tube) is focused by one
or two electromagnetic lensesjlon the polished anode of the X-ray
tube A. which is arranged on a special plate serving as a holder for
the samples. By means of microscrews the anode can be moved hori-
zontally; a motor with a reducing gear is attached to one of the
handles permitting a continuous motion of the anode-sample in the
chosen direction at a speed of 10 to 201A/minute keeping it under the
electron beam. The holder is arranged to carry simultaneously 3
samples, a fluorescent screen and a frame with a net for control
pictures of the focus size. The following items are mounted into the
X-ray tube: A small mirror 3 and a metallographic microscope M of
special construction with a long focus lens; the microscope itself is
arranged outside the vacuum. Its rigid mounting ensures superposi-
tion of the objective cross hair with the mirror image of the focal
spot; on the sample-anode. For measuring the electron current passing
the tube, a Faraday cylinder is used, which is connected to constant
current amplifier. For resolving the X-ray into a spectrum, a
spectrograph with a bent crystal was constructed using the reflection
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Appendix 2 - Page 2
method. The rigid crystal is bent along a cylindrical surface with
the radius of 300mm. 2 movable arms of the spectrograph which are
connected with each other, carry the microfocus tube and the photon
counter. The kinematic and vacuum arrangement permit simultaneous
moving of the 2 arms toward each other along equal angles. The turn-
ing is achieved by hand or by means of a motor with a reducing and
reverse gear.
All leading devices from the low voltage as well as high voltage
side, are stabilized, the stabilization percent being not lower than
.05%. High voltage for the tube can be changed from 30 to 50 kilo-
watt. The electron current within the tube reaches lj4 ampere. The
diameter of the focal point on the anode is 2-4,u (determined b the
method of the shadow image of the wire mesh having 5,,Adiameter).
The average specific charge of the sample anode equals 1 kilowatt/mm2.
For recording intensities of characteristic lines the block appratus
URS-50-I is used, permitting determination of the intensities by
.direct or conversion method, or by recording the spectrum on self-
registering electronic potentiometer. Varying speeds of the sample
motion and of the chart permit to vary widely the "enlargement" of
the observed recording of the element distribution in the sample.
Maximum "enlargement" is 2.104.
At optimum conditions the intensity of the line Kd, of a pure element
is 104-l05 pulses per second. Therefore, at higher contents of the
element to be determined at a given spot of the sample it is neces-
sary to work with smaller specific charges (weaker currents through
the tube). The accuracy of this analysis, determined by the
stability of leading devices and recording arrangement, when checked
experimentally was found to be 2-5%.
In Figure 2 a point spectrogram of a multi-component alloy is shown
illustrating the work of the invented apparatus.
In Figure 3 results of a "point" analysis of another multicomponent
alloy are shown. Curve A shows the intensity changesof the line Ni
K1I(RC=4 seconds, the scale 1000 pulses per second) by moving the
sample under an electron beam. Curve S - shows the intensity changes
of the line tungsten Lot, (RC=2 seconds, scale 200 pulses/second) in
the same area of the sample. Comparing these results with a micro-
photograph of the sample, it is possible to draw conclusions, that
the inclusions observed in the sample represent a phase enriched in
W and with a decreased content of the Ni base.
Thus, the apparatus and method worked out permit not only a quantita-
tive analysis of the composition at the "point" with an accuracy of
.1% (which corresponds to 10=13g of the element at the "point"), but
also the distribution of the given element within the sample. In-
vestigations were carried out with a series of multicomponent alloys
of metals and of metal-ceramics, welds, diffusion layers, to deter-
mine distribution of elements Fe, Ni, Cu,-Zn, Nv, Ms, W, Re in micro
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Appendix 2 - Page 3
samples and in given directions. Results of these investigations
have shown large possibilities of this new method for solving prob-
lems which cannot be solved by other existing methods of physico-
chemical analysis.
Bibliography:
1. I.B.Borovskii, Collective volume. "Problems in Metallurgy",
dedicated to Acad. I.P.Bardin on his 70th birthday.
Publisher Acad. Sciences USSR,1953?
2. R.Castaing, A.Guinier, Anal.Chem. 25,#5 724 (1953).
3. I.B.Borovskii, M.A.Blokhin, X-Ray Spectral Analysis, (1939).
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BHTC51 B pa6o4ee npOCTpaIICTBO npH6opa Ha noUuiKy. Be iH4HHa AaBJIeHHH
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Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
 0
0
Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
APP i~ .
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Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
 Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
B OHOpHOH noAyWKe HJIH B HaKOH 4HHKe nyaHCOHa. OXnaxcI aeMas BOAOH HanpaB-
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Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
 Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
A P' ice..
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Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
 Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
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Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
 Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
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Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
 Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
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(DHr. 152. CTpyKTypa MgZn2 [43]. cocTOBHHHx. B pa6oie OCHOBHOe BHH-
MaHxe 6blJlo yge.nexo AByM BonpocaM:
BJIHHHHIO KHH2THKH yCTaHOBJIeHHH paBHOBCCHH Ha BHA AHarpaMMbl Mg - Zn,
a T8K)Ke AHarpaMM COCTflB - MCXflIIH4eCKHe CBOI3CTBa H H3y9eHH10 BJIHRIIIIH
TeMnepaTypbl Ha MCX8HH4eCKHe CBONCTBa 6oramix McTaJIJIH4eCKHMH COeAHHe-
HHHMH CnJIaBOB.
1'1CCJIeAOBaHHH npOBOAHJIHCb Ha 25 CnjjaBaX, paCno.no)t a cucme.ua.C c ,+ IemannuaecKtLuu ccedunexuR.uu 227
MapKH Mr-1 (99,9% Mg) Ii LHHKa MapKH 4-1 (99,94% Zn). fIJlaBKa Benacb B
THreJIbHOii 3JIeKTponetiii B rpa(pHTOBbIx THr.njix nog nOKpOBOM npe.I BapHTeJIbHO
o6e3BO>KeHHoro KapHaJIJIHTOBOrO (piuoca. COCTaB CnJIaBOB KOHTPOJIHpOBaJlcn
XHMIi4eCKHM aHaJIH30M. O6pa3ubl je(j)opMI1pOBaJIHCb nyTeM ropitlero
npeCCOBaHH53 Ha yCTaHOBKe, nOKa3aIInoii Iia (plir. 27. 3ai atla 3Ta OKa-
3aJ1aCb BeCbMa Tpy. HOii, TaK KaK AJISI noJlygeHHA CpaBHHMb1X AaHHbIX Bce cnJia-
Bbl I aHHOri CHCTeMbI AOJI)KHbI 6bIJII! 6btTb o6pa6OTaHb1 B oAHHaKOBb1x yCJIOBHSIX,
KOTOpble JIHMHTHPOBa.IHCb nJIaCTI1t1HOCTb10 Ha116oJiee XpynKOrO cnjlaBa. 1-103TOMy
npHLHJIOCb npOH3BeCTH npeABapIITeJlbxoe onpo60BaHHe Bcex cniiaBOB,
Har1TH OHTHMaJIbHble YCJIOBH51 nJ1aCTHtieCKOro ,T1e4DOpMHpOBaHH$ AJISI Kaxcgoro
H JIHLLIb noc ie 3TOrO Bb16paTb o61uHe AJI$3 Bcex YCJIOBHH noJlytieHH$3 o6pa3uoB
H HX HCnbITaHHii. Ha Bb1pa60TICy McTOAHKH H YCTaHOBJIeHIie OHTHMaJIbHbIX H
CpaBHHMbIX yCJIOBHA YU1J1O B o61uef4 CJIO)KHOCTH 6oJlblue BpeMenH, tieM Ha HCnbl-
TaHHH.
B pe3yJlbTaTe npeABapHTeJibHbIX OnbITOB 6bIJIO yCTaHOBJIeHO, 11TO npH npa-
BHJ1bHO Bb16paHHb]X YCJIOBHHX npeCCOBaHHH (TeMnepaTypa, CKOpOCTb, CTeneHb
Ae4 opMaLLHH H HaAJIe)KaLuasl CMa3Ka) Bce OTJIHTble cnJlaBbI MOryT 6bITb no iytieHbl
B BHAe Ao6pOKaueCTBeHHbIX npyTKOB. 1-1paBAa, BCe 1Ke HeKOTOpble JIHTbie CnJ1aBb1
He BbIAep)KHBaJIH 60JIbule 50% o63icaTH31. 1103TOMy AJIH no.lytieHHS3 6oJlbwero
3( eKTa OT Ae(popMauMH 6bIJio BBeAeHO npeccOBaHHe B ABa npxeMa. B nepsOM
nepexoAe CJIHTOK AHaMeTpoM 22 M npoIaBJ1HBaJicH 4epe3 MaTpHuy AHaMeTpoM
15 MM, T. e. o6)KHMaJICS1 npH6JIH3HTeJIbHO Ha 50% . BO BTOPOM nepexOAe no.ny-
ti2HHble npyTKH CriJlaBa npeccOBaJIHCb B 11 H6ope c AHaMeTpOM BHyTpeHHerO
OTBepCTHH 15 MM tiepe3 MaTPHL[y C AHaMeTPOM OtiKa 10 MM, T. e. TaK)Ke Ha 50%.
B KatieCTBe CMa3KH npH npeCCOBaHHH npHMeH$IJIaCb CMeCb rpa(pHTa H MaiuHHHOTO
MacJia. 110JIyt1eHHb1e O6pa3ubl HCnOJIb3OBaJIHCb Aim onpeAeJIeHH$ TBepAOCTH H
AaBJIeHHSH HCTegeHH51 CnJIaBOB B Ae(popMHPOBaHHOM COCTOHHHH npH pa3JIHtIHbIX
TeMnepaTypaX. rlpe000BaHHe o6pa3IOB H onpeAejieHHe gaBJIeHHS3 HCTetieHHH
npOH3BOAHJIHCb npH TeMnepaTypaX Ha 15-200 HH)Ke TOYKH nJIaBJIeHHH. J1JI51
npHBeAeHHSH CnJIaBOB B paBHOBeCHoe COCTO$3HHe npHMeHHJICSH OT)KHr. 110 J1HTe-
paTyPHbIM AaHHbIM, AJIA JIHTbIX cniiaBOB 3TOri CHCTeMbI Tpe6yeTCSI OtIeHb AJ1HTeJ1b-
Hb1ik OT)KHr - AO 90 CYTOK [4021. C L1eJlbIO yCKOpeHHR npoueccoB AH(pcpy3HH
>Ke.IaTeJlbHO oT)KHraTb CnJIBBbi npH Han6onee BbICOKHX TeMnepaTypaX. Ho, ytlH-
TbIBasi, t1T0 CnJIaBb1 CHCTeMbI MarHHri - LLHHIC 311agHTeJlbHO pa3JIHgaioTCSI n0 TeM-
nepaTypaM n.IaaneHHR, BO H36e)KaHHe nepe> Kra OHH 6bIJIH pa36HTb1 Ha tleTbipe
rpynnbl; B Ka)KAoii rpynne HaXOAHJIHCb cn.iaBb! C 6JIH3KHMH TeMnepaTypaMH
nJIaBJIeHHH. O'r u r cnJIaBOB npOH3BoAHJIC$3 npH TeMnepaTypaX, YK83aHHbIX
B Ta6J1. 50.
Ta6JIHga 50
YCJIOBHA OT%Hra cnJIaBOB CHCTeMbI Mg - Zn
TeMnepaTypa
oTxcara, ?C
npoAOnx(eTe.nb-
HOCTb OTNCBra
Ycnoaxst ox-
nax(Aexex
o6pa34oa
OT 20 Ao 72,89. .
300
OxJIawAeane
OT 72,89 Ao 84,74.
320
5, 10 H 20
BMeCTe c ne-
OT 84,74 AO 92,7 .
340
f CYTOK
9b1O B Te4e-
OT 92,7 AO 100. . .
335
HHe AByx
CYTOK
0
O6pa3IZb1 HarpesaJIHCb noA cJloeM nopoluxa OKHCH aJIuOMHHHSI; IueJib Me)KAy
KOpnyCOM H KPb1HIKOit My(peJIH 3aMa3bIBaJiacb rJIHHOri. CTeneHb AOCTH)KeHHSI
paBHOBeCHSH KOHTpOJIHpOBaJlaCb meTOAOM MHKpOCTpyKTypbl. Cn.naB C9HTaJICS1
16'
Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
 0
?
0
Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
A- i /,,
Our. 153. MHKpOCTpYKTypa CHJIdBOB CIICTIIMb1 iNg-Zn (B pa3J1H9HbIX COCTORHHHX)X6OO.
a -- 45,6 Bee. % ZH
I) JIHTOII (a + 9BTCKTHKa); 2) J(ef(IOPMHPOBaHHblh-(n + 3HTeKTIIKa); 3) OTOH(M(CHHbI{i ((l + 98TCKTKKa).
6 - 76,8 Bee. % Zn
1) JIHTON (MgZn + 9BTeKTHKa); 2) )I,4OPMIipOBaHHW{I (MgZn + 9BTeKTHKa); 3) OTOH(MCeHHWWIi (MgZn).
a - 85 Bee. % Zu
I) JIIITO6 (MgZ112 + 9BTeKTHKa); 2) JlefpOPMHPOBaIIHFdii (MgZny); 3) OTOB(8(eHHb1N (MgZny).
Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
 ?
?
?
Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
1 5 3 . MHKpocrpyKTypa cnjlaBOB CHCTCMbI Mg - Zn (B p83JIH4HbIX COCTOHHHAX) X 600.
- 93,1 sec. % Zn
1) AecbopMHpoaaHHMA, OTON(NKeuHb11I 5 CYTOK (MgZn,+MgZn,); 2) Ae4)opMnposaHHMN, OTOXC)KeHHMII 10 cyTOK
(MgZn,); 3) Ac()opm1JposanHMA, OTO)K)KCHHMN 20 CyTOK (MgZn5).
a - 96,8 sec. % Zn
1) JIHTON (MgZn, + seTCKTHKa); 2) Ae41opMHpoeansbl(l (MgZn6 + SBTeKTHKa); 3) oroxfxcesxMH
(MgZn, + 9aTeKTHKa).
ropsmaH ge4 OpMaIuis (npeccoBaHHe) pe3KO H3MeJIbgaeT CTpyKTypy (CM,
(pHr. 153), C03AaeT CBe)KHe CTbIKH MexcAy 3epHaMH H Cn0006CTByeT 60JIee 6bICTp6-
My BbIpaBHHBaHHIO COCTaBa o6pa3IjOB. Ho Bee we, B CHJIy McAJIeHHoro npOTeKa-
HHH AH*y3HH, OCO6eHHO B 06JIaCTH COeAHHeHHH MgZn, Aeq)OpMHpOBaHHble He-
OTO)K)KeHHble CnJiaBbI He $IBJIHIOTCH nOJIHOCTbIO paBHOBeCHbIMH. B COOTBeTCTBHH
C 3THM B MHKPOCTPYKType cn.naBOB, B o6JIacTH B03MO)KHOTO cyLgeCTBOBaHHH r0?
MOreHHbIX o611acTefi, etue COAep)KaTCSI He60JIbwHe BKJ1K),IeHHH BTOpOH 4)a3bl
(CM. (MHr. 153), a Ha KPHBBIX COCTBB-MexaHHgeCKoe CBOHCTBO npH 20' TOJIbKO
coeAHHeHHe MgZng HMeeT CHHry.napHYio TO4Ky-MHHHMYM (4)Hr. 155, Ta6J1. 51).
Ha (PHr. 155 H B Ta61I. 51 BHAHO, qTO Ae()OpMHpOBaHHb1e CnJiaBb1 B o6JIaCTH
COeAHHeHHH MgZn npH O6b19HOH H nOBbIIneHHbIX TeMnepaTypax BbI.1 eJ1 HOTCA
BeJIHIqHHOH CBOeH TBePAOCTH H AaB.neHHI HCTe'IeHHH. BepOATHO, B 3THX cnJIaBax
Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
 Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
A pr, /1-
0
111. Cnnaebl a cucmeMax c ,1le1naanuvecnuJlu cceauHeHunniu 231
npH Aec4opMaumi HJIH He6o.IbuIOM Harpese npOHCXOAHT nOArOTOBKa x o6pa3o-
BaHH10 coeAHHeHHH MgZn, a Mo)KeT 6b1Tb Aaa{e ero BblAe.neHHe B McJIxOAHCnepc-
H013 cj opMe, 'ITO Bb13b1BaeT HCKaXCeHHe OCHOBHOII CTpyKTVpbI CnJIaBOB H nOBbI-
?
' Hr. 154. L aBneHHe HCTegeHHH JIHTbIX MarHHI9-IHHKOBbIX cnJIaBOB.
0 , JO LO 30 90 SO 60 70 00 90 100
%Zn
UJeHHe TBepAOCTH Ao 350 Kr/MM2. B npouecce H3MepeHHH TBepAOCTH BblLie 300?
B03MO)KHO yxce nPOHCXOAHT gacTHLIHag cKOaryjmijH5n> coeAHHeHHH, TaK KaK
MaKCHMyMbI TBepAOCTH cr.na}KHBax)TCSI. CKa3aHHoe OTHOCHTCH TaK)Ke H K coeAH-
dieHHK) MgZna. KHHeTHKy npoueccoa CTapeHHSI B 3TOM c.iyqae cJleAyeT H3y-
~r
e.__. --' 300
-------------------
l0 2 J'7f 40 3 947 7~
OHr. 155. TBepj(OCTb A e4 OpMHPOBaHHb1X MarHHA-EXHHKOBb!X CIIJIaBOB
npH pa3JIH4HbIX Te MnepaTypaX.
%Zn
'IHTb (50Jiee nOAp06HO, TaK KaK MgZn H MgZn2 - yfpO'IHHTeJIH HeKOTOpbIX Tep-
MH4eCKH o6pa6aTbIBaeMbIX CnJ1aBOB MarHHH C aJIK0MHHHeM H IIHHKOM.
r1pHMeHeHHe McXaHHqeCKOI H TepMmeCKOI{ 06pa6OTKH 06pa3IjOB 3HaTiHTeJIb-
HO COKpatuaeT BpeMfi npH6JIH)KeHHH CnJIaBOB K paBHOBeCHOMY COCTOHHHIO npH
OT)KHre H, CJIegoBaTeJIbHO, fO3BOJI5ieT BbIHBHTb 6oJiee COOTBeTCTByfOIAHfi AaHHOMy
THny XHMH4eCKoro B3aHMOAeIRCTBHH KOMnOHeHTOB BHA AHarpaMMbl COCTOHHHH
H AHarpaMM COCTaB-CBO iCTBO. TBepAOCTb H3yqaBHIHXCSI CI1JIaBOB 3aBHCHT OT
BpeMeHH oT)KHra (4)Hr. 156).
HaH60JIee paBHOBeCHbIMH H3 H3y'IaBCI1HXC$i HSMH OKa3aJIHCb Ae4)opMHpOBaH-
Hble H OTO>K)KeHHble B Te'IeHHe 20 CYTOK cnJIaBbI. fHTHCyTOTiHbIf OT>KHr He BHeC
npHHuHnHaJIbHbIX H3MeHeHH1 B XOA H3OTepMbI TBepAOCTH no OTHOItIeHHIO K JIH-
TOMy COCTOHHHIO, HO OTAeJIbHble CfJIaBbI yseJIH'IHJIH CBO}O TBepAOCTb. TaK,
cniiaB C 76,8% Zn, COOTBeTCTBy OIII;HII coeAHHeHHK)MgZn, B Ae(OpMHpOBaHHOM
BHAe HMeJI TBepAOCTb 315 Kr/MM2, a noc.ne HHTHCyTO'IHOrO OT)KHra - 357 Kr/ MM2.
.r1ocne AecETHCyTOgHOrO oT)KHra Ae(4opMHpOBaHHbIX CnJIaBOB COeAHHeHHe MgZn
Ha H30TepMe TBepAOCTH CTaJIO BbIAeJISITbCH rJIy60KHM MHHHMYMOM.
Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
 Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
232 BAUAHue me unepamypee Ha .uexaHUaeenue ceoucmea . iema.mmeckux cnAaeoe
?
i
.lHTble cn]laBb
l
TBepAocTb. HE, K1I,l t2
TBep
Bec. % Zn
Te1nepaTypa
HCnb1TaHH9, ?C
aaeneHHe IICTeveHHn
i
6e3 OT)KHra
nocjie om nra
(5 CyTOK)
HeOTO)K)KeHnblx cnna-
BOB, K, Kr(MM'
6e3 oT)Kllra
20
128
102
I
I
118,0
'
24,2
325
20,0
15,9
20
194
138
109,0
45,6
325
17,1
1
15,9
20
260
303
280,0
69,8
325
40,7
38,1
20
303
204,0
70,8
325
43,7
25,9
20
297
280
270,0
72,9
325
25,0
31,2
20
260
225
280,0
74,3
325
13,1
31,2
20
242
270 , 0
74,8
$25
14,7
0
37,0
20
`291
373
} 335
315,0
75,4
325
23,1
34,4
20
303
342
315,0
76,8
325
39,4
38,1
20
233
_
315
303,0
77,0
325
33,4
34,4
20
280
315
303,0
77,5
325
13,1
34,4
20
265
260
303,0
80,6
325
-
36,8
31,2
20'
255
280
280,0
81,5
325
44,7
27,5
20
197
225
270,0
83,;1
325
26,3
27,0
20
200
208
260,0
,
84;3
325
19,7
24
8
20
280
170
280,0
850
325
28,9
47,5
86,6
20
325
197
208
27,6
3650
251,0
38,0
20
237
251
265,0
87,9
325
22,3
25,9
20
150
242
280,0.
89,4
325
11,8
18,5
20
144
260
303,0
90,2
325
33,7 )
23,8
20
142
225
285,0
91,7
325
20,3 1
7,0
20
233
260
280,0
92,6
325
15,8
7,0
92,7
20
325
129
242
}
18,4
345?
159,0
9,1
20
194
121
146,0
93,1
325
14,5
5,6
20
200
218
/
74,0
95,6
325
18,7
9.1
Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
 Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
4p , 41
0
0
JI,OCTb, HE, KClmal'
,4aencHHC IICTC4eHItB K, Krimht3
HOCJIC OT)Kllra
TeMHCPaTYPHW1I IC034)-
[r111g11CHT TBCPAOCTH
5 CYTOK
10 CYTOK
20 CYTOK
CIIJIaBOB, OTOB:)CCHHbIX
20 CYTOK (20-325?)
fC3 OT%IIPa
^OCJIC OT)KHra
(5 CYTOK)
90 7
I
73 2
I
18,4
12,0
-0,26.10-3
29;9
17,7
164,0
126,0
18,4
11,0
-0,35.10-3
23,0
21,1
233,0
138,0
31,2
25,0
-0,2.10-3
57,0
20,4
233,0
159
242,0
28,4
18,9
-
59,8
15,3
280,0
233,0
34,4
45,6
-0,23.10-3
45,4
20,7
303,0
233,0
31,2
31,3
-0,25.10-3
-
19,9
260,0
291
270,0
34,4
65,0
-0,2.10-3
40,8
23,6
280,0
303
280,0
47,5
41,6
-0,27.10-3
38,8
335?
26,1
335?
357
0
150
107
0
}
}
,
,
41,9
37,0
-0,15.10-3
63,7
29,3
303,0
303
246,0
38,1
43,9
-0,25.10-3
42,0
22,1
315,0
315
280,0
41,9
50,0
-0,25.10-3
35,0
23,1
280,0
260,0
38,1
60,4
-0,21.10-3
38,7
23,5
342,0
290,0
40,0
50,0
-0,25.10-3
40,1
14,5
315,0
280,0
38,1
45,6
-0,26.10-3
34,7
22,9
199,0
246,0
31,2
25,2
-0,33.10-3
31,5 J
18,1
290,0
255,0
53,1
45,6
-0,24.10-3
42,3
25,1
233,0
212,0
28,4
25,2
-0,31.10-3
211,6
21,1
303,0
251,0
26,1
22,4
-0,35.10-3
20,4
14,8
270,0
191,0
19,3
15,0
-0,3610-3
24,4
15,3
291,0
20,1
242,0
14,5
-0,4.10-3
33,5
365?
15,1
3650
280,0
242 , 0
17,1
15,7
-0,39.10-3
20,4
16,3
303,0
'251,0
28,4
28,3
-
14,1
22,9
185,0
218,0
15,9
11,0
--0,43.10-3
22,9
15,03
138,0
84,9
15,6
8,0
-0,33.10-3
17,2
14,5
179,0 I
17,1
I
233 0
-0,38.10-3
23,5
345?
.16,9 } 345'
Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
 Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
0
JJaxce npH 6erJIOM B3rJIHAe Ha H30TepMy 20? TBePAOCTH noc.ne 20-cyTOuHoro.
OT)KHra CTaHOBHTCH HCHbIM, I TO, HeCMOTPH Ha HeKOTOPb1e Bb13BaHHble HeoJ'HO-
pOAHOCTb1O CTpyKTypbl KOJIe6aHHH, TBepAoCTb onpege.iHeTC51, B nepayio oqepeAb,
XHMH4eCKOFi nPHPOAOH cnJIaBOB. Bce TPH HMeIOnjHXCH B 3TOI-i CHCTeMe McTaJIJIH-
9eCKHX CoeAHHeHHH Ha H30TepMe TBePAOCTH Bb1AeJ1H}OTCH OCO6bIMH To4KaMH:
MgZn H MgZnb-r.Iy6OKHMH MHHHMyMaMH, MgZn2-He60JIbLHHMMaKCHMyMOM.
B o611aCTH CoeAHHeHHH MgZn H MgZng H3MeHeHHe COCTaBa CnJIaBOB Ha 1,5-2%
MO?KeTnpHBeCTH K H3MeHeHHIOTBePAOCTH B 1,5-2,5pa3a. TaK, HanpHMep, cniiaB
900r 11/00
r
Zee
100 _ .Q ZO ' '' ~' JalraneMM' e
c /3
I*
JIH3epoB, 6e3 yrlea.a coJreB&fd 4acTil,
XapaKTepl13yeTC5I cJIea.yIOu.LHMH w'I(I-
par,Iii (MOJI. o/o) 87 '90 MgO.; 6-
11 Fe; 2-2,5 A12O3,; 1,5-2 Si02.;
1-1,5 ICaO.. flaCCHBH:pOBaHI3e xaTO-
AoB Mar-HueBbIX 3JIeKTpOJIIr3epoB Jnpo-
J1CxoAIIT o6bIgHO n.prr nllTaHHH NO-
C.aeAHHX X.7OpIICTbIM MarHiieM, noJly-
4aeMbIM xjiopnpoB'aHIfieM KayCTH4e-
CKOrO MariieWlTa, H 3Ha'T3iiTemi o pe-
}Ke B c.Iy4ae nHTaHHH HOKVCCTBeid-
HbIM KapHaJIJIHTOM.
IIOCKOJIbKY OCHOBHOIi cocTaBJIHlo-
well KaTOAHOII nJIeHKH 2BJIHeTCH OKHCb
.Marddii1 (Ao 90 MOJI. 'e/o), aBTOpaMH
6bI.no ?cAe.iaHo arpeAno.no}KeHHe, 4TO
dd.pH4HHOII idaCCI BHpOBa'HHS1 Ka'Eo.goB
MarHHeBrIx 9JIeKTpoJIH3epoB HBJIHeTCA
p.a3JIH4He d3 xapaKTepe m noaeAeHHH
a 9JIex rpoJHlTe OKHCH M a rHHx. IS.m-
CJIeAHSISi noABJtxeTCSi 'B HeM 3a C'Qier
iiiAp'OJIH3a XJ1OpHCTOPO MarHI3'Sa HJIH
KapxaxJIHTa, npwUeM o6pa3o:BaHHe ca-
Molt KaTOAHOfd rlJieHKH SIBJISreTCH pe-
sylIbTaTOM nepeHoca qaCTHIu oKHCH
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Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
 Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
,4ppeId -x l3
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Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
 Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
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Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
 Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
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Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
 Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
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Approved For Release 2008/07/31 : CIA-RDP80T00246AO02700010001-0
 Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
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1. FHApo.11H3 xJIOpMCTOro
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cpei[e pacnJlaBJleHHOrO Ka-
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npoBoxcAaloLuHHcR o6pa3o-
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CKOpOCTb1O - ;3HagHTeJIb-,
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ro MarHHH H Mexblueu AJia
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Bo 60 40 20
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Hbie no H3MeHeHH1o BeJIHgHHbI KpII-
CTaJiJIOB KapHaJIJIHTa B 3aBHCHMOCTII
OT TeMnepaType HX KpHCTaJIJIH3auuHIi.
3Aecb xKe noKa3aHO H3Me}IeHHe BeJIH-
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JIygeHHoM 'npH rHApoJIH3e KapHaJIJIHTa
C pa3JIHLIHOfI KpyrIHOCTbIO KpHCTaJIJI06.
HaH.6oJIee KpynHee KpHCTaJIJIbI Kap-
HaJIJIHTa 6bIJIH no.Rygexbl rips 80 H
60?, HaH60Jiee McJIKHe - npH KOMHaT-
HO I TeMnepaType H 95?. IIpH HH3KHX
TeMnepaTypax npoljecc 3apO)KAeHHa
66
2. B pe3yJlbTaTe rHApOJIH3a x iopH-
CTOI'O MarHHR o6pa3yeTC51 TOHKOAHC-.
nepc aR OKHCb AiarHHR (epeAHIIH pa3-
Mep L1aCTHubI 0,0055 xm), Aalowa 1
B 3J1eKTpoJIHTe B3Becb, a' npH rMApo-?
JIH3e KapHaJIJIHTa - KpynHOKpHCTaJi
JIHLIecxaa OKHCb MarHI3R HrOJIbLlaTo
()OpMbI (epeAHRR AJIHHa KpHCTaJIJIa
0,56 MM), ocax 02,3 CHBa 02,1 IIpimeT HanpaBJIeHHe, KacaTeJ ' 100 H HOBepXHOCTLI
MBTa3IJIa. BePTIIKa7IbHaH COCTaBJIHIoll aH 3TOI3
CHJIbr paBHa 02,1 cos (180 - 6 ), n paBHOBe- v. ~ enmponum1 - 1r ~ecjro 1 .
01.3 = 02.3+ 02,1 cos (180- 0),
oe,Cos(h'
2,1 I
Cos(180-0) = Q1.3 a2,3
a
He'HHe 02,3 H 02, yMBHbIIIaeT a6COJIKITHyIO Be- (ZL/)OA ~,
NWIHHy cos (180 - 0). 3TO, oireB1J H0, HMeeT
McCTO IIpH B03paCTa'HHH (180 - 0),'ITo IIIpO-
HCXOR'HT Torj(a, HorJ(a HpaeBog yro.l KaIIJIH
pacnJIaBJIeIHoro meTaJnia 0 yMeHbHIaeTCH. 171.3
I'IHbIMII CJIOBaMH, IIpH IIOBMIIIreHHH MBHC-
(aaHoro HaTJUEOHHH pacinlaBJleHHorO aJIeK-
TpOJIHTa Ha I1paHrn e 0 TBepgBIM KaTOJ1;OM
(02,3) H paCIIJlaBJIBHHHIM MarHHBM (0 2,1)
HOA BJIHHHHBM IIOBepXHOCTHO-HeaKTHBIIbIX
PHc. 9:, :,':eMa CHJI HoBepXHO-
cTHOro TBHSBHHA, AefiCTByIO-
mxx Ha *AHJ110 MarHHH Ha Ha-
Tone
B0IAeCTB, HanpuMep ()TOpHJ{OB (HOHOB F-),
90JIHMHO yjiyLIIIIaTbCH CMa'IHBaHHe KaTOJ{a paCIIJIaBJIe?HHh, IarHHBM, a CJieJ;O-
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IIOBepXHOCTH KaTOJ{a. HaO60pOT, IIOBePXHOCTHO-aHTHBHIII :0MIIOHeHThI 8JI8K-
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p0CTY KaIIeJl,,_ 3arHHH.
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r
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Macce a.leKT. (HTa, . -tITO--'-TaICIce
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9(Ai Co) MarHHH, a CJI .)BaTeJIbHO, H K cry BbIXOAa TORY. IAeJiecoo6-
pa3HOCTb IF 3eHeHHH Jto6aBow
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3JIeRTpOJIH'Ty. bATBepHf eua, Kax
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r1BJIeHHI3 B r. 5'gecce BJIeKTpOJiH-
THgIecicoro pa 1IHHpOBaHHH aJIIo-
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CH, KaK HaBeCTHO, TPH padn3laBJIeHIIEIX. CJIOH: anOAHbII3 IJIaB (Al + Cu),
8JIOKTpOJIHT H tIHC'TbII3 KaT0) Hb113 aJIKIMHHHIi. rlOBepX'HOCTB JIBJIBHHII B 9TOM
iipouecce HpOTOKAIOT Ha rpaiirn a pa3JIH*rHE.Ix (Paa, o6ycji .ZHBaH IIpOHHKHO-
BeHHe COJIOBOr0 paCIIJI3Ba B (yTepOBKy, HOTepH McTa3IJIB B 9JIOKTPOJIHTe .II
J(e41(1pMaljMlo KaTOJ[0B (pHC. 10).
3JieRTpOJIHTbI COBpeMeHHIIX BaHH J{JIH 8JIeKTpOJIHTH'Ie, )FO pa()HHHpOBa-
HHH aHIOMHHHH HPeACTaBJIHIOT co6on CJ1OZKB MO HO COCTaBy -' IIJ1aBu H3 CMeem
(TOPHCTMIX H XJJOPHCThIX COJIeI3. HCCJIeAOBaHHH 17 IIOKaabr :, IT, ZITO CMaiiHBa-
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 Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
4 APP e^'chx /J-
SURFACE TENSION OF MOLTEN SALT MIXTURES FOR AN
ISOCONCENTRATIONAL SECTION (10% BY WEIGHT OF MgCI2)
OF THE SYSTEM MgCls -CaCI5 -KCI -NaC1
Kh.L. Strelets and O.G. Desyatnikov
Measurements of the surface tension of molten salts can be carried out most accurately by the maximum
bubble pressure method, which permits the use of apparatus made of materials of good resistance to the action of
molten salts. Also, in this method it is easy to ensure constancy of temperature in the space in which the measure-
ments are made, since the tip of the capillary at which the gas bubbles are formed is immersed to a depth of only
0.1-0.3 mm.
In its application to molten salts, this method has received its most detailed development in the hands of
Jaeger ti].
V. Semenchenko and L. Shikhobalova [2,3] have used the same method for the measurement of the surface
tensions of pure salts and binary mixtures of Na, K, and Li chlorides and sulfates, but they have improved it by
the use of an electrical contact to determine the moment at which the capillary makes contact with the melt.
For the measurement of surface tension we used the method based on the maximum pressure developed in a
gas bubble.
The accuracy of the method was checked against data for the surface tensions of pure molten KCI, NaCl.
MgCl2, and CaC1s at the interface with the gas phase. In order to check the reproducibility of the results, duplicate
measurements were made: the results agreed within 1?16.
Figure 1 shows the results of our measurements of surface tensions of pure salts in comparison with those of
other authors. For NaCl and KQPthere is good agreement with the results of Zhivov (4] and Jaeger [11 and for
CaCI1, with the results of Barzakovsky (5].
With respect to the magnitude of the surface tension of the molten salt at its interface with the gas phase, the
salts that we have studied may be placed in the following order: MgGls - KC1-- NaCl -p CaCls, in which
MgCls has the lowest and c.:aCls the highest surface tension.
Tables 1-7 give the results of the measurements for all compositions.
In Figure 2 a comparison is made of the surface tension isotherms for all sections at 750?. All of the curves
are smooth and are convex in the direction of the axis of absciss4s. As the KC1 content increases this convexity
also increases.
From these curves it will be seen that with increase in NaCl content the surface tension increases greatly.
Increase in the CaCI= content from 0% to 30-40 by weight at a constant NaCl : KC1 ratio has practically no effect
on the value of the surface tension. In the region of 20 CaCls there is a poorly defined minimum on all of the
curves.
With further increase in the concentration of calcium chloride, a rise in surface. tension occurs; this is most
marked in the range -70-9G%.
Figures 3 and 4 are the concentration triangles for 700' and 750?, and they show the lines of constant surface
tension.
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 Approved For Release 2008/07/31 : CIA-RDP80T00246AO02700010001-0
A
15b I
*-I
su~-
tsr~
Cc,Q
aso
L1
950
data. 4) our data.
Fig. I. Surface tensions of pure salts.
A) surface tension o (erg/ cm2). B) temperature (?C).
1.))aeger's data. 2) Barzakovsky's data. 3) Zlti.vov's
Fig. 2. Surface tension isotherms for compositions in all 140
of the sections studied (750?).
A) Surface tension a (erg/cm2). U) Ca(;I2::oiIt.: it by Ito
weight). Tlr-, lom-in numerals correspond to the numbers
of the sections. too
TABLE I
Surface Tension a (erg/ cm2) for Compositions of Section I (NaC1 = U)
CaCI content ' ? wt.)
806
93.3
717
100.5 7 57
100.00
712
108.9 , 766 11 `J.0
815
138.5
848 89.9
793
95.2 789
97.8
721
108.6
878
114.2
875
136.9
869 88.6
842
92.0 800
96.6
757
107.5
901
113.8
903
135.2
892 8d `6
900
88.0
806
96.5
787
106.1
911
112.3
917
134.8
942
0
85
815
95
9
852
101.0
-
952
133.4
907 85.8
.
.
(
914 84.7
963
84.1
877
92.0
892
100.1
-
-
988
132.9
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 Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
0 APPeNd,x is- ~. 3
9o%CaC12+ 10% McCZ2
I II Mm 60 -1 840 30 ZO in t0 -
90%KCI+lo%MgC1= WAN. By wr.) 9D%nlaCL+10%f1CL
Fig. 3. Concentration triangle fo' 700', showing lines of
constant surface tension.
90%CaCIa+IO%MgC!=
1,28 136
1IO 102
80 ~O
~.bL11A~~
~?e 30 S
q.; '~~ %]ft
50
~O*~
7 aw
VyTA -
8
/~~ I-
7VV
w
\V\AAS)a-
I 8o II 10 M 6o 50 17' 40 30 7 20 M Io
9O%KU+IO%MgCL= Ka.(%bv wT) 9D%tb L+10%M9cl;
Fig. 4. Concentiaton triangle (or 750?, showing lines of
constant surface tension. ,
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 Approved For Release 2008/07/31 : CIA-RDP80T00246AO02700010001-0
TABLE 2
Surface Toulon a (era/ cm') for Compositions of Section ii r J
\KCI 6
4C
a
697
103.0
695
102.1
709
101.6
.672
111.5
732
123.8
758
98.5
705
101.9
722
101.6
685
111.4
802
120.0
768
98.3
7 63
97.6
758
100.0
734
108.9
808
120.8
826
94.3
838
92.4
795
97.7
760
108.0
836
119.2
887
9L 0
865
91.7
895
93.1
827
104.0
895
117.1
954
92.3
900
89.3
907
92.6
875
102.6
901
116.6
TABLE 3
Staface Tension a (erg/cm') for Compositions of Section III NaCI
0
20
40
60
80
?C
a
?C
a
?C
a-
?C
a
?C
a
733
103.0
694
104.1
667
106.9
732
111.6
747
122.9
821
96.8
169
98.7
716
104.9
780
109.5
766
122.6
865
94.9
790
97.6
730
103.9
803
107.0
779
122.0
880
93.1
829
96.2
745
103.1
818
107.1
900
114.2
915
89.8
830
95.3
839
97.4
852
105.1
904
113.9
942
88.9
880
93.2
895
95.4
870
103.9
907
113.3
TABLE '4
Surface Tension a (erg/ cm2) for Compositions of Section IV NaCI 1
C
KCI 1
0
20
40
60
80
?C
a
?C
a
?C .
a
?C
a
?C
a
697
108.1
672
108.5
702
110.2
709
115.0
756
125.9
732
107.1
688
107.8
722
109.2
770
112.5
816
124.0
768
104.2
740
104.0
772
106.4
820
109.6
882
120.3
805
101.6
853
98.8
882
100.9
838
108.9
886
120.7
842
99.4
860 -
97.9
905
98.9
850
108.4
930
119.1
870
98.0
945
' 93.4
972
96.9
866
108.2
968
117.4
TABLE 5
Surface Tension a (erg / cm= for Compositions of Section V
(
NaC1 = 3
KC1 1
0
20
40
60
80
?C
o
'C
a
?C
a
9C
a
?C
a
805
105.8
739
108.9
700
113.5
685
119.7
734
127.7
885
101.4
744
108.2
735
112.9
740
117.7
749
126.0
917
98.4
758
107.5
760
110.4
750
116.4
793
125.3
936
95.9
819
103.4
815
108.1
768
115.9
890
120.0
968
94.6
826
102.7
833
106.7
887
111.3 '
893
120.0
1008
98,2
886
. 98.1
894
102.9
908
1011.5
908
119.0
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wt.
