MODIFICATION OF PHYSICO-CHEMICAL PROPERTIES OF CARBON PRODUCTS IN THE PROCESS OF ELECTRICAL GRAPHITIZATION

• Document Type: CREST
• Collection: General CIA Records
• Document Number (FOIA) /ESDN (CREST): CIA-RDP82-00039R000100100056-9
• Release Decision: RIPPUB
• Original Classification: C
• Document Page Count: 38
• Document Creation Date: January 4, 2017
• Sequence Number: 56
• Publication Date: January 27, 1951
• Content Type: REPORT

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Titl�t r~iODIF'ZC~IThDN D~ PNY9IC0-C~~~CAL PROP~TI ~'S OF CARBON PR DU
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IN TFi~ PROC�~S 0~' ~CTRZCJIL CIt~IPF~xI~ITION by B, V. 1?~~ter
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9otiuro0 = Ru~~iari monthly poriodio~l Tsv~l~ Metal ~ No 12i Mo~oow
Deo 1~3? or 1938. ,
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0~ PKYSICO-CNII~IC PROPgRTtg9 ~
u Mo~~~scATToN -
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n punW pA~DUCTB IN Tidy PROCESS of ELFOTRICAL
r is eF
k ~ GA!?PHITIZATION
by S~ Y. l~inte ~
~Sintsvetmetmoloto ~i~oooow Institute
~i n-Ferrous Metals end sold)
o~ No
arbonacoous material is transformed into
Ae shown b9 Depre (1) f an~? o
e osed to a high temperature for a long time. Howover~
graphite on being xP
~ 2 a high temperature alone is not euftioient
ae has been shown by O~
rboa black (soot): the pre�enae o~ certain
~ for the graphitization of oa ;
a~ elemental eilioon ie oleo neoeesary~
,a~uree such ae Moron, aluminum,
hree different types of ~i
M. ~arthelot (3) Pointed out that there are t
rs hits the graphite of cast iron, and electrioel
graphite: natural g P ,
Volo din showed that these graphitee diner
graphite. LeChatelier and g
ae of a di~'ferent amount of admixtures.
from sash other by the presen
the oxidation of artificial graphite pro-
According to Moisean C5),
ro artional to the temperature to which
duced in are electric furnace ie p P
he sire of graphite flakes obtained by sep-
the gra~ahite had been heated T
~F
ns diminishes with the increased melting temp-
oration from metaled solutio
ices roduced in an electric furnace do not
erature of the metals ~ Qraph P
furs has been merely raised in processing them] while
t swell if the tempera
tem erature swell easily.
r those obtained from molten metal at a high P
states that when cas'bon contains a considerable quantity
Aoheeon (6 )
~ been modified by adding to it 2.5~ of m�ta1. '
of inorganic matter, or hoe
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~ ra . bite fie considerably inareaded~ and fife quality fie
w the field o B A
oxides ~ y -
e an inoreaeed greasineae~ lower hordneei~
improved the graphite exhibit
a ~ raoite
and etron er lueter~ however, Areem (1~y baewehown that ooke and anth
g
ized more readily when their ash oantent hoe been roduoed by
are graphit
abemioal meaner
and De a (8) demonstrated that firs the oouree of the heatin6
Arndt by
ban ra hits orystale are inoreaeed in size by a footer of approximately
of oar ~ 6 p
d that the growth of graphite oryetals depends on the properties o~f
1000 an
aria/ ~ The increase of eleotrioal Qonduotivity begins
the a tartir~g mat
with the evolution of gas, and the point of the greatest increase
together
ncidos with the ma~d~mum evolution of gas. Petroleum and
in oonductivity ooi
e are Basil graphitized; gas coke with greater difficulty;
foundxy aok Y ,
Basil ra hitized and awelle oonsiderably during the process
retort carbon fie y g p
ra hitization~ The anthracite whiol~ is geologioally oldeet~ graphitizes
of g p
as been likened by Rishkevioh ~ 9) and
best. The prooese of graphitization b
Arndt to that of the recrystallization of metals.
h wn in the work by Debye and Scherrer (8), Kohlechuetter (10),
Asso
4
and others amorphous carbon and graphite do not essentially differ from
h others the only difference consists in the diff~brent size of crystals
sac
entiaal as far as their lattice fie concerned. The so-called
which are id
o houe carbon fie composed of graphite orystals which are so fine that
am rp
rem ordin graphite by using any mechanical method
they cannot be obtained f
~ of treatment.
