ELFIN I FINAL REPORT

• Document Type: CREST
• Collection: General CIA Records
• Document Number (FOIA) /ESDN (CREST): CIA-RDP78-05288A000100020002-8
• Release Decision: RIPPUB
• Original Classification: C
• Document Page Count: 109
• Document Creation Date: December 23, 2016
• Document Release Date: August 14, 2013
• Sequence Number: 2
• Publication Date: July 25, 1962
• Content Type: REPORT

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CONFIDENTIAL
25 July 1962
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Dear Sir:
Enclosed are six (6) copies of the Final Report for the
Elfin I Project. This completes the work on the contract and it
would be appreciated if you would notify the contracting officer
of this completion.
Enclosures: C25-7 (6 copies
-,DOCtiME'N'T
-VC C..
Ui
CLAS
"TO: .
?
? ..AUTH:
? q51141
Cc7,7-1C,9
Very truly yours,
Project Manager
.0%
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Co?,./V) 4 ?
ELFIN I
FINAL REPORT
C25 -7
July 25, 1962
ili)CUW.Egr NO,.
NO CHANc.2.E IN
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CLASS. Ci-iANC:E.D 10:
tsiD(T _
1,,TE : REVII-fi?JE12: 73 1.f-7.--1
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TABLE OF CONTENTS
Page
1 Introduction
1. 1
2 Experimental Procedures
21
2.1 Electrode Preparation and Testing
211
2.2 Cell Construction and Cleaning
2.6
2.3 Electrolytes and Materials
2. 9
2.4 Circuitry and Data Taking
2.10
Experimental Results
3.1
3.1 Discussion of Significant Experiments
3.1
3.2 Resistance Measurements of E-cells
3.47
3.3 Discussion of Results
3.58
4 Conclusions and Future Work
4.1
Appendix: Sources of Back EMF of E-cells
A. 1
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I. INTRODUCTION
The purpose of the present study has been to develop electro-
plating cell of sufficient sensitivity to integrate extremely small
electrical signals. The quantity of charge specified as the sensitivity
level was one-tenth micro coulomb. This charge is to be integrated
by passing a small current through the cell in one direction and read-
out by passing a known current through the cell in the reverse direction,
noting when the potential across the cell rises as the result of removal
of all the material plated onto one of the electrodes by the initial current.
The cell is to be used as an integrator of currents from such
sources as antenna-diode combinations, transducers, and recording
instruments. Applications to timers, radiation monitors, and com-
puters have been investigated on other projects.
This report summarizes the final four months of a seven month
study of electroplating cell development. A previous report was issued
at the end of the third month.
The results of the study have exceeded the initial goals for cell
sensitivity. Electroplating cells can be produced which will integrate
quantities of charge as small as a millimicro coulomb, two orders of
magnitude smaller than the original goal. This quantity of charge
corresponds to one micro-microgram of silver plated onto an electrode.
The sensitivity of the technique can be increased even further. Lacit
of available time is responsible for the present limit.
The techniques which have contributed most to the improvement
of sensitivity are the elaborate cell cleaning procedures and electrode
construction methods. Removal of platinum oxides from the electrodes
has yielded consistently cells of high sensitivity.
The organization of the report is' apparent from the Table of
Contents. Section 3.1 is a particularly detailed chronological discussion
of the cell development program during the past four months. Section 3.2
is a report of results of some preliminary work done with determining
1. 1
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cell resistance and other characteristics as a function of current level.
Although the discussion of this section is somewhat tentative, the results
are now thoroughly understood and presented in Section 3. 3. The
Appendix provides a detailed look at some of the theoretical techniques
for calculating cell potentials under various conditions which depart
from the standard eases. In particular, the effect of an electrode
only partially covered with the ionizing metal is considered.
ElThe cell work is continuing with applications being investigated
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and a field test program planned.
1.2
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2. EXPERIMENTAL PROCEDURES
2.1 ELECTRODE PREPARATION AND TESTING
Early in the study electrolytic experiments were performed by
using electrodes made of 20 mil platinum (Pt) wire sealed into soft
glass or pyrex tubing, cut and ground flush with the glass so that
only the cross-sectional area of the wire was exposed. The glass
tubing was either dipped into the electrolyte or sealed into cell walls
of glass. This technique did not result in adequate sensitivity because
of the fracturing of glass around the Pt causing diffusion of the electrolyte
into the seal.
Progressive losses of silver from cycling current between electrodes
were thought to be due to diffusion into the electrode material. Tungsten
electrodes were tried because its crystal structure is different from that
of silver, and some improvement was noticed.
By a chance experiment very fine (3 mil) Pt wire was sealed into
a small soft glass tube and clipped short rather than ground flush. The
result was a considerable improvement in sensitivity, allowing plating
currents as small as 0.01 microamperes to be used.
Numerous electrodes were made of three mil Pt wire sealed in
soft glass tubing with data taken by holding two electrodes in a rubber
stopper inserted in a small medicine bottle. Later cells were made by
sealing the soft glass electrodes into opposing ends of glass "T"'s,
the stem of the "T" used for filling and closing the cell. Pyrex tubes
were tried and found unsatisfactory because the expansion coefficient
did not match that of Pt.
2.1.1 Cleaning of Glass Tubes and Pt Wire
There were three procedures for preparing Pt electrodes and in the
later experiments the Pt wire and the tubing were first cleaned before
fusing the wire into the ends of the glass tubes. The wire and glass
tubing were first cut into suitable lengths using a good grade of alloy
scissors for the wire and a steel file for the tubing. The lengths of
tubing used varied from about one inch to 2-1/2 inches and the wire
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about one inch longer than the tubing in which it was later fused. The
wire was immersed in a beaker containing dilute nitric acid for about
three minutes. The acid was then poured off and distilled water added
until the wire was covered. The water was then poured off in such a
way that the entire inner walls of the beaker were washed. This rinsing
with distilled water was then repeated six times. The wire and beaker,
were then rinsed with reagent acetone three times using the same
techniques as when rinsing with water. Nitrogen was then blown into .
the beaker to dry the wire.
