The Tensile and Shear Properties of Several Solders at Cryogenic Temperatures

J. L. Christian Senior Engineering Metallurgist

and

J. F. Watson Staff Scientist

General Dynamics/Astronautics
A Division of General Dynamics Corporation

The T e n s i l e a n d S h e a r P r o p e r t i e s of S e v e r a l S o l d e r s a t Cryogenic T e m p e r a t u r e s

by
J. L. C h r i s t i a n 8r J . F , Watson

Abstract The t e n s i l e and s h e a r p r o p e r t i e s of e i g h t s o f t s o l d e r s were d e t e r m i n e d a t s e v e r a l l o a d i n p r a t e s a t 7 8 O , -100'.

-320'

and -423'F.

I t w a s found t h a t , i n g e n e r a l , t h e t e n s i l e and s h e a r s t r e n a t h s increased

w i t h i n c r e a s e i n loadinr?: r a t e and d e c r e a s e i n temperature.
Large

d e c r e a s e s i n d u c t i l i t y , a s measured by e l o n g a t i o n and r e d u c t i o n i n a r e a , and d e c r e a s e d t e n s i l e and s h e a r s t r e n g t h s f o r some of t h e solders

a t c r y o g e n i c t e m p e r a t u r e s are i n d i c a t i v e of t h e i r low t e m p e r a t u r e
embrittlement.
A d i s c u s s i o n of t h e e x p e r i m e n t a l d a t a and l i t e r a t u r e

v a l u e s is g i v e n a n d recommendations are made c o n c e r n i n < t h e a i l p l i c a t i o n

of s o l d e r s f o r c r y o g e n i c s e r v i c e .

- 1-

I _. NTRODUCT I ON

I _I -

T h e r e have b e e n a few i n v e s t i g a t i o n s on t h e m e c h a n i c a l p r o p e r t i e s o f s o f t s o l d e r s a t c r y o g e n i c teiiiperatrires (Kef. 1 - 4 ) ; however t h e imrlcity o f t h e l i t e r a t u r e d a t a and t h e need f o r c e r t a i n d a t a which were n o t a v a i l a b l e prompted t h i s i n v e s t i u a t i o n . A d d i t i o n a l d a t a were needed f o r

t h e d e s i g n of e l e c t r o n i c components, s e v e r a l i t e m s of plumbing hardware a n d e v e n for s t r u c t u r a l a p p l i c a t i o n s i n c r y o g e n i c t a n k a n e f o r m i 4 s i l e . s and space c r a f t . These d a t a i n c l u d e d s h e a r s t r e n g t h and t e n s i l e p r o p e r t i e s A l s o , a few a l l o y s were t e s t e d

a t v a r i o u s s t r a i n r a t e s and t e m p e r a t u r e s .

f o r which no p r e v i o u s d a t a a t c r y o g e n i c t e m p e r a t u r e s e x i s t e d . The s o l d e r s t e s t e d i n t h i s i n v e s t i g a t i o n were a l l l e a d - or t i n - b a s e alloys. Because o f t h e e m b r i t t l e m e n t o f p u r e t i n a n d h i g h t i n , t i n - l e a d

a l l o y s a t low t e m p e r t u r e s

e m p h a s i s w a s p l a c e d upon e v a l u a t i n g t h o s e

s o l d e r s which c o n t a i n e d l a r g e amounts of l e a d which i s known t o have Rood d u c t i l i t y a t c r y o ~ e n i ct e m p e r a t i i r e s . Three s o l d e r s having high t i n

c o n t e n t s were i n c l u d e d i n t h e program b e c a u s e t h e y had been r e p o r t e d as h a v i n g s a t i s f a c t o r y low t e m p e r a t u r e p r o p e r t i e s .

