Procurement, development, and testing of nickel- cadmium cell

Baumstark, G. A.

English

NASA Technical Reports Server

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NATIONAL AFJiONAUTICS AND SPACE ADMINISTRATIOrJ 
CONTRACT NU-5-9226 
'J23CHNICAL STATUS REWRT NO. I2 
(May 25 thratgh Auguet 26, 1966) 
"PROCUREMENT AND DEVELOl"T PROGRAM 
FOR NICKEL-CADHIUH CELLS TO 
SPECIFICATION S-615-P-2" 
SUNlURY: 
are being made. 
ing equipent  was modified so t ha t  4.e can be used a t  one time. 
High Reliability operations were re-located and operators were trained 
and cer t i f ied for  all production operations. 
t e s t s  (overcharge a t  -5OC) a r e  given which were done a f te r  several 
types of conditioning procedures. 
Presswe and Voltage on -5OC overcharge, and voltage during c e l l  
"reversaltt w i t h  overcharge behavior. 
behavior during 120 hour overcharge by voltage, pressure and pressure 
decay a t  an early stage of t h e  overcharge. Carbonate content of cell. 
electrolyte was reduced. 
included . 
The cover problems have been solved and superior covers 
More pressure transducers were received and record- 
The 
Results of eight ttscreenhg" 
Correlation was sought between 
Efforts were made .to predict 
A delivery schedule for Item 2 ce l l s  is 
DESIGN AND EQUIPNEXT: 
A. - Cover. 
glass-ceramic-metal seal principally caused by unsatisfactory 
aetall ized ceramic parts and migration of tho braze metal. 
Fhese have been solved by a change of the braze metal and 
special electroplating of  the metdliaed coating of t h e  ceramic 
?art. 
:ontract, was done before the solution of these problems was 
3chieved. We believe t h a t  we now have a cover seal  which is 
iefinitely superior to any other used for sealed cells. We 
mve proved th i s  out i n  the 2 inch diameter stainleas Steel 
:over by making 30 covers i n  the  past few days with a yield 
D f  approximately 9@ t h i s  change, t o  the us8 of gold rather 
than s i lver  in brazing the ceramic element t o  the  positive cup 
terminal and the stainless s t ee l  cover, w i l l  occur with c e l l  
Jo. 231. 
to t a k e  place a t  approximately c e l l  No. 290. 
the use of a cover whose diameter is 0.01 inch greater t o  
be used w i t h  the thin w a l l  (0.025 inch) cell  casea. 
Further problems were encountered w i t h  the  multiple 
Considerable experimental work, not assigned to t h i s  
Another minor change w i l l  be made which is expected 
This involve6 
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Bo Test Eauipnent. We have constructed a switching device 
that pressure and vo1tae;e data for two se t s  of 2.4 ce l l s  
SO 
Can 
be taken on our 24 point recorders. 
transducers were received. We now have 55 transducers f o r  
use ori thiis project. 
Additional pressure 
0,  Re-location of Operation+ The move of the High Reliabil i ty 
operations was made during the period May 26 to June 1. The 
testing i e  being continued with the same personnel a t  the 
Battery R & D Laboratory i n  Elmsford and the production 
equipnent w a s  moved to the plant a t  Cold Spring, N. Y. where 
it is located i n  a separate room of 2,000 square f ee t  apart 
from the other battery operations. 
secured and trained, three for  Production and one for  Quality 
Control. A t  l e a s t  one operator has been certif ied by Mr. George 
LeFloch, the DCASR representative for each of the 16 operations 
according t o  our training program and NASA specification NPC-200-31. 
This was completed between July 6 and July 15. 
s u p e r v i ~ ~ r ,  Mr. Frank Crozier, was assigned t o  the High Reliabil i ty 
f a c i l i t i e s  on June 13. 
Four workers have been 
. 