The glass tubing was immersed in cleaning solution (K2Cr207
dissolved in concentrated sulfuric acid) for about ten minutes and then
well rinsed with Braun distilled water. The tubes were then shaken to
remove most of the water and placed in a beaker containing reagent
acetone. The tubes were then removed from the acetone and blown
dry with nitrogen. ?The object of using acetone in the final rinsing of
the wire and tubes is to remove the water which is soluble in all pro-
portions in acetone. The wire and tubes were then placed in clean,
dry, covered glass dishes. Most of the glass tubing used was soda
lime glass; however, in a few experiments pyrex tubing was used in
preparing the Pt electrodes. The glass tubes, whether previously
cleaned or not, were fire polished at each end before fusing the Pt
wire into one of the ends. One of the following procedures was then
used in preparing the electrodes.
2.1.2 Preparation of "Wire" Pt Electrodes
The Pt wire is threaded through the tube until it extends a little
further out from the end of the tube than its final planned length. The
wire is then rapidly fused into the end of the tube While rotating the
latter. The tube is then quickly removed to a point just beyond the tip
of the outer gas flame and held there a short time to anneal the glass.
A gas-air torch is used for soda lime glass and a gas-oxygen torch
for pyrex. The wire is then cut off with a good grade of alloy scissors
to the correct length.
2. 2
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2, 1. 3 Preparation of "Sphere Type" Pt Electrodes
After threading the Pt wire into the tube as described under
Section 2.1. 2 until the wire extends about half an inch out, the tip of
the wire is held in the flame of the gas-oxygen torch at a point about
half an inch beyond the inner cone until the wire scintillates and a
sphere is formed on the end of the wire by the melting of the platinum.
The wire is retracted into the tube until the sphere is just flush with the
end of the tube. It is easiest to determine if the sphere is flush by
viewing the sphere and tube under the microscope. The Pt wire
and its sphere is then fused into the end of the tube as described
under Section 2.1. 2. The electrode is then examined under the
microscope and if the sphere extends out too far, or not far enough,
the procedure is repeated using another piece of tubing. In some
cases when the sphere does not extend out far enough, it may actually
be covered with a thin film of glass. The preparation of this type of
electrode is difficult because often a fair number of trials are
necessary before a satisfactory electrode can be made. Another
difficulty that presents itself in some cases is that there is apparently
formed on the surface of the sphere a film of an oxide of Pt which is
sufficiently thick or of such a nature that the electrode will not conduct
current. If, upon examination under the microscope, there appear
bubbles or other defects in the Pt to glass interface the electrode is to
be rejected.
2.1.4 Preparation of "Broken Wirer' Type Pt Electrodes
The Pt wire is threaded into the tube until it extends about half
an inch out from the end and is then fused into the tube as described in
2.1.2. After the tube has cooled to room temperature the wire is grasped
with a forceps from about 1/2" to 3/4" from the end of the tube and,
keeping the wire slightly taut, it is carefully bent back and forth until
it breaks off approximately flush with the end of the tube. The end of
the tube and wire are then examined under the microscope and if there
are any bubbles, splintering (due to the bending of the wire), or other
defects in the Pt to glass seal the electrode is rejected,
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2. 1. 5
Testing Procedure
The numbers of the Pt electrodes, recorded in the "Pt Electrode
Log, " are to be noted on the chart; the one with the lowest number being
"L", the other "R".
The materials used in this test consist of (besides the two Pt
electrodes) two medicine bottles, cylindrical in shape; L D. = 18 ?mm,
height = 50 mm; silver wire 0.020" in diameter; a neoprene 'stopper
having three holes drilled in it, one for the silver wire and the other two
for the Pt electrodes; vaseline; distilled water (Puritas and Braun);
conc. HNO3 C. P. and cleaning solution (K2 Cr207 dissolved in conc.
H2SO4 C. P. ).
The two Pt electrodes are to be placed in the two larger holes,
of the stopper by first threading the Pt wire leads into the two holes,
then pushing the electrodes through the holes so that the ends extend
a predetermined distance ", " below the bottom side of the stopper.
A No. 1 stopper is used, the three holes having been previously greased
with a little vaseline by running a nail through them before placing the
electrodes in.
The Pt electrodes (assembled in the stopper) are next dipped in
hot cleaning solution and well rinsed in Puritas water followed by Braun
water.
A short length of the silver wire is dipped in conc. HNO3, heated
in the gas flame and dipped, while hot, in the acid a second time, then
heated carefully in the gas flame until all black Ag20 is reduced to Ag.
Using a small pliers or forceps, the silver wire is then forced through
the smaller hole on the bottom side of the stopper until its end is in a
plane slightly above the lower ends of the Pt electrodes.
In assembling the three electrodes into the stopper, they are not
to be touched or to be in contact with any material except clean forceps
(after being cleaned) on any part which is to be in contact with the water
or water solution of Ag NO3 in which they are later tested.
? The electrode assembly, consisting of the two Pt electrodes, the
Ag electrode and stopper, are then placed in a medicine bottle containing
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5.0 ml Braun water and checked for conductivity using a scale of 0.03
or 0.01 p.a. Depending on the residual currents obtained, the electrodes
may be tested again in 5.0 ml fresh Braun water after first rinsing them
and the bottle in this water.
The electrode assembly is next removed and, after shaking off excess
water, placed in a second bottle containing 5.0 ml of the appropriate AgNO3
solution and tested. The medicine bottles are to be first cleaned in cleaning
solution and well rinsed in Puritas and Braun water.
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2.2 CELL CONSTRUCTION AND CLEANING
The principle problem of cell construction is the necessity of
using soft glass. It was discussed in Section 2.1 (see also p. 3.23 ff)
that pyrex cannot be used to seal the Pt electrodes because of the poor
match in thermal expansion coefficients. The entire cell body must
therefore be made of soft glass which is more difficult to work with
than pyrex. One particular problem is the sealing of a second electrode
into the cell body can cause the first seal to crack from the heat radiation
of the torch. This problem is ameliorated by using the "T" shaped
cell with the electrode seals placed far apart.