CaCI content 3 by
CaC1 content (% by wt.
CaC content (3 b wt.
 Approved For Release 2008/07/31 : CIA-RDP80T00246AO02700010001-0
TABLE 6
CNaCI.6
Surface Tension v (erg/ cm) for Compositions of Section VI KC1 1
APP 1.7 ra 47
0
20
40
60
80
?C
a
?C
a
?C
a
?C
a
?C
v
868
103.6
715
112.1
687
114.4
672
120.8
762
128.9
899
101.3
798
106.8
739
112.1
709
118.8
776
127.4
928
99.6
831
105.0
758
110.4
792
116.2
- 860
125.3
937
99.4
890
100.6
877
105.9
875
112.5
874
123.3
958
97.6
950
103.1
885
111.8
877
124.2
962
102.6
933
109.2
912
123.1
Surface Tension a (erg/cm?) for Compositix>> .,f Section VII (KC1 = 0)
0
20
40
60
80
?C
?C
?C
?C
a
?C
a
871
106.9
769
112.2
720
116.7
721
122.2
723
130.7
892
105.0
797
110.9
737
115.7
733
120.8
747
129.5
920
103.5
828
108.9
779
114.5
787
119.4
758
129.2
947
101.5
880
105.8
837
112t0
815
116.9
787
127.2
961
100.5
900
104.0
868
109.1
846
115.6
852
124.2
922
103.5
905
107.7
877
114.8
900
121.9
LITERATURE CITED
[1] Jaeger, Z. al1g. anorg. Chem., 101. 18 (1917).
[2] V. Semenchenko and L. Shikhobalova. J. Phys. Chem.. No. 5(1947).
(3] V. Semenchenko and L. Shikhobalova, 1. Phys. Chem., No. 6 (1947)
[4] V. Zhivov, Tram. VAMI, No. 11 - 12 (1935).
[5] V. Barzakovsky, J. Appl. Chem., XIII, 8 (1940).
Received October 9, 1953.
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CaC12 content ('1? by wt.
CaCI content (%b b wt.)
 Approved For Release 2008/07/31 CIA-RDP80T00246A002700010001-0
ff ~ e6.id?x i6
.B R I E F C O M M U N I C A T I O N S
DENSITY OF FUSED SALTS ALONG ISOCONCENTRATION SECTIONS
(10 wt. 10 MgC12) IN THE SYSTEM; MgCl2 - CaC12 - KCI - NaCI
Kh. L. Strelets and O. G. Desyatnikov
We measured densities for all the compositions by a ..,ethod of hydrostatic weighing. We maintained an
atmosphere of carbon dioxide gas above the melts in order to avoid the action of oxygen or moisture during the
time of measurement.
The accuracy of density determination, as dependent on concentration, amounted to 0.3-0.5%.
Densities of these pure salts were determined to check the method: KC1, NaCl, MgCls, and CaC)p. The data
are given in Fig. 1, where they are compared with data from other authors.
0_1
s-2
0-5
0-1
LAS 4D 1.0 I.bt) 1.66 1.70 1.75 Lao 1BS 1.% Lgff 2.00 ZAS
DENSITY
Fig 1. Densities of KC1. NaCl, MgC12, anal CaCl2, ac.:ordin to various authors.
1) Abramov; 2) Mashovets; 3) Barzakovsky; 4) present authors.
As can be seen from Fig. 1, our data lie between the data of Abramov [1] and Mashovets [2]. The CaCI; de-.,-
sity data are close to the data of Barzakovsky [3]. All of the controlled measurements we made were in good agree-
ment with the above noted limits of error.
Results of Measurements
We studied isoconcentration sections passing through 10 wt. % MgCns in the system: CaC4 -MgCL-NaCl-KC1.
A total of 72 compositions were measured; they were themselves arranged as secondary sections passing
through the vertex of the ternary diagram (90 wt. % CaCI5 and 10 wt. % MgCI=).
Compositions which correspond to the same CaCns content in these sections differ from one another in their
NaCI: (Cl ratio.
The results of measuring density for all compositions are given In Table 1.
Density isotherms for five sections at a temperature of 750? C are given in Fig. 2.
179
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 Approved For Release 2008/07/31 : CIA-RDP80T00246AO02700010001-0 .
CaCls con-
tent(wti
0
10
20
30
{ 40
50
60
70
80
0
10
20
30
35
40
45
50
55
60
' 70
0
{ 5
10
15
20
30
35
40
45
50
60
10
0
I ! 5
10
15
20
25
30
40
45
50
55
60
80
.- 0
10
20
30
1 3 c' I 40
50
,Densii.of salt At indicated tempetuute: ('C)
715
1.555
1.540
1,524
1.621
1.615
1.603
1.587
1,573
1.680
1.661
1.654
1.639
1.827
1.610
1.748
1.732
1.712
1,701
1.680
1.671
1,656
1.789
1.776
1.760
1.745
1,728
1.711
1.696
1.830
1.816
1.800
1,784
1.768
1.751
1.908
1.891
1.872
1.859
1.846
1.833
1,821
1.806
1.963
1.949
1,936
1,923
1.911
1.897
1,884
1.871
2,007
1.993
1.978
1.966
1.953
1.939
1,561
1.551
1.539
1.526
1.634
1.618
1.805
1,591
1.580
1.5 66
1
891
1.679
1.614
1.654
1.638
1.623
1.613
1
751
.
1.739
2.725
1;713
1.700
1.687
1,674
1,661
.
764
1
1.752
1.740
1.127
1.715
1.703
1.691
1.619
.
1
790
1
777
1,764
1,751
1.739
1.721
1,714
1.101
.
1.815
.
1.801
1.781
1,774
1;761
1.748
1.736
1.724
1
838
1.826
1.813
1,800
1.787
1.774
1.762
1.749
.
1
868
1.855
1.843
1.830
1.817
1,804 1,792
1.779
.
902
1
1.890
1.878
1.867
1.855
1.841 1,821
1,815
.
1.961
1.947
1.933
1.918
1.905 1,891
1.878
1,583
1.570
1,551
1.544 1,530
1.518
1.605
1.591
1.577
1,564 1,549
1.636
1.637
1.623
1.610
1.597
1.584 1,572
1.559
1,873
1.660
1.645
1.631
1.618
1.605
1.592
1.579
1
693
1.618
1.685
1.852
1.640
1,628
1.609.
1.600
.
1.734
1.720
1.706
1.893
1,680
1,667 1.654
1.640
1.755
1.743
1.729
1.716
1.703
1,690 1.677
1.665
1.789
1.776
1.763
1.750
1.737
1.725 1.112
1.700
1.801
1.790
1.778
1.785
1.752
1.739 1.724
1.715
1 839
1
827
1.813
1,800
1.788
1.776 1.783
1.151
1.882
.
1.869
1.856
1.844
1.832
1.820 j 1.808
1.795
1.962
1.948
1.935
1.921
1,907
1.893 1.819
1.866
1.602
1.589
1,573
1,561
1.542
1,530 1.518
1.503
1.615
1.601
1.587
1.574
1.559
1.545 1.532
1,520
1.632
1.622
1.608
1.594
1.582
1.568 1.554
1.540
1.685
1.651
1.636
1.622
1.601
1.594 1.580
1.566
1.691 1.678
1.664 1.851
1.636
1.622 1.608
1.594
1.705
1.891
1.67ub
1,663
1.651
1,637 1.624
1.613
1.129
1.716
1.701
1.890
1.617
1,663 1.650
1,638
1.776
1.762
1,748
1.134
1.721
1.701 1,894
1.680
1.800
1.785
1.773
1.758
1,746
1.732 1.118
1.103
1.820
1 806
1.792.
1 178
1 764
1.150 1,738
1.724
1.840
1.828
1.815
1,803
1.792
1.179
1.767
1.154
1.879
1.868
1.856
1.845
1,833
1.821
1.809
1,797
1.991
1,977
1.963
1.950.
1.935
1.589
1.576
1.561
1.544
1.528
1,514
1,500
1.485
1.629
1.616
1,602
1.587
1,573
1,559
1.544
1,530
1.669
1.656
1.644
1,629
1.615
1.601
1.588
1,575
1.712
1.700
1.686
1.673
1.659
1.646
1.633
1.619
1.765
1.751
1.731
1.723
2.709
1.695
1.681
1,664
1.822
1.801
1.793
1.719
1,164
1.751
1.739
1.724
1.874
1.861
1.846
1.833
1.819
1,805
1.791
1.777
1.947
1.933.
1.920
1.906
1.893
1.897
1.866
1.851
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 Approved For Release 2008/07/31 : CIA-RDP80T00246A002700010001-0
TABLE 1 (Continued)
NaCl: KC1
CaCI con-
Density of salt at indicated tempera re: ('C)
ratio
tent (wt.0k)
675
700
125
150
775
800
825
850
0
-
1. 565
1.551
1.537
1.523
1.510
1.494
1.480
10
1,t22
1.606
1.593
1.578
1.563
1.549
1.532
1,520
20
1.661
1.646
1.630
1.616
1.603
1.589
1,575
1.561
30
1.7GA
1
695
1.681
1.667
1.654
1.640
1.627
1.613
1: 6
40
1.755
.
1.142
1.129
1.715
1.702
1.689
1.675
1.862
50
1.807
1.793
1.780
1.766-
1.753
1.139
1.725'
1.111
60
1.872
1.858
1.844
1.829
1.815
1.802
17 79
1.775
70
-
1 937
1.923
1 913
1.899
1.883
1.869
1.855
w--i--
0
-
-
-
-
1.524
1.500
1,490
1.464
10
-
1.601
1.596
1.578
1.560
1.544
1,527
1,511
20
1.666
1.652
1.6:>
1.620
1.611
1.585
1.513
1.559
30
1.706
1.690
1.613
1.660
1 644
1.631
1.618
1,606
40
-
1.722
1.709
1,694
1.680
1.869
1,650
Nacl = 050
50
-
1.1E'-1
1.774
1.762
1.749
1.129
1.117
1.703
60
-
1.860
1.845
1.830
1.818
1.805
1.792
1.780
70
-
-
1.911
1.900
1.887
1.871
1.858
1.847
80
-
2.011
1.999
1.985
1.969
1.955
1.935
1.924
90
-
-
-
-
2.058
2.045
2.030
2.016
Fig. 2. Density isotherms for sections I. 111, IV. V
and Vll at 150?C. A) Density; B) CaC1 content
(wt. %).
Fig. 3. Isotherm of molecular volume of the com-
position of all sections studied at 750? C. A) molec-
ular volume; B) coiuent CaC12 (in mol.-%).
With increased CaCI5 content, the density curves for all sections increase monotonousl);; the curves are con
vex to the abscissa axis.
The curvature decreased with increase in sodium chloride content (increase in NaCl: KC1 ratio
It can be seen from considering the data presented that electrolyte density also increases with increased sod-
ium chloride content.
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 Approved For Release 2008/07/31 : CIA-RDP80T00246AO02700010001-0
" Timpauttue Coefficients of Density for Melts in the MgC1e - CaC>s - KCl - NaCI System.
NiClt`[
ratio
CaCig.
content
(w1.%)
Density
at ' '
800' C
0.10s
Range of
measuring
tempera-
tures (9C)
NaC1:KC1
ratio
Caclr
content
(wt.'%) -
Detiiiti'at
8000 C
at . 106
Range of
measuring
tempera-
Wes (*C)
0
1.555
62.5
100-860
40
1.708
55.0
700-850
10
1,595
59.0
700-850
1:1
45
1.731
55.0
676-850
20
1.660
56.0
725-850
50
1.751
55.0
700-850
30
1.685
60.5
700-850
60
1.822
48.5
675-850
KCl
40
1.727
61.5
-700-850
80
1.963
55.0
150-850
50
1.786
60.0
700 -850
60
1.833
53.0
675-850
0
1.515
60
650-850
70
1.898
52.0
675-850
10
1.560
57.5
675-850
80
.1.966
64.0
700-850
20
1.602
55
675-850
30
1.643
53.5
675-850
0
1.551
49.0
775-850
1;3
40
1,694
57.5
675-850
10
1.593
52.5
725-850
50
1.752
56
675-850
20
1.638
55.0
700-850
.60
1.805
55.5
675-850
30
1.688
50.5
675-850
70
1.880
54
675-850
6:1
40
1.726
50.0
700 -850
45
1.750
51.5
675-850
0
1.510
56.5
675-850
50
1.775
51.0
700-850
10
1.550
57.5
675-850
60
1.840
50.0
675??850
20
1.589
57,
675-850
70
1.906
55.0
700-850
30
1.640
54.5
675-850
1:6
40
1.689
63
675-850
0
1.544
52.5
725-850
50
1.739
55
675-850
10
1.584
53.0.
700-850
60
1.802
55
675-850
20
1.626
53.0
675450
70
1,882
55
675-860
30
1.667
53.5
675-850
40
1.125
51.0
700-850
0
1.502
67.5
700-850
3:1
45
1.740
51.0
675-850
10
1.544
68
700-850
50
1.778
50.5
700-850
20
1.581
63.5
700.850
60
1.821
49.5
615-850
30
1.630
60.5
700-850
10
1.823
55.5
675-850
40
1.680
58
700-850
0
1.532
56.5
675-850
aCl = 00/6
50
1.731
56
100-850
10
1.568
54.5
675-850
60
1.805
54.5
725-850
1:1
20
1.623
52.0
675-850
70
1.872
55
700-850
30
1.662
53.0
675-850
80
1.954
59
100-850
K)
2.044
58
700-850
The nature of the density change is linear for all compositions. Data for density at 8000 C and temperature
coefficients are given in Table 2.
Considering the molecular volume isotherms (Fig. 3), shows the presence of characteristic points of
inflations on the isotherms at CaClj concentrations of 40-45%. The clearest point of inflexion appears on the Iso-
therm for the section from which NaCl is lacking. With further transition to sections corresponding to smaller KC1
contents , this point is less readily determined, and it disappears in the section which does not cont.in KCI. The in-
dicated character of the isotherms may be explained by forming the compound KCl ? CaCla. The characteristic point
on the molecular volume isotherms is somewhat shifted to the left from the composition KCI ? CaC>s because of the
presence of MgCla in the system which also forms a compound with KCI.
LITERATURE CITED
[1] G. Abramov. Metaf?urgy. No. 8 (1935).
[2] V. Maahovets and Z. Lundina, Trudy Scientific Research Institute of tight Metals, No. 10 (1935).
[3] V. Barnakovsky, 1. Appl. Chem., XIII. 8 (1940),
Received October 9, 1953
102
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 ?
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Ffppe.i d i * / 7
CONDUCTANCE OF THE FUSED SALTS OF ISOCONCENTRATED MIXTURES OF THE SYSTEM
MgCl2 - CaCl2 - KCI - NaCI (10010 MgCl2 BY WEIGHT)
Kh. L. Strelets and 0. G. Desyatnikov
Many studies have been devoted to determination of the conductance of fused salts. Karpachev, Stromberg
and Poltoratskaya [1] have studied the conductance of the system. KCI- MgC12. They made their measurements in a vessel
"i tttr-a quartz capillary having a constant of 230. A Ruhmkorff coil provided them with alternating current. The
vessel was calibrated in terms of fused CdCI2.
Batashev [2] studied the conductivity of mixtures of fused chloride salts of Na. K and Mg. A generator having
the frequency of sound was employed in this work. A flat-b ttomed cylindrical platinum vessel served both as-
container and as one of the electrodes. A platinum disc served as the other. The electrolytic capacity of the vessel
was 0.322. The accuracy of the measuremen? v Aluated as being within 316.
Shcherbakov and Markov [31 measuring the conductance of the same system, developed a more exact method.
They used cells with both U-shaped and vertical capillaries. The conductivity of the vessel walls was taken into con-
sideration in making these measurements, and the drop in temperatures through the thickness of the melt was reduced
by improving the thermal insulation of the furnace.
Barzakovsky [41 studied the conductance of binary systems of fused salts, including CaCl2 - NaCl.
The present work employs a system of measurement which satisfies to a maximum the conditions resulting from
the theory of the alternating current bridge. We have employed vessels with capillaries, capacity being from 100
to 400.
EXPERIMENTAL
Method of measurement. For our measurements, we employed quartz vessels of the vertical type with capi-
llaries 5 to 20 mm long and 1 and 1.5 mm in diameter. Fig. 1 presents a drawing of the vessel.
The electrolytic capacity of the vessels we used varied from 100 to 400 with the diameter and length of the
capillaries, and the resistances of the salts from 25 to 250 0.
The vessels were calibrated with 301o sulfuric acid.
The use of vessels'having capillary portions 5 to 7 mm in length assured that the temperature differential through
the thickness of the measured layer of salt would be negligible (about 2 ?C); this was confirmed by special readings.
In calculating the conductance we allowed a correction for the conductivity of the walls of the vessel, the value
of which was determined for all the vessels over a large temperature interval.
An equimolecular mixture of NaCl and KC1 was adopted as the control. An identical level of salt in beaker
-aad_vessel was maintained in all expenments.
To make our measurements we employed a bridge supplied with alternating current at the speed of sound
(Fig. 2). The theory of systems of measurement has been analyzed in adequate detail by Semenchenko [5], Polyakov
-and-Ivanov [61 and Barzakovsky [4]. Our design made it possible to determine the sound minimum within 1 mm
of the rheochord scale. The accuracy of measurements was to 0,5.0.8%.
The reproducibility of the results was verified by measurement of the conductance of the control mixture.
In Fig. 3 we show our data for the conductance of pure salts of KC1, MgCiz,-NaCl and CsCI= in comparison with
that of other researchers.
cases taken at a number of temperatures
Conductance measurements data of pure complete alts anof mixtures in thereof
both at heating and cooling. The
Results of measurements. Tables 1-7 adduce the data arrived at and Fig. 4 compares the isotherms of specific ntent
from 0 to
markedelevation
ted conductance of all the samples studied at 75C?TheGradual
minimumCwaslshown with materials havingla com-
first in a drop and then in a rise in conductance.
position lacking in NaCI (Mixture 1).
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 Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
o tint esu. ,the position of the minimum shifted in the diradtion of lowu cac 1 c
WE `I. the amlhimum was found in the region of CAC12 concentration of between 48 ,and 5S
approximately to that In which the chemical compound KCI ? CaC1s is formed.
iii
teMipl.eft
1 lAtte-
Fig. 1. Position of furnace and vessel at moment of
measurement.
TABLE 1
Specific Conductance (X) of Type I Mixtures (NaC1= 0)
1.67
1.73
1.76
1.82
1,90
687
718
777
7 98
818
860
1.295
1.40
1.55
1.61
1.65
1.725
Fig. 2. Electrical circuit of system for determination
of conductance.
(in 11'1 cm-1)
'
717
1.26
715
1.175
740
1.33
759
1.29
778
1.25
798
1.3115
788
1.45
825
1.455
860 1
1.61
870
1.535
708
D%IYCI?/0%14sCt=
$0 Iv 40
Wt % KCt
30 ya0 , 10 VII
X%n4C2 flvxl A2
Fig. 5. Concentration triangle with lines showing equal Fig. 6. Concentration traingle with lines showing equal
specific conductances at 700 ?C. specific conductances at 750?C.
LITERATURE CITED
?
x%CCC1,?ro%wjC2:
S. Karpachev. A. Stromberg, and V. Poltoratskaya, J. Gen. Chem., V, 621 (1935).
K. Batashev. The Metallurgist. 7 (1935).
A. Shcherbakov and B. Markov. J. Phys. Chem, XIII. No. 5, 621 (1939).
V.,Barzakovsky. Papers on the Electrochemistry of Fused Salts. 1940.
V. Semenchenjo. B. Erofeev and V. Serzhinsky, J. Gen. Chem., II. 10 (1932).
V. Polyakov and A. Ivanov. Bull. USSR Acad. Sci.. No. 5-6. 1119 (1938).
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r
 Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
VISCOSITY OF FUSED SALTS ALONG AN ISOCONCENTRATION SECTION.
( 1 0 W t . ? l o MgClt) I N THE MgC12 - CaCI= - KC1 - NaCl SYSTEM
We selected the Kulon method for measuring viscosities since it is most convenient for determining the viscosity of
.This method is based on observing the damping of harr...,,,ic vibrations of a solid of revolution suspended in the
liquid by an elastic fiber. By observing a series of successive vibrational amplitudes and calculating the logarithmic
decrement of the damping, we can compute the viscosity of the liquid using the following equations given by
Fershaffelt:
fused salts,
where n is the viscosity being determined, d the density of the melt under study, 6 the decrement in vibrational
damping, Rthe radius of the sphere (the solid, of revolution), Tthe period of vibration of the system in the salt being
studied. T the period of vibration of the system in air, and Kthe moment of inertia: of the system.