~Iowever the finely orystallized graph~.tee (amorphous carbons) differ
he coarse/ crystallized modifications as far as chemical behavior is
f rem t Y
~r Ruff su Bated tZlat the name amorphous carbons f
concerned For that reasons 66
be retained for the f irgt (ll)
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8a?~foux and Riley X12) ostablished that ~Y organio eubetanoee whioh
. are u,ouall ro~forrad to as amorphous are aotually oongloc~oratoo having a
y
aryatalline lattiao that is similar to tho epeoe lattioe or graphite.
1
3
Those eubetanoee oontain firmly sound hydrogen botwoen the oarbon l~exagone �
` The hydrooarbone in question exhibit a aonoidereblo stability and begin to
a
deoompooe only at 600�700�~ An additional proof for the exietenoe of a
hydrooarbon having this degree of stability ie in the authors ~ opinion the
faot that anthraoite rather than graphite ie the end produot of the prooeee
of ooal formation
The brief historical aooount given above illustrates the mein trends in
the field whioh is of interest to ue~ Th� question of tt~e etfeot of inorganio
admixt~~res on the process of graphitization oan by no means be regarded as
soived~ This fact induced our present investigation.
1. Physico�Chemioal Properties of Carbon Produate~ Oraphitieed at the '
3
Temperatures 1800, 2000, 2200, and 2500�.
We submitted to in~~��tigation products prepared according to 8 dif�
{
ferent presoriptions~ The crude material for the first product consisted
t
of petroleum coke, that for the second of mixtures of petroleum coke with
anthraoite~~ Then cams two grades of anthracites foundry coke, and a mixture
of foundry ooke with petroleum coke The mixtures were prepared on the
principle of gradually raising the ash content of the mixture
All materials had the same partials ei~e oomposition and the eiee of
the particles was in all oases lower than O~15 mm� The physioa�ohemieal
properties of these materials are listed in Table 1. The temperature of the
i
preliminary heating was the same in all cases and amounted to 1300� � Asa
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~ binder 25~ of soft pitch with a softening temperatiure olf 1~1�!~7' were used.
Mixtures were made up using equal quantities of the ingredients in the dry
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e oombinod with 50~ o~ petroleum Doke, and
part, i ~ e ~ 50~ oP anthracite wer
in redients had been mixed thorou~h~ with eaoh
ao ~orth~ Auer the solid 6
r
itoh the mixture was pressed ~ an enolosed
other and with the molts p ,
to 60,.65, A momentary rather than oustainod
mold w~~ioh had been preheated
~ a lied ~ For eaoh temperature atudiad j ~ sampleo
presage of 100 kg/am was pp
0 0 mm were prepared Auer being pressed the
having the dimensions 40~ ~
ordin Ritthammor ring furnaoeo and submitted
samples were heat�treated in ~'y
to examination, a.
4
heat treated matorial was carried out in speai
Qraphitieation of the
into the production furnace and removed
carbon equipment which was inserted
mined tern �rat�re had been reached The
from it as soon ae the predeter P
f
eared through a carbon tube by means o� a platinum- f
temper~?ture was mea
tioal rome't~r~ ,N,thcugh we attempted
platinumi rhodiwn thermooouple cr ~ op ~
satin at a definite tome�rature and the oondi~bions ~:'i
to keep the period of h g
lace constant, it was nevertheless necessary for
under whioh cooling took p ;
car out heating at higher temperaturesfor alonger ~
teohnical reasons to ry
time ~ j
able 2 a considerable reduction of meohanioal
As can be seen from T ~ i
ion below the temperature of 1604' This
strength occurs in graphitizat ~ ,
s reatest in the samples made from anthracite ha ng
reduction o� strength i g ~
r this in the order of mechanical strength redact
slow ash content Afte ~
oleu~n coke mixtures, anthracite with a high ~
Lion, follow anthracite petr
~ sum Doke mixtures and
eh content foundry coke, foundry Doke pei~rol
a ~
The factor by which the mechanical strength is
f inal~Y petroleum Doke
case of anthracite having a low ash content
reduced comprises 3.0 in the
in the case of petroleum Doke ~ The absolute figures ,
.r and amounts to L�~
en th differ to a considerable extent It is note-
measuring mechanical str g
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worthy that oven ~rhen graphitization f e waz'r ied out bel~r l~~' ~ Chore ie a
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1'airlsr votive reorystallieation~ as oan be seen froaa the roeittivity o~
ear~ples and ~owdera ~ Graphitization proceedo m�at aotive~y in materi~!
