design, development, and fabrication of a functional ... · cation in the space adhesive bonding...

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WHITTAKER CORPORATION Narmco Research & Development Division Advanced Composites Engineering Department 3540 Aero Court San Diego, California 92123 DESIGN, DEVELOPMENT, AND FABRICATION OF A FUNCTIONAL ADHESIVE BONDING REPAIR EXPERIMENT TO BE PERFORMED DURING SPACE FLIGHT (Covering Period November 1966 through May 1968) S. Feher, Author Final Report Contract No. NAS-8-20677 Control No. 1-7-30-12604-Sl(lF) PO June 1968 FSTl Hard copy (WC) I _PI ff 653 July 65 Prepared for GEORGE C. MARSHALL SPACE FLIGHT CENTER Huntsville, Alabama 35812 13 P I & =! 3 (NASA CR OR TMX OR AD NUMBER) https://ntrs.nasa.gov/search.jsp?R=19680028429 2020-03-27T16:36:38+00:00Z

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Page 1: DESIGN, DEVELOPMENT, AND FABRICATION OF A FUNCTIONAL ... · cation in the space adhesive bonding repair experiment. systems are suitable for application in the zero-g, hard vacuum

WHITTAKER CORPORATION Narmco Research & Development Div i s ion

Advanced Composites Engineering Department 3540 Aero Court

San Diego, C a l i f o r n i a 92123

DESIGN, DEVELOPMENT, AND FABRICATION O F A FUNCTIONAL ADHESIVE BONDING REPAIR EXPERIMENT

TO BE PERFORMED DURING SPACE FLIGHT

(Covering Period November 1966 through May 1968)

S . Feher, Author

F i n a l Report Contract No. NAS-8-20677

Control No. 1-7-30-12604-Sl(lF)

PO June 1968

FSTl

Hard copy (WC) I _PI

ff 653 July 65

Prepared f o r GEORGE C. MARSHALL SPACE FLIGHT CENTER

H u n t s v i l l e , Alabama 35812

13 P I &

=! 3 (NASA CR OR TMX OR AD NUMBER)

https://ntrs.nasa.gov/search.jsp?R=19680028429 2020-03-27T16:36:38+00:00Z

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Three s p e c i a l l y formulated adhesive systems were developed f o r a p p l i - c a t i o n i n t h e space adhesive bonding r e p a i r experiment. systems are s u i t a b l e f o r a p p l i c a t i o n i n t h e zero-g, hard vacuum space en- vironment over a temperature range from 30°F t o 130"F, y i e l d i n g t e n s i l e shea r s t r e n g t h s i n excess of 1000 p s i .

The t h r e e adhesive

A s u i t a b l e adhesive package, d i s p e n s e r , and vacuum glove box were de- veloped t o c a r r y o u t t h e adhesive bonding r e p a i r experiment i n t h e S I V - B Work Shop.

iii

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*

TABLE OF CONTENTS

INTRODUCTION . . . . . . . . . . . . . . . . . . . . . . . . . . . 1

TECHNICAL DISCUSSION . . . . . . . . . . . . . . . . . . . . . . . 2

Adhesive Development . . . . . . . . . . . . . . . . . . . . . . . 2

Adhesive Formulations . . . . . . . . . . . . . . . . . . . . . . 2

Experimental Evalua t ion . . . . . . . . . . . . . . . . . . . . . 3

Adhesive Package . . . . . . . . . . . . . . . . . . . . . . . . . 11

Adhesive Dispenser and Glove Box Development . . . . . . . . . . . 11

Adhesive Dispenser . . . . . . . . . . . . . . . . . . . . . 11

G l o v e B o x . . . . . . . . . . . . . . . . . . . . . . . . . . 12

Proof P res su re and Leakage Test . . . . . . . . . . . . . . . . . 15

CONCLUSIONS AND RECOMMENDATIONS . . . . . . . . . . . . . . . . . 16

V

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LIST OF ILLUSTRATIONS

Figure

1

2

6

7

8

9

10

T e n s i l e Shear S t r eng th ve r sus Aging Time

T e n s i l e Shear S t r eng th ve r sus Aging Time

T e n s i l e Shear S t r eng th ve r sus Aging T i m e

Tens i l e Shear S t r eng th ve r sus Aging T i m e

T e n s i l e Shear S t r eng th versus Aging Time f o r Adhesive System B S e t and Aged a t

Epoxy Aluminum Tens i l e Shear S t r eng th ve r sus Exposure T ime of S i l i c o n Car- b i d e Abraded Aluminum Exposed t o A i r

f o r Adhesive System A . . . . . . . . . . . . . . . . . . 7

f o r Adhesive System B . . . . . . . . . . . . . . . . . .