A Quality Control 
111. ITEM 1 CELLS (PROTOTYPE EVALUATION 1: 
Tests are being continued on cel ls  130 throuEh 135 which have the 
"filler tribe-gage adapter" integral with the-cell cover togother with 
the ce l l s  of Item 2. 
a t  t h e  adapter to transducer connection, were tested for several 
weeks w i t h  Item 2 ce l l s  and then the tes t s  were discontimed due to 
the leakage problem And the uncertainty of c e l l  pressure readings. 
We expect tha t  we can get more than enough ce l l s  t o  sat isfy the . 
contract requirements for  Itom 1 cells. 
ditioned" ce l l s  from those with adapters not integral with the cover, 
probably a t  l ea s t  10 of the 15 (approximately) available. 
there w i l l  be cella from the group Nos. 130 through 135 which have 
adapters integral w i t h  the cover. In the remainder we pOp08e that 
cella from the Item 2 group which do not  sat isfy some minor require- 
ment of the Acceptance Tests be used. T h i s  would be done after 
mutual agreement with DRTE and NASA-Goddard engineers. 
The other cells, which were subject to leakage 
Some of them w i l l  be "con- 
Then 
IV. ITEM 2 CELLS (PROTOTYPE  INSTALLATION^; 
More ce l l s  were assembled so that we now have 31 ce l l s  (Nos. 200 
through 230). 
separator assemblies have not been completed due t o  the cover 
problems mentioned in section IIA. 
have completed "open cell" tests. These plates (80 each positive 
and negative) constituted a t e s t  fo r  effect  of the special treat- 
ment during open c e l l  test which was described in section B of 
the "Summary of the Design Review Meeting of April 12" which waa 
submitted with Report No. ll. 
The remaining 4 l  ce l l s  which exist as plate- 
Plates for 25 more ce l l s  
O f  the 31 celle which have been assembled 24 are being subjected 
t o  t e s t s  described in Section V. 
damaged ab followe: 
The remaining 7 cel la  were 
PORTABLE POWE$ FOR PROGRESS - -  
Cell 204. 
Cell 205. 
Cell 222. 
The adapter broke away from the cover during the 8/1 
t o  8/5 overcharge. 
The c a l l  "bulged" on the overcharge t e s t  of 6/13 t o  
6/17. 
This c e l l  'Ibulgedn due t o  excessive pressure on the 
initial charpe. 
no defects were noted. Ye believe it was t1rever8e* 
connected during charge. 
The adapter broks from t h o  cover on 6/l4/66/ 
The adapter broke a t  the start of the filling operation 
in early June. 
These ce l l s  llbulpedll while on overcharge of 6/13 to 
6/17. There was no record of excessive pressure on 
these ce l l s  and ce l l  205. The cause was probably a 
leak at  the connection t o  the transducer so tha t  the 
true pressure was n o t  recorded. 
Thoro was no record of excessive pressure. 
The c e l l  was cut open, examined and 
Cal l  225. 
C e l l  226. 
Cell 229 
and 230, 
V. TEST DATA; 
A. General. 
t e s t s  described here were done chiefly on Item 2 cells. 
Because of the difficulty, described i n  Reports 10 and U, 
with the n120 hour overcharge" t e s t  a t  -5OC and the sug- 
gestion made by Mr. W. E. Yhreinen of DRTE we have concen- 
trated on th i s  t e s t  as a llscreeningl' method. 
uated a mmber of conditioning treatments f o r  the ce l l s  
such e8  wreversalll, overcharge and "n3VerSa11', repeated 
charge-discharge cycles, overcharge a t  +2roC, discharge a t  . 
a high rate, increase of amount of electrolyte and reduction 
of LiOH content of electrolyte. Eight overcharge t e s t s  were 
conducted for periods of 40 t o  134 hours. 
ment which show8 promise ia overcharge in a vented s ta te  
followed by discharge and t@reversal". 
in progress and effor ts  are being made t o  predict the effi-  
ciency of the reversal from the voltage during reversal. 