which have the lowaet natural aeh oontent. When graphitization is oarried
out up to the temperature o#' 2000' (o~~ Table 3)~ there ie further reduotion
t
of meohanical strength in all samples with the exoeption oP that mode from
foundry aoke~ It is true that this reduotion is not ae great ae in the
former series of experimenta~ The atxangest reduotion ie observed in the
case of anthraoite ha~ring a high aeh oontent (an ef~eot whioh is 1�I~ times
e ter than that in the graphitization at 1800�) ~ while the strength of
gr a
produats made from foundry ooke is even increased by a faotor of 1.1.
The meahanical strength of samples ~aade from petroleum ooke remains
unohan ed. There is further reduction of the speoifio eleotrioal resistanoe
6
and of the total ash oontent In graphitization up to the temperature of
2200� an interesting phenomenon is observed: the meahanical strength off'
roducts increases (of. Table as distinguished from all other samples
p
the one made from foundry coke shows a alight reduction of strength here
This m be due to the foot that in the case of foundry ooke the ohange of
curvature in the ourve expressing meahanioal strength begins somewhat earlier
In graphitization up to 2200� intensive recrystallization takes plaoe
in products prepared from foundry coke, anthracites, and mixtures� Further-
more, there is additional reduction of the vol~~me weight and of the ash
oontent, as can be seen from Table 4~
In the ra hitization temperature range 2200-2500� (af~ Tables 4 and
g P
there is a second abrupt drop of the mechanical strength occurring after the
i
first reduotion which takes place below 1800�~ The Volume weight and the
aeh content of the material drop sharply Its specific electrioal resistanoe ~ y
r.
is also reduced, as can be seen espeoially olearly from the speaifia elea~
I.;'.
ri al resistance of owders~ ~
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tfn
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purin the whole grapt~~titiation period outing wig the temperature
6
o#' nbur~ng" (preliminary heat treatment,] whlah was 100' and eliding Kith
200', the mechanical strength of the product prepared from petroleum ooke
dropped by a factor of 1.7, that of the product ~roro mixtures of anthracite
and petroleum ooke on the average by t factor of 3�7 ~ that of the product
from mixtures of foundry ooke and petroleum ooke by a factor of 4.8, in the
product resulting From anthracite with a high ash content by a factor of ~
.6 and in the redact from foundry ooke by a f sate r of ~ ~ 8 ~ of, figure 1 y
7, p
i
Changes of the specific electrical resistance in the process of graphiti-
i
i
nation can be beet determined on powders because the Batt obtained in this
manner are the moat reliable The resistance of samples usually depends on
3
a number of fortuitous circw~atances such as the presence of craoks~ the ~ ,
~ the surface etc. while in powders interference due
degree of burning o : :
to these causes naturally dose not arise.
xt is evident from what has been said above that at~~800� the speaifio
electrical resistance drops sharply. F1~rth~r on, at 20C~0�, it increases
to some extent, but not on the samples made from petroleum coke Thie ie
probably due to the formation of crystalline metal carbides as distinguished
i
from amorphous metal carbides ~ The latter m~ form even at temperatures
lower than 1100�~ When the temperature is raisad to 2200�, the resistance
of the material begins to drop again and continues to drop anti]. 2500�
t increase Burin the whole
The specific weight of the material does no g
process of graphitization. After the material has been heated to a certain
temperatures the specific weight has a tendency to drop Ad can be seen
from Tables 2, 3, and 5y the highest specific weight is shown by samples
which have been graphitized at 2200� ~ The ash content drops to an insigni-
ficant extent up to 2000�? The reduction of the ash content becomes strongly
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ronounood at 72v0~ and higher temper`t~~ros (of ~ figure ~ ~ ~ ~f a oomparison
A
of the eiao-ohemiaal oharaoteristioa is oarriod out f one may arrive at
the folla~ing oonolusione �
P.