2.2.1 Cell Construction Procedures
Two kinds of electrolytic cells have been standardized. The series
"A" cell has three electrodes of relatively large surface area to operate
in the 10-100 microampere region. The series "B" cells are the high
sensitivity cells made in the inverted "T" shape. They are designed
to operate in the 10-100 millimicro ampere region. The procedures for
making these cells is as follows:
Series "A" Cell
Three twenty thousandths platinum leads are cut approximately one
inch long. Hold the three leads, properly spaced, and imbed in the end
of a glass rod. Using the rod as a holder, wind hot glass around the three
leads approximately in the center of the leads. Heat the bead just formed
and flatten into a round button using tweezers. The platinum is then
cut off approximately 1/4 inch above the button.
The seal is made into a tube end with a small gas-oxygen flame
and annealed in a soft gas-air bunsen flame. The leads are then cut
off above the glass rod.
Series "B" Cell
Cut a piece of 2 1/2 mm 0.D, lime glass tubing approximately 6
inches long. TwO "marias" are then formed about 1/2 inch either side
of the center of the tube. The so-called "maria" is formed by slowly
rotating the tube in a pin-point flame and pushing the two ends toward each
other. Next, two small holes are blown approximately 1/2 inch from each
maria on the outer sides. The tube is then cut in two, either in the flame
or with a file. Gas-oxygen is used for these steps.
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A piece of three thousandths platinum, three inches long is inserted
into one of the above tubes and sealed at the end with the maria, leaving
about 1/2 inch extending past the seal. After the seal is cooled the
wire is broken off as close as possible by bending back and forth with a
pair of tweezers. The glass tubing is then cut about one inch from the
maria on the side of the small hole. Next cut a piece of twenty thousandths
platinum wire about 3/4 inch long. The fine wire is wrapped around
one end of the larger wire about six or eight times the excess wire clipped
off. This coil is then inserted into the end of the tube and the glass is
sealed around it, imbedding the coil and the larger platinum in the seal.
Gas-air is used for this step.
The cell envelope is a "T" tube made of eight mm tubing with a
constriction in the center tube. Gas-oxygen is used.
The electrodes are sealed in one at a time using gas-oxygen and
annealing well with a gas-air bunsen burner flame.
Once the cells have been cleaned, filled with electrolyte, plated
with silver on one electrode, and tested, the cell is sealed at the tube
constriction by applying a hot flame and pulling or pinching the con-
striction. If this is done quickly and the electrolyte level is below
the constriction, the liquid will not rise to its boiling point.
2.2.2 Cell Cleaning Procedures
In general the cells were cleaned by an application of cleaning
solution (sulfuric acid and potassium dichromate), nitric acid, and
liberal rinsing with distilled water. Later it was found that substitution
of the nitric acid with aqua regia removed and Pt oxide layer, giving
excellent reproducibility. The details of cleansing some of the B-series
cells which were used as examples in Section 3 are listed below.
Pt Cell 31 - Exp. D, III, 6-4-62
Prior to above cell was dumped from Parts I - II of Exp. D,
6-4-62, rinsed and cleaned
hot cleaning solution, H20,
Pt Cell B1 - Exp.
Cell tested
Pt Cell B1 - Exp.
Cell tested
A, 6-5-62
directly without
C, I, 6-8-62
directly without
as follows: Warm 1: 1 HNO3' H20'
H20 (stand).
any cleaning since Exp. D, III, 6-4-62.
any cleaning since Exp. D, III, 6-4-62,
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Pt Cell B10 - Exp. D, I - III, 6-11-62
Cleaning solution, H20 (stand), H20.
Pt Cell B16 - Exp. C, 6-13-62
Cleaning solution (-'-'1 - 1/4 hrs), H20, H20 (stand 45 minutes),
17120?
Pt Cell Ell - Exp. E, I - III, 6-11-62
Cleaning solution, H20, H20 stand, H20.
Pt Cell B19 - Exp. B, III, 6-14-62
Cleaning solution ( 1 hr), H20, H20 (stand..-2 hrs), H20.
Preliminary Testing of Electrodes (later Sealed into Pt Cell B5) Exp, D,
II, 6-5-62
Hot cleaning solution (electrode dipped in), H20 (stand), H20.
Pt Cell B5 - Exp. F, I, 6-6-62
Hot 1: 1 HNO3, 1-120, hot cleaning solution, H20, H20 (stand), H20,
Pt Cell B6 - Special Exp., 6-11-62
Cleaning solution 2 hrs), H20, H20 (stand 15 minutes), H20
prior to running. Prior to running Ag NO3 solution used, dumped and
cell rinsed with H20 first, then reagent acetone and dried with a stream
of N2. Cell then constricted and filled with fresh 0.10 N Ag NO3 and run
with right electrode charged with Ag about five minuates at 1.03 p.a.
Next, cell was sealed and used.
Pt Cell B10 - Exp. B, II, 6-12-62
See P 3.42. No cleaning since.
Pt Cell B24 - Exp. I, 6-15-62
Cleaning solution 1 hr), H20, H20(stand 2-1.2 hrs), H20.
Pt Cell B24 - Exp. 3, 6-18-62
0.10 N Ag NO3 solution dumped from the cell rinsed and cleaned
as follows: 1: 1 HNO3 HC1 ( I min), H20 (stand), H20.
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2.3 ELECTROLYTES AND MATERIALS
In general the electrolytes were made using analytical reagent
grade Ag NO3 and KNO3 packaged by Mallinckrodt Chemical Corp.
The chemicals were mixed the distilled, deionized water packaged in
polyethylene containers by Braun Chemical Company. Weighings were
done with an analytical balance and solutions mixed in volumetric flasks.
The electrolytes were generally prepared fresh for each experiment.
However wh.e1-73:-Fe-gh 6 - ere not used no de radation
was noted.
The silver wire used as the initial anode was specified as 99.999%
pure by the supplier, The Wilkinson Co. of Santa Monica. The wire
was cleaned thoroughly in hot, concentrated HNO3 to remove any contaminants
from the drawing process.
The platinum wire was also supplied by the Wilkinson Company with
no quantitative specification of its purity. The B series cells were made
using thermocouple grade Pt drawn to .003 inches.
11.1.1 2.9
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2.4 CIRCUITRY AND DATA TAKING
The circuitry and data taking procedures are very similar to
those described in the previous summary report. The circuit used is
somewhat simpler than that used before and is shown in Figure 3. 32
of this report.
