Best Available Copy - dtic. · PDF fileSeven adhesives were evaluated for their lap shear,...

%AF TR-804183

AD A 0 9'9 4 9(f} DHESIVE ,RONDING FOR JHELTERS.

D. Robert/Askins James C/McKiernan.

UNIVERSITY OF DAYTON RESEARCH INST DTiC300 COLLEGE PARM AVENUE DTIDAYTON, OHIO 45469 Q--LLCi

4 .- " " -.---.... . --.'- -

DECE d /8-JJJ/7 /- y4 y/. -

INT.TM CI_-'jTr21 $•,F.POjT DECEMBER 1977 AUGUST 1980•Final• Surnw-try epet, fn Shelter Adhesive Program)

> Approved for public release; distribution unlimited.

S"I •/ " / I'" /, j•v•,• t• ' ._. :•/ . r . ~ ,, ... ... .

___ I) ,,-.,.- * # ; ,••I . . . .

t!TERIALS LABORATORY=mIR FORCE WRIGHT AERONAUTICAL LABORATORIES

AIR FORCE SYSTEMS COMM4ANDWRIGHT-PATTERSON AIR FORCE BASE, OHIO 45433 / ) "" "'

8i 3 30 099

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NOTICE

When Government drawings, specifications, or other dataS:are used for any purpose other than in connection with a

definitely related Government procurement operation, theUnited States Government thereby incurs no responsibility

-nor any obligation whatsoever; and the fact that the Governmentmay have formulated, furnished, or in any way supplied thesaid drawings, specifications, cr other data, is not to beregarded by implication or otherwise as in any manner licensing7: ~the holder or any other person or corporation, or conveying ;

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This technical report has been reviewed and is approvedfor publication.

O RHODEHAMEL-- A. OLEVITCH, ChiafProject Engineer Nonmetals Engineering BranchNonmetals Engineering Branch Systems Support Division

I

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A''A-TR-so0-4183 -1p 911674. TITLE (and S.btl Its) 5. TYPE OF REPORT & PERIOD COVERED

Interim Technical ReportADIHESIVE BONDING FOR SHELTERS December 1977-August 1980

6. PERFORMING O1G. REPORT/ UMBER

UDR-TR-80- 887. AUTHOR(&) 8. CONTRACT OR GRANT NUMBER(.)

F33615-80-C-5011 ,'$t.

D. R. Askins and James C. McKiernan F33615-78-C-5002

9. PERFORMING ORGANIZATION NAME AND ADDRESS 10. PROGRAM ELEMENT. PROJECT. TASK

University of Dayton Research Institute AREA & WORK UNIT NUMBERS

300 College Park Avenue 24210315

Dayton, Ohio 45469It. CONTROLLING OFFICE NAME AND ADDRESS 12. REPORT DATE

Air Force Wright Aeronautical Laboratories/ December 1980Materials Laboratory (AFWAL/ML) 13. NUMBER OF PAGES

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IS. SUPPLEMENTARY NOTES

19. KEY WORDS (Continue on r-'otae side if nece.saty and idenltify by block rnumber)

Adhesive Lap Shear PrimerBond 1Peel Crack ExtensionDurability Stress-Durability Metal EtchingEqvironmental Aging Failure Mode Shelter PanelModified Epoxy Surface Preparation

20 UYSTRACT (Coriot,. on ,eoe, oside It nec.- -,y and Identify by block n.,mber)

As a result of work done over the past several years with adhesives ingeneral and shelter adhesivem, in particular, a testing scheme for evaluatingcandidate shelter adhesives ha; been developed and generally accepted by the *1

shelter industry. Thi:; includes agreement upon the types of tests, testconditionsj, and ton:,t ,,cim ,;tl! whlich will b(' utilize'd to valuate candidatev

((:nltiluad On oth('23 side)

DD O' 1473 DITIO,. 0' 1 NOV 6 IS OtISOLE:TL UNCLASSIFIED

-,t CURITY CLASSIFICATION OF THIS PAGE f*W7.n Voef F,,ftrod)

i :j

\ UNCLASSIFIED$CCUV TCLASSIFICATION OF THIS PAGE(I"?ae Date Enter~d)

The work undertaken in this program was aimed at identifying adhesiveswhich have the capability of retaining a substantial portion of their struc-tural integrity after prolonged exposure to the combined effects of elevatedtemperature and high humidity, and also to evaluate tae effects of severaladherend surface preparation variables upon the interfacial durability of

bonded joints.Seven adhesives were evaluated for their lap shear, peel, and stress-

durability characteristics. No single adhesive ra-iKed high in all categoriesbut a relative ranking of the adhesives was developed, based on their relativeperformance in all of the tests.

Two surface preparation va~ables weru uvaluated, the type of etch bath"sweetener" and the type of rinse\water used. The type of etch bath "sweetener"

was found to have a dramatic effect on interfacial durability, with the coppercontaining 2024 alloy required regardless of the alloy being etched. Thedifference between rinsing with tap water and deionized water was marginal.

71NCLASSIPIED

Stc $ '.'• CL• A •IICATIONi OP ," P Or.rWhen Data Ep0topdl

iI F

PREFACE

This report covers work performed during the period from

December 1977 to August 1980 under Air Force Contract Nos. IF33615-78-C-5002 and F33615-S0-C-5011, Project 7381. The work

was administered under the direction of the Systems Support

Division of the Air Force Materials Laboratory, Wright

Aeronautical Laboratories, Wright-Patterson Air Force Base,

Ohio. Mr. John Rhodeharrel (AiWAL/MLSE) was the Program

Project Engineer.

The Principal Investigators on this program were D. Robert I

Askins and Ronald J. Kuhbander. The major portion of the labora-

tory work was conducted by Messrs. James McKiernan (specimen

fabrication and data documentation) and Lonald Byrgn (testing).

This report was submitted by the author in October 1980.

The contractor's report number is UDR-TR-80-88.

-JAeCe ItNOn F 0i•TI 3 G.<,& I -•

A i 1 'l 'l.ty tq:los •"

iI

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= l

TABLE OF CONTENTS

SECTION PAGE

1 BACKGROUND AND INTRODUCTION 1

2 APPROACH 3

2.1 MATERIALS AND PROCESSES 32.2 SPECIMEN FABRICATION PROCEDURES 52.3 TEST METHODS AND EXPERIMENTAL DESIGN 5

2.3.1 Lap Shear Testing 52.3.2 Floating Roller Peel Testing 92.3.3 Stress-Durability Testinq2.3.4 Thick Adherend DCB Crack

Extension Testing i3

3 DISCUSSION OF RESULTS 18

3.1 LAP SHEAR TEST RESULTS 183.2 PEEL TEST RESULTS 293.3 STRESS-DURABILITY TEST RhSULTS 323.4 CRACK EXTENSION TEST RESULTS 41

4 SUIMARY AND CONCLUSIONS 48

APPEN DICES •

I ADHEREND SURFACE PREPARATION PROCEDURES 51

II PRIMER APPLICATION PROCEDURE 57

III PANEL LAY-UP AND BONDING PROCEDURES 59

IV SPECIMEN MACHINING PROCEDURES 62

V ADHESIVE PROPERTY DATA FROMMLANUFACTURERS' LITERATURE 64

VI INDIVIDUAL SPECIM<EN LAP SHEAR TEST DATA 66

vii INDIVIDUAL SPECIMEN FLOATING ROLLER PEELTEST DATA 89

ViII INDIVIDUAL SPECIMEN STRESS-DURABILITY TESTDATA 94

IX INDIVIDUAL SPECIMEN DCB CRACY i',OWTHTEST DATA 103

V

LIST OF TABLES

TABLE PAGE

1 Lap Shear Test Matrix 7

2 Lap Shear Test Results for 6061T6 Adherends withMachined Specimens and FPL Etch 20

3 Lap Shear Test Results on 6061T6 Adherends with1Machined Specimens and OFPL Etch 21

4 Lap Shear Test Results on 50521134 Adherends withNMachined Specimens and FPL Etch 22 -

5 Lap Shear Test Results on 5052H34 Adherends withMachined Specimens and OFPL Etch 23

6 Lap Shear Test Results on 6061T6 Adherends withFinger Specimens and FPL Etch 24

7 Lap Shear Test Results on 6061T6 Adherends withiFinger Specimens and OFPL Etch 25 -

8 Lap Shear Test Results on 5052i134 Adherends withFinger Specimens and FPL Etch 26

9 Lap Shear Test Results on 5052E34 Ahercnds .. ithFinger Specimens and OFPL Etch 2-1

10 Floating Roller Peel Test Results 30

11 Stress-Durability Test Results

12 Stress-Durability Test Results for Extra Retested

Specimens J0

1.3 DCB Crack Extension Results 42

14 Sunn•ary Ranking of Adhesives 4T,

kA[A=iSl n

• .win: iwi

LIS" OF ILLUSTRATIT ONS

FIGURE PAGE

2. Lap Shear Specimens (from ASTM D]1002) 6

Lap Shear Testing Plan 8 -.