(100'F t o 150°F) f o r Adhesive System C . . . . . . . . .

€or Adhesive System C . . . . . . . . . . . . . . . . . . 9

8

8

1 0 0 ° F . . . . . . . . . . . . . . . . . . . . . . . . . . 10

a t 20% Oxygen and 50% R e l a t i v e Humidity . . . . . . . . . 10

Exploded View o f Adhesive Dispenser . . . . . . . . . . . €1

Welded Sheet Metal Frame and P a r t i a l l y Assembled Glove Box . . . . . . . . . . . . . . . . . . . 13

Glove Box wi th T e n s i l e Test Unit . . . . . . . . . . . . € 4

Complete Experiment System . . . . . . . . . . . . . . . 14

v i

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INTRODUCTION

Adhesive bonding has found wide acceptance i n t h e aerospace indus t ry as an e f f i c i e n t method f o r j o i n i n g va r ious components ranging from p r i - mary s t r u c t u r a l members t o d e c o r a t i v e w a l l pane l s . Adhesive bonding o f f e r s unique p o t e n t i a l f o r a p p l i c a t i o n i n a c t u a l i n f l i g h t repair o f damaged space v e h i c l e s . With the u t i l i z a t i o n of s u i t a b l e adhesives , very compact and w e i g h t - e f f i c i e n t r e p a i r k i t s could be developed f o r pa t ch ing up micormeteoride impact craters i n the s k i n of a space v e h i c l e , f o r example. Bonded j o i n t s could a l s o be u t i l i z e d f o r in-space assembly of l a r g e s t r u c t u r e s r e q u i r i n g minimum t o o l i n g . Adhesive-bonded c l i p s o r b racke t s on t h e e x t e r n a l s u r f a c e o f the v e h i c l e could g r e a t l y improve t h e mob i l i t y and s e c u r i t y of an a s t r o n a u t du r ing e x t r a v e h i c u l a r a c t i v i t y .

A l l t he se p o t e n t i a l a p p l i c a t i o n s depend on the s u c c e s s f u l demonstra- t i o n t h a t s p e c i a l l y formulated adhesives are s u i t a b l e f o r bonding i n an a c t u a l space environment a t zero-g and hard vacuum, over a wide range of temperatures . It was t h e purpose of t h i s program t o develop adhesive sys - tems t h a t could be u t i l i z e d under t h e s e cond i t ions and would y i e l d u s e f u l mechanical p r o p e r t i e s .

The demonstration of t h e f e a s i b i l i t y of adhesive bonding under a c t u a l space environmental cond i t ions i s planned as one of t h e experiments i n t h e Saturn I V - B Work Shop program.

This experiment w i l l involve mixing of t h e two-part adhesive by t h e a s t r o n a u t and us ing i t t o bond t e n s i l e l a p shea r specimens. The specimens w i l l la ter be t e s t e d by t h e a s t r o n a u t , who w i l l u se a s m a l l hand-operated t e n s i l e t es t appa ra tus . The i n t e r i o r of t h e work shop i s planned t o be p re s su r i zed t o 5 p s i a . Thus, i n o r d e r t o conduct t h e bonding experiment under a c t u a l space environmental c o n d i t i o n s , a s p e c i a l l y designed vacuum chamber w i l l be u t i l i z e d . This chamber w i l l be vented t o the e x t e r i o r of t h e v e h i c l e . The a s t r o n a u t w i l l work i n t h i s chamber by means of f l e x i b l e arm i n s e r t s and gloves, as i n a convent ional l a b o r a t o r y glove box.