Although some tes t s  were run on Item 1 cel l s  the 
We have eval- 
The only treat- 
These t e s t s  are s t i l l  
We have a l s o  attempted t o  correlate voltage with internal 
pressure during the -5Oc overcDarge t e s t  with negative results. 
Neither do pressure decay measurements on open c i rcu i t  during 
early phases of the overcharge t e s t  prove useful i n  predicting 
behavior for  the f u l l  120 hours. Some success was had based 
on pressure af ter  40 hours of the test .  
the K2CO3 content of the electrolyte t o  less than 3$ by nelec- 
t rolyte  exchange1'. 
We were able t o  reduce 
B. Outline of OvercharEe Tests a t  -5OC. 
1. Test of 6/13 throunh 6/17. On th i s  t e s t  f o r  106 hours, 
5 of 19 cells or  26% remained below 200 PSI. 
2. Test of 6/27 throuRh 6/2q. This t e s t  of 40 hours waa 
reversal to -1.5 volt. performed following "open 
Seven of the 21 ce l l s  or 33% remained below 200 PSI. 
PORTABLE POWER FOR PROGRESS 
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These resul ts  are the same as  i n  the previous test ,  allowing 
for  i t s  shorter duration, so we condider the "open cel ln  
reversal t o  be without benefit. 
Test of 6/30 throuEh 7/1. This 40 hour t e s t  was done af te r  a 
discharge t o  0.6 volts a t  2C (20 amperes). Seven of 22 ce l l s  
or 32% remained below 200 PSI, so this  conditioning, al80, ie 
fruitless . 
Test of 7/12_cIbc3 thrcr uEh 7/12 for  78 and 128 hours. Prior t o  
this teet a l l  the cella were oharged st +25OC for  89 haurs. 
During this charge 11 of 22 or 5C$ remained below 200 PSI and 
pressures were approximately 2/3 the pressures shown a t  -roc. 
Since only 4 of 24 or 25% survived this  charge, we judge that 
+2S0C overcharge is not productive. 
were: 7 cycles of automatic charge-discharge a t  -5OC which 
w a s  not advantageous as only 2 of 10 ce l l s  remained below 
200 PSI a t  35 hours overcharge; an "open cell" overcharge 
of   AH a f t e r  which only 1 of 5 ce l l s  was below 200 PSI; and 
an "open cellt1 overcharge of 12AH which gave 4 of 6 ce l l s  
below 200 PSI af te r  128 hours overcharge. Only this last 
procedure shows promise. 
Included in th is  t e s t  
Also before t h i s  t e s t  we increased the mount of electrolyte 
t o  17 and 17% from l@$ (% by weight of the plate-separator 
assembly weight) for  four cells. 
no better on th i s  overcharge than they had done on the 6/30 
through 7/1 t e s t  we conclude that there i s  nothing t o  be gained 
by increasing the amount of electrolyte, 
Test of 7/19 through 7/20. 
charged open f o r  l2 and 18 ampere hours a t  1 and 2 amperes. 
This treatment did not result  in low pressures on th i s  40 
hour overcharge. 
Teat of 7/24 throuprh 7/29/66. This t e s t  of 120 hour duration 
for  18 ce l l s  was pcrformed, following reversal for 1, 3 a d  5 
AH a t  2 amperes. 
overcharge. Of the aix cells reversed for 1 AH only one stayed 
below 200 FSI. O f  the six c e l l s  given 3 AH, two remained below 
200 PSI and of the six given a 5 AX reversal, four stayed below 
200 PSI. 
than 1 or 3 AH. 