I t is d e s i r a b l e t o e v a l u a t e a m a t e r i a l a s i t is a c t u a l l y u s e d i n a
component. However, t h e c o m p l e x i t y and s i z e o f t h e procram f o r e v a l u a t i n l r

many s o l d e r s a s a f u n c t i o n of s t r a i n r a t e and t e m p e r a t l i r e became o v e r whelming when o t h e r p a r a m e t e r s s u c h a s t h e many v a r i a b l e s i n v o l v e d i n s o l d e r i n g a p p l i c a t i o n s , f l u x e s , t y p e a n d c o n d i t i o n of m a t e r i a l s b e i n g s o l d e r e d , s o l d e r g a p , e t c . were added. T h e r e f o r e , this i n v e s t i g a t i o n

w a s l i m i t e d t o t h e e v a l u a t i o n of t h e p r o p e r t i e s of t h e b a s i c s o l d e r s .
The o b j e c t of t h i s f)rouram, t h e n , w a s t o p r o v i d e d a t a on t h e m e c h a n i c a l p r o p e r t i e s of s e v e r a l s o l d e r s f o r t h e p u r p o s e o f s e l e c t i n g t h e b e s t s o l d e r f o r a p p l i c a t i o n s a t room and c r y o g e n i c t e m p e r a t u r e s .

-2-

MATERIALS AND -I

-- -PROCEDURE
10%-9OPb;

The s o l d e r s t e s t e d in t h i s i n v e e t i r a t i o n i n c l u d e : 20Sn-80Ph; 95Sn-5Sb; 30%-70Pb; 60Sn-40Pb; lSn-97.5Ph-l.SAg;

45Sn-32Pb-18Cd-5Bi;

and 6OSn-36Pb-4Ag.

The t r a d e n a m e s and chemical compositionfi

are g i v e n i n T a b l e 1.

F i v e of t h e s o l d e r s a r e l i s t e d u n d e r F e d e r a l

S p e c i f i c a t i o n QQ-S-571c, and t h e s e s o l d e r s m e t t h e c h e m i c a l c o m p o s i t i o n r e q u i r e m e n t s of t h a t s p e c i f i c a t i o n . The s o l d e r s were t e s t e d i n t h e a s - r e c e i v e d c o n d i t i o n i n t h e form of 16 gauKe (0.063 i n c h d i a m e t e r ) w i r e . T e s t s p e c i m e n s were made s i m p l y T n n s i l e and

b y s h e a r i n g one t o t h r e e i n c h long p i e c e s o f t h e s o l d e r .

s h e a r ( d o u b l e s h e a r ) t e s t s were performed on s t a n d a r d u n i v e r s a l t e s t i n n machines, The t e s t f i x t u r e s used f o r g r i p p i n g t h e specimens durin,q Elonaations reported are total eloncatione

t e s t i n g a r e shown i n F i g u r e 1.

a s measured o v e r a one i n c h aauge l e n g t h which w a s marked by means o f a

dye and gauge b l o c k . R e d u c t i o n i n area measurements were d e t e r m i n e d by T e n s i l e and
by

use of a f i l a r e y e - p i e c e and m e t a l l u r g i c a l m i c r o s c o p e s .

s h e a r t e s t s w e r e performed a t 78'F

(room t e m p e r a t u r e ) , a t -100'F

immersion i n a b a t h of d r y i c e and a l c o h o l , a t -320'F l i q u i d n i t r o g e n and a t -423'F

by immersion i n A full

by immersion i n l i q u i d hydrogen.

d e s c r i p t i o n o f t h e t e s t i n g a p p a r a t u s and e x p e r i m e n t a l p r o c e d u r e i s r i v e n i n r e f e r e n c e 5. The t e s t s a t c r y o g e n i c t e m p e r a t u r e s were performed a s

soon a s t h e specimen had r e a c h e d e q u i l i h r i u m t e m p e r a t u r e , as measured

b y t h e r m o c o u p l e s ; t h e r e f o r e , a r e c o n s i d e r e d " s h o r t t i m e " e x p o s u r e tests.

EXPERIMENTAL RESULTS T a b l e 1 g i v e s t h e c h e m i c a l c o m p o s i t i o n of t h e s o l d e r s t e s t e d . The

a w

t e n s i l e a n d s h e a r p r o p e r t i e s a t 78'. i n T a b l e 11.

-looo,

-320'

and -423'F

are given

The s h e a r s t r e n g t h s ( o b t a i n e d i n d o u b l e s h e a r b u t r e p o r t e d

as s i n g l e s h e a r ) a n d t e n s i l e p r o p e r t j e s a r e Riven f o r t h r e e d i f f e r e n t
-3-

l o a d i n g rates:

0.1, 1.0 and 10 i n c h e s / m i n u t e .