1

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TECHNICAL DISCUSSION

The work under t h i s program w a s divided i n t o two major areas. The o b j e c t i v e of t he f i r s t p a r t of t h e program w a s t he development of adhe- s i v e systems s u i t a b l e f o r bonding r e p a i r a p p l i c a t i o n s i n space . This work w a s performed by t h e Polymer Chemistry Department of Narmco R&D. The second p a r t cons i s t ed of t h e des ign , f a b r i c a t i o n , and t e s t i n g of a vacuum chamber (glove box) and adhesive d i s p e n s e r , which were t h e respon- s i b i l i t y o f t h e Engineering Department.

ADHESIVE DEVELOPMENT

The goal of t he adhesive development e f f o r t w a s t o formulate an ad- hes ive system wi th a working t e m p e r a t u r e range from 30°F t o 130°F i n hard vacuum. Short c u r i n g c h a r a c t e r i s t i c s were a l s o considered d e s i r a b l e f o r f a c i l i t a t i n g quick r e p a i r ope ra t ion r e s u l t i n g i n bond shea r s t r e n g t h s of a t l e a s t a 1000 p s i w i t h i n a few hours a f t e r a p p l i c a t i o n .

ADHESIVE FORMULATIONS

Attempts t o s a t i s f y t h e requirements o f a s i n g l e space adhesive sys - t e m capable of being used between 30°F and 130°F l e d t o the conclusion t h a t such a system i s no t p r e s e n t l y a v a i l a b l e . Those systems which worked w e l l a t 130°F were s o l i d a t 30°F o r had inhe ren t low-temperature cu re times whose d u r a t i o n w a s p r o h i b i t i v e . Conversely, t hose systems which were usable a t 30°F degassed badly a t 130°F or se t up so f a s t t h a t they could no t be app 1 ied .

With t h e s e problems i n mind, t h r e e matched adhesive systems were formu- l a t e d . Each system a c t s i n e s s e n t i a l l y t h e same manner as t h e o t h e r s i n i t s own temperature range. Mixing and a p p l i c a t i o n must be completed w i t h i n 7 minutes, and c o n t a c t p r e s s u r e must be appl ied r a p i d l y and he ld 30 minutes from mix i n i t i a t i o n . The 1000-psi t e n s i l e shear s t r e n g t h l i m i t i s reached i n a l l cases w i t h i n 90 minutes from mix i n i t i a t i o n . There is a 5°F overlap i n the usab le temperature ranges o f t h e s e systems.

System A w i l l be used between 30°F and 77°F. According t o the l i t e r a - t u r e , t h i s system w i l l a l s o work a t 15"F, but r e q u i r e s a 3-day cure t o reach a s t r e n g t h l e v e l of 1000 p s i . System B w i l l be used between 72°F and 107°F. System C w i l l b e used between 102°F and 130°F. This l a t t e r system s t i l l has a usab le p o t l i f t and vapor p r e s s u r e a t 150°F.

The formulation chosen f o r adhesive System A i s :

1.00-g Epirez 5109 r e s i n 1.00-g Epicure 861 c u r i n g agent 1.00-g MD 105 aluminum f i l l e r

2

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The formulat ion chosen f o r adhesive System B is:

1.000-g Epon 828V r e s i n 0.353-g Genamid 2000 f a t t y amidoamine c u r i n g agent 0.758-g Epicure 861 polymercaptan c u r i n g agent 0.03-g Bisphenol A cu re c a t a l y s t 1.07-g ND 105 aluminum f i l l e r

The formulat ion chosen for adhesive System C i s :

1.000-g Epon 828V r e s i n 0.158-g Genamid 2000 f a t t y amidoamine c u r i n g agent 0.237-g S h e l l U polyamine c u r i n g agent 0.027-g Bisphenol A cu re c a t a l y s t 0.711-g MD 105 aluminum f i l l e r

The formulat ions of t h e adhesive systems were v a r i e d t o permit proper po t l i v e s and high t e n s i l e shea r s t r e n g t h a f t e r aging.

Adhesive System A i s b a s i c a l l y a 50/50 mixture of Epirez 5109 and E p i - c u r e 861. A-1100 p re t r ea tmen t of t he bonds d i d n o t i nc rease t h e t e n s i l e shear s t r e n g t h s apprec i ab ly upon aging.

Adhesive System B presented a problem i n t h a t t h e i n c r e a s e of Epicure 861 l ed t o weak bonds upon aging. The i n c r e a s e of Genamid 2000 increased the aged t e n s i l e shea r s t r e n g t h b u t slowed t h e r e a c t i o n t ime. This w a s compensated f o r by adding a c a t a l y t i c amount of Bisphenol A as an a c c e l e r - a t o r .