Current is controlled through the electroplating cell by means
of a large resistor in series with a potentiometer across an ordinary
dry cell. The potentiometer insures that the voltage across the
electroplating cell does not exceed a specified value when the cell is
in the open circuit condition. The current through the cell is measured
by a Hewlett-Packard Microvolt-ammeter, the output of which is dis-
played on a Varian Chart recorder with a tape speed of one inch per
minute.
Once the maximum open circuit voltage across the cell had
been set and the cell connected in place, the shorting switch across the
cell was closed and the proper current setting made. A silver wire or
silver rod which had been thoroughly cleaned in nitric acid, oxidized,
and reduced in a hot flame is then inserted into the cell and connected
to the positive side of the cell terminals in order to serve as an anode.
The series switch in the circuit is opened and the shorting bar across
the cell is opened and the chart recorder operating with the Hewlett-
Packard Microvolt-ammeter is started. At the appropriate time on
the recorder the series switch is closed and current passes through
the cell plating silver from the inserted anode onto the negative electrode.
At the end of a two or three minute_ lati,the series
switch is opened and the silver rod is removed from the cell. The
reversing switch is thrown causing the previous cathode to become
an anode and the other electrode is connected into the circuit so that
it may become a cathode. The series switch is then closed and the
current causes the silver previously deposited to be plated from the
anode to the cathode and be recorded by the chart recorder. At the
end of this deplating period the potential across the cell rises and
the current is reduced nearly to zero. When the current has become
sufficiently small the reversing switch is thrown and the process
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is repeated. This sequence continues several times depending on
the character of the data and the purpose of the experiment.
No difficulty was experienced using this technique or circuitry
except for occasional failure of the switches. The switches were
replaced periodically if the data gave evidence of poor contact or
corrosion effects.
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3. EXPERIMENTAL RESULTS
3.1 DISCUSSION OF SIGNIFICANT EXPERIMENTS
The following set of figures are chosen from a large group of
experiments to illustrate some of the typical problems and effects met
in the electro-chemical work. The figures themselves are reproductions
of part of the Varian chart recorder data showing the current versus
time behavior of some of the cells. The experiments are arranged
chronologically and are summarized in Table 3.1 with all the pertinent
data. This section will be a discussion of the experiments individually
to indicate their significance to the cell development program.
Much of the significant work during the past three months was
accomplished using bottle cells described in Section 2.1. These cells
are composed of a medicine bottle with a rubber stopper. Into two
holes of the stopper are inserted glass covered electrodes. The
electrolyte and the wire size used in the electrodes are indicated in
Table 3.1. The maximum current indicated in the table is that current
which passed through the cell during most of the time it was conducting.
As the current dropped to zero, the back voltage across the cell increased
until it reached a value opposing the driving voltage of the circuit. This
maximum voltage which is equal to the circuit driving voltage is also
listed in Table 3.1. Finally, it is important to keep in mind that the
chart paper moves through the recorder from left to right in the orien-
tation of the figures as given. This means that the direction of time
on the charts is from right to left, in a sense opposite to what is usually
encountered in graphical analysis. The time scale is one minute per
inch,
Figure 3.1 indicates some rather good data taken with a carefully
cleaned cell and cleaned electrodes. The electrode diameter was
20 thousandths of an inch; however, the left electrode was 32 millimeters
in length, considerably longer than the 2 millimeter length of the right
electrode. The effect of this longer electrode can be seen-in the figure
3. 1
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TABLE 3.1 SIGNIFICANT EXPERIMENTS WITH PT-130T,TLaCELLS
Maximum Max. Figure
urip3e Experiment Cell Number Electrolyte Electrode Current Volt. No. Comments
1 A-II- Pt Bottle 0.10 N 20 mil 1.6 pa 0.2 3.1 Effect of low current density
3/6/62 Cell No. 2 AgNO3 Pt Wire L = 32 mm, R = 2 mm
2 Pt Bottle 0? 10 N 20 mil 0.16 p.a 0.0777 3.2 Effect of low current density
3/13/62 Cell No. 2 AgNO3 Pt Wire and and low voltage
0.10 pa.
3 E-I-
3/16/62
Pt Bottle 0.10N 20 mil 1.38 ma 0.93 3.3 Effect of large driving voltage
Cell No, 4 AgNO3 Pt Wire
4 A-II-
4/10/62
Pt Bottle
Cell No. 9
5.0 :N
ANO
g 3
3 mil
Pt Wire
.0179 p.a. 0.358 3.4 High sensitivity due to small
electrode area
A-II- Pt Bottle 1.0 N 3 mil 0.0155 0.358 3.5 Effect of "broken-wire" electrode
4/13/62 Cell No. 16 AgNO3 Broken p.a construction
6 A-III- Pt Bottle 0.10 N 3 mil 0.0152 0.358 3.6 Erratic current behavior
4/17/62 Cell No. 18 AgNO3 sphere
7 A-I- Pt Bottle 1.0 N 3 mil 0.0152 0.358 37 Good behavior with sphere
4/18/62 Cell No, 19 AgNO3 sphere pa.
electrodes
8 A-II- Pt Bottle 0.11 N 3 mil 0.0145 0.358 3.8 Effect of supporting electrolyte
5/1/62 Cell No. 24 AgNO3 sphere pa.
and O. lON
KNO
3
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ILT3 173 I Declassified in Part - Sanitized Copy Approved for Release 2013/08/14: CIA-RDP78-05288A000100020002-8 1=1 1=11 1=1
TABLE 3.1 (cont.)
Maximum Max. Figure
Example Experiment Cell Number Electrolyte Electrode Current Volt, No.