H R C EM CLORS
Ffg. 1 Arrangement of equipment for viscosity
determinations.
QoZo
Fig. 2. Viscosity isotherms for compositions:i long :all
sections studied at 750.0.
A) Viscosity n (centipoises), B) CaC4 content (wt.
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 Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
Fig. 3. Viscosity isotherms for compositions along all
sections studied at 750'C.
A) Viscosity Ti (centipoises). B) CaCl2 content (mol. %)
9o%W11.10% MfAj
9D%W1+1096MgCL; WT.%KCL 9D$NdCL+10%f4$Lt
"rig. 5. Triangular concentration diagram with
lines of equal viscosity (700').
app.
Fig. 4. Viscosity isotherms for composit?ors.ailong all
sections studied at 750'C.
A) Viscosity n (centipoises), B) CaClz content (01?).
.3 cl cle+1096 MtCLK
9b
R6
2,4
2.0
18
20
r %I %r %I xdb%
1
.9D%KCL ? 10% MJCLx WT. % KCL 9%NotCL* 10`)6MIjCLa
Fig. 6. Triangular concentration diagram with lines
of equal viscosity (750').
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 TABLE I
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Viscosity. (11) for Compositions along Section 1 (NaCl = 0) (centipoises)
0
1
0
20?
30
40
50
60
10
80
9
0
?C 1
n
'C
n
'C
n
'C
in
'C
T1
'C
n
'C
in
'C,
in
'C
in
'C
n
729
748
780
802
852
1.24
1 .17
1.05
1.00
0.85
692
720
755
785
810
833
1':70
1.48
1.36
1.29
1.16
1.07
618
642
685
721
159
793
2.83
2.51 '
2.11 1
1.77
1.54
1.39
640
674
712
742
774
814
3.12
2.71
2.22
'1.97
1.75
1.54
680
703
729
754
778
800
2.96
2.65
2.37
2.15
1.96
1.'17
6 724 76
156
783
811
833
3.37
2.74
2.44
2.25
1.98
1.85
709
131
'159
810
832
854
3.34
3.05
2.73
2.28
2.11
1.95
694
719
744
766
789
809
3.94
3.63
3.32
2.99
2.75
2.60
120
744
790
817
838
85.6
3.83
3.52
3.03
2.77
2.59
2.51
'14p5
776
800
820
854
3.74
3.20
3.02
2.91
2.60
855
0.99
827
1.21
844
1.41
824
1.67
861
1.73
834
2.36
TABLE 2
fNaC1 Viscosity Viscosity (n) for Compositions abng Section 11 \ KC 1 6J (centipoises)
682
712
742
772
800
826
85?
1.44 1 674
1:.28 700
1.19 727
1.09 762
1.05 793
1.00 828
0.88
1.74
1.59
1.50
1.32
1.24
1.06
661 : 2.23
692 ' 1.97
732 1.72
752 1.56
782 1.46
813 1.32
846 1.25
TABLE 3
NaCI_1 \
Viscosity (n) for Compositions along Section III KCI 3) (centipoises)
660 1.46 1 666
690 ` 1.41 :710
730 ; 1.20 752
761 1.12 816
796 1:06 849
822 0.98
852 0.93
n
1.87
1.55
1.35
1.14
1.06
667
690
718
748
784
820
856
656 2.64 680 2.8.`,
666
3.47
684
2.37
706,
2.56
703
2.87
711
3.28
708
2.16
726
2.34
742
2.56
754
2.71
746
1.89
748 2.16
780
2.22
781
2.43
787
1.61
780 1.96.
803
2.12
816
2.24
814
1.57
804 1.84
861
1.78
846
2.06
824
1.39
824 1.72
843 1.63
CaClt Content (wt. ?b)
'C 1 .nom n
T!
11
2
660'
2.64
680
2.79'
666
3,44
689
3.47
683
4.03
720
3.84
.
96
1
708
2.11
710
2.41
717
2.67
720
3.09
700
3.55
753
3.45
.
80
1
745
1.88
744
2.17
764
2.29
748
2.79
731
3.31
786
3.00
.
64
1
792
60
1
777
1.90
804
2.04
779
2.44
754
2.96
810
2.71
.
42
1
816
.
50
1
809
1.72
827
1 .85
813
2.13
778
2.62
824
2.59
.
1
27
857
.
1.32
833
1.60
852
1.71
849
1 .99
822
2.32
845
2.46
.
844
18
2
1.16
855
1.49
.
_
(KCI 1 (centspoases)
Viscosity (n) for Compositions along section IV NaCl 1
?b
Ca
T
ent (oft
)
,
688
1.38
668
1.83
666
2.06
680
2.31
23
2
686
716
2.57
2.30
713
1.30
689
1.62
693
1.95
692
.
99
1
745
2.01
759
1.11
712
1.54
730
1.73
724
.
77
1
7
199
1.88
37
1
174
1.45
752
.
5
786
1.08
7
511
.
35
849
17
1
796
1 .57
810
g
1.5574
822
0 .90
758
5
8
826
1.
1 :?
.
8
1.36
3
4
856
:52
50
-C n
n
640
3,47
630
&37
660
4.35
670
3.05
668
3.61
687
3.92
710
2.67
696
3.08
726
3.25
74
7
2.42
6
3
7
2.76
766
2.84
2
1
6
5
2.
789
2.66
.
1
4
4
g
p
2
7
4
812
4
4
810
1
838
2:02
IN
1
1
60
:
611
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TABLE 5
Viscosity (11) for Compositions along Section V 1 KC1 T (centipoises)
0
10
20
30
4
0 50
60 70
8
0
'C
n
'C
11
'C
"C
C
n C
C
C
n
C
tl
728
1.28
708
1.61
691
1.81
679
2.21
675
2.53 691
2.85
6561 3.73 } 671
4.21
698
4.44
754
1.11
730
1.47
725
1.65
716
1.87
699
2.37 730
2.45
668 3.43 686
3.84
722
3.76
773
1.11
777
1.26
750
1.56
748
1.81
722
2.22 750
2.33
703 3.20 722
3.24
755
3.28
799
1.06
808
1.18
769
1.50
779
1.60
752
1.97 790
1.99
743 1 2.71 754
2.93
790
2.83
816
1.02
808
1.35
793
1.53
778
1.80 838
1.74
776 2.50 780
2.67
832
2.52
826
1.00
802
1.67
815 2.12 800
2.49
866
2.23
852
0.94
823
1.61
850 1.87 847
2.10
0
1
0
20
30
40
50
60
7
0
'C
t
'C
ri
C
n
'C
n
'C
n
i
?C
n
?C
752
1.18 739
1.42
702
1.81
672
2.21
680
2.53
656
1 3.26
640
4.09
678
4.25
780
1.11 764
1.31
725
1.69
724
1.94
706
2.30
680
2.98
680
3.37
707
3.61
800
1.08 784
1.25
758
1,48
758
1.71
732
2,05
704
2.56
702
3.04
716
3.39
815
1.03 796
1.23
788
1,35
797
1.51
752
1.94
740
2.31
734
2.75
745
3.00
835
0.99 819
1.19
816
1.31
807
1.48
777
1.77
776
2.08
760
2.47
775
2.65
848
0.95 840
1.09
800
1.69
802
1,96
790
2.23
805
2.46
824
1.57
840
1.77
818
2.13
832
2.25
844
1.48
833
2.05
847
2.14
Viscosity (ti) for Compositions along Section VII (KCI = 0) (centipoises).
20
30
40
50 60
70 80
'C
n
''C
r
r
"C
'G
n
n
?C
T?
'C
T)
n
788
1.13
758
1.34
724
1.69
693
2.09
664
2 67
665
3 02
670
3,33
647
4,26
697
3,88
807
1.04
777
1.26
744
1.59
720
1.91
686
2,42
686 1
2 76
6841
3,20
691
3.59
734
3.42
822
0.98
802
1 18
766
1.49
743
1 .75
716
2.20
731
' 1
720
2,91
722
1
3.25
775
2,97
843
0.94
820
1.13
784
1.41
766
1.63
747
1 98
-:.J9
754
2.53
751
2.87
829
2.58
850
0.93
840
1.05
800
1.35
787
1.52
778
-.77
801
1.85
788
2,29
801
2.53
865
0.89
861
0.98
840
1.20
811
1.44
802
.65
836
1.73
811
2.20
830
2.37
863
1.17
838
1.35
824
1.55
859
1.62
846
1 98
847
2.26
858
1.31
846
1.46
The method described is suitable for the condition where the solid of revolution vibrates so slowly that turbulent
motion is not produced in the liquid.
The Kulon method was developed in detail and irnproved by 17antuma Ct ] for measuring the viscosity of fused NaCl.
Karpachev and Stromberg [2] used this method for nicasuriug viscosity in the NaCl system,
Berenblit [3] studied viscosity in the fused MgC12 -KCI -NaCl System by the same method,
The arrangement of our equipment is shown in Fig. 1. The measurements were performed in a porcelain vessel
with D= 55 mm and h = 105 mm. The diameter of the platinum ball was 25 min.
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CaC12 Content (wt.
CaCI Content (wt. %
 It can be seen from Fig.. 2. that the viscosity of the quatenary electrolyte studied by us is not an additive function
The results, of our measurements are, given in Tables 1 -7. Isotherms for all sections at 750'C are given`in Fig. 2,
of composition. Electrolyte viscosity sharply increases with increased CaCl2 concentration.
The effect of KCl and NaCl concentrations on viscosity of the electrolytes studied is readily seen in Figs. 3 and 4,
on which the viscosity isotherms for all sections at 750'C are compared. Triangular concentration diagrams with lines
of.constant viscosity are given in Figs. 5 and 6.
it can be seen from Fig. 2 that when calcium chloride is present in the electrolyte, the viscosity increases with
increase in the NaCl content in the MgC1=-KC1-NaC1 ternary system. In the MgCla-CaCI,-KCI-NaCI iguatenary
system with CaCls concentration greater than 10 wt. % the nature of the effect of KCI and NaCl on viscosity
changes; in this, the system viscosity increases with increased KCI concentration. t
The shape of the viscosity isotherms confirms the fact that the compound KC1 ? CaCI2 is formed.which leads to
increase in the electrolyte viscosity. '
L1 T'.KATURE CITED
[1 ] Dantuma, Z. allg, Chem., 1, 175 (1928).
[2] S. Karpachev and A. Stromberg, 1. Gen. Chem., 5, 625 (1935).
(3] V. Berenbilt, Trans.. All Union Research Institute for Aluminum. Magnesium, No. 14 (1937).
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APPENDIX 19
"MAGNESIUM CAST IRON"
K. I. Vashchenko and L. Sofroni
State Scientific-Technical Press
of Machine-Construction Literature
Kiev 1957 Moscow
421 Pages.
412 Literature References, of which 184 are Russian.
0
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Appendix 19 - Page 2
Table of Contents
Page
INTRODUCTION
3
Chapter I - Crystallization and Structure Formation
14
1. Cooling Curves and Phase Diagrams
14
2. Structure and Properties of the Base Metal
31
3. Structure and Composition of the Graphite
Graphite Formation
60
Chapter II - Treatment of Cast Iron with Magnesium
92
1. Theoretical Basis for the Modification
92
2. The Determination of the Quantity of Magnesium to be
125
Introduced into the Cast Iron
3. Methods of Introducing Magnesium into the Cast Iron
134
Thermal Losses in the Process of Modification
162
5. Removal of Sulphur from Cast Iron before the
Introduction of Magnesium
171
?
Chapter III - Chemical Composition of Cast Iron
178
1. Composition of Basic Elements
178
2. Changes in the Chemical Composition of the Cast Iron
When Treated with Magnesium
191
Alloying Elements
2 02
Elements with Anti-Modifying Action
206
5. Gases in Cast Iron
211
Chapter IV - Casting Properties. and the Making of Castings
216
1. Fluidity
216
2. Linear. Shrinkage
222
3. Design of Mold to Take Care of Shrinking
Internal Stresses
2k3
5. Casting Rigging
250
6. Risers and Chills
252
7. Some Sample Diagrams of the Technology of Casting
Molds and Feeding of the Castings
255
Chapter V - Physical Properties
266
1. Specific Weight
266
2. Coefficient of Thermal Expansion
267
Heat Conductivity
2 67
Electrical Conductivity
267
5. Magnetic Properties
269
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Appendix 19 - Page 3
Page
Chapter VI - Thermal Treatment of Cast Iron
274
1.
Graphitization of the Eutectic and Eutectoid Cementite
275
2.
Isothermal Decomposition of Austenite
282
Annealing of Cast Iron
284
Thermal Treatment of the Castings
287
Chapter VII - Mechanical and Service Properties of
Magnesium Cast Iron
304
1.
Mechanical Properties of the Cast and Thermally-
Treated Cast Iron
304
2.
The Influence of the Chemical Composition and the
Speed of Cooling and Other Factors on the Mechanical
Properties of the Cast Iron
318
3.
Mechanical Properties of Magnesium Cast Iron at
Elevated and Lower Temperatures
339
4.
Resistance to Wear
3148
5.
Corrosion Resistance
360
6.
Heat Resistance and Resistance to Growth of
Magnesium Cast Iron
365
18
Chapter VIII - Austenitic Magnesium Cast Irons
373
Chapter IX - Welding and Heat Treatment of Cast Iron
381
1.
Welding
381
2.
Heat Treatment of Magnesium Cast.Iron under Pressure
385
3.
Cold Treatment
390
Chapter X - The Occurrence of Scrap and Methods of
Eliminating It
398
Chapter XI - Application Fields and Results of Prototype
Castings from Magnesium Cast Iron
x+02
BIBLIOGRAPHY
410
?
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?
i
Appendix 19 - Page 4
INTRODUCTION
Cast iron is one of the most widely used materials in the construc-
tion of machines.-- The weight of cast iron parts of the majority of
machines forms 45-85% of the machine weight. Cast iron is.used in
almost all fields of the national economy. The cast iron castings
which are used nowadays are quite complex: Their weight ranges
from a few grams to 250 tons; the thickness of the castings varies
from 2 to 500 mm. and up (Reference 1).
The widespread use of iron castings is explained by their low cost,
good casting properties, and particular properties of the cast iron
as a construction material (versatility, high resistance to wear,
low sensitivity to concentration of stresses and resistance to
vibration).
However, for a long time an important obstacle in the widening of
the spread of cast iron parts were the low mechanical properties
of the cast iron. This was contrary to the basic tendencies of
modern machine construction, which is to lower the machine weight
and, in particular, to lower the number of cast parts. The develop-
ments in machine construction require castings from alloys which--are
more stable and have a higher ductility than the regular sulphur-
containing cast iron. The production of castings from steel and
malleable cast iron.is connected with a series of technological dif-
ficulties and is less economical than the production of castings from
gray cast iron.
Steel as a casting material is not as good as cast iron because it
has a high melting temperature, large degree of shrinkage, and low
fluidity, and has a tendency to form porosity and internal stresses,
which lead to the formation of hot and cold cracks and to liquation.
Therefore, the production of formed steel castings is one of the most
complicated problems in the castings technology. Castings of steel
require a large amount of metal, the castings have to be annealed,
cleaned, and there are many losses. All of these operations raise
the cost of steel castings and prolong the production cycle.
Cast iron can be looked upon as steel which has graphite inclusions.
As is known, the strength of graphite is very low, and, therefore,
these graphitic inclusions can be regarded as cavities.
Therefore, the low mechanical properties of cast iron are mainly due
to the presence of graphite flakes. Consequently, the casting and
metallurgical technician was faced with the problem of increasing
the strength of cast iron by lowering the influence of graphite. In
principle, the strength of cast iron was increased by changing the
shapes, sizes and the distribution of graphite inclusions in the
base metal. For this purpose, superheating and holding the liquid -
east iron at high temperatures for extended periods of time, the in-
troduction of a large quantity of steel, modification, etc., were
used. The application of all these methods allowed us to improve
the mechanical properties of cast iron considerably.
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Appendix 19 - Page 5
There are numerous patents and methods in the literature for the
production of cast iron with nodular graphite. Most typical of
these are shown in Table 1, in which it can be seen that as modi-
fiers a variety of additives can be used and the nodular shape of
graphite can be obtained by treating the cast iron with such ele-
ments as magnesium, cerium, calcium, lithium, zinc, barium,
potassium, sodium, selenium, tellurium, and thorium.
TABLE I
ADDITIVES AND METHODS OF CAST IRON TREATMENT
Additives and Methods of Cast
Iron Treatment
Magnesium Additives
?
?
Metallic magnesium added in .4 thru
1% (Ref. 8)
Scra of magnesium alloys (Elek-
tron) in the amount of .5-1.0%
(Ref. 9)
Alloys of magnesium with FeSi, with
a higher content of magnesium (over
20%) (Ref. 10 and 11)
Alloys of magnesium with FeSi, with
a low magnesium content (from 5-1590
(Ref. 12-16)
Alloys:
Mg Cu (from 15 to 50% Mg Ref 17
Mg Ni (from 20 to 50% Mg) (Ref 18,
Mg2Ni-C (17% Mg, 81% Ni, 2% C)
.(Ref 22,23)
Mg-Ni C (17% M, 10 47% Ni 5% C,
remaining Fe (Ref 22,23)
Mg-Cu-Ni-FeSi 33% Cu, 20% , 13%
Ni 26% Si, remaining Fe) M(Ref
22)
Violent reaction; absorption of
Mg is not great; it is mostly
used for casting of large sec-
tions; cast iron is considerably
cooled down.
Absorption not large; reaction
violent; cast iron is consider-
ably cooled down.
Lower absorption of magnesium by
cast iron; violent reaction;
pyrotechnics increase with in-
creased magnesium content in the
alloy.
Good absorption of magnesium by
cast iron; quiet reaction.
Specific wt. 7.40 Heavy alloys
" if 7.38 good absorp-
" if 7. 5 tion of Mg
Specific wt. 4.20; good absorption
and quiet reaction.
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Appendix 19 - Page 6
TABLE I (CONTINUED)
?
Additives and Methods of Cast
Iron Treatment
Notes
Alloys:
Mg-Ca (Ref 25)
The addition of Ca together with
Mg-SiCa (20% M$) (Ref 26)
Mg insures stable results; reac-
Mg-Ca-Ni-FeSi (15% Mg, 15% Ca,
tion is quiet; the modification
15% Ni, 45% Si, 10% Fe)
of cast iron by FeSi is not neces
(Ref 22)
sary; reduction of cementite for
20% Cu,
Mg
-20
~
~
u
C
mation on the surface; minor py-
~7 j
(R
f
60
68%
SiCa)
rotechnics.
Mg-Si-Ca-FeSi (12% Mg, 38%
SiCa, 50% FeSi) (Ref 27)
Mg, 13% Mn, 55%
25%
Mn from the alloy removes sulphur
)
Si) (Ref
from the cast iron, partially re
Mg-Ca-Si-Al-Mn-Fe (30% Mg, 20%
.
placing Mg.
39% Si, 2.5% Al, 0.5% Mn,
7% Fe ) ( Ref 2k )
Alloys:
Mg-Li (Ref 28, 55)
tion is quiet; the ratio of
Reaction
Li to Mg equals 1:30 up to 1:3.
mixture of Mg and Zr
The quantity of the introduced
10 30%
-
~
mixture is calculated from the re
5~ Si) (Ref. 62)
~
Zr,
1o
maining Mg content in the cast
iron which is in the range of 0.0
to 0.1%, Zr from 0.03 to 0.3%.
Mg-Bi (Ref 28 29)
(
Alloys of Mg and Cu and Al are no
15% Mg~ (Ref 17)
Mg-Al
because Cu (more than
recommended
15% Mg) (Ref 17)
Mg-Cu-Al
and Al (more than 0.3%) have
3%)
(
Mg (2-20% , Ca, Bap Sr, Li (2-15%,
an antimodifying effect.
each one or the ..sum of it) Si
(5-50%), Cu (3-50%), Fe (5-65%)
`Ref 2.9 )
Mg together with Ce (Ref. 30, 31,
and Ce have a combined effect;
Mg
32, 33)
modification results are stable;
the detrimental effect of element
with anti-modifying effects is
neutralized; spherical graphite i
Mg and at 0.001%
formed at 0.005%
Ce.