Adhesive System C a l s o r equ i r ed Bisphenol A due t o t h e a d d i t i o n of Genamid 2000.

The v a r i a t i o n s i n t h e po t l i v e s and the r e a c t i o n t i m e s of t h e s e adhe- s i v e systems wi th d i f f e r i n g concen t r a t ions of r e a c t a n t s can be found i n Table 1.

I n no c a s e was an at tempt made t o f ind a cu re c y c l e which would in- crease t h e t e n s i l e shea r s t r e n g t h . It w a s f e l t t h a t t h i s would be inap- p r o p r i a t e f o r space bonding due t o i t s added complicat ions.

EXPERIMENTAL EVALUATION

A l l bonds made were on s i l i c o n c a r b i d e abraded aluminum i n an at tempt t o d u p l i c a t e a c t u a l space bonding techniques. Eight bonds were made a t one t i m e and the t e s t i n g of t h e s e bonds w a s i n d u p l i c a t e f o r each elapsed time i n v e s t i g a t e d .

3

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A summary of t h e r e s u l t s of t h e experimental eva lua t ion of t he va r ious adhesive formulat ions i s presented i n Table 1. The r e s u l t s of aging s t u d i e s on the t h r e e s e l e c t e d systems are given i n Figures 1 through 3 . Af t e r aging f o r 13 days, 4 days a t 30°F and 9 days a t 75"F, System A had an average ten- s i l e shea r s t r e n g t h of 1180 p s i which d id no t show a d e c l i n e from a rerun aged 3 days g iv ing 1025 p s i i n t e n s i l e s h e a r .

A f t e r 1-day aging a t 100"F, System B gave a 1370-psi t e n s i l e shear s t r e n g t h va lue ; a f t e r 4 days, t h i s v a l u e increased t o 1570 p s i . There was no s i g n of d e c l i n e i n t h e bond s t r e n g t h .

.I4 VI a ,2000

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The shea r s t r e n g t h f o r System C a f t e r 1-day aging a t 150°F w a s 1260 p s i , a f t e r 4 days was 1220 p s i .

-

- -a--

Figure 1. Tens i l e Shear S t r eng th versus Aging T i m e f o r Adhesive System A. an average of two v a l u e s )

(Each d a t a p o i n t r ep resen t s

7

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0 30 90 15 0 1 4 8 12 16 20

(minutes) (days 1 Elapsed Time from Mix I n i t i a t i o n

F igure 3 . Tens i l e Shear S t r eng th versus Aging Time (100°F t o 150°F) f o r Adhesive System C

8

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A s u r f a c e a c t i v e agent was employed i n an at tempt t o i n c r e a s e t h e t en - s i l e shea r s t r e n g t h of aged bonds. The r e s u l t s are given i n Table 1 and Figures 3 , 4 , and 5. From Figures 3 and 5, one would surmise t h a t A-1100 d e f i n i t e l y improved aged t e n s i l e s h e a r s t r e n g t h s bu t from F igure 4 t h i s would n o t seem t o b e t h e case. The d i f f e r e n c e i s t h a t t h e u n t r e a t e d bonds (Figures 3 and 5) were exposed t o t h e atmosphere f o r over 1 hour be fo re adhesive a p p l i c a t i o n , whereas t h e u n t r e a t e d bonds (Figure 4 ) were exposed t o the atmosphere f o r less than 10 minutes. A look a t t h e l i t e r a t u r e re- veals t h a t a i r a t 50% r e l a t i v e humidity w i l l s e v e r e l y d e t e r i o r a t e t h e s u r - f ace of s i l i c o n c a r b i d e abraded aluminum (see Figure 6 ) . In t h e c a s e of t h e long-term exposure (Figures 3 and 5 ) , the A-1100 p ro tec t ed t h e aluminum. In t h e case of F igu re 4 , however, t he aluminum w a s coated wi th adhesive be fo re s e v e r e exposure d e t e r i o r a t i o n could occur. It can be surmised t h a t t h e bonds formed i n space w i l l be s t r o n g e r than those formed on e a r t h due t o a l a c k of oxygen and humidi ty; t h e r e f o r e , a primer i s no t recommended.