The v a l u e s r e p o r t e d i n

T a b l e I1 a r e a v e r a g e s of a t l e a s t two, and g e n e r a l l y f i v e , r e p l i c a t e

tests.

P h o t o g r a p h s of t y p i c a l t e n s i l e f r a c t u r e s a r e shown i n F i g u r e 2 .

These c l e a r l y i l l u s t r a t e t h e e f f e c t of t e s t i n g t e m p e r a t u r e on t h e e l o n g a t i o n s and r e d u c t i o n i n area.

DISCUSSION OF RESULTS The most n o t i c e a b l e r e s u l t s of t h e t e s t ( T a b l e 2) a r e t h e l a r g e d i f f e r e n c e s i n t e n s i l e a n d s h e a r s t r e n g t h s a s a f u n c t i o n of t e s t temperat u r e and l o a d i n g rate. The t i n - l e a d s o l d e r s are a p p a r e n t l y v e r y s t r a i n and t o a l e s s e r e x t e n t a t

r a t e s e n s i t i v e , p a r t i c u l a r l y so a t 7' 8F
cryogenic temperatures. i n s t r e n g t h a t 7' 8F minute t o 10 in./min.

The s o l d e r s e x p e r i e n c e d a 20 t o 80% i n c r e a s e

upon i n c r e a s i n g t h e l o a d i n g r a t e from 0.1 i n c h e s / The i m p o r t a n c e of t h i s t y p e of d a t a c a n be

r e a d i l y u n d e r s t o o d s i n c e l o a d i n g r a t e s may v a r y from v e r y low t o impact c o n d i t i o n s d e p e n d i n g upon t h e s e r v i c e a p p l i c a t i o n . To t h e a u t h o r s '

knowledge t h e s t r a i n r a t e s e n s i t i v i t y of commercial s o f t s o l d e r s h a s n o t been p r e v i o u s l y r e p o r t e d . I n o r d e r t o b e t t e r d e t e r m i n e t h e e x t e n t of t h e s t r a i n r a t e s e n s i t i v i t y of t h e s o f t s o l d e r s , a few tests were made on t h e 95Sn-5Sb ( S b - 5 ) s o l d e r a t l o a d i n g r a t e s o f 0.01 in./min. s t r e n g t h of 2620 p s i a t 7' 8F T h i s s o l d e r had a t e n s i l e Compared

when l o a d e d a t 0.01 in./min.

w i t h t h e d a t a i n T a b l e 2, i t may b e s e e n t h a t t h e t e n s i l e s t r e n g t t i o f t h e Sb-5 s o l d e r a t 7' 8F i n c r e a s e d by 165% upon i n c r e a s i n g t h e l o a d i n g

r a t e from 0.01 t o 10 in./min. The e x p l a n a t i o n o f a m a t e r i a l ' s s e n s i t i v i t y t o s t r a i n r a t e g e n e r a l l y i n v o l v e s a d i f f u s i o n mechanism. T h e r e d o e s n o t a p p e a r t o b e any c l e a r l y

-4-

d e f i n e d dependency of t h e m o u n t of s t r a i n rate a e n a i t i v i t y of t h e s o l d e r s

upon t h e i r c h e r i e t r i e 8 .

However, t h e d e c r e a a e in s t r a i n r a t e s e n s i t i v i t y

w i t h d e c r e a s e i n t e s t i n g t e m p e r a t u r e is i n d i c a t i v e t h a t d i f f u s i o n ia r e s p o n s i b l e f o r t h e e o f t s o l d e r s ' s t r e n g t h dependency upon l o a d i n g rate.

A s would be expecte'd, t h e t e n s i l e and a h e a r s t r e n g t h increase w i t h

decrease i n t e s t i n g temperature, The t e n s i l e and s h e a r s t r e n g t h s , a t a c o n s t a n t l o a d i n g rate, of t h e t i n - l e a d s o l d e r s is d e p e n d e n t upon t h e amount' of t i n p r e s e n t . The depen-

dency of t h e s t r e n g t h upon t h e t i n c o n t e n t is s m a l l as compared t o its dependency upon l o a d i n g rate, p a r t i c u l a r l y a t 78OF; however, of t h e Sn-Pb a l l o y 6 (e.g.