Mixture of 10% magnesium chips
High absorption of magnesium by
and 90% reduced in size ferro-
cast iron; quiet reaction.
silicon (Ref 12, 13)
-
-
1
t
s
s
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Appendix 19 - Page 7
TABLE I (CONTINUED)
?
Additives and Methods of Cast
Iron Treatment
Notes
Mixture of calcium cyanamid and
Calcium removes the sulphur from
the alloy of (10% Mg) and Ni,
the cast iron and replaces magne-
Cu, and Si. Weight ratio of
sium partially.
calcium cyanamid and the alloy
is 0.5:1 or 6:1 (Ref 35)
Mixture of Mg and MgO (3-10% Mg)
Quiet reaction; natural MgO can
with liquid glass (Ref 314)
be used.
Briquettes made from 31+% Mg, 33%
Compressed at pressures of 140
cast iron chips and FeSi
3%
tons, the briquette diameter is
(Ref 36,
(which itself is 75%~
140 mm.; its height is 120 mm.
37)
(Ural-Zis).
Briquettes made from M , Si, and
Reaction quiet; small magnesium
MgO (1:14:0.6 and 1.3) (Ref 38)
losses; absorb magnesium up to
Briquettes made from Mg. Si and
80%.
graphite (?) (1:4:1) (Ref 39)
Briquettes made.from Mg Si, and
~
(Ref 39)
CaC2 (1:14:0.6 and 2.5
Briquettes made from Mg powder
(Ref 39)
Melting under a layer of MgO or
At high temperatures (1700 deg.)
dolomite (2 MgO. CaO) (Ref 30)
Mg and Ca are introduced in the
cast iron during the melting.
Gaseous magnesium alone or to-
Introduced through a tube into
ether with an inert gas
the ladle or into the furnace.
Ref 4o)
Magnesium powder together with an
Introduced into the ladle by
inert as such as nitrogen or
means of feeders; good absorp-
argon (Ref 141)
t ion of magnesium.
Calcium Additives
0
Ca (Ref 142, 143)
Ca together with Ce (Ref 22, 51)
Ca-Cu 10% Ca) (Ref 142)
Ca-Si 20-25% Ca) (Ref 142)
Ca-Si Ref 44)
Amount of Ca introduced is 0.125
to 0.650%; reaction is quiet;
cast iron has to be hot.
Is introduced in the amount of
3-5% as a powder into the ladle
or into the mold.
CaC2 (Ref 145, 146, 49)
Nitride, Cyanamid and calcium hy-
dride (Ref 149) CaF2 (Ref 47)
Blow into the cast iron together
with nitrogen and try to avoid the
formation of CaO.
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Appendix 19 - Page 8
TABLE I (CONTINUED)
?
0
Additives and Methods of Cast
Iron Treatment
Notes
MgO. CaO (fired dolomite) (Ref.
Mg and Ca are introduced into the
48)
cast iron from the slag, from the
CaO (lime) (Ref 48)
lining, or from the flux cover.
Alloys:
Ca-Si-Cu (24% Ca, 56% Si, 20%
The addition of Ca together with
Cu) (Ref. 43)
Mg insures stable results.
Ca-Si-Cu-Ni (20-26% Ca 46-59%
f 4+
)
l
3
(Re
Si, 20% Cu, 14-5% Ni
Ca-Si-Mg-Cu-Ni (10-35% Ca, 140-
65% Si, 1-5% Mg, 0-50% Cu,
0-30% Ni) (Ref 43)
Ca-Si-Li-Mg-Cu-Ni (20-22% Ca,
10.50% Si, 6-15% Li, 2-1+% Mg,
12-20 Cu, 13-20% Ni) (Ref 4+3)
1.5% SiCa; 2% CaF2 0.5% Zr (as a
Calcium fluoride is added as a
mixture or separately) (Ref 50)
flux reagent; zirconium for the
increased strength and obtaining
of spherical graphite.
Other Additives
Cerium alloys (mischmetal) 45-52% Is usually applied for modifica-
Ce, 45-48% rare earth (La, Pr, tion of hyper-eutectic cast irons.
and ?) 0.5-1+% Fe, up to 1.6% Mn,
up to 3% Si, Cu, Al (Ref 51)
Metallic Bi (Ref 52) Is added to the ladle in the amount
of 0.2-0.3%.
Te,
B
(Ref
22)
K,
Na
(Ref
22,
Li (Ref 54255)
53)
Reaction products of TeS, Teo and
BS are difficult to remove from
the cast iron.
Violent reaction; absorption very
low; sodium vapors are toxic;
alloys based on K and Na are diffi-
cult to make.
Spherical graphite is obtained if
Li from 0.005 to 0.1%. Sulphur
content has to be higher than
0.08%.
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TABLE I (CONTINUED)
0
0
Additives and Methods of Cast
Iron Treatment
Notes
Zn (Ref 56)
Mn content in the cast iron shoul
be less than 0.1%, carbon less
than 2.6%; under these conditions
spherical graphite is obtained at
0.kk% sulphur.
Blowing of gases through cast
Spherical graphite is obtained
iron such as: Argon, chior-
only in part.
ine, nitrogen and hydrogen
(Ref 56, 57)
Superheating of cast iron in the
Superheating at 1600-1700 deg.;
furnace,--melting under vacuum
vacuum 5.10-k atmospheres; when
and high-speed of cooling
casting the iron into the shell
(Ref 57)
mold, the formation of spherical
graphite can be observed.
Pre-Treatment of Cast Iron
before the Introduction
of Magnesium
Preliminary removal of sulphurs
Ca. Ce, or CaC2 (Ref 58, 59)
Preliminary
oxidation
of
iron by
(for
~
ing
annealing.
)
(Ref 60
cast
?)
Blowing oxygen or air through
cast iron (Ref 61)
d
The content of sulphur is lowered
and less Mg and Ce is used. The
amount of introduced Mg can be
lowered down to 0.005%. The in-
crease of the range of the compo-
sition of the 'charge as far as
sulphur is concerned. Calcium
carbide is introduced into the re-
ceiver of the cupola by means of
a gas (N2, Ar, but not in
air or 02) through a graphite tube.
For 1 kg. S, 10 kg. of CaC2 are
introduced.
Absorption of Mg'by cast iron is
increased.
Magnesium absorption is increased;
the amount of non-metallics is de-
creased.
The name for this cast iron has not yet been defined in literature.
It is called either "Cast Iron with Spherical Graphite", "High Strength
Cast Iron", "Super Strong Cast Iron", "Cast Iron with Nodular Graphite",
"Cast Iron with Plastic Properties", "Malleable Cast Iron with Spheri-
cal Graphite in the Cast Structure", "Ductile Cast Iron", "Magnesium
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Cast Iron", "Cast Iron Treated with Magnesium", "Cast Iron Modified
by Magnesium", etc.
In order to differentiate between the lamellar form of graphite in
the regular gray cast iron and the flake graphite in malleable cast
iron, the graphite in cast iron treated with magnesium is called
"globular", "round","spheroidal", "spherical", "granular", etc.
According to GOST 7293-54, in castings made from high strength cast
iron the graphite is called "spherical" and the cast iron is called
"high strength". However, the term "high strength cast iron" is too
general and can refer to different cast irons; therefore, in the
present work the term "magnesium cast iron" and the term "spherical
graphite" are used as the shortest and because they most completely
reflect the technology of the product of cast iron and the shape of
the graphite.
The mechanical properties of the magnesium cast iron, due to the
spherical form of graphite, differ very much from the starting gray
cast iron. In Table 2 the properties of cast steel, and magnesium,
gray and malleable iron are shown. From this table it can be seen
that the range of tensile strength of magnesium cast iron is close
to that of carbon steel (70-80% of the steel strength) and is con-
siderably higher than the strength of the gray and the malleable cast
irons. The ductility or plasticity of magnesium cast iron is much
higher (5-15 times) than the plasticity of the gray iron and is close
to that of steel and malleable cast iron. Impact toughness of magne-
sium cast iron is higher than that of gray and malleable cast iron,
but is lower than that of steel, but as we are going to see in the
following, it depends to a higher degree on the chemical composition
and the conditions of the cast iron cooling, in particular on the
phosphorus content. As to the casting properties of magnesium cast
iron (Table 3), they represent a peculiar combination of properties
of regular gray cast iron (good fluidity small linear shrinkage, no
tendency for the formation of hot cracks), properties of steel (the
tendency to form shrink cavities) and the properties of the white
cast iron (tendency to form cold cracks).
TABLE 2
Steel Gray Malleable Magnesium
Properties Castings Cast Iron Cast Iron Cast Iron
GOST 977-53 GOST 1412-48 GOST 1215-41 GOST 7293-54
Limit of Tensile
Strength in
kg./mm.2 ......... 4o-60 .... 12-38 30-4o .... 40-60
Elongation in % ... 10-28 .... (to 0.5) .... 3-12 .... 1.5-10
(to 20%) (to 20%)
Limit of Bending
in kg./mm.2 - .... 28-60 .... - .... (70-110)
Amount of Deflec-
tion at Fracture (3~5-30)
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TABLE 2 (CONTINUED)
Properties
Steel
Castings
Gray
Cast Iron
Malleable
Cast Iron
Magnesium
Cast Iron
GOST 977-53
GOST 1412-48
GOST 1215-41
GOST 7293-54
Impact Toughness in
kgm/cm.2 .........
2.5-5
...
(to 0.5) ...
0.5-3.0
...
1.5-3.0
(to 10)
Brinell Hardness ..
-
...
143-262 ...
149-201
...
156-269
TABLE 3
Properties
Steel
Gray
Oast Iron
Malleable Magnesium
Cast Iron Cast Iron
Linear Shrinkage in % 2.0-2.2 0.8-1.2 1.5-2.2 0.8-1.4
Tendency to Form Shrink-
age Cavities Large Small Large Large
Tendency to Form Stresses " " if 11
Liquid Fluidity Satis. Good Satis. Good
From the economic point of view, the use of magnesium cast iron is very -
satisfactory. If the basic cost of the regular cast iron casting is con-
sidered to be 100%, then the corresponding basic cost of magnesium cast
iron castings equals 130% and of steel castings 160% (Reference 63).
Thus, the high mechanical properties and the good casting properties of
magnesium cast iron, the lower cost and the possibility of producing it
by way of the regular casting process make it possible to consider it as
a new construction material. From this cast iron, in many cases, products
can be cast which have a great industrial and economic effect which
usually are made from steel, malleable cast iron,.bronze, or other non-
ferrous metals. The use of magnesium cast iron makes it possible to re-
duce the weight of iron castings and increases their service properties
and strength.
The widening of the range is noticeable at the present time in the use of
? magnesium cast iron in various branches of machine construction such as
Diesel construction, compressor construction, ships, auto and tractor con-
struction, etc.. Rolling mill rolls made from magnesium cast iron have 2-3
times greater strength than those made from lamellar. graphite. Magnesium
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cast iron can be used advantageously in several fields as a heat and
corrosion resistant material. Great possibilities are open for mag-
nesium alloy cast iron of the austenitic type, "Nirezist", which have
high mechanical properties and are resistant to heat and corrosion
(Reference 64, 65).
In spite of this and all of the advantages of magnesium cast iron.,
there has been only limited application in the foundries of the USSR
as well as abroad. For instance, in the United. States the production
of castings from magnesium cast iron in 1951 was only as high as
100,000 tons per year, which is only 0.77% of the gray cast iron out-
put and 11% of the malleable cast iron production (Reference 66);
however, at the present time the production of magnesium cast iron
castings is increasing rapidly and in 1955 magnesium cast iron was
produced in 334 foundries in various countries (Reference 412). This
can be explained by the lack of systematic data on properties, pro-
duction and application fields for magnesium cast iron, as well as by
some particularities of the process for its production and casting
which remain either unclear or unfinished. The following problems
are still open:
(a) The method of introducing magnesium, as well as the
introduction of other additives and, in connection
with this, the determination of the amount of these
additives which would be sufficient to obtain stable
results;
(b) Chemical composition of the cast iron and, in par-
ticular, the influence of the alloying additives on
the structure, mechanical and other properties of
magnesium cast iron;
(c) Mechanism of structure formation and occurrences during
the modification;
(d) Investigation of other additives besides magnesium
which favor the production of spherical graphite;
(e) Studying the mechanical, physical and casting
properties of this cast iron from all viewpoints;
(f) Study service of the castings at normal conditions
of use;
0
(g) Improvement of the technology of good quality cast-
ings from magnesium cast iron;
(h) Rationalization and economic conditions of the
thermal treatment and other treatments.
There are many publications on the theory and the practice of casting
production from magnesium cast iron in the USSR as well as abroad.
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For further development and improvement of the production of castings,
of great importance will be the general and scientific analysis of
the experimental. and theoretical material collected.
The scope of the present publication is to give a generalization and
a systemization of the basic parts in the composition, the proper-
ties, the production and the fields of application of the castings
based on our own investigations as well as on the literature.
The authors hope that their modest work will contribute to wider in-
troduction in industry of this new construction material.
The authors will be happy for some notes or corrections. Please
address to: Kiev
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CHAPTER XI
?
THE FIELDS OF APPLICATION AND THE RESULTS OF THE EXPLOITATION
OF MAGNESIUM CAST IRON CASTINGS
Magnesium cast iron possesses high mechanical properties, for which
reason castings made from it will be stronger and more durable than
the castings made from gray cast iron, or they can have a smaller
wall thickness than the castings made from gray cast iron. In other
words, the use of magnesium cast iron in place of the gray form is
one of the decisive ways to reduce the weight of cast articles and
increase their length of service.
Magnesium cast iron on a ferrite base also possesses high plastic
,properties, which are absent for the ordinary gray and modified cast
'irons. Nearly all of the exploitation properties of magnesium cast
iron are considerably higher than for the gray and modified cast
irons. The alloying of magnesium cast iron leads to obtaining new
types of cast irons, possessing high service properties, which sub-
stantially exceed the properties of the alloyed gray and modified
cast irons.
When compared with wrought iron, ferritic magnesium cast iron, with
similar values for the elongation and toughness, shows higher strength
properties and especially the elastic limit. In addition, the dimen-
sions of the castings from magnesium cast iron and their thickness
do not possess the limitations inherent to wrought cast iron.
Magnesium cast iron, having nearly the same strength as cast steel,
shows better casting properties, which facilitates obtaining sound
castings. Together with this, magnesium cast iron retains the good
service properties inherent to gray cast iron (high abrasion resist-
ance, high cyclic tenacity, low sensitivity to the influence of
stress concentrations, good workability, etc.).
Magnesium cast iron can be used to cast a series of complicated
articles (crankshafts, cam shafts, etc.) instead of their being
forged or stamped out.
It should be mentioned again that in recent years the criteria used
to evaluate the strength of cast irons and steels have been changed.
In order to correctly evaluate the durability it is necessary to take
local stress concentrations into consideration. Practice shows that
the failure of parts during operation bears in most cases a fatigue
character and is associated to less degree with elongation. Conse-
quently, a small elongation for cast iron, when compared to steel,
in most cases is not a disadvantage. For this reason machine build-
ers should turn their attention mainly to the resistance offered by
the fatigue limit to factors that reduce its value, producing local
stress concentrations. In this respect magnesium cast iron differs
but slightly from wrought steel.
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Some orienting data are given in Table 112 on the cost of articles
made from cast iron and steel prior to mechanical treatment, relat-
ing to plants building medium machines and to those with assembly
line production (the cost of a ton of cast iron articles from gray
iron is taken as 100%). The cost of casting, heat treatment and
supplementary equipment enters into the cost of the castings made
from magnesium cast iron. From Table 112 it can be seen that mag-
nesium cast iron is cheaper than either wrought iron or steel.
TABLE 112
Cost of the
Metal Article article in %
Cast from gray cast iron ................ 100
Cast from modified gray cast iron ....... 110
Cast from magnesium cast iron ........... 130
Steel forgings 185
? Wrought iron 226
Steel casting 252
According to the data of the Syzran hydroturbine plant (Russian
Ref., 1955), the manufacturing cost of a ton of cast iron castings,
prepared from magnesium cast iron, is approximately 2.5 times cheaper
than the cost of a ton of steel castings of the same degree of com-
plexity, while according to the orienting data of the Novo-Kramatorsk
machine-construction plant it is cheaper by only 25% (Russian Ref.,
1955). The cost of manufacturing castings from magnesium cast iron
depends to a considerable degree on the scale of production. It is
quite obvious that after becoming familiar with the technology of
preparing castings from magnesium cast iron the cost of their manu-
facture will be only slightly above the cost of manufacturing the
castings from gray iron.
A comparison of the mechanical, casting and exploitation properties
of cast irons and steel permits explaining the exceedingly great in-
terest shown in cast iron containing spherical graphite and visual-
izing the broad perspectives for its use in machine construction.
We will present some examples of the practical application of magne-
sium cast iron, proceeding from those requirements as apply to the
conditions for the exploitation of various parts.
Crankshafts. In recent years magnesium cast iron has been used to
replace wrought steel in the manufacture of crankshafts for station-
ary ship, automobile and tractor engines and compressors.
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Crankshafts can be fabricated either by casting, hot stamping or
forging. For technical reasons, the stamping of fabricates is
possible only for comparatively small shafts and is practical only
for the mass production of the same type of shafts. Of these
methods for the fabrication of crankshafts that of casting shows an
advantage, since here there is a substantial reduction in the amount
of metal loss and in the time of subsequent mechanical treatment.
In addition, the employment of special and general equipment for the
mechanical treatment of the shafts is reduced, the output of the
forge press equipment is set free, the need for cooperation of the
plants without forge press equipment is eliminated, etc.
Cast iron is the material usually used for cast shafts, since their
casting from steel, due to the much poorer casting properties of the
latter, requires extremely complex technology.
Gray cast iron, due to its low mechanical properties and associated
inadequate reliability during operation, has failed to find exten-
sive use in the casting of crankshafts. From literature data it is
known (Russian Ref., 1953; Russian Ref., 1954; French Ref., 1951;
and German Ref., 1955) that the casting of crankshafts from magnesium
cast iron is both most progressive and expedient.
To obtain the least amount of wear during use a magnesium cast iron
with a pearlitic structure (VH 60-2) is usually used for the casting
of crankshafts.
Some comparative technical-economic data are given in Table 113 on
the production of forged shafts from 30 XM steel and of shafts from
magnesium cast iron for diesels, relating to the tested portions of
the castings (Russian Ref., 1953).
TABLE 113
Designation
Forged
Steel
Shaft
Cast
Cast-Iron
Shaft
Weight of ingot in tons
12
--
Weight of blank in tons
6.3
2.7
Pure weight in tons
1.9
1.7
Work load in norm-hours
1495
694
Included in this:
Preparation of the blanks
439
480
Heat treatment
15
6
Mechanical treatment
1050
208
Length of the fabrication
60
20
""' 1 f n ? ri a -Ira
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It should be mentioned that in the transition to serial production
both the work load and the cost of the cast shaft from magnesium
cast iron will-be reduced by 25-30%. In addition to effecting a
three- to four-fold reduction in the cost, the replacement of wrought
steel by magnesium cast iron in the fabrication of crankshafts per-
mits replacing the molybdenum steel alloy by a cheaper and more
abundant material (with a simultaneous saving of more than 4 tons of
metal), results in a smaller load through the special annealing
machines for mechanical treatment (approximately a 5-fold decrease),
etc.
As had already been mentioned (see p. 357), a three-year testing of
magnesium cast iron crankshafts for D-5 engines, operating on trac-
tors in the MTS, revealed that the average wear of the shaft
journals made from magnesium cast iron was one-half that shown by
steel journals, while the average total wear of the shaft journals
and bushings was 35-40% less than that shown by the steel shafts.
For crankshafts, operating at high speeds, the fatigue endurance is
of extreme importance. Actual tests made on shafts (Russian Ref.,
1954) with alternate symmetrical flexing reveal that the fatigue en-
durance of"shafts, cast from magnesium cast iron, and the fatigue
endurance of shafts, fabricated from steel 45, are practically the
same and approximately twice as great as that of shafts fabricated
from gray cast iron CH 21-40.
According to the data of Kudryavtseva (Russian Ref., 1954), the
fatigue cracks in magnesium cast iron spread from one graphite inclu-
sion to another, and chiefly permeate the graphite inclusions having
the least roundness and substantial size. Consequently, in fabricat-
ing shafts from magnesium cast iron much attention should be given to
the structure of the metal base and the form of the graphite.
Gamma rays are used to control the casting density, while control of
the mechanical properties is run on the cast specimens.
As a result, from the presented data it can be seen that magnesium
cast iron is a very valuable substitute for wrought steel in the fab-
rication of. crankshafts.