30 90 150 (minu t es )

A Sanded bonds, no s u r f a c e agents

m Sanded bonds, A-1100 treated

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I I I I I 1 I 1 4 8 1 2 16 20 25

(days 1 Elapsed T i m e from Mix I n i t i a t i o n

F igu re 4 . Tens i l e Shear S t r eng th ve r sus Aging Time f o r Adhesive System C

9

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0

(minutes ) Elapsed Time from Mix I n i t i a t i o n

F igure 5 . Tens i l e Shear S t r eng th ve r sus Aging Time f o r Adhesive System B S e t and Aged a t 100°F

3000

2500

2000

1500

Condi t ion ing Time , minutes

Epoxy Aluminum Tens i l e Shear S t r eng th ve r sus Exposure T ime of S i l i c o n C a r - b i d e Abraded Aluminum Exposed t o A i r a t 20% Oxygen and 50% R e l a t i v e Humid- i t y . Source: Adhesives Age, 2 1 (1967)

F igu re 6 .

.-r

10

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ADHESIVE PACKAGE

A Tedlar* f i l m package and mixing chamber h a s been designed and satis- f a c t o r i l y t e s t e d a t 30"F, 75"F, and 100°F. two compartments, t h e r e s i n i n one s e c t i o n and t h e cu r ing agent i n another . The o u t e r p o r t i o n of t h e package i s made of 2-mil' Tedlar and the d i v i d e r i s made of 0.5-mil Tedlar . A l l p o r t i o n s a r e h e a t s ea l ed . Mixing is accom- p l i shed by b u r s t i n g t h e 0.5-mil d i v i d e r and kneading the package. This has been accomplished success f u l l y wh i l e wearing heavy a s b e s t o s gloves , however, n o t w i thou t some d i f f i c u l t i e s . While t h i s adhesive packaging and mixing system i s considered workable by an a s t r o n a u t wearing a space s u i t and gloves, f u r t h e r op t imiza t ion of t h i s concept is recommended. A mechani- c a l c l i p type s e p a r a t o r f o r example would f a c i l i t a t e easier mixing of t h e two p a r t adhesives .

ADHESIVE DISPENSER AND GLOVE BOX DEVELOPMENT

The package i s d iv ided i n t o

Upon the s u c c e s s f u l completion of t he adhesfve development e f f o r t , the des ign and f a b r i c a t i o n of a s u i t a b l e adhesive d i spense r and vacuum chamber w a s undertaken.

Adhesive Dispenser

The primary cr i ter ia governing the des ign of the adhes ive d i spense r u n i t was t o make the a p p l i c a t i o n of t he adhes ive as easy as p o s s i b l e f o r t h e a s t r o n a u t .

The gun l i k e u n i t shown i n an exploded view i n F igure 7 , i s simple t o ope ra t e and r e q u i r e s a minimum e f f o r t on the p a r t of the a s t r o n a u t t o c a r r y out the adhesive bonding ope ra t ion .

F igure 7. Exploded View of Adhesive Dispenser

* Product of DuPont.

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The mixed adhesive s t i l l contained i n t h e Tedlar package i s folded i n h a l f and placed i n s i d e t h e p l a s t i c c y l i n d e r of t he d i spense r . This p l a s t i c c y l i n d e r and nozz le s l i d e s i n s i d e t h e r e t a i n e r and threads on to the g r i p p a r t o f t h e gun. When the t r i g g e r i s squeezed t h e p i s t o n advances in t h e c y l i n d e r pushing the adhesive package a g a i n s t t h e sharp edges of t h e nozz le which p ro t rude i n t o t h e c y l i n d e r . The Tedlar package i s punctured and the adhesive i s skeeted through t h e nozz le .

The p l a s t i c c y l i n d e r and p i s t o n cap are t h e only p a r t s d i r e c t l y i n con- t a c t w i th t h e adhes ive , and can be disposed and replaced a f t e r each app l i - c a t i o n , making the d i spense r r euseab le , r e q u i r i n g no so lvan t c l ean ing .

Glove Box

Due t o t h e requirement f o r conduct ing t h e adhesive bonding r e p a i r ex- periment i n s i d e t h e Work Shop, a s u i t a b l e chamber has t o be provided t o conduct t h e experiment i n vacuum.