Floating RollKr ("Beli") Peel Scectmen andFixture (from ASTM D3167) 10

"4 Peel "tin.1(' Plan _i

5 Lap Shear Specimen and Stress-DurabilitCyFixture (from ASTM D2919) 12

o Stress-Durability Testing Plan 14

7 Thick Aiherend Double Cantilever Beans (DCB)Crack uxtension Specimen (fro,•, AF-IL-TR-76-173) 15

Crack-Extension- Testina Plan

3 ':-ianation of Failure Mode Notation ]>)

1 Streess-Derabi iit' Behavior on 6061T6 BareAdhe rends r s

ii Stress-Durab i tv Behavior on $052H3: BareAuhierends 36

12 Stress-Durability Behavior of LR00-252 andEA9601NW Adhesives on 50521134 Bare Adherenas 39

13 Stress-Durability Behavior Sun-mary 40

14 Effect of Ltch Bath Sweetening Alloy onInterracial Durability 4'

Ef ._fect of Rinse Water Type on InterfacialDurability 44

16 Effect of Aheus ive/i rimer Type on Durab iitv 45

V i

SECTION 1

BACKGROUND AND INTRODUCTION

The Air Force, as well as the other services, has beenu'tilizing lightweight, air transportable shelters for a wide

variety of purposes for a numtber of years. Some of the many

uses for these type shelters include the housing of personnel,

hospital facilities, offices, and electronic instrument stations.

Modular building concepts incorporating such features as

sandwich wall construction and adhesive bonding are routinely

used for these structures to reduce production costs. Walls

can consist of honeycomb or foam cores between aluminum skins.

In addition to the skin-to-core bonding found in honeycomb-

stiffened wall construction, adhesives are also used for metal-

to-metal lap-type joints, and frequently serve both as a load

bearing structural member as well as a joint sealant against A

environmental infiltration.

Shelters of this sort are used in r.;any locations through-

out the world, and consequently are sWbjected to a wide varietyof environmental exposure conditions. These rangje from subzero 4

arctic tem[lertures to hot, dry desert climates as well a- hot,

humid tropical conditions. Besides exposure to these various

climatic extremes, the shelters are periodically subjected to

abnormal stresses of transport from one location to another,

exacerbating the dermtnds made upon the structural members and

bonded joints.

The shelter desian requirements w'hich most heavily in-

fluence the type of adhesives selected for use in structural

bonding are

(a) Maximum and minimum exposure temperatures of -40'F

(-40'C) to 200 0 F (93 0 C) with concomitant interior-to-exterior

thermal gradients coupled with varying humidity conditions up

to saturation,

(b) Water resistance,

(c) Overall stress loads ranging from 300 to 1200 psi

(2.07 to 8.27 tMPa) , and

w•) L.onj-terrn durability 01. up t;. tel, yeats ot in-the-I

1_'NPCVi ncflCC iICs has icnS th, Lit the chot--hAnu d onvironlich.Lt

] S tU O m sL<St d,_2;.,alL12 Id~ll .li-] im 1 a, t ile ,. g I 'c I, y: iV,)-' Ill U1.

these structures are tLhe sitms most suscuptibie to f.ailure as A

o sGu1t ,D oxmposur.o to tUl aiSld LMi], t ccoarl ticiios

describeL a bVe,

The primary objective of this in-,,entiuation was to identi y,

copimerciaily available adhesives whicih have the capability Ur

r 1t.ainin~j a subs t..nts1 .)rtien, :;, their st.i2te.a] tnt jrit '1

after p)rcloniejk3a exposure_ L(_ t'lcibn- lei ; i~t

tLmuerature and hi-,h hujvaiitv. A secondary objective was to

evaluate the eFfect e:f so cted surface I)ro;laratd , . vaI Iab ,a2s

u;,on the interlacial k:iaabiit..y of bonded joints. a

u. the work undetLacn was in direct response to the expressee

concerns cie desi . es o ) both Lhc snelter manufacturers and

aehesiv:e v.':Jdrs *]:-. ,,el' .- s t n.-. ,>f thc'var ious serviec3.

II

2

1-4

SELCCTION 2

APPROACH

Two Vlhesivc characteristics were of Las)ic interest in this

,_val uat ion Ortort: (1) the a' i • tv to resist thc cum -in'ation 0!

L2eI vatuo tenL• Leup u r, at" I t P hieh I l'li i t4, (<I 'Id at In I, ptj (2) 1rnw

tenl~'ratt'L( toughness. Althu1h .]aait a tL iv'C acC, c /c U ct

':ite ia fto., thoese tVo .Chn2 ctor A.C.. h've rIot vCot v 03C) i on,

the \"Iri cuI adc!hes Iv' f a C nat) d can ,it. e:'u;t bI cn L-ar d t, oa Ct

other and civen some sort of overall rankinc.

Pirc,' ty o ts.st.s we're Ust'eG ikr !i~c adhJ .SiVti ecv'atiu

Conductmcd dur-inii this pro; ran: 1) aj s],ax, (2) floati1!ng

rl1oer poel, and (3) stress-duo-abilit. .I ai shIear tests wereconduc ted1CC -,(, l:U_.IStl IC t!wlo 0.f 1,)0 "!b , t], c]<v'ate, te2l;,_: ratu'L -C

"10.1 ' L',id t \, .,i1'. u1on adLil'si<.t: w.,o ,., t 202s. The :iv ic ntalIex;,osUaro conc1itio.-s1 \l e Wk , otd to Coa-r.spono to tIose measured

in t~ic field [ 200", ()'-3C") and 95-100 2-rCcellt reiat, yve huimn ,i tYv .

ncss oa the adhhcsives at low tem;era turcs [-65°IT (-541C) ] Stress-

durability tcsts wcrc conducte(, to ,"',ca.sur- theC sin'ultaneous cffccts

of stress, elevatod tonr',Irature, ad taa hu',, ui t% U'DO1m adhesC1vc.

bond life. The c'V, vrornentaJ exosurc conditions for these were

the same as for the lap s'near tests.

A fourth type of mechanical test was used in the evaluation

of the various surface. preparation parafl'ters. This was a thick

adherend, double-cantiicver-boarr (DCB-) crack extension test.

The results of these tests measured the influence of surface

preparation variables upron thC end.'iro'.ental d(ueradation of a

bonded Joint.

2.1 MATERIALS AND PROCESSES

There are four major categories of materials and processes

which were of interest to this investigiation: (1) adlierund alloy;

(2) adherend surrace preparation p)roceuure; (3) adhesive surface

primer; and (4) adhesive.

3

The1 t ,:Co pi Cli I)l t aiher•cndO ,tci- als wore har (2 5075'21134 and

oil'i0 aluTi6uU, alloys. These represent the two priinciple

dlUfl.u,,1 alloys ISId i 5h•I tel construction today. A third

dultuminum • llov, bare 20i.4T3 was used to a limited extent during

the program Lecause of extensivt, P1rar- exerience- w1th1 this

a 1 10,: in ad1•< yeI bonding work It is nci generally used in

shlel toz c,)IlstrUCtioiI, bccauso rn eith,_r tlo 2000 or 7000 ser ias

a lu:!inom 1111 Lo arc easily w, tld or arc as corros, on resi stant nt-is thc, 5000 or 6000 sc~ri zs A 1 1o'.Y

The primary surface preparation procedure tsed for the fo

,1,; h 0S 1v 1-0 Fý-' I "I' W.Ok nI t 1. 1s i oý -k•\ r-,m• w,'-is tho op i,-. i 7_(_,,<'t 1',

(Yorest Products Laboratory) Ltcfl treatment, althouqh the non-

o-t imized FPL Ctch treatment kASTM D2151, method A) was used for

some of *hI( earlv work. The oq-timized FP1, etch treati.ent a

sodi im dichr.,-o, suiliuric acid sol ut io:) is beono ale: ted by

the shelter ma.uufactur-n-.; •ndustrv as the standard aluminum,

suriface trI, at:r2nt for adhesive bondino. Details of theso two

surface treatment tcchn 'ues a:.d the signifi:cant 01- ifc.rrnce

between the two are i)rcsonted in Aooendix I.

Two corrosion inhibiting primers were used durino the program:

BR127 by American Cyanamid and :KA3950 by 3M. The BR127 was usedSthrouqhout the program while the X]A3950 was used only in the lap

shear portion. In addition, some specimens were prepared without

primer durinq each part of the investigation. Appendix IT describes

the primer application procedures.