Comments
9 A-I- Pt Bottle 0.11 N 3 mil 0.0141 0.358 3.9 Effect of supporting electrolyte
5/2/62 Cell No. 24 AgNO3 sphere 1.ta
and O. 10N
KNO3
10 A-IX- Pt Bottle 0.11 N 3 mil 0.0128 0.161 3.10 Lowered driving voltage with
5/2/62 Cell No. 24 AgNO3 sphere ?a supporting electrolyte
and 0.10N
KNO3
11 A-V- Pt Bottle 0.11 N 3 mil 0.00178 0.229 3.11 Very low current data
5/2/62 Cell No. 24 AgNO3 sphere 1-La
and 0.10N
c.),) KNO3
12
A-VIII- Pt Bottle 0.11 N 3 mil 0.00240 0.161 3.12 Very low current data with
5/2/62 Cell No. 24 AgNO3 ? sphere i-La low residual current
and O. 10 N
KNO3
13 B-I- Pt Bottle 0.10 N 3 mil 0.010 ?a 0.161 3.13 Sensitive "broken-wire"
5/25/62 Cell No. 28 AgNO3 Broken electrodes
and 0.10N
KNO3
14 B-III-
5/28/62
Pt Bottle 0.10 N 3 mil 0.0086 0.161 3.14 Effect of pyrex
Cell No, 28A A NO Pt. wire ?a
g 3
and O. lON
KNO3
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C:11
I Declassified in Part - Sanitized Copy Approved for Release 2013/08/14: CIA-RDP78-05288A000100020002-8
TABLE 3.1 (cont.)
Maximum Max.
Figure
Example Experiment
Cell Number
Electrolyte Electrode
Current
Volt.
No. ?
Comments
15
B-I-
Pt Bottle
5.0 N
3 mil
0.0083
0.13
3.15
Testing of electrodes for cell
5/17/62
Testing. Cell
AgNO3
sphere
?a for
of Figure 3.17
No. 2
16
B-IV-
Pt Bottle
5.0 N
3 mil
0.0104
0.161
3.16
Testing of electrodes for cell
6/4/62
Testing Cell
AgNO3
broken
of Figure 3.18
17
A-III-
Pt "S"
5.0 N
3 mil
.008
0.13
3.17
Erratic performance after
5/18/ 62
Cell No, 2
AgNO3
sphere
assembly of electrodes into cell
18
Pt Cell B1
5.0 N
3 mil
0.0103
0.161
3.18
Better result with'broken-wire"
6/4/62
AgNO3
broken
ta
electrodes
4 19
A-I-
Pt Cell B1
5.0 N
3 mil
0.0108
0.161
3.19
Accumulation of silver on
6/5/62 .
AgNO3
broken
standing overnight
20
C-I-
Pt Cell B1
5.0 N
3 mil
0.010
0.161
3.20
Accumulation of silver on
6/8/62
AgNO3
broken
standing three days
(No. 2)
21
D-I, II, III-
Pt Cell B10
0.10 N,
3 mil
0.0094
0.161
3.21
Effect of changing electrolyte
6/11/62
1.0 N
broken
0.0097
thru
concentration
and 5. ON
0.0100
3.23
AgNO3
?a
22
E-I, II, III
Pt Cell B11
0.10 N,
3 mil
0.0100
0.161
3.24
Effect of electrolyte concentration
6/11/62
1. 0 N
broken
0.0102
thru
5.0 N
0.0103
3.26
AgNO3
?a
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lEji I Declassified in Part - Sanitized Copy Approved for Release 2013/08/14: CIA-RDP78-05288A000100020002-8 1=1 t=11
TABLE 3.1 (cont.)
?:7,:amp1e
Experiment
Cell Number
Electrolyte Electrode
Maximum Max.
Current Volt,
Figure
No.
Comments
23
C-I-
6/13/62
Pt Cell B 16
0.10 N
ANO
g 3
3 mil
broken
0.0101
pa
0.161
3.27
Large progressive losses
24
D.-II
6/5/62
Pt Cell B 5
5.0 N
A NO.
g
3 mil
broken
0.0100
0.161
3.28
Large loss with later recovery
25
6/6/62
Pt Cell B 5
5. 0 N
Ag NO3broken
3 mil
0.00995
La
0.161
3.29
High sensitivity cell with
capacitance surge
26
UI
Special
6/11/62
Pt Cell B 6
0.10 N
ANO
g 3
3 mil
broken
0.0090
ta
0.161
3.30
Progressive loss of silver
27
B-II-
6/12/62
Pt Cell B 10
5.0 N
AgNO3
3 mil
broken
0.00090
a
0.161
3.31
Correction of cell behavior
shown in Figure 3.30
1=1
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ASSOCIATES. PALO ALTO. CALIF.
INSTRUMENT DIVISION
111111 EMI 8-Z000Z0001-000V88Z90-8Zdal-VIO 'bi-/BO/CI-0z eseeiej -10j panaiddv Ado pez!l!ueS u! Pe!4!sse1087.1 11 111111 6.1
Declassified in Part - Sanitized Copy Approved for Release 2013/08/14: CIA-RDP78-05288A000100020002-8
as a result of the increased length of the tail in the run from left to right*
and the less-than-vertical slope of the trailing edge of that particular run.
This effect was reproduced over and over again in succeeding runs of
the data which, however, are not presented here for the sake of concise-
ness. The explanation for this length and tail of the curve as a result
of the larger surface area and lower current density at this electrode
is not entirely understood. One mechanism can be postulated, however.
When the silver is initially deposited from the smaller electrode onto
the larger electrode, some of the silver is deposited at distances along
the large electrode considerably removed from the small electrode.
When the current through the cell is reversed, that silver nearest the
small electrode is removed from the large electrode first. As we
approach the tail of the curve, it is necessary for silver to be plated
off of the large electrode at the remote points. This would result in
larger resistive drops through the electrolyte causing_ov,9rvoltages to
tY
be required to remove this last bit of silver. Thpilvoltage across the
cell would then be reduced and the rate at which this silver is removed
would be considerably less than the rate of removal of silver from those
points near to the cathode.
In Figure 3.1 the current density at the large electrode was a
maximum of ------3 micro amperes per square centimeter. In Figure 3.2,,
thelower current level overall so that
the current density has become as small as two-or-three-tenths of
a rni.....c_r_p_anap_er square centimeter. The difference, in effect,
between the right electrode being the anode and the left electrode being
the anode is still apparent. Another effect can also be observed in
Figure 3. Z. The series resistance of the circuit is sufficiently large
and the sensitivity of the microvolt ammeter is sufficiently high so that
one can see the effect of charging up of the capacitance layer at the
electrodes. That is to say, the initial peak on each of the charging
curves is due to a surge of current into the double layer at the inter-
face between the electrodes and the electrolyte. Once this layer is
):c Indicated on the chart by L--) R.