A glove box was designed which i s capable t o wi ths tand an e x t e r n a l p re s su re of 5 p s i , r e p r e s e n t a t i v e o f t h e p r e s e n t l y planned 5 p s i a oxygen atmosphere f o r t h e Work Shop. a 15 p s i e x t e r n a l p r e s s u r e load i n case a two gas one atmosphere system i s adopted fo r t h e Work Shop program. The c u r r e n t glove bo:: des ign has a proof p r e s s u r e r a t i n g of 10 p s i and an u l t i m a t e load of 15 p s i d i f f e r e n t i a l p re s su re .

The des ign could be e a s i l y upgraded t o c a r r y

The glove box (Narmco Drawing No. NR 370) h a s a welded s h e e t metal frame wi th two major bonded s t i f f e n i n g channels which c a r r y the loads along t h e window cu tou t . A l l s i d e pane ls a r e aluminum honeycomb cons t ruc- t i o n t o minimize weight . F igure 8 shows t h e w e l d e d s h e e t metal frame and t h e p a r t i a l l y assembled g love box i l l u s t r a t i n g t h e t y p i c a l honeycomb w a l l pane l s . The completed glove box i s shown i n F igure 9 , i nc lud ing the hand opera ted t e n s i l e t es t u n i t i n s t a l l e d on the back w a l l of t h e chamber. Two modified Apollo hard s u i t arms w i l l adopt d i r e c t l y t o t h e p o r t ho le s i n t h e f r o n t of t h e box. The l a r g e hold i n t h e bottom, covered w i t h a f i n e mesh screen i s t h e opening of t h e ven t tube which w i l l be connected t o o t h e r hardware i n t h e Work Shop vented d i r e c t l y t o the e x t e r i o r of t h e v e h i c l e .

The complete experimental system fo r t he adhesive bonding r e p a i r ex- periment (except gloves) i s shown i n F igu re 10 w i t h two t y p i c a l adhesive packages , t h e d i spense r u n i t and blank t e n s i l e shea r t e s t specimen blanks i n f r o n t of t h e glove box.

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Figure 8 . Welded Sheet Metal Frame and P a r t i a l l y Assembled Glove Box

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Figure 9 . Glove BOX wi th T e n s i l e T e s t U n i t

F igure 10. Complete Experiment System (Except gloves)

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PROOF PRESSURE AND LEAKAGE TEST

The glove box w a s submitted t o a 1 minute d u r a t i o n , 10 p s i d i f f e r e n t i a l proof p r e s s u r e load by p u l l i n g approximately 20 inches of mercury vacuum i n s i d e the chamber. Visual i n spec t ion of t h e s t r u c t u r e showed no s i g n o f damage of permanent deformation o f any component.

Following t h e proof p r e s s u r e t e s t , t h e glove box w a s l e a k - t e s t e d a t 5 p s i d i f f e r e n t i a l p r e s s u r e . p r e s s u r e was less than 1 inch of mercury i n s i d e t h e chamber. ra te i s w e l l w i t h i n t h e al lowable value o f 5 cc/minute.

During t h e 24 hour t e s t , a change i n vacuum This leakage

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CONCLUSIONS AND RECOMMENDATIONS

The t h r e e adhesive systems developed under t h i s program provide a wide temperature range from 30°F t o 130°F i n which a c t u a l i n space adhe- s i v e bonding ope ra t ion could be performed.

The glove box and adhesive d i spense r are bel ieved t o be s u i t a b l e t o c a r r y o u t a r e a l i s t i c adhesive bonding r e p a i r experiment on board t h e SIV-B Work Shop.

The fol lowing a d d i t i o n a l work i s recommended t o improve t h e u s e f u l l n e s s and inhance t h e success of t h e experiment:

1. The working temperature of t h e adhesive systems should be increased i n both d i r e c t i o n s . A temperature range of 0°F t o 160°F appears f e a s i b l e wi th mod i f i ca t ion o f t h e adhesive systems developed under t h i s program.

f a c i l i t a t e easier and f a s t e r mixing. 2 . The adhesive package design should be improved t o

3 . Accessory f i x t u r e s and devices should be developed t o provide a i d i n performing t h e experiment i n s i d e the glove box under zero-g c o n d i t i o n s .

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