Seven vendor-supplied adhesives were evaluated. These, to

the best of our knowledqe, were all modified epoxies. Six of the

adhesives were supplied in the form of a supported film while one

(IR]00-172) was a low viscosity, two-part system applied as a

thin unsuppurted film by hand after mixing. The seven adhesives

were,(1) LR100-172 (two part paste) Hysol(2) R7114 (0.081b/iftL, 0. 39Kgn/'m 2 ) Reliable (Ciba-Geigy)"I XAl80 (0.0 61bLft 2 , 0.29Kg/9 2 ) 3M(4) LR100-252 (0.091bft 2 , 0 44Kg/mr) }iyso] (currently

designated EA-9652)(5) MIA-429 (0.06lb/ft 2 , 0.29Kg/rm2 ) McCann(6) R382-7 (0.081b/ft 2 0.39Kg/mn) Reliable (Ciba-Geigy)(7) EA960iNW (0.0851bift4, 0.42Kg_/o, 2 ) 11vsol

4

soon

These seven adhesives were selected because they were either in _

current use in shelter construction or because they had beenidentified as likely candidates to replace those which were beingused. Appendix V presents Manufacturers' data provided for each of

these adhesives.

2.2 SPECIMEN FABRICATION PROCEDURES

The fabrication of the specimens used for data generation inthis piogram consisted of a sequence of five distinct processes:

(1) Adherend surface preparation,

(2) Priming of freshly prepared adherend surface, J:

(3) Bonded joint panel layup,(4) Curing of adhesive joint panel, and

(5) Machining of individual speci[,iens from cured panel.Each of these five processes is described in detail in AppendicesI through IV, respectively. These include step-by-step descriptionsof each procedure, as well as the quality control criteria used toaccept/reject a part or finished panel at each stet in the fabrica-

tioii sec.uence.

2.3 TEST METHODS AND EXPFRIMENTAL DESIGN

All testing conducted during this investigation was performed

in accordance with standardized procedures. Thus, the lap shear,peel, and stress-durability tests followed ASTM test methods,while the crack-extension tests were in accordance with a methoddeveloped by the Boeing Corporation.

2.3.1 Lap Shear Testinq

Lap shear tests were conducted in accordance withASTM method D1002 on specimens from boLh the btandard (fullymachined after bonding) and the preslotted (finger) types oftest panel (see Figure 1). Specimens were used only if theapplied primer thickness and the cured glue line thickness fellwithin specified limits. The techniques used to measure these

41

[ I I

F

I

I I

Wa) MAC (IN GE SPECIMENS

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S h2 c iI s ,'L -.ii

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Ib I PR ESLOT T(E. (FI GE•lR ) SIPECIMErN S

F i q ud r e 1. ta p S h e a r S p e c i m e ni s ( tr o m l A S T P I 1) 10 0 2 ) .]

thicknosses are described in Apjijedices II and 1I, respectively. ,

The specimens primed with BR127 were used only if the primer

thickness fell within the 0.0002-0.0004 inch (0.005-0.010 mm)

rancge. The specimens primed with Xt-3950 were used only if the

primer thickness fell within the 0.0001-0.0003 inch (0.003-0.008 mm)

range. Both of these primer thickness ranges were recommended

by the respective primer manufacturers. The bonded specimens

were_ used only if the cured glue line thickness fell in the

0.004-0.007 inch (0.10.-0.18 nur,) range. This glue line thickness

range was established by a consensus of shelter manufacturers

at thu s Lar of theL 7rO:I iiii

Fiaure 2 lists the materials, processing, and test

conditions included in the lap shear testincg portion of this

i;ro.J ram.

With the exception of two adhesives, the test matrix

consisted of a full factorial deSieLn incorporating five replicate

Sp:ecimens of each combination of adhesive, specimen type, adherend

alloy, surface preparation, primer, and test condition. The two

excepted adhesives (LR100-252 and MIA-429) were not tested on

finger specimens or with the standard FPL etch surface prepara-

tion. A full factorial design would have involved a total of

1,680 lap shear specimens. Table I indicates the actual test

matrix, the omitted combinations accounting for a reduction of

240 in the specimen total.

TABLE 1

LAP SHIEAR TEST MATR[X

Specimen Typ:e__ Surface PreparationAdhesive Machined r Finr 1 FL t. FPL

LRIO0-172 X X X x IR7114 X x , XXA180 X X I X X

LR]0O-252 X -NOT TLSTED-- XNMA-429 x -NOT TIESTED�-- XH382-7 X X N x X

E A 9 60 N'V W Xx X X

NOTVS: All indicated combinations were prepar,'i using all threeprimer conditions (none, B13127, and XA- 3950) , and twoadherend alloys (6061T6 and 50521!34) , ind tested at twotent conditions [720F (22C) and 200%F ()3'C) after hot-burri~l ag ing,.

7 Adhesives 2 Surface Preparations

LRIO0-172---Hysol FPL Etch (except for LRI00-252 and MA-429) i

R7114----Reliable Optimized FPL Etch

XA180-2---3M

LR100-252--Hysol 3 Primer ConditionsMA-429----McCann

R382-7 ---- Reliable No primer

EA9601NW---Hysol BR127-----American Cyanamid

XA 3950------3M

2 Adherend Alloys2 Test Conditions

6061T6 Bare

5052H34 Bare 72-F (22 0 C)

200OF (93 0 C) after two weeksat 200OF (93 0 C) and 95-100

2 Specimen Types percent R.H.

Machined

Preslotted [Finger] 5 Replicates(except for LR100-252and MA-429)

TOTAL- 1,440 Specimens

Figure 2. Lap Shear T,3sting Plan.

•I

8

'I

2.3.2 Floating Roller Peel Testing

Floating Roller Peel (frequently referred to as

"Bell" peel) tests were conducted in accordance with ASTM

method D3167 (see Figure 3). Specimens were tested only if the

applied primer thickness fell within the manufacturers recommended

limits [0.0002-0.0004 inches (0.005-0.010 mm) for BR127]. Cured

glue line thicknesses were not measured but the same shimming

process was used in the manufacture of these panels as was used

for the lap shear panels. This procedure results in about

95 percent of the cured bondlines falling within the desired

thickness range of 0.004-0.007 inch (0.10-0.18 mm) (Appendix

III). Tests were conducted at both 72 0 F (22'C) and -651F (-54'C).

Seven adhesives, three adherend alloys, one surface preparation,

and one primer were involved in the peel testing for a total

of 21 combinations. Additionally, one of the adhesives was

used without a primer, adding three more combinations for a

total of 24. Four specimens of each combination were tested at

each of the two test temperatures. Figure 4 lists the materials,

processing, and test conditions included in the peel testing

portion of this program.

2.3.3 Stress-Durability Testing

Stress-durability tests were conducted in accordance

with ASTM method D2919 (see Figure 5). The same accept/reject

criteria regarding primer and glue line thickness were followed

with these specimens as with the lap shear specimens mentioned

in Paragraph 2.3.1.

Stress-durability tests consisted of mounting the

specimen in the fixture illustrated in Figure 5, imposing a

predetermined shear stress upon the specimen, and placing the

specimen-fixture assembly in an elevated temperature, high

humidity aging environment until the specimen failed as the

exposure period reached a preselected limit (1000 hours in this

program). In the event that the exposure period reached the

9

PEEL -

TESTHANEL

:. i 254 CIA1254C AFLEXIBLE

MEMBER

""27 CM(OSO IN)I

NOTE A 1.5 TO 3.0 IN (38.1 TO T4.1 MM) SHIM CAN BE USED TO FACILITAT'E

THE START OF PEEL.

(a) TEST PANEL AND TEST SPECIMENS

(1/8 IN) 095-096 CMS0 316 CM ALUMINUM - r- (038-039 IN)

OR STAINLESS STEEL IN DIAMETER

-330 CM

E'N WIH IN

2~ 54 CM- 305 CIVI(IOOMIN (120 IN)

3/6 IN - 16 STUD BEARINGS3/B I 16 NT I DUBL&ROLL EXTRA1

SYNTHETIC SEAL BALLBEARING WITH EXTENDEDINNER RACE

-- RIGID ADHEREND

- .I(0.064 IN.)

JII

WIDTH ---- FLEXIBLE ADHEREND I(0.50 IN.) - (0 025 IN.)

(b) ROLLER DRUM PEEL TEST FIXIURE

i.gure 3. Floating Roller ("Bell") Peel Specimen and Fixture(from ASTM D3167).

10 i

S... ... .. .. ...•:" -. ...- .... • • '-"-•"• •=• F [ " .