3. 7
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8-Z000Z0001-000V88Z90-8Zdal-VIO 'bi-/8O/CI-0z eseeiej .104 panaiddv Ac100 pazWueS u!Pe!PsseloaCI
z aa-rvId
?
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_I --1-L1,11-.-?;:):::_HT -1_1-4-21--11---7,_--- -4:----?---i=1.-----1: -I'll '-'1- ----1-1-i'-i- -1-
r -I I-- ! ! ! -1-- -7-1 1 .
rl, -7= ! ; j
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; . ? I- I- I-
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; 1-4-
II '1,---L 1 _t_h -' ' i ' i -1 --; __Li 'k- ti ', -r- -4 --'-' ; ? ?
' -F1-1-1
=- - 1-1; -I --i -I- j-
17-21 I,-t --: I- -r-Th-1 ; i ..;4 7=-1 '_,L_Th _- -I i ' --1-1 ' ! 1 "
. ?--; ? : ' 1 1-- ' 1 1-- 1--- '-I- -1-1---H-- _7_1=11=
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; t I- , ;___1 ? 1-__L.7 -,` _.1_1_1=. _,-..,, i___r_ ::::?.:=F_,_. r-t-. -1-!--1 t , -
H--1 4-1 1. t L , , __. ,..,,,___ ?
1 -4-4 ;--,- ;-1 I- H- --i_J__i ; HT- 1---F-c 4 1 -I
-,--j--i -t ;_, -----1-.-1H -I ff-:
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'ALO ALTO. CALIF.
INSTRUMENT DIVISION CHART NO. 4-A
-7-4'
1-1
; I
PRINTED IN U.S.A.
8-Z000Z0001-000V88Z90-8Zdal-V10 'bi-/8O/CI-0z eseeiej .104 panaiddv Ado pezWueS u! Pe!4!ssepa-c-11
Declassified in Part - Sanitized Copy Approved for Release 2013/08/14: CIA-RDP78-05288A000100020002-8
Li
a
charged and current begins to flow at a rate determined by the cell
resistance and back voltages, the current level drops down. The time
constant for this drop of the capacitance charging current is consistent
with a value of approximately 20 to 40 microfarads capacitance per
square centimeter of electrode area.
Figure 3.3 illustrates an entirely different effect. In this experi-
ment the current density was considerably higher than the previous one,
the experiment here having a current density of approximately 2 milliamperes
per square centimeter or four orders of magnitude higher than that of the
previous experiment. A long tail, however, still appears on these data
but has clearly a different characteristic. The trailing edge of the
charging curves is still rather vertical in spite of the long tail. The long
tail in this experiment cpn be explained by the high maximum voltage that
was used across the cell being over 0.9 volt. The effect of this large
voltage across the cell is to cause spurious reactions to take place in the
cell so that silver can be deposited at the cathode as the result of other
oxidation reactions taking place at the anode other than the removal of
silver from the anode. It will be noticed as we proceed from right to
left in Figure 3.3 that the area under the block type curves gradually
increases due to the contribution of these spurious reactions.
The lessons learned from the previous experiments with various
current densities suggest that if low current data were to be obtained,
it would be necessary to use very small electrodes. Accordingly, an
electrode was made of 3 mil platinum wire embedded in a soft glass rod
and clipped short with a pair of scissors so that approximately only 1
millimeter length was exposed to the electrolyte. The electrodes were
carefully cleaned in cleaning solution, nitric acid, and distilled water.
The results are indicated in Figure 3.4 for one of the experiments with
electrodes of this type. The current level, it will be noted, is less than
0.02 microamperes so that the integrated charge under the curves is
of the order of 2 microcoulombs. The reproducibility of this data,
however, appears to be approximately one percent of this, or 0.02 micro-
coulombs. This cell, then, will exceed the sensitivity of the initial goal
of 1/10 of a mierocoulomb. It was learned by experience, however,
that electrodes of this sensitivit could 0- ?_. _ - roducibly and
3. 9
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8-Z000Z0001-000V88ZBO-BLdCII-VIO 'bi-/BO/CI-0z eseeiej -104 panaiddv Ac100 paz!4!ueS u!Pe!PsseloaCI
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? C:)-1"---71 L._
iy,?....T-1----_L--
,,
i
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r--i---j -
!.....
___I -.1
.--1'
11-1
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!
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1.---F4-- -
.C.7P, --i=4-
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that a, somewhat different procedure would have to be employed in order
to accomplish this goal.
One technique that was followed to obtain reproducibility has its
results indicated in Figure 3. 5. Here the electrode was prepared by
embedding the 3 mil platinum wire in soft glass allowing a centimeter
or so of the wire to extend beyond the glass and then breaking the wire
off at the base near the glass by fatigue; that is, bending the wire back
and forth until it was broken at the glass metal interface. Almost all
electrodes made in this manner seemed to yield fairly good results and
the data indicated in Figure 3.5 shows a current level of 0.015 micro-
amperes with a form to the curve nearly as good as that obtained in the
previous example.
Not all our results at this time were entirely satisfactory, how-
ever, as is indicated in Figure 3. 6. This shows what can happen
during the run when the current level no longer maintains itself at a
constant value until all the silver is removed from the electrode. The
electrodes of this cell were fashioned by heating the 3 mil platinum wire
in a very hot flame until a little sphere of molten platinum is formed at
the end. This sphere is then mounted at the tip of the glass tube to serve
as the electrode. This erratic effect was occasionally noticed with other
electrodes made by different techniques, but not so frequently as it was
with this technique. It was found that this erratic behavior of the current
was not the result of any loss of silver during the plating process or
any increase in the cell resistance but, rather, the effect of some kind
of an erratic back ?*?? o lt a g e which opposed the driving voltage through the
cell and lowered the current accordingly. Figure 3.7 indicates some
good results obtained with sphere type electrodes. Here, the maximum
current level is also about 15 millimicroamperes.