Test of 8/1 and 8/2 throwh 8/5/66. 
were done for  th i s  94 hour overcharge. 
not been on test for  more than two weeks (including Item I ce l l s  
130 through 135) received "open cell11 overcharges for 12 AH 
followed by reversal of 5 AH and gave four cell0 which remained 
below 200 PSI during the overcharge. In  another group of 5 
ce l l s  which had been in the 7/24 through 7/29 test and had 
received the overcharge and reversal, only 1 of the 5 gave 
pressures below 200 PSI, In 6 ce l l s  the LiOH content of the 
electrolyte was reduced t o  0.3 N or l e s s  by nflushin&' the c e l l  
with 7.2 N KOH solution. None of these ce l l s  stayed below 200 
PSI on th i s  overcharge. Thia tes t ,  although apparently negative, 
w i l l  be respected when further ce l l s  are assembled, 
Since these ce l l s  performed 
Prior t o  this tes t ,  18 ce l l s  were 
The reversal  was done without an open c e l l  
Apparently, a reversal of 5 AH gives bet ter  resul ts  
Several pre-treatments 
Seven ce l l s  which had 
PORTABLE POW R FOR PROGRESS -5- 
8. Test of 8/10 through 8/16/66. 
on 21 cells,  8 of which had exhibited low pressure on one or 
two prior -roc overcharge tes t s  and 13 ce l l s  given reversal 
f o r  5 AH without a prior "Open cell" overcharge. Of the 8 
ce l l s  with ear l ier  low pressure characteristics, 6 stayed 
wi th in  200 PSI; of the cel ls  subjected t o  reversal, only 2 
of 13 showed low presaure. 
preceding vented overcharge, is not helpful. 
This t e s t  was run for  134 huurs 
Apparently, reversal, without a 
C* Cell Voltage and Pressure on -5' Overcharze. Since voltage 
measurements are made much more easily than c e l l  pressure 
measurements, it was hoped, and expected, that  rather close 
correlation would be found between them, Previous work had 
indicated that low pressure would be associated with volt- 
ages of 1.52 t o  1.55, with the voltage becoming lower with 
longer periods of overcharge. Unfortunately, t h i s  is not 
the case, a t  l ea s t  for  these cells. In  the Appendix t o  
th i s  report, we have summarized, on pages A-1, A-2, and 
A-3, the results of the four l a ten t  overcharge testa, 
. 
D. Pressure Characteristics i n  Early Stages Of -5' Overcharge Test. 
We a l s o  examined the data with a view t o  determining whether 
some forecast cuuld be made af te r  shorter periods of charge, 
8.8.) 20 or 40 hours, about behavior on the full 120 hour 
charge 
1. 
2. 
Pressure Decey. 
c i rcu i t  was determined af te r  the ce l l s  of the 8/1 through 
8/5 t e s t s  had exceeded 200 PSI or af te r  the end of the 94 
hour t e s t  showed very good correlation - - those tha t  
exceeded 40% were the ce l l s  that  remained below 200 PSI. 
In the following test ,  of 8/10 through 8/16, the charge 
vas interrupted several times and the pressure decay 
ra te  determined, the  low pressurett and the "high pressure" 
cells did not show sharply different behavior. 
that  th i s  method is not promising enough t o  warrant fur- 
ther work. 
the Appendix. 
Pressure a t  Early Stapes. 
four overcharges a t  -5OC which are given i n  summary form 
on pages A-6 and A-7 of the Appendix and find that the 
behavior can be predicted from the pressure a t  40 hours 
charge. If 170 PSI is taken as the criterion, no "low 
pressure" cells would be rejected and 8,!$ of the "high 
presmre" ce l l s  were above 170 PSI a t  40 hours. 
The pressure drop i n  one hour on open 
We fee l  
The data are given on pages A-4 and A-5 of 
We studied the results of 
E. Voltage During Reversal. The data on voltage during the 
"reversal" or ttoverdischargett was reviewed and summaries 
are included i n  the Appendix as pages A-8, A-9 and A-10, 
f o r  the three l a s t  overcharges. Three types of behavior 
took place: 
direction) slowly to-0.24. to-0.39 within the 5 ampere hours; 
the voltage became more negative a t  first and later became 
less negative (e ,g .  - 0.24 volts a t  
the voltage continued t o  r i s e  (in a negative 
AH and -0.18 at 5 AH); 
PORTABLE POWER FOR PROGRESS 
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or the voltage became more negative than -0.40 volt  bafore 
5 ampere hours of reversal. 
l i t t l e  correlation wi th  overcharge characteristics vas found. 