7 Adhesives 1 Surface Prepoaration ]LR100-172 Optimized FPL etch ]R7114

XA-180 1 Primer Condition

LR100-252 BR127 (except for LR100-172)

MA-429

R382-7 2 Test ConditionsEA9 6 0 lINW

72 0 F (22 0 C)

3 Adherend Alloys -65 0 F (-540 C)

2024T3 Bare 4 Replicates

6061T6 Bare A

5052H34 Bare

TOTAL - 192 Specimens

A

A

Figure 4. Peel Testing Plan.

41

A,

11i

I 6ram (0064")

I-*i- -'?7m-n/5" . .

--------- 4 76m-/-

/-2 7mrr( 112Z" 1IT

I.• ... ... ... 2 .9m int8 /2')-

LOD Sre3r igpec.rne',

Spr rq

: , -. T P, e.e3, ed ["1hC

~___

Figure 5. Lap Shear Specimen and Stress-Durability Fixture(from ASTM D2919).

12

1000 hr. limit without specimen failure, the fixture was removed

from the environmental cabinet, and the specimen unloaded and

removed from the fixture and tested for residual strength. This

test was aimed at providing additional data on the effect of

environment upon adhesives. While not necessarily providing

real-life design type data, it did provide a comparative ranking

of adhesive resistance to environmental degradation.

Standard lap shear tests were conducted at 720F

(22'C) and 140QF (60 0 C) on dry unaged specimens to provide base-

line data. Stress-durability tests were conducted in a 140^F

(601C) and 95-100 percent R.H. environment at two stress levels:

(1) 40 percent of 140'F (600C) dry ultimate strength, and (2) 60

percent of the 140OF (60 0 C) dry ultimate strength. Times to

failure were recorded and any specimens which had not failed

wi0h1n i,Ouu nours were removed and tested for residual strength

at 140OF (60 0 C). Seven adhesives, two adherend alloys, one

iurface preparation, and one primer were used for these tests;

a total of 14 combinations. Additionally, as before, one of the

adhesives was used without primer, bringing the total number

of combinations of 16. Three specimens of each c•,mbination were

tested at the two baseline conditions and five specimens of each

combination were tested for durability at the two stress levels.

Figure 6 lists the materials, processing, and test conditions

included in the stress-durability testing portion of this program.

2.3.4 Thick Adherend DCB Crack Extension Testing

Crack extension tests were conducted with the

thick adherend DCB specimen, and in accordance with the pro-

cedures described in AFML-TR-76-173. This specimen is illustrated

in Figure 7. Specimens were used only if the applied primer

thickness fell in the 0.0002-0.0004 inch (0.005-0.010 mm) range.

As with the peel specimens the glue line thicknesses were con-

trolled during fabrication but not measured. The objective of this

A),Licnl of the ')ro•i-c7 was t: examine the effects of surface

preparation variables upon the bond between the metal oxide and

the surface primer. Only one adhesive (FM73) was used. This

13

_/I;

3WJ

7 Adhesives 1 Surface Preparation

LR100-172 Optimized FPL etch

R7114N AI U 0 1 Primer Condition

LR100-252 BRI27 (except for LRi00-172)

PIA-4 29

R382-7 2 Test Conditions

EA960INW40% stress level

60% stress level2 Adherend Allovs

6061T6 Bare 5 Replicates

56521134 Bare

TOTAL - Stress-durability - 160 specimens

Baseline statics - 96 specimens(3 ieplicates)

Figure 6. Stress-Durability Testing Plan.

, .

I

T. -

, 4

jNN J -

DOeAN, of rhtk Adherend DGB Spe-nen

Figure l7. Thick Adherend Double Cantilever Beam (DCe) CrackExtension Specimen (from AFRL-TR-76-173)

15

adhesive had been shown in the Primary Adhesive Bonded Structures

Technology (PABST) program to be highly resistant to elevated

temperature, high humidity degradation, and was selected to

maximize the probability of failure along the oxide/primer

interface. Only one primer kBRI27) was used. One exception

to this work plan was the use of a second adhesive (LRI00-172)

without primer in a few tests. The tests were conducted in a

140OF (603C), 95-100 percent R.H. environment and crack lengths

were measured as a function of time. The crack propagation locus

was also recorded (i.e.: interfacial or within the adhesive

layer). Fjiure 8 lists the materials, processing, and test

conditions included in the crack-extension portion of this

program.

1

161

I

I I_•:• • • ,•n 7• :L -: i: : ...• •• -- =,..-: • • • •¢ -•--.••• -- " "' -,,• , •'• •"• " ,,,,,

9 Adhesive/Primer/Adherend Alloy/Surface Preparation Combinations

Adherend OFPL Sweetening Rinse

Adhesive:Primer Alloy Alloy Water

0 FM73:BR127 2024T3 2024 Tap

* FM73:BRI27 2024T3 2024 Deionized

* FM73:BR127 5052H34 2024 Tap

* FM73:BRI27 5052H34 5052 Tap

a FM73:BR127 6061T6 2024 Tap

* FM73:BR127 6061T6 6061 Deionized

* FM73:BRI27 • ')•,IT6 6061 Tap

* LR100-172:None 5052H34 2024 Tap

* LRIOO-172:None 6061T6 2024 rap

1 Test Condition

140 0 F (600C) and 95-100% R.H.

5 Replicates

TOTAL - 45 Specimens

Figure 8. Crack-Extension Testing Plan.

DISCIUSSION 01' RdESULTS

intcrpretitiui alnd assessment oi thu results obtained

in this investigation are based upon the measured strengths, -A

times-to-lailurc, ano strain energy release rates measured in

thc various tests as well as the observed tailure modes in the

bonded joint interfacial areas.

Traditionally, bonded joint failures have been reported

as adhesive, cohesive, or some combination of the two. In

this context, adhesive. failure referred to . failure locus

along the interface Letween the substrate and the adhesive

layer, while cohesive failure referred to a failure locus

compietely within the adhesive layer. It was felt that witil

the inclusion" of a primer layer in the bond, along with bet

cistinct from the adhesive iay'er, the traditional means ot

report:.ng failure mode was inadeouate. Accordingly, a

differient format for reportir':z faiiirt mode was adopted

during this investigation. This format is illustrated andexplained in Figure 9. T]••i:lz petto J[ • ointfailure modes is very subjective. It is dificult, with the

naked eye, to ascertain the exact failure mode unless it is

totally cohesive (within the adhesive layer). Interfacial

failure modes may appear obvious but one cannot be sure, short

of resorting to expensive surface instrumental analysis, that

a very thin layer of primer or adhesive has not remained adhered

to an otherwise clean appearing surface. Since the primer laver

is so thin, the only evidence of its presence, to the eye, is

generally color. In this investi.,ation the only 6iscriwinations

made regarding failure mode were those dctctable by eye. Thus,

it is to be recognized that reuardless o. the di fferent presen-

tation format, the failure modes reported a.:, this document are

still subjective.

3.1 LAP SHEAD .TST !LSULTS

The data obtai:ic ] frun. the testing ,i the lap shear specimens

are surnmarized in Tables 2 through 9. The values presented in

'M

For Bonds Made With No Primer

x-x

cohesive failure within the adhesive layer (%)

L .adhesive (interfacial) failure between the adhesiveand the substrate oxide (%)

"-For Bonds Made With a Primer on the Substrate Surface

X-11-X-X

cohesive failure within the adhesive layer (%)

adhesive (interfacial) failure between theadhesive and the primer (%)

L- cohesive failure within the primer layer (%)

adhesive (interfacial) failure between the primerand the substratv oxide (%)

Example: 5-0-30-65 indicates that, according to the observer'sestimate, the failed joint exdhibits the followingfailure mode.

The primer pulled cleanly off thc metallic oxide

on 5% of the bond area.

At no poine alorng the bondline did the failurelocus run cohesively within the primer layer.

The adhesive debon-ied cleanly from the primer on30'. of the bond area.

T'ie faii ur, iocis run cohcsivc.1 withln thledaoi:s jv'. 1.1ur o2 65 oi Le bond ,v~-A..

I, . r . ) *

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these tables represent averages of five replicate specimens.

A comprehensive listing of all of the individual specimen-by-

specimen lap shear test data is presented in Appendix VI.

In general, three adhesives (LRI00-172, XA-180, and LR100-

252) withstood moisture attack very well, exhibiting residual

strengths after exposure of greater than 1000 psi (6.89 MPa)

in every case.