Qoifio olootrioal r�eietanoe of the powdered
A pertain increase in tho ep
dteriale taken plane at 2000' when apparently intensive diseooiation and
m
et oocurred� The latter pan be ee,n From
sublimation of oarbidea have not y
f the material ~ This indicates that there is a oonneotion
the ash oontent o
e eatrioal resistance and the quantity of ash which
between the speoifio 1
is present in the material
f meohanioel strength ~ the range 2000-2200' is aooom-
The increase o
anted b an increase of the apecifio weight and followed by a reduction o
P y
uent heatin � This leads to the aonelusio~a that the
the latter on subeeq 6
hanical strength is incr�ased due to the formation in the material of a
men
i
ids lattice. Then the mechanical strength of the product depends only
Garb
e siren th of the carbide lattice independantly of the absolute quantity
on th g
of carbide contain�d in the product The carbide forming this lattice rep-
resents a special modification of the ordinary carbide
Thus at a definite temperature in the neighborhood of 2200� in the gas
~ able va or assures carbides gay fog which contribute
phase and at apprec. p
f the mechanical strength and of the specific weight of the
to an increase o
jS
material.
s.
ed Substances on the ~'hysica-Chemical Properties of
2 � Effect of Add 4
roducts Graphitized at the Temperatures 1800�, 2200�, and 2500�~
P
C
r
e have shown above that the ash contained in the material has aeon-
W
ble influence on the physical properties of carbon products, particularly
eiders
he 2040-2200� temperature range of graphitization, ~'or that r�ason it
in t
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oh in not what manner indl~d~ o~ddea which
is of imPortanoe ~ eetabli ~
f oarbonaoeoua materials afFoot the moat important prop
oompooo the soh o
s of tho roduota~ In ordor to investigate the influence of ash oo~?-
ertio p
me it was neoeaeary to ael~t a oarbonaoeoue material having a low
pone ~
ntent and showing only a small reduotion of meahanioal strength in
ash ao
tion� Thio made it pQOeible to eliminate extraneous faotore auoh
graphitize
aettlin ewelling~ formation of here, eto � ~ whioh might
ae the effeote of g,
the matter of drawing a oorreot oonclueion from the experimental
oomplicate
table material from this point of view seemed to be
reeulte~ The moat eui .
Tn order to permit a eomparieon of the now method wit~? the
petroleum coke
es of the reeul ding product are oonnerrled f the
old ~ ae far ae the prrperti
ration and relimin8ry' heat treatment of the se~mples was
proceeB of preps P
t unchan ed with the sole exoaptivn #?hat l0~ of ferric oxides magnesium
lef ~ ,
r silicon oxide were added to the starting material
oxide, caloium oxides o
rom Table 6 that with the exception of products prepared
Tt can be seen f
oxide all samples showed an increase in elQCtrical
with the addition of ferric
stance after heating Upon graphitization at 1900� there wa$ no alter-
resi
rioal roperties, except that the specific resieta~~ee of products
anon of phy P
to which ferric oxide had been added dropped sharply
s can be seen from Tabl� 7, heating at a temperature whioY~ was higher
A
~ � re�ulted in a considerable deeraase of the mechanical strength of
by 100
acts ~ As compared with products processed at 1800�, the results on
the prod
1'~ om a mixture of petro~.eum cake and ferric oxide show�d a
samples made fr
on samples with oalcium
i reduction of mechanical strength by a factor of 4�7f
factor of 3.9 w~.th magnesium oxide by a factor of 3�~, and with
oxide by a ~
~
n d~.oxide b a factor of 3.7 ~ ~
silica Y
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4 f
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orvao ed 2 ~ 6 timoo on the {
cal oonduativity of all oampleo in ~
The elootxi f a ~~'~''a"~~
and the aoh distilled os ~
ed c~rta~derably
a e. Tha velum! waS~~~t drape
aver g
a~;moot oompletely~ i~ont
with thooe obtain�d earlier ~exP�r
If th�so reoults are aompaxed
ro ort~os in thi� inotanoo differ
l one notioeo thst the physics/ p p
No. ) ~
from those observed �a~'lier~
aaneidorably
oam lee were graphitized in the furnaoe ,I
Notowithstanding the facts the p
the roducto listed in Tt~bleo ?