Figures 3.8 and 3.9 indicate the effect of adding a supporting electro-
lyte, in particular potassium nitrate, to the silver nitrate electrolyte,
the idea being in principle that the supporting electrolyte will not be
reactive in the electroplating process because of the voltage required to
reduce potassium at the cathode. However, the addition of the supporting
electrolyte should have an effect in lowering the over cell resistance
3.12
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and may be of interest if the cell resistances obtained with the silver
nitrate alone are too high. It can be seen from Figures 3.8 and 3.9
that one of the effects the supporting electrolyte has is to raise the
residual current in the tail of the curves which is undesirable. This
effect can be eliminated, however, by lowering the driving voltage
through the cell which was done in Figure 3.10. The effect of lowering
the residual current by reducing the driving voltage allowed us to
improve our current sensitivity by an order of magnitude and data was
taken as shown in Figure 3.11 and 3.12 at current levels of the order of
a millimicroampere. Also in Figures 3. 11 and. 3.12 can be seen the
effect at this level of sensitivity of lowering the driving voltage and
reducing the residual currents. In Figure 3.11 the driving voltage
was .229 volts whereas in 3.12 it was .161 volts. The residual
current was reduced by approximately a factor of 2 accordingly. It
will be observed that in Figure 3.12, the residual current is of the
order of 5 x 10 amperes which correspond to 1/20 of a micro
microgram of silver per second. This is an amazing sensitivity for
the detec _III_ ? _ silver itself an
than anything reported in the literature with similar technictu_e_s_2,
.s
?
er
4w.a.s_fo_und that it was not pas.sible_to make cells of the sensitivity
of Figure 3. 12 in a consistent and predictable manner. These cells had,
as was escribed previously, electrodes of small spherical shape embedded
in the tips of glass rods inserted into the cell. Many erratic results
were obtained from these electrodes and it wp.p I owld that mcro reprQdqci,-
bility, consiatency, and the same level of eenaitivity could be obtained by
making the electrodes in the manner described in Section 2.1 with the
broken wire technique. In these cells the electrodes were given a fresh
surface by breaking the 3 mil wire through metal fatigue after the wire
has been sealed into the glass. It was not understood at the time the
reason for this improvement in results but later it was shown to be due
to the formation of an oxide surface on the platinum if it is heated in the
flame to seal the wire into the glass envelope. The breaking of the wire
in this manner gave a surface more or less free of an oxide layer.
Figure 3.13 illustrates the results of a cell made with broken wire
electrodes. It can be seen to be of comparable sensitivity and reproduci-
bility of those shown previously.
3. 18
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CHART NO. 4-A
,PRIN
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About this time in the development program, it was decided that
sufficient sensitivity was obtained with the electrodes inserted in the
bottle cells. It was decided that the next step should be to assemble
these electrodes into sealed glass containers for operations use. Several
electrodes were prepared in the usual way and assembled into T-shaped
fl cells and filled with electrolyte to be tested before sealing. The results
with these cells were completely inadequate. The cells performed many
orders of magnitude less sensitivity than previous cells and in a manner
which was completely new to us. Several days of experiementing did not
reveal any insight into the problem, this experimenting including various
cleaning procedures and techniques for removing any oxide layers that
might have accumulated on the cells during assembly. The electrodes
themselves were tested before assembly into the cells and, surprisingly
enough, they were found also to behave rather poorly although not so
badly as when assembled in the cells. It was realized at this time that
the one
11
d han ed from previous experiments was that
...????=m.10?1?.?
the electr des were being made out of platinum sealed into thin ? rex
tubing where a soft tubing had been used before. In order to better
understand the effect of pyrex and whether or not it was decisive in the
inferior operation of the electrodes, a specially designed experiment
was performed in which the conventional bottle cell was operated using
three electrodes; two made of soft glass, one made of pyrex, and all
prepared, cleaned, and treated in exactly the same manner. A partial
result of this experiment is illustrated in Figure 3.14. Silver was
plated onto one of the soft glass electrodes, then plated onto the other
soft glass electrode, and then plated onto the pyrex electrode and cycled
among the electrodes in that manner. The result of plating from the
left electrode to the pyrex electrode was found to be a nice square-shaped
curve of the type usually encountered with soft glass electrodes. How-
ever, when the silver was removed from the pyrex electrode and plated
back onto the previous electrode, the curve had the unusually long tail
shown in Figure 3.14. However, although not shown in this figure,
there appeared to be no loss of silver since plating from the left electrode
onto the right electrode gave an area comparable to the earlier amount.
This is also confirmed by a planime4r measurement of the curve of
which the silver was plated from pyrex to soft glass showing the total
3. 23
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Declassified in Part - Sanitized Copy Approved for Release 2013/08/14: CIA-RDP78-05288A000100020002-8
area under the curve and the tail to be approximately equal to the
rectangular curves obtained previously. Since the problem of making
the cells of soft glass was of sufficient difficulty that it was worthwhile
investigating whether or not the problems with pyrex could be eliminated,
a series of experiments were undertaken in order to determine what the source
of the difficulty with pyrex was. These experiments indicated that the
electrodes using pyrex exhibited a considerable back voltage which was
somewhat erratic in nature and which opposed the driving voltage through
the cell. Elimination of chemical sources for this back voltage left
the only explanation that the voltage was the result of the difference in
the expansion coefficient of pyrex and platinum. When the electrode is
sealed into the pyrex tube, it contracts on cooling at a rate faster than
pyrex, leaving a separation of perhaps only a few hundred angstroms,??.
between the platinum and the pyrex. This separation is sufficient, \\
however, to allow electrolyte to diffuse between the platinum and the
pyrex but at a sufficiently slow rate that the concentration of the electro-
lyte in this region would be expected to differ from that in the main
solution. This concentration gradient sets up a concentration potential
which it is theorized is responsible for the potential opposing the driving
voltage through the cell. Since it was not known how to control the
diffusion or the concentration potential that was set up, the use of
pyrex for electrodes and consequently for the cell body had to be
abandoned. Cells were manufactured of soft glass from this point on-
ward.