Two other adhesives (R382-7 and MA429) withstood moisture

attack well but did exhibit a few residual strength values less

than 1000 psi (6.89 MPa). The residual strength after aging of

the R382-7 system fell below 1000 psi (6.89 MPa) in five out

of 24 cases. Two of these aere on unprimed FPL etched surfaces

and exhiDited interfacial failure. A third was on an unprimcd

OFPL-etched surface and exhibited considerable interfacial failure.

The other two were on BR127-primed surfaces and very narrowly

missed the 1000 psi (6.89 MPa) level. The residual strength

after aging of the MA429 system fell below 1000 psi (6.89 MPa)

in two out of six cases. One of these was on an unprimed surface

and exhibited interfacial failure. The other very narrowly

missed the 1000 psi (6.89 MPa) level.

Another adhesive (EA960lNW) exhibited marginal moisture

resistance. In 14 of the 24 cases, the residual strength atter

aging of this adhesive fell below 1000 psi (6.89 MPa) . Twelve

of these 14 cases, however, exhibited interfacial. failure between

either the adhesive and the primer layer or between the adhesive

and the unprimed adherend. The other two were cohesive failures

within the adhesive layer. This indicates that with the EA9601NW !

adhesive system, the interfacial bond degrades more rapidly than

the adhesive itself during hot humid environmental r-ging.

The last adhesive (R7114) was very susceptible to moisture

degradation. Tn 23 out of 24 cases, the residual strength of

this system after aging fell below 1000 psi (6.89 MPa) and the

one exception reached cnly 1100 psi (7.58 MPa) . Most of these

failures are within the adhesive layer (cohesive failure).

- - -O-

The optimized FPL etch produces consistently higher

strength levels than the standard FPL etch on the machined lap

shear specimens. On the preslotted type specimens, however,

some adhesive/primer combinations exhibited higher strengths

on the FPL etched surface than on the OFPL etched surface.

In general, specimens made with the 6061T6 alloy exhibit

higher joint strengths than those made with the 5052H34 alloy.

Since the 6061T6 has a higher yield stress than the 5052H34,

the bending at the end of the lap area is postponed until a

higher load is reached during a lap shear test. This, in turn,

postpones the introduction of peel stresses into the joint and

leads to the higher joint strengths.

Although moisture degradation appears to be slightly more

severe on the preslotted finger specimens than on the machined

specimens, the differences between the two is not substantial.

In general, the specimens with primed surfaces resist

degradation better than those with unprimed surfaces. In some

cases, iowever, the reverse is true but the overall difference

is not sibstantial. There seems to be little difference in

the residual property results shown by either the BR127 or

AA3950 primers.

3.2 PEEL TEST RESULTS

The data obtained from the testing of the peel specimens

are presented in Table 10. Probably the most obvious feature

of this data is the fact that the bond formed between the BR127

primer and the LR100-172 adhesive has very little resistance to

peeling stresses! All of the specimens primed with BR127 and

bonded with LRIOO-172 failed along the primer/adhesive interface

at low loads.

The peel properties of the unprimed specimens bonded with

LRl00-172 were significantly higher than those of the primed

specimens. Failures were predominantly along the metal/adhesive

29

TABLF 10

FLOATING ROLLER PEEL TEST RESULTS

I Fee! StreŽngt (lb/inch wi 0dU)

sublstratx, 720F "25_______

Pl __ix" Ad_ si taiai. ,iohd strfl .ai .

20 24T3 :jone 1,Rj0o-1 7 2 2). u5-5 205,

2024T3 BRI27 LRI00-l7 2 4.0 0-0--1 -D 4.7 O-9- .-

2024T3 SR127 R71).4 41.3 -0--o4-lOU 24 3 1-0-

2024T3 BR127 XISv80 33.7 60-0-40-0 21.7U -D

2024T3 BR127 100-252 44.9 30-30-0-7C 11 .8 s-0- 1- Is

.OJ24T3 a3}1427 .'.A I 4~,0-}5-12 3c . -7--7-3

2u24T3 BRi27 3,:, -7 1 I.4 c 0-' -43 -

:-)024T3 B27 EA6I NW 43.38 Q-0 -j-100D 33.6 3Y-)-I .- 60

IG1TG None LRIO-1 2 11• i. 1 0- - 14.4

606 116 BR127 LRIO0-1 7 2 - 3.0 -'-'

6061T6 6R127 7 114 .37. 2 2 -0--7 T -

606 T P12R27 XA 18 0 142.4 60-0-43-3 26.3 -,- 16-0

606 1T6 IiRl27 00-2f 2 2.' l30--u7. ".-.

3 '2 - 7 22

61T(0.5 512 3- .7 10606 16 B R127 EA) U I' 2-0- i 5 26 0. -,)- -0,',

17

BR] lO0-t1 7 I.-

L)JJ."(S4 [Jozr1 7 71 .i]. [ -- [--t - I%• ]' [-l-6 -•

-)::i 34)

,i34 B 3 KI 2 ' 2- - -

.,t

503 ' 2.; n~13 i I:

interlace on the unprimcd LR1l00-172 specimens hut at relatively

high loads compared to the primed specimens, which failed along

the adlhesiveiprimer interface.

The lap shear test results, discussed previously, and tne

lap shear stress-durability test results, discussed later, failed

to provi.e any indication ,of tie BR127//LRl00-172 adhesive/primer

incompatibility manifested by the peel test results in Table 10.

In general, the LA96,]6-W and the XAI80 adhesives gave the

best peel strength levels at -65-F (-54 0 C) . Tnese were followed

by the un:primed Ll1100-172 system, then R7114 aind LIM00-252.

NNt 1.-1 1n11?, al, the aR382-7 a A-429 sy'stemTis and the lowest

was the 'rir.med LRIOO-172 system.

Generally, the failure locus becomes more interfacial in

natare as the test temperature changes from 72'F (22CC) to -635F

(-5 40 C) . Thus, the primer layer, and its assouiated interfaces,

appears to have been the portion of the bond most susceptible to

low temperature poelinq stresses. After the teLsts were completed,concern was expressed that the primer thickness should have beenr reduced. Since we were, however, interested in joints iepresen•ta-

tive of those present in shelter structures, and not those ideal

for best peel properties, our specimens were prepared with the

same primer layer thickness as used for the lap shear joints.

In addition to the strength levels exhibited by each adhesive

system, a consideration of the failure node and relative amount

of strength decrease from room temperature to -65'F (-54°C) is

also useful. Hence, a brief, general, adhesive-by-adhesive

description of the results follows.

The EA9601NW loses about one-third of its room temperaturepeel strength at -65OF (-54 0 C'.. At room temperature, it failspredominantly within the adhesive layer (cohesive), while at

the reduced temperature, the failure mode becomes more primer

and more interfacially oriented with a mixture of all four of

the modes explained in Ficiurc 9 evident.

The XA180 adhesive system loses about one-third of its

room temperature peel strength at -65 0 F (-540 C) also. This

3 - 1

system exhibits relatively little failure within the adhesive

layer at either test temperature. Rather, the failure locus

is principally along the adherend/primer interface and to a _

lesser extent along the primer/adhesive interface, with a small

amount appearing to be within the primer layer itself.

The R7114 adhesive loses about one-half of its room

temperature strength at -65'F (-54'C). While its failure mode

is primarily cohesive (within the adhesive layer) at both test

temperatures, a substantial amount of primer/adhesive interfacial

failure appears at the lower temperature.

The unprimed LRIOO-172 adhesive loses very little of its

room temperature peel strength at -651F (-54'C) . At both test

temperatures, however, the failure mode is predominantly inter-

facial along the adherend/adhesive interface.

TThe LR100-252 adhesive loses between one-half and three-

quarters of its room temperature peel strength at -65'F (-54'C) .

Its failure mode at room temperature exhibits substantial amounts

of adherend,'primer and primer/adhesive interfacial failure as

well as cohesive failure within the adhesive layer itself. At

-651F (-54*C) the failure shifts entirely to the adherend/priirer

interface and to the primer layer.

Both the R382-7 and MA-429 adhesives exhibited failure loci

in peel which were predominantly along the primer/adhesive inter-

face at both test temperatures. Both adhesives also exhibited

peel strength reductions of over 50 percent when tested at

-65OF (-54 0 C).

Comparing these peel results with the lap sheai results

discussed in Paragraph 3.1, one notes that only the XAI80

adhesive ranked high in both peel and lap shear.

3. 3 STRLSS-DURkBILITY TEST RESULTS

The data obtained trom the lap-shear stress-durabi litY

tests are sunn-narized in fable 11 and illustrated in Frigur-es 10

32

___________________ _________ I _____________--

(A

c c oo n 0C nI o D -m-"u) 0I I - 0 - 'fn en I." o I. -4r4a)I0... .... 4:.. .~0

4 s . . . . . . . v," ,7- l i ,.