10/90, 20/80, 30/70 and 60/40)

t h e o n e s c o n t a i n i n g t h e most

t i n are t h e s t r o n g e s t .

It i s a l s o q u i t e a p p a r e n t t h a t t h e t e n s i l e and

s h e a r s t r e n g t h are d e p e n d e n t upon t h e p r e s e n c e of o t h e r e l e m e n t s s i n c e t h o s e a l l o y s c o n t a i n i n g large amounts of A g , Cd, B i and Sb are s t r o n g e r

t h a n t h o s e s o l d e r s c o n t a i n i n g p r i m a r i l y Sn and Pb.

The s t r o n g e s t s o l d e r

is C l a u d e M i c h a e l ' s #275 which c o n t a i n s l a r g e amounts of Cd and B i .

A l s o , i t a p p e a r s t h a t t h e s t r e n g t h of l e a d b a s e a l l o y 8 is a p p r e c i a b l y i n c r e a s e d by s i l v e r , i n amounts a s s m a l l as l.5%, s i n c e t h e s t r e n g t h of C l a u d e M i c h a e l ' s #20 (lSn-97.5Pb-1.5Ag)

is g r e a t e r t h a n t h a t of t h e

Sn-Pb s o l d e r s c o n t a i n i n g as much as 30-6046 Sn. I n comparing t h e s t r e n g t h d a t a o b t a i n e d i n t h i s i n v e s t i g a t i o n w i t h t h a t r e p o r t e d i n t h e l i t e r a t u r e on s o f t s o l d e r s , t h e r e a r e s e v e r a l p o e s i b l e discrepancies.

For example, Kaufman (Ref. 4 ) r e p o r t s t h e t e n s i l e

s t r e n g t h of Claude-Michaels #20 as 3,600 p s i a t 80F and 9,OOO p s i a t

-320OF; and C l a u d e - M i c h a e l s #273 as 8,750 p s i a t 80. and 7925 p e i a t -320OF.

The r c a a o n f o r t h e s e , a s w e l l as s e v e r a l o t h e r d i s c r e p a n c i e s w i t h l i t e r a t u r e d a t a , i s b e l i e v e d t o be p r i m a r i l y d u e t o t h e s t r a i n r a t e s e n s i t i v i t y , Much of

-5-

the literature data does not include the strain rates or loading rates and thus inhibits direct comparisons. Although commercial solders were

not tested in the investigation by Jaffee, et a1 (Ref. 3 ) , the tensile data (obtained at a loading rate of 0.06 in./min.) on alloys similar to

those tested in this investigation compare more favorably. The ductility of many of the soft solders is severely affected by the testing temperature. "Ductilitp, as discussed herein, is the

ability of the material to plastically deform prior to fracturing, and is measured by elongation and reduction in area. All of the solders

tested have adequate ductility at 78' and -100'F; however, the ductility of many of the solders sharply decreases from -looo to - 2 ' . 30F The

photographs of typical tensile failures as shown in Figure 2 clearly illustrate the effect of testing temperature on the ductility of several of the soft solders. Although the minimum amount of ductility required

for satisfactory performance is dependent upon the particular application, it is recommended that soft solders have a minimum of about 10% total elongation and 3046 reduction in area for structural type applications. The toughness of many soft solders is also severely affected by the testing temperature. "Toughness is defined as the ability of a The best test to determine a material's

material to resist brittle failure.

toughness is the low temperature impact test since this test involves a high strain rate, a stress concentration and low temperature, all of which promote brittle failure. of determining toughness. There are, however, several other methods

The methods ueed in this investigation include

an analysis of the tensile fractures to determine the amount of plastic deformation as compared to the amount of brittle cleavage failure; an analysis of the tensile strength data as a function of increasing loading
-6-

.
rates and decreasing temperature (in some cases the strength decreased

instead of increased which is indicative of embrittlement); and primarily, an analysis of the shear strengths at high loading rates and low temperatures. It is believed that the high loading rate, low temperature shear The stress concentration is imposed

tests simulate the impact test.

by the relatively sharp edges of the shear testing fixture.