Articles of the Piston Group. Magnesium cast iron is successfully
used for the fabrication of such parts as the crankgear and gas dis-
tribution mechanism of engines, connecting rods, connecting rod,
covers, crossheads, pistons, piston rings, sleeves, camshafts,
plunger, etc. These articles are usually fabricated from pearlitic
magnesium cast iron and are cast in dry molds. The transition in
the fabrication of this group of parts to their casting from magne-
sium cast iron is accompanied by a substantial reduction in the
amount of work required for their fabrication and leads to a saving
in the consumption of rolled steel and nonferrous alloys (Russian
Ref., 1953).
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The piston is one of the important parts of the connecting rod-
piston group that is exposed to wear, corrosion, action of high
temperatures, etc. The pistons of the YAZ-204 en ine, fabricated
from pearlitic gray iron, have a short life span (on the average a
mileage of 15-30 thousand kilometers) due to the appearance of
cracks, scorching. of the bottoms, and also wear of the piston
grooves (Russian Ref.', 1953). When these pistons are fabricated
from magnesium cast iron with a pearlitic ferrite structure for
the base metal their length of service is sharply increased. Most
of the tested pistons looked well after being run 65 thousand kilo-
meters: The pistons failed to show cracks, scorching of the bottoms
or wear of the piston grooves. In addition, the piston pin operated
without bronze bushings on the cast iron, and showed less wear
(0.03 mm.) than is customary for a bronze bushing in the upper head
of the pitman (0.11 mm.).
Pistons, cast from magnesium cast iron, are long-lived, and their
service life is three to four times that of pistons fabricated from
wrought iron with a granular pearlite.
As regards piston rings, fabricated from magnesium cast iron, then,
as had already been mentioned (see Figure 240), their wear, as tested
in the performance of automobile engines GAZ-AA and ZIS-5 (Russian),
is considerably less than that shown by rings made from gray and
alloyed cast irons.
The installation of a top compression ring from magnesium cast iron
on the piston of diesel engine YAZ-204 assured reliable performance
of the diesel engine during operation, which could not be obtained
with rings fabricated. from alloyed gray cast iron.
The wear resistance and reliability of operation of camshafts and
plungers, fabricated from modified gray cast iron, and even more so
when fabricated from magnesium cast iron, is considerably greater
than that shown by the same parts when fabricated from steel (Russian
Ref., 1955). And here also magnesium cast iron proves to be a com-
plete substitute for steel with a substantial economic advantage.
Tractor and Automobile Parts. Magnesium cast iron is also success-
fully used in the fabrication of other tractor and automobile parts:
Differential crankcase, front and rear wheel hubs, brake shoes, brake
system supports, spring su ports, rear transmission housing, armature,
Jack parts (American, 1952), etc.
According to the data of Gosteva and others (Russian Ref., 1951), the
casings for the divided axles of tractors U-1 and U-2, tested under
conditions more drastic than the usual field conditions, showed ade-
quate strength and reliability.
The sockets of tractor cross arms are also fabricated from magnesium
cast iron, replacing Bronze OCS 5-5-5 (Russian Ref., 1951). As is
known, the cross arm sockets operate under conditions of inadequate
lubrication and abrasive wear. The results obtained in the testing
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of cross arm sockets under exploitation conditions on DT-54 tractors
for two seasons of field operation reveal that the'wear of sockets
made from magnesium cast iron is approximately 30-40% less than the
wear shown by serial sockets, fabricated from bronze Br. OCS 5-5-5.
Bearing Separators. As the data of Belkova and Kaminarskii show
(Russian Ref., 1955), magnesium cast iron can be recommended as a
substitute for brass LS 54-1 in the fabrication of massive separa-
tors for roller bearings.
The roller bearing separators, cast from magnesium cast iron by the
centrifugal method and heat treated on ferrite and pearlite (20%
sorbitic pearlite), were tested under the conditions operating in
medium sized section mills and in the machine assemblies used in
the coal, lumber and machinery construction industries. All of the
bearings with cast iron separators operated satisfactorily, and
destruction of the separators and escape of the bearings from the
machine assembly was not observed.
Metallurgical Equipment Parts. Magnesium cast iron is successfully
used for the fabrication of many metallurgical equipment parts:
Rollers, roller conveyor and rolling mill frames, casting molds, gear
casings of rolling mills, hammer presses, anvils, frames, boxes,
wheels of casting machines, etc. (French Ref., 1951 and German Ref.,
? 1955).
According to the data of Ezerskii (Russian Ref., 1950 , Balle (Ameri-
can Ref., 1955) and others (Japanese), the durability of rollers,
cast from magnesium cast iron, exceeds the durability of ordinary
rollers by'2.5-3 times.
Magnesium cast iron is also successfully used for the rollers of
blooming mills in the production of rails, and also in the mills for
the production of sheet steel (American Ref., 1955).
As Pisarenko indicates (Russian Ref., 1955), for the production of
molds with a wall thickness of 100-150 mm. the composition of the cast
iron after its treatment with magnesium is taken as the following:
3.1-3.6% C; 2.2-2.8% Si; 0.3-0.9% Mn; 0.1-0.18% P and up to 0.02% S.
To remove the internal casting stresses and impart plastic properties
to the cast iron the molds are subjected to graphitization annealing
(heating to 910-930? at a rate not exceeding 150? per hour, holding
at this temperature for 6-10 hours, cooling to 650 at a rate not ex-
ceeding 25? per hour, and further cooling with the furnace).
The average durability of molds made from magnesium cast iron for
small and medium sized ingots as 2-2.5 times greater than the dur-
ability of molds made from ordinary gray cast iron. The introduction
of magnesium cast iron into the production of molds made it possible
to reduce their consumption from 12-14 to 5-6 kg. per ton of steel.
The use of magnesium cast iron for molds also made it poss.bie to cast
them in metal molds, which led to a simplification in the fabrica-
tion technology and to a substantial improvement in the mechanical
properties when compared to casting in sand molds. It should be
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mentioned that attempts to use metal molds for the casting of molds
from ordinary gray cast iron have been unsuccessful. The high dur-
ability possessed by molds cast from magnesium cast iron is also
indicated by other investigators (American Ref., 1951 and American
Ref., 1951).
Machine Construction Parts. Mounts, carriages, drums, the casing of
hydraulic pumps, gears, shafts, chucks and other parts, cast from
magnesium cast iron, have recommended themselves well in use
(Polish Ref., 1953).
Agricultural Machinery Parts. Rollers of harvesting machines, coni-
cal and cylindrical gear wheels and gears of various sizes with
cast teeth, sprocket wheels, plowshares, harrow teeth, harrow disks
and other parts can be successfully fabricated from magnesium cast
iron instead of steel (Japanese Ref., 1953).
As Nikolaenko indicates (Russian Ref., 1954), plowshares that had
been cast from magnesium cast iron are in no way inferior in use to
plowshares that had been fabricated from steel L65 and L53. The
plowshares are chill-cast, after which they are subjected to
graphitizing normalization. To temper the cutting edges the plow-
shares are heated in a salt bath of 920 and 950? and then quenched
in water. The annealing temperature is 240-280?. That plowshares
? made from magnesium cast iron possess good durability is also indi-
cated by other investigators (French Ref., 1953)?
"Zigzag" harrow teeth, cast from magnesium cast iron instead of being
forged from rolled structural steel, when tested under field condi-
tions, showed a durability that was on a par with that shown by
steel teeth.
?
Harrow disks, cast from magnesium cast iron, can also be successfully
used instead of stamped steel disks. Magnesium cast iron can also
be used in the fabrication of cultivator blades, levers and frames
for the tractors, etc. (French Ref., 1953)?
Use of Magnesium Cast Iron in Other Branches of Machinery Construction.
Magnesium cast iron can be successfully used in the fabrication of
various equipment parts in the petroleum industry (parts of drilling
machines, valves and fittings of cracking installations, etc.); in
the fabrication of parts for hoisting and moving equipment (the wheels
of overhead cranes and cars, pulleys, flywheels, drums, etc.); loco-
motive parts (valve sleeves, parts for the steam-distribution assembly,
etc.); parts for steam turbines (diaphragms, condensate drains,
separator valve boxes, rotors, etc.); parts for compressors and pumps
(housing for compressors and pumps, propellers, etc.); parts for hy-
droelectric turbines (vanes, controls and regulating links of the
distributor, etc.); pile-driver heads; vises, anvils, etc. (American
Ref., 1955 and French Ref., 1953)?
The condensate drains for steam turbines, fabricated from magnesium
cast iron instead of the earlier used L30 steel, consist of a float
chamber and cantilever, have a rough weight of 450 kg., a shell
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thickness of 20 mm, are tested for a pressure of 28 kg./sq. cm.,
operate in a hot medium under a pressure of 16 kg./sq. cm., and
fully justify themselves in use.
The h droelectric turbine vanes consist of a streamlined portion
(fins), cast as one piece with the top and bottom trunnions, the
overall length of the vanes is about 3 meters, the weight is about
1.8 tons, the greatest thickness in the trunnions is 240 mm., and
the wall thickness of the fins is 40 mm. One hydroelectric tur-
bine requires 24 such vanes with a total weight of 43.2 tons. Dur-
ing operation the vane is loaded by hydrostatic pressure and the
power transmitted from the servomotor (relay) through the distribu-
tor winding mechanism. Vanes, fabricated from magnesium cast iron,
have been installed as replacements in several of the water tur-
bines in one of the hydroelectric stations (Russian Ref., 1955).
Pile-driver hammers, manufactured from magnesium cast iron and
weighing 1.8 and 3 tons, after two years of operation, with the
hammer falling a distance of 16 meters, fail to show even a single
crack or chip (Russian Ref., 1955).
Anchors for river vessels, cast from magnesium cast iron instead of
being fabricated from wrought steel, showed excellent results when
tested for dropping a distance of 8 meters.
Magnesium cast iron is successfully used in the fabrication of parts
that operate under high temperature conditions and in corrosive
media.
According to the data of Girshovicha and others (Russian Ref., 1954),
armature parts, cast from magnesium cast iron (flange ventilators),
are extremely close to cast carbon steel in their properties. Conse-
quently, magnesium cast iron with a ferritic base is fully suitable
for armatures, operating at temperatures up to 425? and pressures up
to 40 kg./sq. cm.
Parts made from cast iron with a ferrito-pearlitic or pearlitic base
are completely graphitized with an increase in volume when heated for
extremely long periods of time, and consequently rapidly escape from
the assembly. Thus, the valve seats in a tractor head, operating at
a temperature of up to 350-450? and fabricated from pearlitic magne-
sium cast iron, escaped from the system after 100 hours of engine
operation.
Since magnesium cast iron operates better than steel in various
corrosive media, and has a high strength and plasticity, it is used
to fabricate pipes for sewer systems, the transfer of petroleum,
etc. (American Ref., 1955; Indian Ref., 1953). The pipes are cast
by the centrifugal method. The pressure in pipes made from magnesium
cast iron can be increased two-fold when compared with pipes made
from ordinary gray cast iron.
As had already been indicated, the austenitic class of magnesium cast
iron alloys possesses wide utilizati.n perspectives for the manu-
facture of parts that operate at high temperatures and in corrosive
media.
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Appendix 19 - Page 22
Magnesium cast iron can be successfully chill-cast, which makes it
possible to expand the nomenclature for the parts that lend them-
selves to serial production. In chill-casting the outer zones and
even the whole cross-section of the casting are obtained with a
white color; by means of graphitizing annealing and subsequent heat
treatment it is possible to obtain any desired structure, and conse-
quently, the desired mechanical properties. Chill-cast parts,
operating under rubbing conditions (bearing separators, sockets, etc.),
showed better antifriction properties than did the corresponding
parts when cast in sand molds, due to the more homogeneous surface
structure (Indian Ref., 1954).
It should be mentioned that at the present time magnesium cast iron
is used to produce castings of different configuration, varying in
thickness from 3 mm. to 1 meter, and weighing from several grams to
tens of tons. The variety of parts, being transferred to castings
of magnesium cast iron, is constantly expanding.
At the present time the production of castings from magnesium cast
iron is utilized by many plants of individual and small serial
manufacture. However, the question of this cast iron finding broad
acceptance in the casting sections of massive manufacture, and fore-
most as a substitute for wrought iron and steel, is of greater im-
portance.
From the presented data it can be seen that the broad introduction
of magnesium cast iron in machinery construction, as a substitute
for cast, wrought and rolled steel, and also for wrought iron and
the nonferrous metals, can result in a substantial saving of metal
and in a reduction of the work load and cost.
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APPENDIX 20
"USE OF RADIOGRAPHIC METHOD IN INVESTIGATING
THE STRUCTURE OF MAGNESIUM ALLOYS"
By M. E. Drits, Z. A. Sviderskaya and E.S. Kadaner
Zavodskaya,Laboratoriya (Industrial Laboratory,, 1955,
#7, 831-833.
."Application of the (contact auto-) radiographic method to the
study of structural Mg alloys"
?
?
Usual metallographic etching methods are not useful in bringing out
the segregation of an alloying element in the inter-dendritic
interstices of magnesium alloys. However, if the inter stalline
distribution of Ca is being studied, radioactive Ca (Cag may be
used in conjunction with an autoradio-graphic technique. The'radio-
active Ca is used as an alloying material, and, if the macro-distri-
bution is being studied, x-ray film is placed in contact with a
polished surface-of the cast alloy and exposed for several days. For
a study of the micro-distribution, a highly polished surface is put
in contact with a fine-grained nuclear emulsion and exposed 10-15 days.
The resulting film is enlarged in the microscope and photographed by
transmitted light.
Fi . 1 - Slices of a sand-cast. billet containing varying per-
centages Ca show changes in the distribution of Ca. The most uni-
form distribution is obtained with the concentration in the range of
hundredths of a percent (la). The dendritic growth of segregation of
the Ca in the dendritic interstices is clearly shown as the Ca is,
raised to the level of tenths of a percent (ib). Segregation toward
the center of the billet is shown as the Ca is raised to one or more
percent (lc).
In a ternary alloy of Mg-Mn-Ca, etching shows very little (2b) of the
Ca distribution. However, contact auto-radiography of a slice (2a)
clearly shows the segregation. The cone of segregation is particularly
interesting.
The effect of cooling conditions and Ca content can be shown by micro-
contact autoradiography. The clearest dendrites are formed in the region
of tenths of a percent Ca. (Fig. 3A - tenths of percent Ca. 3b -
higher Ca content) In a Mg-Ca-Mn ternary, the Ca distribution varies
with position in the casting. Fig. 4a shows a spot from the upper
section of a casting and 4b from the lower section.
If a 4-component alloy is east in a heated mold instead of a sand mold,
different segregation patterns are present (6a,b). 6a is from the
center and shows 'grains that have grown practically equiaxially from
the liquid. These grains are fairly uniform in Ca distribution but
are surrounded by material richer in Ca; but this Ca-rich material
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Appendix 20 - Page 2
is also non-uniformly distributed, as can be seen from the Fig. 6b
taken at higher magnification.
Contact auto-radiography may also be used to study the effect of
heat treatment on the Ca distribution. Fig. 7a shows the cast state,
and Fig. 7b after heat treating 24 hours at 600C. The Ca is some-
what equalized by the heat treatment.
Figure -Captions
Fig. 1 - Autoradiograph (macro) of a binary Mg-Ca alloy (X 3/4)
Fig. 2 - Autoradiograph (macro) of a ternary Mg-Mn-Ca all.oy.X 3/4
Fig. 3. - Micro-autoradiographs from a binary Mg-Ca alloy X9
Fig. 4 - Autoradiographs of different spots from a sand-cast
ingot of a ternary Mg-Mn-Ca alloy X8
a - top
V - lower part
Fig. 5 - Micro-autoradiograph of a 4-component alloy
Fig. 6 - Micro-autoradiograph of the center of a special 4
component magnesium alloy
a enlarged 25 times
b - enlarged 750 times
Fig. 7,. - Micro-autoradiographs of magnesium alloys
a - as cast
b - heat treated 24 hours at 6000
Note: In the radiographs, the Ca is in the light regions for
the macrographs, but is in the dark regions for the micro-graphs.
(For the micrographs, the surfaces of the alloys were protected
from corrosion by coating with a 3% solution of Japan lacquer in
amyl acetate.)
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a
?
is
Appendix 20
a 6
PHC. 1. MaicpopaAHorpaMMw ABOAllb,X cnnaeoa Mg-Ca, X%
PHC..?2. Mau Koc y p~cnHTKa;,T.pq,'ixoro;,cnnaaa
ri
Pile. 3. MuKpupa:ui,n pa.nua
0111:I14n1, \~~~ ~? ,
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Appendix 20
PHc. 4. M11KpopaAHorpaMMw pa3JtH4HbIX McCT CJIHTKa
TpoilHOro cnnaBa Mg-Mn-Ca:
a - HepXllafi '30118 C.OBTKa, 6 - IIH)KHHH 30H1 QAfITKa; XA
PHC. 5. MHKpopaAHorpa1Ma 4eTbi?
peXKOMnOHeHTHOrO MarnueBOro
cn.Taea; X8
PHC. 6. MHKpOpaAHorpaMMM ueHTpaJII,HoA 4aCTH CJIHTKa 4eTbIpexKOMII0HeHT-
Horo MarHHeBoro cnnaBa:
a - npii yeenn4ennii 25. 6 - npii yaeawleniitl 750
?
[I O
PHc. 7. MHiKHra apH 6000 B Te4ennn 24 'Inc.; X5(
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INFLUENCE OF CRYSTALLIZATION RATE ON THE MICROHETEROGENEITY
OF MAGNESIUM ALLOYS
Technical Science Candidates Z. A. Sviderskaya and M. E. Drits
and Engineer E. S. Kadaner
The A. A. Baikov Institute of Metallurgy
of the Academy of Sciences of the USSR
?
?
Metalloved. i Obrabotka Metal. (Metallography and Metal Working),
No. 5, pp. 23-29 (1957).
Many investigators (/l/-/5/) indicate that the physical and mechanical
properties of alloys depend to a considerable degree on the microhetero-
geneity, observed in the structure of the cast material. A. A. Bochvar
/1/ indicates that a change in the cooling rate of alloys leads to a
change in the degree of intradendritic liquation, which is associated
with diffusion of the alloying elements in the liquid and solid states.
Very high cooling rates (for example, at the points of contact of the
metal with the cold mold) do not permit passing through primary diffu-
sion in the liquid phase and the structure of the metal is obtained
more or less homogeneous. At some average cooling rate, the progress
of diffusion processes is facilitated, creating a difference in the
composition of the solid and liquid solution, and here the intra-
crystalline heterogeneity reaches some sort of maximum value.
Further reduction in the cooling rate facilitates secondary diffusion
in the already hardened metal, which leads to some smoothing out of
the microheterogeneity. However, up to now a similar character of the
rule for change in the degree of intracrystalline liquation with
change in the cooling rate has failed to receive sufficiently clear
experimental confirmation.
Olsen and Hultgren /6/ believe that a reduction in the microheterogeneity
of alloys with increases in the cooling rate also facilitates super-
cooling, which retards the formation of crystalline centers and reduces
the degree of liquation. Using the x-ray analysis method, these
authors were able to show a regularity in the change of the micro-
heterogeneity as a function of the rate of cooling for the copper-gold
system of continuous solid solutions, depicted as a curve with a
maximum.
However, they failed to establish a similar relationship for the cop-.
per-nickel alloys.
To experimentally prove the existence of a curve with a maximum in the
change of the intracrystalline heterogeneity with change in the rate
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Appendix 21 - Page 2
of cooling N. E. Bolotov, M. I. Gol?dshtein and others/7/ made an
attempt to use the autoradiography method, which in recent years is
finding constantly increasing use in metallurgy and metallography.
These authors studied the distribution of phosphorus, sulfur, and
tungsten in steel with different rates of cooling, but failed to con-
firm the existence of a curve with a maximum.
On the basis of analyzing the data obtained in studying the dendritic
heterogeneity of a steel casting I. N. Golikov /8/ expressed the theory
that the reason for the observed divergence in the opinions of dif-
ferent investigators on the question of the existence of a maximum
on the curve "degree of microheterogeneity - rate of crystallization"
is the fact that in practice cases are considered where the rate of
cooling changes on different sides of the maximum. Here to the right
of the maximum an increase in the rate of cooling should cause a
reduction in the microheterogeneity, while on the other hand, to the
left of the maximum an increase in the rate of cooling should cause
an increase in the microheterogeneity.