Io s. A

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ca i

- ( A..-.-- -, o ,, V•aj~

_ _ _ -, aH

• ,4 "o 44

'0__ --- 0 040I .,0 uID a

o ' ? I i01 I" I -4-,4.,-' ,3

4 - Q 0 0 440 0

. 4 ''' 111 '-1 1o40 4 11 11 1 0 a

0. o414 1 C, 1 o 0 II

.' 0 c0 I I -'4

'0tr

33)

a, 4.

W 0

> V

, .... -1--4... . ..... -. . .. . .. - - - 4I I I

> 4

L14. Z * 4) 1:

-~~~~~~L j- ~ . 4 44 ( 4

0 44 '. 14 Y0 - I j Q4 KI 10 4~ "'44f'-

0 0 c 0f4 c0D'- ' 4 4 ~

and 11. The values presented in this table represent averages -

of at least five replicate specimens.In addition to the hours-to-failure exhibited by each adI

Atesive, the stress level to which the specimens were subjected

during exposure are noted. Since each adhesive system exhibits its Iown characteristic strength and since the exposure stress levels

were set at a percentage of the adhesives lap shear strength at

1401F (601C) , one must consider the stress during exposure as

well as the tirm--to-failure and failure mode in assessing

relative stress-aurabilitv of the various adhesives. IThe lap shear control strength values, upon which the

exposure stress levels are based, are presented in Appendix VIII

along with the individual stress-durability results. The 140'F

(60'C) lap shear control strength values were used to compute

the 40 percent and 60 percent stress levels for use during the

durability exposures. The room temperature values were measured

primarily to provide a means of chccking the quality of the

panels from which these specimens were obtained against theroom temperature lap shear results for the same combinations of

adherend, surface preparation, primer, and adhesive tested durina

the lap shear- portion of the program and discussed in Paragraph

3.1. In 14 of the 16 cases, the room temperature strength values

obtained from the stress-durability panels are within 10 percentof the value obtained previously in the lap shear testing. The

two exceptions both occur on 5052H34 adherends with one (XAI8O)

being ].7 percent lower than the original lap shear result and

the other (R382-7) being 42 percent higher. There are more

frequent differences in the apparent failure mode with 11 of

the 16 cases exhibiting substantial differences in failure mode

froui the original results. For the most part, these differences

in failure mode consist of more failure along the metal/primer

interface in the control specimens for the durability tests than

in the original lap shear results.

II

IA q !fl 00 0)//41- / -- :-

< / C,)

'AI I r o ®l

./ I -4q •

1 / ". % .o ,-,/ / / 00)1 ,.

/<

/ /

>

0 O( -, a

/ - H 'q

r'"" C') 'l e.

Co

N ( -. ,

c43 (-L

(*d '~ rL-• d~ h•il IS-.. -] -I.

4ý

.0:

U)

o 0 ) 0 0 0U() - r-III) ro N~ N - H(!sd ) Ur j0X3 qNQ~lG SIjS Vo

35

roIU, _,0w

0

CN .

C4 ". .,-.

,c--- -- ' (N

O NCT ) r- f,

0 l N-IO Lflto 1c

- C4

:>1

""-I =1 --

o4 I

CC3

I-4

w -4

, J,

C• r- 'r I

o N 0

0N N co-

(isd) 3UflSOdX3 ONIUflO SS~IUS 8V3HS

36

The single most obvious feature of the data plotted in

FirqcurosIQ and 11 is the reversed slope of the curves fo• LRl00-

252 and EA9601NW on 5052H34 adherends. No explanation for this

can be offered unless the times-to-failure and stress levels were

inadvertently interchanged for these two combinations. These

tests were rerun however, using extra specimens left over from the

original LRI0O-252 and EA9601NIW panels. The data from these tests

are presented in T 1 and FilUre 12 and are consistent with

the trend one would expect.

It will be noted in Fiurel0 that the 6061T6 stress

durability curves seem to fall into three general groupings.

One, representing those adhesives with the best stress-

durability behavior includes LRI00-172 (with primer), LRl00-252,

;A4 29, and EA9601N•. The second, representing those adhesives

w..ith inter.Tediate stress durability behavior, includes XAl80,

R7114, and R382-7. The third includes only the LR100-172

adhesive used on an unprimed surface and represents a very

short time-to-failure.

Assuming that the second set of tests with the LR100-252

and EA9601NW adhesives on 5052H34 adherends (Tjah_.) is more

indicative of their stress-durability behavior than the first

set (Table 11) , the stress durability curves for 5052H34 adherends

(Figure 11) also fail into three general groupings. The first,

representing those adhesives with the best stress durability

behavior includes .,1%429, LRI00-252, and EA9601NW. The second

grouping, representing those adhesives with intermediate stress-

durability, includes LR100-172 (both with and without primer),

XAIS0, and R382-7. The third group for the 5052 adherends is

composed only of R7/114 and represents a very short time-to-failure.

Figure 13 superimposes the 6061 and 5052 data groupings on

a single graph for greater ease in visualizing the relative adhe-

sive/adherend stress-durability behavior. It can be seen here

that the general location of the high, intermediate, and low data

yroupings coincide fairly well for both adherend alloys.

In summary, three adhesives (LRI00-2 5 2 , MA429, and EA9601NW)

exhibited consistently higher stress durability than the others

37

A

rJ

W n 000 00 D 0 w

ol 1 1 .1.

41 i I t

V) w 4 -n 4 (N4 .-4 .-4 .

M • t oo t,, .

4J

zI

o -4 to C

0C'J - a0- C 04

-, a ID In• •

N o

r4l (N 0N C4 (N 40

S2•)i. - n- 0 - 4

-,- • {

0• u t n

4 , 4 0 ci

1-4 4

4- k D 40C) '

U, -

0)--"' Q)4~- 0 -4 0A 0 0

0. ý U) -4 -4 04 0 --

(N (N ( N ( 0 4) 0)

24 4 ON 40 )t -

(N C, oo o c0 n '(3

'-4 *I'"~ - -

~!

LI) Q -

W~ C) A

co4 ýC c-*i '4 1 : 9

F-1

u A.

Elg 0

14 -4 (j uP

w 0 0"4

IDI38

,ifi

O---0

-68 8 1:<0

00

(,r) C) I.)

H-r

0 ~ 0000.,-t

39

Ln~

000 0 00000 0 0 0

OC 0 0 A~

(ISd) 36rlSOdX3 ONidfl SS38iS 6V3HS

39

t_,•--,i __. • • .•+~~~~~~~~~... ..... •• _ ++'-••-"','• +•m+,m ,, . .

ADHEREND

GROUP ALLOY ADHESIVES

1 60616 Al, A4, A5, A7 5052H34 ADHEREND ALLOY

2 606116 A2. A3, A6 - 6061T6 ADHEREND ALLOY

3 5052H34 Al . Al. A3.A6

V)

ui 3400 -GROUP I

LL u3 400-

U)

GRU 2• RU

o 3000 A5__-

w2600-

(r 2200I

U) 1800LLJ

o1400

1I000,II1 10 100 1000

TIME TO FAILURE (HRS)

Al* LRlOO-172-NO PRIMER A4 LRI00-252:BRI?7Al LRIOO-172 BR127 A5 M,-A-429.BR127A2 R 71141 BR 197 A6 R382-7-BRI27A3 xAl80O'BRI?7 A7 EA61V;~2

Figure 13. Stress-Durability Behavior Summary.

40

tested in this program. One adhesive (LR100-172 with primer)

performed well on the 6061T6 alloy but only moderately well Aon the 50521134 alloy. Two adhesives (XA180 and R382-7) fellinto the intermediate time-to-failure regions on both adherend

alloys. The last two adhesives (R7114 and LR100-172 without

primer) fell into the low to intermediate groupings on each

a'Therend alloy.

There does not seem to be a consistent relationship

between failure mode and stress durability. The three better

adhesives in this type test exhibit markedly different com-

binations of failure. The MA429 exhibited considerable adhesive-

to-primer failure, the EA960INW considerable failure within theadhesive layer, and the LR100-252 considerable primer-to-metal

failure as well as failure within the adhesive layer. The two

lower durability adhesives displayed dramatically different

failure modes with one being exclusively interfacial between theadhesive and the unprimed metal while the other was predominantely

within the adhesive layer.

3.4 CRACK EXTENSION TEST RESULTS

The data obtained from the testing of the double cantilever

beam (DCB) crack extension specimens are summarized in Table 13

and presented graphically in Figures 14 to 16.