usl in a limited epees,, and that p I
simultanoo y
ietributed in different please of
res votively were intentionally d
and p sia~+-
em stature for all samplee~ th� phY
s s ace oo as to achieve the same t p
thi p
ve roduete wer� entirely different.
hemiosl rroperties of the r~speoti p
c
I
of samples made from petrol�um ooke
Thus the mechanioal strength
00' was 228 kg/cm2, while the average
�hout ~ addition and heated et 22
wit
aoke with the addition of 10~ oxide
ran tb of samples made from petroleum
st g
s to only 80 kg/cm2, i~ e ~ is lower ~a.
tad at thQ sam� temperature amount
and. heo
a,cteristic that in the second instance
b Erector of 2 ~ 8 ~ It is char t
Y
volume weights Zf the volume weigh
there is a greater reduction of the
ed at 2200� and leaking metal oxide
of samples from petroleum coke prdpar
e ared from the came material and
is 1+4 the volume Weight of samples pr p
e addition of metal oxides is on t e
' r the same conditions but with th
ands
average only 1 � ~6
of the samples listed in Table 7
The specific electrical resistance
lea listed in Table W'hen the
is much higher thin 'that of the camp
0 2 00�) ~ there were further lows 6
as raised still higher (t 5
temperature w
~,sl, reduction of the ash content,
f the mechanical strength of th� mate
o the almost
cal conductivit~'~ Notewithstandir?g
crease of the e1e atri
and in
erial cf � Table 6) ~ the eleatria~. con-
I ~ ~ bsence of ash in tt~e mat ~
complete a
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Declassified in Part -Sanitized Copy Approved for Release 2012J05/25 :CIA-RDP82-000398000100100056-9

 Declassified in Part -Sanitized Copy Approved for Release 2012/05/25 :CIA-RDP82-000398000100100056-9
A
duotivit off' the eamploa to which oxides had been added done not in a
Y ,d
Binge case reach the comparatively high value obtained in the ease of pure ~
e meohanical etren th is on the average times lowor~
petroleum aoke~ Th ~
t Dan be seen from the above that with temperatures highor than 1800'
I
t~~e mechanica3 strength of products from pure petroleum Doke ie higher thou
that of products obtained after admixing oxide to the same crude materiel
The same situation obtains with r@gard to the electrical aonductivity~
In order to determine the effeot of the quantity of oxide whioh had =r~-:';
beon added to the crude matQrial on the meohanical etr�neth of tho graphitized
. roduete we have carried out the following investigations To potrol�ura
p ,
coke w~iich had a slightly higher ash cantent Q0~80~) than b�for�, metal
oxides were added alternately in sufficient quantity to brine the conoen-
trationa up to l~ 2, 5, and l0~ respectively
i
9
The technological process of preparing the samples remained the same
as before. The temperature of graphitization was 2500�~ It turned out
that the physical properties of the product made from petroleum Doke changed
1
oongiderably even if only 5~ of oxide were added
The ehat~pest reduction of mechanical strength (by a factor of l.8)
occurs upon addition of ferric oxide The reduction is somewhat lase }
pronounced in the case of magnesium oxide (by a Factor of 1~3), and is still
f
b a factor of l.2 ~ Taking the average reduc-
Less with aluminum oxide ~ y ) I
ion of mechanical strengt~i resulting from the addition of of these
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metal oxides, we get a red~tiction by a factor of 2 ~ 2, and with 10~ of metal
oxide added a factor of ~,~6~ On the other hand, the mechanical strength !
of the product from pure petroleum coke is reduced by a factor of only 1.1
upon graphitization at 2500�~
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of a~hraczte la�
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Declassified in Part -Sanitized Copy Approved for Release 2012J05/25 :CIA-RDP82-000398000100100056-9