To study the structure heterogeneity of magnesium alloys, containing
calcium, we'used the radioactive calcium isotope, which permitted us
to follow the change in the character of the micro-heterogeneity ob-
served in these alloys as a function of a number of factors.
We observed (/9/,/10/) that a change in the conditiorisof cooling the
alloys during their hardening exerted a sharp influence on the distri-
bution of calcium in the micropores (microspaces). A rapid cooling,of
the alloys when cast in a metal mold led to a very uniform calcium
distribution when compared with the sand-cast specimens, where sub-
stantial intradendritic heterogeneity was. observed. To establish the
relationship between the rate of cooling magnesium alloys and intradert--,
dritic liquation we used the quantitative autoradiography method, based'
on determining the amount of elements contained in a micropore (micro-
space) of the alloy by the method of photometric examination of the
radioautograms (/11/-12/).
First we constructed the characteristic curves, expressing the rela-
tionship between the intensity of radioactive radiation and the densi-
ty of blackening of the photoemulsion. With the assistance of these
curves we determined the region of blackegming, within the limits of
which there existed a direct relationship between the density of blacken-
ing and the radioactive calcium concentration. An M F-2 mic?ophoto-
meter with a square slit having an area of 1 sq. mm. was used in the
photometric examination of the radiograms at a magnification of 24X,
on a 5 mm. portion of the autograph.
The blackening density was measured at 0.01 mm. intervals, i.e. 500
determinations were made.
For studying the microheterogeneity we took three series of castings,
the variation in the cooling rate of which was achieved by different
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Appendix 21 - Page 3
methods. In the first case the binary alloys of magnesium with calcium
were cast in a metal mold, heated to different temperatures. The
second and third series of castings represented quaternary alloys of
the system magnesium-manganese-aluminum-calcium. In this case a
change in the cooling rate was achieved by using different types of
casting molds copper, steel with immersion in water, cast-iron with
heating to 5300, and dry sand molds), while in the last series of
alloys a difference in the cooling rate. was created by using sand molds
of variable cross section--having a diameter of 11, 30, 50 and 80 mm.
respectively.
Curves, showing the change in the blackening density along the length
of the photometered portion of the structure, were constructed for
all of the alloys studied by us. The curves for the binary magnesium-
calcium alloys, cast in. molds that had been heated to different tem-
peratures, are shown in Fig. 1. The character of the blackening
curves clearly shows the calcium distribution in the microspaces of
the alloy as.a function of the rate of cooling.
When cast in a cold metal mold at 200 the calcium is distributed very
uniformly and the blackening curve has a monotonic shape (Fig. 1).
With increase in the temperature of the mold the intracrystalline
heterogeneity increases, and large fluctuations in the blackening
values, i.e. in the calcium concentration are observed on the blacken-
ing curves. By making a statistical analysis of the photometric results
it was possible to estimate the degree of microheterogeneity present
in the structure of the studied alloys. For this the blackening
density values were converted into concentration values, and then
the distribution frequency curves were constructed. The frequency
curves, corresponding to all three cases of varying the cooling rate
of the alloys, are shown in Fig. 2. The maximum on the frequency
curves corresponds to the average amount of calcium in the given series
of alloys and determines the number of microspaces found in the photo-
metered portions with an average concentration. The higher the maxi-
mum on the frequency curve and the smaller the distance between its
branches, the more sharply expressed is the intracrystalline hetero-
geneity in the structure of the alloys. The frequency curves, corre-
sponding to the binary alloys of magnesium with calcium (Fig. 2,a),
show that with decrease in the mold temperature, i.e. with increase
in the cooling rate of the alloy during its crystallization the liqua-
tional microheterogeneity decreases. When the alloy is cast in a cold
mold, having a temperature ranging from 200 to 2000, the amount of
microspaces with an average calcium concentration is 80-90%. With
retarded cooling, when the mold is heated to 600-6750, only 35-38%
of the alloy microspaces have an average calcium content (for the
given series of alloys 0.06%).
On the whole, the curves shown in Fig. 2b for alloys of the magnesium-
manganese-aluminum-calcium system confirm the rule established for
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binary alloys relative to the change in the microheterogeneity as a
function of the rate of cooling.
An increase in the cooling rate when casting the alloy in either a
copper or watercooled steel mold results in substantially less micro-
heterogeneity than when cast in a sand mold or a heated cast-iron pot.
In the first case the amount of microspaces with an average calcium
content (equal to 0.13% for this series of castings) is 70-88%, while
in the second case this value is reduced to less than 30%. However,
it should be mentioned that for slow cooling rates the maxima on the
frequency curves for the discussed series of castings lie extremely
close to each other. With casting in a sand mold the maximum is even
situated somewhat aboveothat obtained when the casting is in a cast-
iron pot, heated to 530 , although the cooling rate in the sand mold
was minimum. Evidently, a deviation from the direct relationship
between the cooling rate and the degree of microheterogeneity shown
by a cast material is observed here. This deviation is shown more
clearly in the frequency curves (Fig. 2c), which relate to the four-
component magnesium alloy, cast in sand molds of different cross-section.
The maximum degree of microheterogeneity is obtained with the smallest
and largest diameters of the castings. The castings with average
diameter dimensions, and consequently with average cooling rates, show
a greater intraccrystalline heterogeneity.
For the rods with a diameter of 11 mm. the amount of alloy micro-
spaces, having an average concentration, is 55%. With increase in
the casting diameter from 30 to 50 mm. this value shows a corres-
ponding reduction to 32-27%, but then whmithe diameter of the casting
is increased to 80 mm. it again rises-to 41%, which is evidence that
a more homogeneous structure is again being obtained. The micro-
radiograms of-an alloy, taken with specimen diameters of 11, 50 and
80 mm., and at the same magnification as was used in making the photo-
metric measurements, are shown in Fig. 3. With increase in the
diameter of the casting from 11 to 50 mm. the intracrystalline hetero-
geneity becomes more sharply expressed. The interaxial layers, in
which the calcium concentrates, become thicker and the branching of the
dendrites increases. Further increase in the diameter of the casting
to 80 mmo leads to redistribution of the calcium in the alloy struc-
ture, conditioned by a quite slow crystallization and the possibility
of diffusion processes prevailing in the grain body. From the micro-
radiogram shown in Fig. 3c, it can be seen that the calcium is con-
centrated in the intergrain boundary zones, while inside the grain the
structure becomes more uniform.
As a result, the study made by us shows that a more uniform distribu-
tion of calcium in the microstructure of magnesium alloys can be
obtained either in the case of high cooling rates or, on the contrary,
with a sufficiently slow crystallization.
0 An intermediate cooling rate determines a large degree of intracrystal-
line heterogeneity for the calcium distribution.- To generalize?the
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obtained data the results of the statistical analysis of the curves
for calcium distribution were depicted in the form of two coefficients
K and C. Coefficient K characterizes the degree of microheterogeneity
shown by an alloy structure and is determined by the formula
K 1OO-n,
100
where n corresponds to the maximum on the frequency curve and repre-
sents the number of microspaces with an average cona,entration, while -
the 100 represents the number of microspaces in which the calcium con-
tent had been measured. Coefficient C is the ratio of the maximum
calcium concentration Cmax to its minimum concentration Cmin in the
individual microspaces found on the investigated portion of the structure:
C Cmax-
n
In Table 1 we give the values of the coefficients K and C for all of
the alloys studied by us, with the different cooling rates that were
employed by us in the present investigation. The cooling rate was
calculated as the quotient of dividing the temperature difference of
the start and end of alloy hardening by the.cooling time. The curves
showing the relationship between the cooling rate and the microhetero-
geneity of the alloys studied by us, constructed from the data given
in Table 1, are plotted in Fig. 1. As an. analysis of these curves
shows, in two cases (Fig. 4b and c) the relationship between the co-
efficents K and C and the cooling rate is expressed by'curves with a
maximum.
It should be mentioned that for the series of castings, relating to the
binary alloys of magnesium with calcium, the curves do not pass through
a maximum, i.e. the microheterogeneity of the structure constantly
decreases in measure with increase in the cooling rate. Evidently,
the curves obtained by us with a maximum correspond to the more general
case of a relationship existing between the cooling rate and intra-
crystalline dendritic heterogeneity, arising in the crystallization
of alloys of the solid solution type.
A study of the microstructure of the alloys cast by us reveals that
in all cases the. amount of a second phase were'very small, and con-,
sequently in their structure the investigated alloys were extremely
close to one-phase solid solutions.
If here it is considered that the photometric measurements of the
microradiograms were made at comparatively low magnifications, and
that the inclusions of the manganese ebmpone!t in the Mg-Mn-Al-Ca alloys
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Appendix 21 - Page 6
do not give a blackening on the microradiograms, then evidently it is
possible to assume that the obtained rules reflect the character of
the calcium distribution., conditioned by intracrystalline liquation
during crystallization of a solid solution.
As a result, the use of the quantitative radiography method permitted
not only estimating the magnitude. of the observed microheterogeneity
in the casting of magnesium alloys with calcium, but also permitted
obtaining experimental verification of the general character of the
change in the microheterogeneity with change in the cooling rate,
systematically mentioned by A. A. Bochvar /1/. As regards the devia-
tions (including the curve obtained by us and shown in Fig. LFa) from
this rule,, observed under actual conditions, then, in addition to
the above indicated reasons /8/, other no less important factors, such
as, for example, the physicochemical properties of the alloy itself,
should show influence here. It is probab]a that for the same diapason
of change'in the cooling rate different materials will be differently
inclined to show more or less developed dendritic crystallization,
which cannot fail to be without influence on the extent of micro-
heterogeneity arising during freezing. There is no doubt as to the
importance of establishing a relationship between the degree of micro-
heterogeneity and the cooling rate of alloys for solving individual
practice problems.
Many of the physical and mechanical properties of alloys depend on
the change in their structure heterogeneity. As is known the heat
resistance is one of the properties that belongs here. We determined
the heat resistance (endurance limit) of a number of alloy specimens
that had been cast in molds of variable cross-section. The structure
microheterogeneity of the tested specimens is clearly seen when the
microradiograms shown in Fig, 3 are examined. The conditions of
casting the specimens, the value of the microheterogeneity coefficient
and the values obtained for the endurance limit at 2500 are presented
in Table 2.
As can be seen from the data in this table, the heat resistance of the
investigated alloy shows substantial change with change in the cool-
ing rate. Here the highest values of the endurance limit are obtained
with average values of the cooling rate, i,e. with the greatest
degree of heterogeneity for the structure of the cast alloy. Evidently,
at high cooling rates,the same as with extremely slow cooling, a more
uniform distribution of the structure components facilitates the.
progress of diffusion processes and to a certain degree lowers the
heat resistance.
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Appendix 21 - Page 7
LITERATURE CITED
/1/ Bochvar, A.A., Principles of the Heat Treatment of Alloys,
Metallurgy Press, 1934.
/2/ Petrov, D. A., Problems in the Theory of Aluminum Alloys,
Metallurgy Press, 1951.
/3/ Dobatkin, V. I., Continuous Casting and Casting Properties
of Alloy, State Press of the Defense Industry, 1948.
/4/ Livanov, V. A., Metallurgical Principles of Continuous
Casting, Transactions First Technological Conference,
State Press of the Defense Industry, 1945.
/5/ Fridlyander, N. N., Transactions MAI,.No. 95, 1949.
/6/ Olsen, W. T., and Hultgren, R., Journal of Metals, Sect. 1, 1950.
/7/ Bolotov, N.E., Goldshtein, M.I., Popov, A.A., and
Fedorov, A.B., Zavodskaya Lab., No. 6, 1956.
/8/ Golikov, I.N., Monograph "Heat Treatment of Metals", State
Press of Literature on Machine Building, 1952.
/9/ Drits, M. E., Sviderskaya, Z. A., and Kadaner, E.S.,
Zavodskaya Lab., No. 7, 1955.
/10/ Drits, M.E., Sviderskaya, Z. A., and Kadaner, E.S.,
Investigation of Heat Resistant Alloys, Academy of
Science USSR Press, 1956.
/11/ Studnits, M. A., and Malyuchkov, O.T., Metalloved. i
Obrabotka Metal, No. 6, 1955.
/12/ Bokshtein, C. Z. Gudkova, T. I., Kishkin, S.T., and
Moron, L. M., Zavodskaya Lab., No. 4, 1955.
TABLES AND FIGURES
(1) Blackening curves for magnesium-calcium alloys:
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Appendix 21 - Page 8
1--320 min; 2--160?/min.; 3--105?/min.; 4--470/min.;
5--200 min.
(2) Density of blackening
FIGURE 2
(1) Calcium distribution with variation in the cooling rate:
a--as the result of differences in the mold temperature
(binary magnesium-calcium alloys); 1--320?/min.
2--1600/min.; 3--105?/min.; 4--47?/min.; 5--206/min.;
b--as the result of using different types ofocasting molds
(Mg-Mai-Al-Ca a~1o160b/min,1-1000/min.; ~ the 2 resu~t/ofn varying
3--450/min.;
the diameter of the sand mold (Mg- lCa alto s);
1--120?/min.; 2--4?/min.; 3--450/min.; 4-22 /
(2) Relative frequency
FIGURE 3
(1) Microradiograms of Mg-Mn-Al-Ca alloys, cast in sand molds
with different cross-sections. x25:
a--diameter of the mold 11 mm; b--50 mm.; o--80 mm.
0
FIGURE 4
(1) Relationship between the microheterogeneity and the cooling rate:
a--with different mold temperatures (Mg-Ca alloys);
b--with different methods of casting (Mg-Mn-Al-Ca alloys);
c--with different diameters of the sand molds (Mg-Mn-Al-Ca
alloys).
(2) Rate of cooling
TABLE 1
(1) Alloy (2) Average calcium content in %
(3) Rate of cooling in ?/min. (4) Coefficient of microheterogeneity K
(5) Ratio of the maximum concentration to the minimum C
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(6) Casting conditions (7) Remarks (8) Temperature of the mold in 0
(9) The cooling rate was varied by varying the temperature of the
mold
(10) Sand mold (11) Cast-iron mold 5300
(12) Steel mold with immersion in water (13) Copper mold
(14) The cooling rate was varied by using different types of molds
(15) Diameter of the mold in mm.
(16) The cooling rate was varied by changing the diameter of the
sand mold
TABLE 2
(1) Alloy casting conditions (2) Rate of cooling in o/min.
(3) Heat endurance limit 0" 250 kg./sq. mm.
100
(4) Coefficient of microheterogeneity K
(5) Cast in sand d 80 mm.
(6) Cast in sand d = 50 mm.
(7) Cast in sand d = 11 mm.
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TeMnepaTypbI H3JIONCHHUbt BHyTpHKpH- OxJiaN(AeHI15I cnJIaBOB. MaKCH,MyM 4a-
CTaJIJIH4eCKaH HeOAHOPOAHOCTb B03pa- CTOTHbIX KpHBbIX OTBetiaeT cpeAHeMy
CTaeT, H Ha KPHBbIX nO4ePHeHHH Ha- co iep KaHH10 KaJIbUHH B CnJ1aBaX AaH-
6JIK)AaIOTCSi 6oJiblulte KoJIe6aHHH B Be- um' :epMn H onpeAeJisieT KOJPH4ecTBo "
MH,KpOo6,beMOB Ha 4)OTOMeTpHpye-
MbIX ytiacTKax, o6JiaAaiouxHx cpeA-
He4t KOHueHTpauHeH. 4eM Bb1IIIe JIe-
)KHT Ma'KCHMy'M 4aCTOTHOH 34pHBO}i
H 4eM McHbuie paOCTOHHHe Me)KAy
ee BeT'SIMH, TCM Mexee pe3Ko BbI-
cHr. I. KpHBble nOtiepHeHH2 Ana
MarHMA-Kaj1bWwfl:
I - 320 rpaA/MHH; 2 - 160 rpaA/MHH; 3 -
106 rpaA/MHH; 4 - .47 rpalt/MHH; 5 - 20 rpaA/MHH.
pa Kelia B CTpyKType cnnaaoB B'HyT-
pHKPHCTaJIJIHtieOKasi HeoAHOpo)q-
HOCTb. 4aCTOTHbie iKp}6Bbie, OTBe'4aio-
IUHe ABONHbIM c-nJlaBaM MarHHA C
KaJIbUHeM ((4HT. 2, a), nOKa3bIBa1oT,
LITO C 'nOHH?KeHHeM TeMnepaTypbI
H3JIONKHHUbI, T. e. C yBeJIHMeHHeM
CKOpOCTH Ox.Ia)KAeHHW' CnJlaBa npH
ero KPHCTaJIJIH3aIHH, yMeHbnlaeTCH
JIHKBauHOHHaR MHKPOHeoA'HOPOA-
HOCTb. IIpH OTJIHBKe c'IIJiaiBa B
JIH',4HHax nO4epHeHHSI, T. e. B KOHueHT- XOJIOAHy1O I(OpMy, H'Meiouuyio TeM-
pauHH KaJibuxsl. nepaTypy or 2Q Ao 200?, KOJIH4e-
Ilp(yBeAsl CTaTHCTH4eOKy1O o6pa6OT- CTBO MHIKpOO6'beMOB CO cpeAHeA
Ky pe3yJibTSTOB. I)OTOMeTpHpoBaHHA, KOHUeHT auxe# KSJIbUHS1 COCTaBJiSIeT
MO)KHO '6bI10 OUeHHTb CTeneHb MH'xpo- 80-900 . II-pH saMeAJleifHOM oxiia]K-
?
0,04 408 412 Ca X143 ca?~ 012, ~4 ca/
cHr. 2. Pacnpejeneaae K8JIb4Ha III H 'H3MeHewwH 'CKOpOCTH OXna0KAeHtta:
a-sa ewer pa3JCH4HH a TeMneparype H3JCOHCHH4bi (ABOBHde CnJBBbW MarHHB-Kanb4xa);
1 - 320 rpaA/Mxx; 2 - 160 rpaA/MHH; 3 - 105 rpaA/MHH: 4 - 47 rpaAIMnH;
6 - 20 rpaA/MnH; 6 - sa ever Hcnonb3oaaHHH pa3nHVHb!x nHTelxbix 4)opM (cnaaBbt
Mg - Mn - Al - Ca): I - 1000 rpaA/MHH; 2 - 500 rpaA/MKH; 3 - 45 rpap/MHH;
4 - 160 rpaA/MHH a - as ever AxaMerpa aeMAHHOa (bopMbt (cn.nanw Mg-Mh-Al-Ca);
I - 120 rpaA/MHH; 2 - 4 rpaA/MHH; 3 - 45 rpaA/MHH; 4 - 22 rpaA/MnH.
HeOAHOpOAHOCTH B CTpyKType BccJie-
AyeMblx CnJIaBOB. AJIH 3TOH ueJlli 3Ha-
4eHHH 3IIJIOT?HOCTH InO'qepxeHHSi inepec4H-
TbIBaJIHCb B Ko2HueHTpauJH;H, H CTpoH-
lIHCb 4aCTOTHble Kp'H?Bble pacnpeAeJie-
HHH. Ha I~Hr. 2 InpeACTa'BJIeHb1 4aCTOT-
Hb1e Kpnabie, COOTBeTC'IIByiOIuHe BceM
TpeM CJIy4aHM } 2MeHeHHR CKOPOCTH
~- _i.Ed1e
AeHHH, KorAa H3JION(HltUa ?HarpeTa.'Ao
600-675?, TOJIb'KO 35-38% MHKpo-
o16'beM?OB cnJIaBa HMeIOT cpeAliee co-
Aep3Ka'HHe KaJIbuHH (AJnn AaHHOFI ce-
pHH CJIJiaBoB 0,06%).
KpHBbie, noKa3aHHble Ha (IHr. 2, 6,
Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
 Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
?L i
a
?
Am cnJiaBa CHCTeMbi MarHH{i-Mapra-
HeiB-aJIK)M'HHHM-KaJIbUHfi, B OCHO'B-
HOM; noATBepwAaIOT 3a'K0H0MepHOCTb
H3MeHeHH5I MHlKpOHeOAHOPOAHOCTH B
3&BHCH?M0CTH OT CKOpOCTH OXJIa}KAeHHH,
yCTaHOBJIeHHYIO AJIH ABOt1HbIX cn.iaBoB.