One of the differences between the standard and optimized

FPL etching solutions is that the optimized solution is "sweetened"

by dissolving 2024 aluminum in the acid solution before it is usedfor panel etching (see Appendix I). This "sweetening" has been

found to provide significantly improved bonding. One question

which arose in the course of this investigation was whether the"sweetening" of the initial etch solution should be accomplished

by dissolving 2024 aluminum alloy (as the normal optimized FPLprocess calls for) in the etch solution regardless of the type

of alloy to be treated, or whether the solution should be"sweetened" with the same alloy as that which is to be etched.

Three different alloy "sweeteners" were consequently utilized

in this portion of the program.

41

I

I~ IIC3

r . C C , I I I , 1

o o40 0

. ... ,

"0* -• • '-" • , -

-- A

--1 + 2(N th

'-i 4-4 (N ý 0 N ( C) f -0 CN + + o

, 4. . u a b, ,J7 -17 to 4..C -

(N 'o 0) r- ,' ) ) U

IN 0( a, 0 '

CA I;

0 -o

U' CL4)

q' -4 .4 N -4 - 4 -j c.4 (

.44

c-4- t'- r. t

I) U

In o ) I) o o <3c3. CC) 0V o

3.-t o. o.4 0.. 0

II 2(

L77

CD

C) (M

CD

ci- -r-- -- -

Lt')

C) C)C)

CD U

4---4

L;i I C-

RU -2

LUn

C')ý LO 0

uj -4 V.' I& L, '• C)

(2) CD CD C'L

LmU

C~C3

CD

0

U

C)-

7- (-) CDD C-- CD .CD CD

-41

-4

43

a-

CDJ

ccz3

vC-)v-I

So - c .,.-

.. --- - L1J I--- C

C)) I-

c .. s.l .--I • 1 I.. -11 •,

S-T- C€ J C: )(0 DD

~~CY CNDI OL

t- )

II •I

LLjc:• ,• :•Uo::1

C--, 0I

Ll~j j CjC,,j ~,,LLU 0

CDD

'-4C-4 w- -

(V I4-._

44

__________ ___________________ ____ ______ _____"_

I- T

CDLf. u)LU... . I-. (N .. _ __I"--'- 0--- I-

Lr-r

Lii C ' I--- , (C

2_ 41Q~

' .CL C..C CD

F-J

Sa :knJ

-LJ C-4 (-,j (NJCID CD. _C- ).LUJ C1404C (NJ

LUJ E-'uL-i

CO -

•D CKCI .,-

434

IL

Q) ,

SLtC\ Lfl (CL >CC--)C COý CD (CL

C: CD CCD

45J

After etching, the adherends are rinsed before drying. This

rinse can be accomplished with either tap water or deionized water. -

Some question existed as to whether deionized water rinsing leads

to significant bond improvement considering its considerably

higher cost. This was also examined.

The principle conclusion of the results presented in Table i3 =1and Figures 14-16 is that regardless of the aluminum alloy being-

etched, the etch bath should be sweetened with 2024 alloy for 2

highest bond durability. The reason for this is generally felt

to be the presence of copper in the 2024 alloy, in fact, some

investigators believe that sweetening the bath with copper alone

is sufficient. Examination of the failure modes for these tests

corroborate the differences in interfacial bond quality obtained

when the etch bath is sweetened with 2024 rather than a non-

cop!)r•- containing alloy. The baths sweetened with the

ccpper containing 2024 alloy I.reduced bonds which failed pre-

dominantly in the adhesive layer, while those sweetened with

tthc non-coPer a... ys p rca.Dccl bonds which failed predominantly

at the adherend-primer interface.

The use of a deionized rinse rather than a tap water rinse

appears to be marginally worthwhile. On a 2024 alloy adherend

etched with a 2024 sweeteneC, bath, a deionized rinse produced a

more durable bond, the difference becoming relatively greater as

the aging time increased. Further, the tap water rinse resulted

in substantially more failure along the metal-primer interface

than the deionized water rinse. On a 6061 alloy adherend

etched with a 6061 sweetened bath, however, the deionized

rinse produced a less durable bond. Since these latter two

bomds were both poor due to the use of a non--cojpezi containing

sweetener, the relative effects of the two rinse methods may

have been obscured by the poor bonds.

The last observation available from these results is that

the LR100-172 adhesive without primer is very inferior to the

FM73/BRI27 combination insofar as its initial (up to 504 hours

and more) ability to withstand crack extension is concerned.

46

The LR100-172 adhesive bond, however, degraded less during

exposure than the FM73/BR127 system. It is conceivable that.

had the exposures been extended to a long enough time (60-100

days if the data in Figure 16 is extrapolated) the LR100-172

may have proven the more durable. The fact that these LR100-172

bonded joints fail.ed predominantly within the adhesive layerrather than at the adherend-adhesive interface indicates that

this adhesive forms a bond directly to the bare etched metalwhich does not require a primer layer to impart environmental. . . ...

durability when loaded in a cleavage mode at 140°F (60"C)

47

-1

SECTION 4

SUMMARY AND CONCLUSIONS-1

It was stated in the introduction that the primary objec-

tive was to identify adhesives which have the capability of

retaining a substantial portion of their structural integrity

after prolonged exposure to the combined effects of elevated

temperature and high humidity. This judgement must be based -.

upon the overall performance of the adhesive in a variety of

loading modes and environite.ntal conditions as well as upon

the anticipated requirements of the particular application.

Hence, it is felt that comparing the relative performance

of the adhesives tested in this program in the various different

loading modes and environmental conditions is an appropriate

way to conclude. This comparison is presented in Table 14 as

a subjective rating of each adhesive in lap shear, peel, and

stress durability.

It can be observed in Table 14 that no single adhesive

ranks high in all categories. Henze, the use of only one or

two types of tests for evaluating adhesives for shelter applica-

"tions is inadequate since some adhesives can display good

property levels in one type test and poor property levels in

another. Indeed, the adhesives can be formulated to exhibit

superior characteristics under one or two stress conditions

and environments.

A secondary objective was to evaluate the effect of

selected surface preparation variables upon the interfacial

durability of bonded joints. Two variables were evaluated:

the type of aluminum alloy dissolved in the FPL etch solution

to "sweeten" it, and the type of water used to rinse the

panels after etching. The most significant result of these

tests was that regardless of the aluminum alloy being etched,

the FPL etch bath should be sweetened with 2024 alloy, presumably

because of its copper content. Unless this dissolved copper

is present in the etch solution, bonding surfaces resistant

48

-i

TABLE 14

SUMMARY RANKING OF ADHESIVES

Relative Ranking in Comparisonto Other Adhesives Tested

Aged Low Temp. StressAdhesive Lap Shear Peel Durability

LR100-252 high intermediate high

XA180 high high intermediate

NA 429 high-to- low-to- highintermediate intermediate

EA960INW low-to- high highintermediate

LR100-172 1 high high-to- low-to-intermediate intermediate

R382-7 high-to- low-to- intermediateintermediate intermediate

hJ LR100-172 high low high-to-

intermediate

R7114 low intermediate low-to-intermediate

lon unprimed adherend surfaces.

49

to humidity degradation will not be obtained. The use of

deionized water for rinsing during adherend surface preparation

provides some improvement in bond durability but the added cost

must be weighed against the amount of improvement attained in

large industrial processes. This judgement must also take

into account the quality of tap water available in order to

determine the degree of durability achievable without

deionized water rinsing.

One other testing variable evaluated in this investigation

was the type of specimen used in the lap shear tests. The use

of the preslotted (finger) specimens for lap shear testing

offer no advantages over machined specimens in the development

of shear data since the adhesives evaluated were ranked in

the same order of decreasing strength by both types of specimens. ]Since the finger specimens are more expensive, there is no

advantage in their use.

-50

/S

IFI

APPENDIX I

ADHEREND SURFACE PREPARATION PROCEDURES

Two different surface preparation procedures were used inthe preparation of the test specimens, a standard and an optimized

FPL etch. The standard basic (or non-optimized) FPL etch treat-

ment is described in ASTM D2651, Method A. The optimized FPLetch treatment is described in ASTM D2651, Method G. The

step-by-step procedures utilized in this investigation are

described as follows.

Adherend Etch Procedure

1. Solvent wipe with MEK or acetone.2. Vapor degrease fcr 10 minutcz in trichloroethylene.

3. Alkaline wash for 10 minutes at 155 + 50 F (68 + 30 C)(Note 1).

4. Water rinse for 10 minutes in a continuous flow bath(Note 3).

5. Etch for 10 minutes in the FPL (or optimized FPL) etchsolution at 155 + 5'T (68 + 3'C) (Note 2).

6. Water rinse immediately after removal from etch solutionfoz 10 minutes in an agitated continuous flow bath(Notes 3 and 4).