Except f o r  the third type, 
In  the  f i r s t  group where the voltage slow* became more neg- 
ative, 9 cella &owed t l l o ~ t l  ( eas than 200 PSI) pressure on 
subsequent -5OC overcharge and 7 ce l l s  hhow6d "highf1 pressure. 
In  the second group, where the voltage became more negative 
and later lee8 negative on reveraal 3 cells were t l l o ~ n  and 
3 were "high" pressure i n  the next -5OC overcharge. 
In the th i rd  group there were 9 ce l l s  which were more neg- 
ative than -0.40 vol t  before 5 ampere hour on reversal and 
they all gave "high" pressure on -5OC overcharges. 
Amount of Electrolyte. 
Battery Research Laboratory in which the effect of electrolyte 
contents of 13 t o  21% (based on the weight of the plate-sepa- 
rator assembly) on capacity a t  several rates of discharge and 
temperatures, overcharges for  extended periods and charge reten- 
tion is being studied. Our S-lO3 ce l l s  are being used, assembled 
with plates of the I s i s  type. 
A t e s t  i s  nearing completion in  the 
Reduction of Carbonate i n  Cell Electrolyte. 
was conditioned several tbesduring the course of c e l l  tests.  
From the data, summarized on page A-ll of the Appendix, it 
appears t h a t  the potassium carbonate can be reduced t o  3 
percent by weight in three conditioning operations. 
The electrolyte 
VI. MEETINGS: 
Promess vas reviewed with Mr. W. E. Threinen in weekly telephone 
ca l i s  and during a v i s i t  t o  Elmsford on August 21. 
- 
VII. SCKEDULE: 
We have prepared a delivery schedule for  Item 2 ce l l s  which appears 
on the next page, 
5% yield for  a ttscreening*l t e s t  which consists of the 40 hours, 
-5OC overcharge t e s t  mentioned in Section V D2; and 8G% yield 
for the Acceptance Test. With normal operations, both assembly 
and tes t ,  and l i t t l e  o r  no allowance for conflicts between t e s t s  
or for  unforeseen delays, we expect that the t e s t s  w i l l  be fin- 
ished by November 17. 
work on weekends which w i l l  move the completion date forward to 
November 10. There are technical people avallable for one extra 
day of t e s t  each week duringthe period September 15 t o  November 
15. I t  is not l ikely that  we can expect t o  extend t h i s  to a 
seven dsy week and move the date forward t o  November 3. 
This is based on 90% yield i n  c e l l  assembly; 
We have made arrangements f o r  overtime 
The data presented i n  section V D2 show t h a t  the screening t e s t  
can be done i n  40 hours instead of 120 hours as was stated i n  
our last report. 
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We propose tha t  consideration be given t o  t h e  following 
modifications in the t e s t  procedure so that the work can 
be completed within the scheduled time: 
A, 
B, 
C. 
Rcmoval of the requirement for pressure readings 
during the charge-discharge cycles when t h e  equip- 
msnt is  needed for "overcharge" or  l'screanin@# tcots  
which are proceeding simultaneously, We find that 
tho prebmre during a n6-d charge of 12 to 13 
hours i a  invariably very low, rarely more than 50 
PSI. 
Increase of the 100 PSI pressure during the 120 hour 
overcharge a t  -5OC t o  200 PSI, 
i n  t h e  Appendix indicate tha t  pressures often become 
constant or increase very slowly in the region of 
130 t o  180 PSI, 
Decrease of the time for the -5OC overcharge t e s t  
from 120 hours to 40 hours. Section V 02 and A p  
pendix pages A-6 and A-7 show that, in most casea, 
high pressure is ovidenced within 4.0 hours of charge. 
The data presented 
George A, Baumstark 
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Procurement and development program for nickel-cadmium cells to specification s-615-p-2 Technical status report no. 12, May 25 - Aug. 26, 1966

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