It is

therefore believed that this test is quite severe since there was a decrease in shear strength at the high loading rates for 60/40, # 2 7 5 , Sb-5

10F and 604-Ag solders at - 0 '

whereas the ductility and failure appearances However, at -320'F each of these solders

do not indicate embrittlement.

lacked toughness and ductility and therefore are not recommended for structural use at -320'F or below. Shear tests at -320'F indicate severe

embrittlement of these solders as well as possible embrittlement of the

30/70 solder.

Analysis of the test results and fractured edges of broken

tensile specimens definitely indicate a lack of toughness of t h e 60/40,

#275, Sb-5 and 6 0 4 A g solders at -320'F
30/70 at -423'F.

and of the same solders as well as

These results are not surprising since those solders contained primarily lead.

which remained tough and ductile t o -423'F

It is recommended that only those Sn-Pb solders containing 70% or more

lead be used for critical applications at -320'F. for use at -423'F, and 80% or
more

lead

SUMMARY
The tensile and shear properties were determined on several soft solders at 7 ' , -looo, -320' and -423'F. 8F From the results obtained

in this investigation the following conclusions and recommendations are made ;

-7-

1.

The s o f t s o l d e r s t e s t e d i n t h i s i n v e s t i g a t i o n a r e s t r a i n r a t e sensitive;

v e r y much so a t room t e m p e r a t u r e and t o a lesser e x t e n t a t c r y o g e n i c temperatures. The amount o f s t r a i n r a t e s e n s i t i v i t y d o e s n o t a p p e a r t o

b e d e p e n d e n t upon t h e l e a d or t i n c o n t e n t . 2. I n g e n e r a l , t h e t e n s i l e a n d s h e a r s t r e n g t h s of s o f t s o l d e r s i n c r e a s e

w i t h i n c r e a s e i n l o a d i n g r a t e and decrease i n t e m p e r a t u r e .
3.

The t e n s i l e a n d s h e a r s t r e n g t h s of t h e Pb-Sn s o l d e r s a r e d i r e c t l y

proportional t o the t i n content. 4.

A d e c r e a s e i n t h e t e n s i l e or s h e a r s t r e n g t h w i t h r e d u c t i o n i n t e m p e r a -

t u r e and i n c r e a s e i n l o a d i n g r a t e is b e l i e v e d t o b e i n d i c a t i v e o f e m b r i t tlement.

A s h a r p d e c r e a s e i n t h e d u c t i l i t y is a l s o i n d i c a t i v e of low

temperature embrittlement.
5.

The low t e m p e r a t u r e e m b r i t t l e m e n t of Pb-Sn s o l d e r s is d e p e n d e n t upon The s o l d e r c o n t a i n i n g t h e l a r g e s t amounts of t i n a r e

t h e t i n content.

t h e most b r i t t l e a t a n y g i v e n c r y o g e n i c t e m p e r a t u r e .
6.

Hased upon t h e t e n s i l e and s h e a r s t r e n g t h s and d u c t i l i t y d a t a t h e

f o l l o w i n g recommendations are made:

a.) A l l of t h e s o l d e r s t e s t e d i n t h i s i n v e s t i g a t i o n a r e s u f f i c i e n t l y

tough f o r u s e a t 78' and -100'F. b.) The f o l l o w i n g s o l d e r s a r e s u f f i c i e n t l y t o u g h f o r u s e a t -320'F: 10Sn-9OPb; 20Sn-80Pb;

c.)

lSn-97.5Pb-1.5Ag.

The f o l l o w i n g s o l d e r s a r e s u f f i c i e n t l y t o u g h f o r u s e a t -423'F: 10Sn-9OPb; lSn-97.5Pb-1.5Ag.

ACKNOWLEDGEMENTS The a u t h o r s w i s h t o acknowledge t h e a s s i s t a n c e of t h e i r a s s o c i a t e s

who c o n t r i b u t e d t o t h i s p a p e r a n d , i n p a r t i c u l a r , t o A.

H u r l i c h , who

-8-

. .
supplied technical counsel throughout the course of this investigation.

The solders were supplied by Claude-Michael, Inc.

The work was performed

under the sponsorship of General Dynamics/Astronautics, whose permission to publish this paper is gratefully acknowledged.