It was the rule initially that before assembling the electrodes in
? the sOft glass cells, that they be tested in bottle cells to see if their
performance was adequate. Figure 3.15 and 3.16 illustrates the testing
of such soft glass electrodes in bottle cells prior to assembly. In the
case of Figure 3.15 the electrodes were made having small spheres
of platinum extending just beyond the glass tubes which held the platinum
wire. In Figure 3.16 the electrodes were made by the broken wire
technique. The results of these experiments are illustrated typically
in Figures 3.17 and 3.18. Figure 3.17, the spherical electrodes
rit showed a considerable degradation in performance with various erratic
backvoltages being generated, when the spherical electrodes were used
as anodes. The broken wire electrodes, however, showed very little
3.25
Declassified in Part - Sanitized Copy Approved for Release 2013/08/14: CIA-RDP78-05288A000100020002-8
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tendency to give this kind of erratic behavior. A typical result is
illustrated for the electrodes of Figure 3.16 after they were sealed
into cells and obtained the results of Figure 3.18. Even so, in
Figure 3.18 it can be seen that when the right electrode is the anode,
there, is still some erratic behavior at the beginning of the plating
process. Another problem with the electrodes when assembled into
soft glass cells is illustrated in Figure 3.19 and Figure 3.20. This
problem is the apparent accumulation of silver on an electrode as a
result of standing overnight or for several days. The cell of Figure 3.19
had all the silver removed by plating from the right electrode onto the
left electrode. The cell was then allowed to stand overnight and a
current put through the cell to move material from the right electrode
to the left electrode. It was found that the current was able to pass as
a result of apparent accumulation of silver on the right electrode.
However, this accumulation could have been the result of another chemical
process which was reversed as the result of the applied voltage across the
cell. This effect is even more pronounced in Figure 3.20 wher e the
accumulation was quite significant in size as the result of standing over
a three day period. The exact mechanism of this apparent silver
accumulation is not yet understood, however it is believed to be related
to the formation of oxides, or hydroxides on the electrode as a result
of standing. The apparent accumulated current-time product then represents
that charge which is necessary to decompose these oxides or other chemical
products which were formed.
Among the experiments which were performed with the cells con-
structed for operational use are a set of experiments used to investigate
the effect of changing concentration of the electrolyte on the performance
of the cells at low current. An example of this kind of experiment is
illustrated in Figures 3.21, 3.22 and 3.23. In these three figures the
same cell was used and experiments were performed successfully by
first electroplating silver with tenth normal silver nitrate concentration,
removing the electrolyte, continuing the plating of silver from one electrode
to the other with one normal silver nitrate, removing the electrolyte and
finishing the experiment by plating the silver back and forth between
electrodes with five normal silver nitrate. It will be noticed that not only
3. 35
Declassified in Part - Sanitized Copy Approved for Release 2013/08/14: CIA-RDP78-05288A000100020002-8
Declassified in Part - Sanitized Copy Approved for Release 2013/08/14: CIA-RDP78-05288A000100020002-8
1
1
1
1
is there little change in the shape of curves, the effect of the residual
current and the height of the curve, but there is also little loss in the
amount of silver plated onto an electrode when the electrolyte was ?
completely removed from the cell and replaced with new electrolyte.
A careful examination will reveal however that as expected the higher
concentration of electrolyte does increase the current through the
cells somewhat due to its lower resistance in the circuit controlling
the current level. Another set of experiments illustrating the effect of
varying concentration is indicated in Figures 3.24, 3. 25 and 3. 26. With
this cell it will be noticed however that increasing the concentration
of the electrolyte does produce miscellaneous random variations in
voltage, both while current is being conducted through the cell and
after the apparent shut-down of the cell by the completion of the silver
plating. These miscellaneous background variations are probably
due to effects of oxides or other chemicals formed in minute quantities
during the electroplating process. This formation of spurious compounds
is evidently enhanced somewhat by the use of higher concentration of
silver nitrate.
Occasionally some of the cells made by the broken-wire technique
gave very poor results when subjected to tests. One such cell, indicated
in Figure 3.27, shows very large progressive losses as the silver is
plated from one electrode to the other. There appears to be no anomalous
ack voltages and the shape of the curves is very good. There is also
Occasionally a catastrophic loss of silver from one of the electrodes
will occur during the cycling process and then reappear at a later time
when more silver is added to the cell. This is illustrated in Figure 3.28.
In area 10 can be seen a reasonably good shaped square pulse as the
silver was plated from left to right. However, when the right electrode
was made an anode, the silver apparently disappeared and area 11 is
almost nil. In area 12, the silver wire was inserted into the cell and
a new current time product of silver was plated onto the left electrode.
The silver was then cycled in area 13 from the left electrode to the right
electrode and when the right electrode was made an anode and the silver
plated onto the left electrode, not only was the current time product of
3.36
Declassified in Part - Sanitized Copy Approved for Release 2013/08/14: CIA-RDP78-05288A000100020002-8
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area 13 reproduced, but the area under the curve suggests that what
appeared to be lost in area 11 was now reappearing and adding to the
amount of silver in area 13 so that the silver was not lost at all, but
merely made passive in some way. It is now understood that these various
forms of losses of silver are due to the most part to chemical impurities in
the cell which can be removed by more careful cleaning procedures or
due to the formation of oxides on the electrode during the assembly process
or on standing in an electrolyte which has been saturated with atmospheric
oxygen.
Figure 3.29 indicates results from one of the more sensitive cells
with a electrolyte concentration of five normal silver nitrate. This
cell was made by the broken wire technique and performs reasonably
well at a current level of less than one millimicro ampere!. The large
spike at the beginning of each curve is the result of the capacitance surge
caused by the current charging up the electrode's face before silver ions
begin to move through the solution. This spike is often noticed at these
low current levels because the large series resistance in the circuit
allows the RC time constant to be significantly greater than the micro-
volt ammeter time constant. The residual current in this figure appears
to be very small. Indeed, there is some suggestion that it is actually
negative as the result of miscellaneous potentials in the cell.
Figure 3.30 shows a progressive loss of silver in one of the
sensitive cells when a current level of less than a millimicro ampere
was used. However this loss can be rectified as is illustrated in
Figure 3. 31. The electrolyte was removed from this cell, the silver
plated on the electrodes was dissolved with acid, the cell cleaned with
acqua regia, and rinsed several times with distilled water. The
aqua regia treatment produces exceptionally good results and it is now
known that this is due in part to the removel of platinum oxides from the
surface of the electrode. The residual current in Figure 3. 31 ap_p_ears
der of 10-11
amperes corresponding to a flow of silver
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through the cell of 1/100 of a
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am per second-. This is
exce tionally
good results for an electrol tic
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1
sensitive means
of measuring the quantity of silver and deposited onto the electrode.
3,42
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