11OBbinieHHe CKOpOCTH oxJia}KAeHHH
npH OTJIHBKe CnJ1aBa B McAH'IO HJIl
cTaJwHylo BoAoox.na)KAaeMyIO H3JI0)K-
HMUbI 06ycJIOBJIHBaeT 3Ha4HTeJlbHO
McHbIIIyIO MHKpoHeOAHOpoAHOCTb no
CpaaHeHHIO C o1JIHBKOf1 B 3eMJIHHylO
ipOpMy HJIH BarpeTylo gyryHHyIO H3-
JIo)K'HHuy. B nepBOM CJiytiae KOJIH4e-
CTBO M61Kp0ofteMOa co cpe,AHeA KOH-
ueHTpauHet% KaJIbuHH (paaHOt 0,13%
AJIH OT0~1 CepHH OTJIHBOK) COCT8BAHeT
70-88%, a Bo BTOpQM cJiy4ae sTa se-
JIH4HHa CHHHCaeTCH AO 3H&4eH'Hf1 McHee
a) 6) B)
0HT. 3. MHK'popeAHOrpaMMbl CnnaBOa Mg--Mn-AI-Ca, OTJINTUX .B 3 MAAHbIO $opMa
paaw x ce4eHHIi. X28:
a-AHsMeTp 4OpMM II MM; 6--80 MM; a-80 MM..
49
30%. 0AHat00 CJIeAyeT 3aM@THTb, WO
AJIH -MaJIbiX CKOpocTe11 OXAa4KAeHNH
MaKCHMyMM gaCTOTHbi'X XPHBbIX AJia
paCCMBTpHDa9MOA CepHH OTJIHBOK Jte-
HfaT 04eHb 6JlH'3K0 Apyr X Apyry. nPH
OTJfl6Ke 41 8eMJIHHy1o tpOpMy MaKCHMy'M
9ICI1OJ1O$CeH Aawe Qte0KoJibxo 'ebiwe
4eM npH JitTbe a '4y~-yHHyte 4f3JI0HCM' 1'
ny, HaPP&rY1O AO 630?, xorn a CieMJIH-
nob 4 OpMC: OKOpOCTh OXJIa'1KAeHHH 6bi-
J1a WMHMaJ1bIIOA. O4eaHA'Ho 9ACCb 'Ha-
6JiIOJiaercC O`rxJlo0eHHe OT inpHMO% CBN-
aH McNCAy. 'CHOpOCTbIO oXJIa*AeHHH H
OTeiteiw6 MHi poneo HOpOA'HOCTH J1H'-
TODD MaTepHaJta. 9TO OTKJIOHettHe 13b1-
pa)KCHO home 6aMeTHO a 4eC'I'OTHbix
apHBux (4I4P. 2, d), KOTbpbie OTHOCfiT-
CH K '1 rMpCXKOMflOHCHTIIOMy MarHHe-
HOMy onJIaBy, OTJIHTOMy B eeMJ1AHble
4 opMbl pa3HOro cegeHHH.
MaKCHMaJIbHan CTeneHb MHKpOHeOA-
HOpOAHOCTH AOCTHraeTCH'npH HaHMeHb-
weM H 'Ha116OJIbweM AHa'MeTpax oTJIHA-
KH. CpeA'HHe pa3Me'pbi cetieli'Hfi, a c ie-
AOBaTeJIbHO 4i cpe(AHHe CKOpOCTH
oxjlaHCAeHHH, o6yCJioBJIH'BaIOT 66JIb-
wylO BHyTpHKpECTaJIJIHtIecK IO HeOAHO-
pOAHOCTb.
Ko.IHUecTBO 'MHKpoo6'beMOB OnJiaaa,
o6JIaAaI0MH'X cpeAHe# 'KORiieHTpa'uae6
AJIH CTep)K'HH AHaMeTpO.M 11 MM, COOT-
BeTCTByeT 55%. C yBeJIH'4eHHeM AHa-
McTpa OTJI'HBKH Ao 30 H 50 MM 9T8 se-
JIH4HHa CH'H)KaeTCH CoomeTcTaeHHO AO
32-27%, MHO 3aTeM c yaeJIH4eHHeM
AHaMeTpa CJlHTKa Ao 80 MM OHOBa B03-
pacTaeT Ao 41 %, rro cBHAeTeJIbcTByeT
o no,iytieHHH BHOBb 6onee oA'HOpoAHO1k
cTpyKTypbl. Ha 4Hr. 3 npeAcTaB-
JIeHbl MHKpopaANorpaMMbi cnJiaaa
CHHTb1e CO CJIHn9COB -I(HaMeTpoM 11, 68
H 80 MM, npH TOM )Ke yAeJIH4eH'HH, npH
KOTOpOM 41pON3BOANJK)Cb 4)OTOMCTpHpO-
BaHHe. C a03paCTaioeIM AHaMeTpa OT-
JIHBKH OT 11 AO 60 MM auyTpHKpHCTaJI-
JtH4eCKaH 'HeoAaopOAHOCTb 4TaHOaHT00
dbjiee peaxo abrpaHceHH09, Mexct yoc'
-
Hble 11pOCJ10 'KH, B HOTOpbIX COCpeA0TO
4HBaeTcH 9CBJIbuotl,'YTOJ ll alorc 1 4C noa-
paCTaeT pa3Be'rBJICH'HOCm AeHAPHTOB.
lpH AaJIbHe$weM yaeJIH.IeHHH AHa'MCT-
pa OTJIN'BKH Ao 80 MM npOHCXOAHT fie-
pepacnpeAeaetlHe 'KaJIb11HH B CTpyXTy-
pa CnJiaea~t o6ycJIOBJ1eHH06 AC ra?o4Ho
McAJteNH0B HpICT*J1JIHaet1He11 ? H aOa-
MOHtHOCTb10 npOTeka rHH 0-000OH-
HbIX 1npoateCC611 B 061eMe 3e4Ha. 14a
np'HBeAeHHOt Ha c4Hr. 3, b :MHxpopa-
AHorpaMMbl BIf'A'H0,'4T0'KaJIbuH11 COCpe-
Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
 ?
S
Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
AOTO4eH B ?nOrpaHH4HbIX Me)K3epeHHbIX
30Hax, a BHyTPH 3epHa CTpyKTypa CTa-
HOBHTCR 6onee OaHOpOAHOf1.
TaKHM o6Pa3oM, BbInoJIHeHHOe HaMH
HCCneJOBaHIie noKa3bIBaeT, MTO 6ozee
oAHOpo,lxoe pac[ipeJieJleHHe KaJIbUHH B
MHKpocTpyKType MaPHHeBbIX cnnaBOB
MO)KHO ?1IOJIytIHTb 'HJIH B cnyqae IBbICO-
KHX CKOpOCTeEi oxJIa)KAeHHR HJIH, Ha-
060pOT, npH AOCTaTO' HO meAJIeHH01i
KpHCTaJIJIH3auHH.
IlpoMexcyTOaxoe 3Hagexxe cxopocJrH
oxJlaN{AeHH1 o6ycJIoBJu BaeT 6oJIbLUy10
B'HyTpHKpxcTaJIJI'HgeCKy1O nneOAHOpoA-
44
0 80 160 240 ?C MUM 0
CKOpOCmb O.aAOMrOeMUp
a)
11 V
C
ra
1.3
40 80 120 160 CHUM
200 400 600 800 ?CMUM 0
CI(OpoCmb OxAdweOKUP
6)
CKOpOCmb OAI10.YrOesuP
0)
(DHr. 4. 3aBHCHMOCTb MHXpoHeoA'HOpo.HOCTH OT CKOpOCTH OXAa)KAeHHB:
a - npH pasnHgHbtx TeMneparypax Hsdo?KHH?d (cnnaabt Mg-Ca); 6- npH pasaHVHMX cnoco6aX
eH (cnnaabl Mg - Mn - AI - Ca); e - npH pasnn4Hdx AHaMerpax aeMJlSHbIX
(cnaaabt Mg - Mn - Al - Ca).
HOCTb B pacnpegeJleHH1H KaJIbuHR. Anf
o6o6uAeHHR nojlygeHHblx A8HHbIX pe-
3YJIbTaTbl CTaTHCTH4eC1K0g o6pa6oTKH
KpHB&X pac'npeAeneHHR KaJIbuHR 6b1nH
npeACTaBJleHbl B BHAe AByx KO4(pH-
UHeHTOB K H C. Ko344 HuHeHT K Xa-
paKTepH3yeT CTeneHb MHKpoHeOAHO-
POAHOCT.H CTpyKTypbl cnnaBa H onpeAe-
J1HeTCH no (popMyne
K= 100 - n
100
rAe n coOTBeTCfByeT MaKCH'MyMy iia-
c1FOTHOH K HBOi1 H OTBegaeT .xoJIH4eCTBy
MHKpoo6,beMOB, %MeioutHX Cpe1 Hlolo
xoaueHTpauHlo, a 4HCJIO 100 (1peAcTaB-
JIHeT CO6Ol ?KoJlH'teCTBo MH'Kpoo6beMOB,
B ?KOTOpbIX l13MepHJlocb coAepxca'HHe
KaJIbuHR. KO344 HUHeHT C HBJ1ReTCR
oTHOIueHHeM MaKCHManbHOR KO'HueHT-
pauHH KanbuHR CmaX K MHHHMaabHOIA
ero KOHueHTpauHH C min B OTAQJ1bHbIX
MlfKpOO67>eMaX Ha HccneAyeMOM y4aCT-
Ke CTpyKTypbl:
C = CmaX
Cmin
B Tab i. 1 npIIBe.lenbl 3Ha'icHHR
Ko3(p()HL I1eHTOB K H C An1I BCeX H3y-
'1eHHbIX HaMil CnJIaBOB -npH pa3JIHgIHbIX
CKOpOCTRX ?ox.na)KAeHHH, KOTOpble ocy-
I. eCTBJI51JIHCb B yC.IOBHRX 11aHIioro HC-
cJIeJ oBaHH1I. CKOpoCTb oxnaN(AeHHR
BbtgiicJIRJIacb 'Ka'K 4aCTHOe OT JAeJIeHHR
pa3HOCTH TeMnepaTyp HaHana m xoHua
3arBepAeBaHHH cnnaBa Ha BpeMR
oxna KgeHHR. KpHBble, ?Bbipa)Ka101UHC
CB93b McN;aTenbHO Ha BeJIHTIHHe 3((eI{Ta yIIpOTlHeHHFI'IIpH TepMHLIeCRoH
O6pa6oTKe, TITO IIPHBOAHT K CHHHfeHHIO IIp04HOCTHbIX XapaKTepHCTHK 3THX'
cIInaBOB, Hapf'Ay c ,yxyAiueHHeM HX TexHOnorl3TiHOCTH. OAHaKO B yCnOBHHX
pa60Tbl IIPH HOBSImeHHbIX TeMIIepaTypax )Keiie3o OKa3MBaeT IIOno)KHTenbHOe
BJIHHHHe, CIIOCO6CTByH TOpMO HOII1'IO AH((Jy3HOHHbIX IIpOgeCCOB IIOn3yHeCTH
B anIOMHHHH Hero cn ianax. B pa6oTe A. A. BOTiBapa H AP. [2] 3T0 HOnOMH-
TeJIuHOe AeuCTBHe 7iceJie3a CBfl3bIBaeTCfi C. IIOBbIIIIOHHeM TemnepaTypbI pexpH-
CTanJIH3aI[IIH a3IIOMHHIIFI 6nar0Aapfl BbIAeJIeH111O 11HTepMeTanurHTIecRoro CO-
eAIIHOHHfI FeA13 Ha noBepxIIOCTli pa3ACJia Me?KAy 3OPHaMII H BHYTPH aepeH.
Ha pa3BHTIte IIJIII TOpMOH1O111IO gif())(Dy311OHIIbIx MexaHII3MOB IInacTHTIHOCTH,
HapHAy C OCHOBHbIMII JIer1[pyIOH(1IM1I IOM1I013e11Ta\ill, BBOAIIMLIMH B CIInaB
B KaxieCTBe yIIPOTIHIITeJIeli, BCCLMa 3aMCTI1oe BJlilfilIHe MoryT OKa3LIBaTb AeCH-
Tbie, COTELO HJIH Aame Tblc)ITlllbie AOJII[ 11pOI[ClITa IIp1IMeceH, coAepmauSHxcn B
HCXOAHJIX MaTeplIaJiax. Hogo6hIoc AOlieTBI[e 11e6Ommoro KOJIHgeCTBa IIpIIMe-
ceH, OTieBnIAHO, CBf13aIIO C Xal)UETOPOM 1[x paCHpeAOJIeHIifi B OCHOBe, T. e.
C TOM BnmgHHeM, IiOTOPOC 01111 OI:a3bIBalOT Ita CTpYKTy]?HOO COCTOHHIIe OCHOBBI
CIIJIaBOB, Ha CTOIICIIb rcTCpOrCI1113aL(I[ll, a TaHHte Ha xapaKTep B3aIIM0AeIICT-
BHH OTAenbHLIX COCTaBnf11OU 11x CIInaBOB (3).
B JIHThIX U Ae(J)OpM11pyeMbIx CIijIalax lla aJIIOMiuHneBOIi OCHOBe, upeAHa-
3HaTieHHbIX Ani pa60TLT Iipit HOBmIB.I0I11IbIx TCMIIepaTypax, AOIIYCKaIOT IIpH-
CYTCTBHe )Keiie3a B KOJIIITIeCTBax, npeBbI naioiwxx 0.8-1 %. IIpH 3TOM, XOT$1 H
C03AaIOTCfi onpeAeiiOlIHble 3aTPYAl1CII1Ifi B OTHOHIeHHII HX o6pa6OTKH, HO 3aTO
o6ecneTifBaeTCH 661niuafi IIaAei{IIOCTb MaTeplIana B 3KCIIHyaTarkHH. I-IoJio-
)KHTenbHag ponb )KeJC3a B O6ecneTIOHHH HSapOIIPOTIHOCTH aJIIOMHHHeBLIX cujia-
BOB AOJI)KHa paecMaTpHBaTbCSI, C OAHOII CTOpOHbi, B CBH3H C ero pacnpeAene-
HHeM B OCHOBO, T. e. B QJIIOMHHIIH 11, c Apyro3i CTOPOHbI, B CBH3II C TCMII H3Me-
HOHHHMH, KOTOPMIe BHOCIIT )Kene3O B ()a3OBbiff COCTaB CIInaBOB.
HHme IIPHBOAHTCH pe3ynbTaTmI IICCneAOBaHIIfI, Harnf1AHO IIOHa3bIBaIomae
pacnpeAeneHHexceme3a B TIHCTOMainoMHHIIH, a TaKHienepepacupeAeneHHeerouOA
? BJIHHHHeM HarpeBa.IlpHMeHeiHe MOTOAa KOJIHTIeCTBeHHOH aBTOpajiorpa(HH (,4,o]
IIO3BOJIHno OIIeHIITh H3MeHeHHe MHKpoHeOAHOpOAHOCTH B CTpyKType
aJIIOM13HHH no Mepe YBeJIHqeHHH COAepH{aHHH B HeM )KeJIe3a.
B qHCTe13HIHi3 aJIIOMHHHl3 MapHH AB000 (99.985% Al) BBOAHJICH paAIIO-
H30TOH mene3a Fe5B C TaKHM paCTIeTOM, TITO6LI o6edletulTb aKTHBHOCTb o6pa3-
ILOB 6 mCu Ha 1 x2 cu Tana. CJIHTH11 aJITOMIIHHII C pa3JIHLIHbIM coAepHcanII[eM
meJIe3a OTJIHBaJIHCb B 3eMJi5IHyIO (lopMV pnaMCTpOM 30 .MM H BTICOTOLI 60 m n.
Approved For Release 2008/07/31: CIA-RDP80T00246AO02700010001-0
 Approved For Release 2008/07/31: CIA-RDP80T00246A002700010001-0
IIay'ei(i:e pa fnpea'.1eI ( 7Ife.1e3a a 0.1110.1111111.1111
,JIfI Han6oaee IIOJIHOro paCTBOpeHHH iKeJIe3a B amOMHI11In 0110 3anpeccoBbI-
BaJIocb B a:IIOMIIHneBbie CTaKaIIgIIIKII, KOTOpLIe BBOAIHJIIICb B IIeperpeT1 L. AO
900' aJIOMIIHIIn. 1'ICTHHHoe eo epwaHIie ;KeJIe3a B uOJIy'ICIIHbIX 0TJIHBHaX
?
Bbjq!IC:If1:10Cb 113 COOTHOIIICHnfI
C=aC' (1)
r;ie x - K03IH(IIIIneHT yCBOHeMOCTn, C' - cogepH;aHHe 9HeJIe3a B CJIIITKe
110 iuIIXTe (B %)?
Iioa44i J I1eHT yCBOFIeMOCTI1 oupeLe IfIJICH paA1ToMeTp1LIecHII, Kai OTHO-
BICHIre 06uieil aHTIIBHOCTH IIOJIy'IeHHOrO CIIJIaBa K alTIIBHOCTII 3JIeMeflTa,
BBeueHnoro B cUJIaB pagiioaKTnBIIHHM upehapaTO\i.
PaegeT IIpOH3BOAHJICfi n0 I OpMy3Ie
aQ100% (2)
rAe it - yAeJIbHaH aRTIIBHOCTb CHJIaBa [uMn/.ALuK. e], a'- yAeJibHAfi aKTIIB-
HOCTb paAHOH3OTOna [u,un/Mu1], Q - Bee cnJiasa [2], q - Bee paAHOH3oTOna,
BBeAeHH0r0 B CIIJIaB [2].
McTOAHKa H3MepeHHfi y) eTIbHOII aHTHBHOCTH COCTOflJIa B CJIeAyIOBieM.
CTpy?KHa CIIJIaBa, 3apaHee B3BerneHHafl (C TOLIHOCTbIO Ao 0.0002 2), paCTBOpfI-
Jiacb B OnpeAeiieHHOM 06'beMe 50 %-Horo pacTBopa COJIfIHOH KHCJIOThI. 3aTeM
paCTBOp HeuTpa1In30BaIICq aMMHaHOM AJ1H yCTpaHeHHfi BpeAHoro AeuCTBIIR
IIapOB HHCJIOThI Ha pa6oTy. ct1eTHHKa. I4aMepeHHe aHTHBHOCTH npOH3BOAHJIOCb
Ha yCTaHOBKe (b') C TOpIIeBLIM CgeTgHKOM. )Iafi BTOH IIeJIH H3 IIOJIytieHHOrO pac-
TBopa IIOCpeACTBOM 61opeTKH OT6HpahICfI CTporo OIIpeAe1IeHHIII3 06'beM (1.5 C.At3)
B CTeKJIHHHyIO HIOBCTy, KOTopafi yCTaHaBJIHBaiiaCb IIOA OHOHIHOM CAeT-
,gKKa. Bee paAHOaKTHBHOr0 npenapaTa H o6'beM pacTBopa IIOA6HpaJIIICb Ta-
KHM 06pa30M, iIT06bI CKOpOCTb CLIeTa BO BCOX CJIyiIafJX He npeBbiHlaiia
3000 uMn/.htuu. YpoBelrb (,oHa npI1 H3MepeHHfix KohIe6aJIcq B npeAe1IaX
40-45 It.Mn/.tuft.
Onpe)jeileHne yAeJIbH0I1 allTIIBHOCTH cfJIaBOB H caMorO npenapaTa npo113-
BOAHJI0Cb 110 d 0pMyJIaM
NV , _ N'V'
a
kk1P'
)ck1P
(3)
rAe. N - CKOpOCTb CueTa pacTBopa cnJlaBa [u.htn/.htun], N'- CKOpOCTb CneTa
pacTBopa npenapaTa [uMn/Mutt], P - HanecHa pacTBopeHHoro CIIJiaBa [2],
P - HaBecxa pacTBopeHHoro paAHOanTHBHoro npenapaTa [2], V - o6'beM
pacTBopa, B HOTOpOM paCTBOpeH CIIJIaB
[CAM, V' - 06'beM pacTBopa, B KOTO_ Ta6Auifa 1
p0M paCTBOpeH npenapaT [c.nt3], k - CoAep,iaHHe
Ro3I (HB;HeHT, ytIHThIBaIOH.IIIY1 pacuaA CoAep,1 aline Koa(D(DmnHeHT Hsenesa no AaH-
Hfene3a no yCBOHeMOCTN HuM paAHOMeT-
MOTOna, k1 - K030HAIIenT, yqHTbIBa- maxTe, % a M) pHV. ananH3a,
10UL11 0006eHHOCTII Ir3MCpeHIIf aKTIIB-%
HOCTH.
Tali KaH npH co6JIIOAOHHI1 IIOCTO- 0.01 85 0.0085
5
IIHHbIX CJIOBHi3 OHLITa KO3 HIiIIOHT k 0.20 96.8 0.1945
Y ~~ I 0.2 96.8 0.194
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