-9-

.
UFERENCES
1 . Kostenete, V 1 .. and Ivanchenko, A.M., "Mechanical Properties of

Metals and Alloys in Tension at Low Temperatures (-196 and -253.C.). Part IV

- Solders,"

Journal of Technical Physics ( U S S R ) , Vole 16,

NO. 5 , 1946.
2 .
Kalish, H S and Dunkerly, F.J., .. "The Low Temperature Properties of

Tin and Tin-Lead Alloys1q, Metals Technology, Vol. 13, No. 6, September 1948
3 .

Jaffee, R.I.,

Minarcik, E.J.

and Gonser, B W , ..

"Low-Temperature

Properties of Lead-Base Solder6 and Soldered Joints", Metal Progress, December 1948. 4 . Kaufman, A B , .. Welecting Solders for Low Temperature Service",

Materials in Design Engineering, November 1958.

5 .

Watson, J.F.

and Christian, J.L.,

"Cryostat and AcCesSOrie6 for Tension

Testing at -423OF", Materials Heeearch and Standards, Vol. 1, No. 2, February 1961

rl

I
i

I I

v,
U
01)

a
I I

v
I
I

d
I I

I I

a0

e
M

I I

~
I

rl

I I

0
e

v
I
I

0
M

v
I I I I

I I

M
I I 1 I 0

I I

v
I

k Q, a

0 9 ,
4

cu
3
I I I I

s
d O

I I

0
IO

d 0

\J
v)

0 V
d

cn

I I

0
b

v cu
0

d
01

I I

a
V

0
V
0

rc

I9
4

v
Q,

v
rl

I I

cu

0 V
Q,

u,
co
0
CD

I I

b
d

c u r l
V

cs'o
I9

. o.
b

G
v)

8
d
rl rl

. .
0
4

d
d

rc O *
3

M
e

.
r-0
C

Q,

4 Q

rl

.
e
M

0 07

Ip

cp

P
b

4 a0
Q,

rc

Q,

Q
Q,

v)

.
I

10

0 10

a
0

v)

co

cu

r/l

0
\

OD

2
1 1 1

e O 0

e n cp
1

w 0

I P

" 0 4
O O

l W

l W

m a 3 0

0 0 0

0 4 a

O
W

0 0 0

b
cp

N a o
O

Q
C

P
C

1 r, w.
cp

0 0 0

ocnco

r n
0 cr,

o o c

v,
0
I

N U l N

cl,

r,

v,
0
cp

n
1

8 8 0 0

oco

I U W Q Q ,

O N C I C D

0 0 0 0

e m m M

8 S 8 8
L C L C

e
8 8 8M5 d : m N
L L L L

M m a D M

d ' Q P o b

0 0 0 0 a 0 4 0 0 OOaQe

0 0 0 0

m 4 Y ) a

e o 0 0

0 0 0 0

ePocr>o

0 0 0 0

4 e e *
L C C

b o o 0

l n n o aaolo

N M r l

e e o
b P o

0 0 0
P o 0 3

m o o a m a

0 0 0

0 0 0 0 0 0
0 e a D
C C

< l o o
4

c J Q b O N u )

8o 8a 8 c8 b l o o

Q Q ,

0aDe

M
*

$ 8 8 4 a ,
L

0 0 0

e a 4

0 0 a Q ,8 0 N O

e 4 3 4 M

* 3 e

0'

. .
L

b,

c
cp 0
C

G l o o m
lu l u a u
0 . 0

" 0 4

c o o 3 4

8 0 0

cow

J a
w

3 0 .

ID

Ig
Y

Fixture Used for T e n s i l e T e s t i n g of S o l d e r s

Fixture Used for Double Shear T e s t i n g o f S o l d e r s

Figure 1 .

T e s t Fixtures

b
x

1 Sn-97.3 Yb-1.5

A& (C-M #20) Solder 15X

LO Sn-90

Pb (10/80) Solder

1SX

Figure 2 .

Photographs of Typical Tensile Fractures

^.

I .

78%

-1ooOF

-32OoF
L

60 Sn-40 Yb (60/40)

Solder

15X

-3 2ooF
.

_.._

95 Sn-5 Sb (Sb-5)

Solder

15X

Figure 2, Photographs cf T y p i c a l Tensile Fractures (conto)