7. Force dry with a heat gun or in an oven for 10 minutesat 150'f (600C).

:.otes:

1. Alkaline solution consists of:

a. I qalilon tap waterh. 173 gramis Tujrco 421-5C. 7. u7jco 4215 additivc

.FP? c 3)r 1tLutioC" con sist-ed of:

, ' ½•;2 Ir 2H2 r" . 2.. iiwr.•: ;>-•2O4, (rc•.vlnt•

c. 2s c,- ol ]1qs Lv(2v d 21124 a: ,

. - , 2 ;-1-t 1i o ;I . I , -" -

;I a :

dz

part of the Crack Extension, Paragraphs 2.3.2-4,and 3.2-4) a deionized water rinse was used.

4. At the conclusion of the rinse step, cleaned partswere observed for water break. A panel passed ifa continuous film of water was maintained on thesurface for not less than 30 seconds. Parts failingthis water break inspection were reprccessed throughthe acid etch procedure described above. If the partfailed a second time, it was discarded.

It will be noted that the only kifference between thestandard and optimized FPL etch procedure is that the etchsolution used in the optimized procedure has 2024 aluminum alloydissolved in it while the standard solution does not. The

significance of this difference seems to be in the coppercontent of the starting etch solution imparted by the coppercontaining 2024 alloy. If a non-optimized FPL etch solution

is used to treat a copper containing alloy such as 2024, thecopper content of the solution will increase and the solutionwill gradually become optimized. A copper concentration equi-valent to that obtained by dissolving 0.20 ounces or more of2024 aluminum alloy per gallon of solution (1.5 gn/liter)

is required for an FPL etch solution to be considered optimized.During this investigation, the non-optimized FPL etch solutionswere discarded before the copper content reached this level.

Titration to Determine Sodium Dichromate Concentrationof FPL Etch Solution

Materials: - Sulfuric Acid, concentrated - 96.4 percent- Potassium Iodide, crystals- Sodium Thiosulfate, 0.1N (purchased)- Starch Indicator Solution- Deionized Water

All materials to be reagent grade.

Hardware: - Mettl.er Balance- Pipette: I ml, 1/100 ml graduations- Pipette: 2 ml, 1/10 ml graduations- Pipette: 5 ml, 1/10 ml graduations- Pipette: 25 ml, 1/10 m! graduations- Pipette: 50 ml Transfer- Burets: 2 ca. 100 ml Automatic- Burets: 1 ea. 50 ml t,.utomatic- Burets: i ea. 50 ml

52

- Magnetic Stirrer i- Magnetic Stir Bar- 250 ml Ehrlenmeyer Flask- Pipetting Bulb- 250 or 500 ml Holding Bottles- 125 ml Ehrlenmeyer Flask I- 1000 ml Ehrlenmeyer Flask

- 100 ml Volumetric Flask

Procedure:

1. Clean all glassware with Alconox and water, rinse severaltimes with distilled or deionized water and allow to drythoroughly.

2. Insure that glassware is at room temperature.

3. Make sulfuric acid, 10 percent, by weighing 100 grams ofsulfuric acid (concentrated) into a flask (125 ml). Filla 1000 ml flask with 500 grams of deionized water (weighit). Pour the acid into the deionized water while stirring.Weigh additional deionized water into the flask until youhave 1000 grams of solution.

4. Make 20 percent potassium iodide by weighing 20 gramsinto a 100 ml volumetric flask. Add a little bit ofdeionized water and swirl until the crystals dissolve.Add deionized water until the 100 ml volume mark isreached by the bottom of the meniscus. Store in a darkplace -- it is light sensitive.

5. Pipette 2 ml of acid etch to be tested into a 250 mlEhrlenmeyer flask. Drop a magnetic stir bar into thebottom and place on a stirrer.

6. Add 50 ml of deionized water by transfer pipette.

7. Add 12.5 ml of 10 percent H2 SO 4 (by pipette or buret).

8. Add 3 ml of potassium iodide [20 percent solution] (bypipette or buret).

9. Titrate with 0.1N sodium thiosulfate until a straw colorappears -- do this very slowly so as not to overshootthe end-point (from buret).

10. Add 2 ml starch indicator by pipette.

11. While stirring rapidly, add 0.1N sodium thiosulfatedropwise very slowl' until color changes to a light blue.

12. Record the number of ml of sodium thiosulfate usea.

53

Calculations:

Determine the sodium concentration by the followingformula:

rJ of sodium thiLosulfate (0.14 x 4.967 Sodium dichromatelofsoiuhsufae01Nx4.6 - concentration in

2 grams per literof solution

Safety:

Wear safety glasses, acid proof gloves, and a lab coat.

Use Pipetting bulb for transferring liquids. Decontaminate

spills with Alconox and water. For skin contact, wash

thoroughly with soap and water. For eye contact, rinse

15 minutes with water, get medical aid.

Titration to oetermine Sulfuric Acid Concentration ofFPL Etch Solution

Materials: - 0.lN NaOH Solution (purchased)- Deionized Water

Hardware: - Pipette: 1 ml, 1/100 ml graduations- Pipetting Bulb- 250 ml Beaker (2)- Magnetic Stirrer- 50 ml Transfer Pipette- Magnetic Stir Bar- pH Meter- 100 ml Automatic Buret- pH7 Buffer Sclution

Proc~edure:

1. Clcan -li .l lassw.-J.ru with Aiconox a:.d water, ur":thorou;i -.lv n £C- brin.I , t,-L, rooLi tempo rar.u :Th

2. 1 am, ia.:e , s~l ba~cr in a 250 :'i beaker.

Transfcd . :. o" acii Otc'I te the:', aký' us.n:; ý

-6J. .. u, ;', " :n .. 'Wiul rs n:. a tr lfl 2.

V, ] -n:r . ",• L J. ': ], -. l•.•• "- - .' .-! ,- "'. l } - a ! :[ U ' [

7. Rinse electrodes and wipe dry.

8. Iumerse electrodes in the acid solution which you have

placed on a stirrer.

9. Add NaOH (0.1N) dropwise until pH 3.5 is reached.

i0. Record the number of ml on NaOH (0.1N) used.

Calculations:

Determine the sulfuric acid concentration as follows:

ml of NaOH (0.1N) x 49.04 _ Sulfuric acid concentration in5 grams per liter of solution

Safe ty: IWear safety glasses, acid proof gloves, and a lab coat.

Pipette liquids using a bulb. Decontaminate spills with j

Alconox and water. For skin contact, wash thoroughly with

soap and water. For eye contact, rinse 15 minutes with water,

get medical aid.

Adjustment of FPL Etch

Materials: - Sulfuric Acid (Reagent)- Sodium Dichromate (Reagent)- Deionized Water (needed only if measured

concentrations are too high and solutionsmust be diluted)

Hardare: - Graduated Cylinders - size as needed

Procedure:

1. After titration, the concentrations determine how much Isodium dichromate and sulfuric acid to add using thefollowing specification:

Sodium Dichromate 28.5 grams/liter (27.0 - 30.0)

Sulfuric Acid 295.0 grams/liter (280 - 290)

2. Adjust the acid first - remember adding acid changesthe volume.

3. Add dichromate according to the new adjusted volume.I

455 1!I

:I

Calculations:

Example: Sodium dichromate was 21.5 grams/liter.

Sulfuric acid was 215 grams/liter.

To add acid 285-215 = 70 grams per liter

70 _

5- 42.4 ml of acid

(10 percent sulfuric acid has specific gravity of

1.65 grams/ml)

(pour acid slowly - it will get hot as you add it to

the solution)

The new volume is now 1.04 liters.

To add sodium dichromate

28.5-21.5 = 7 grams/liter7 x 1.04 7.28 grams

After adjustment, recheck concentrations by titration.

If the concentrations measured by titration are too high,

the reverse procedure (add water to dilute) must be followed.

Safety:

Acid gloves and aprons, safety glasses. Spills decon-

taminate with Alconox and water. Rinse skin or eyes with

water - get medical aid.

56

IAPPENDIX II

PRi•MER APPLICATION PROCEDURE

The primer was applied to the adherends using the following

equipment and procedures.

2.1 Equipment

The Brinks Wren B (air brush) was used in priming the smaller

bonding area panels (lap-shear and stress-durability adherends)

because it would conserve primer (less over-spray) and give a

similiar spray pattern as obtained with the Brinks Model 15

spray gun used on the larger panels. tl

The Brinks Model 15 (spray gun) was used in priming the

larger bonding area panels (floating roller peel and DCB crack A

growth adherends) because it covers a larger surface area with

each pass of the gun, saving time and giving a moLe uniform

thickness control of the primer.

A Dermitron D-9 (Eady Current) by Unit Process Assemblies

Inc. was used to measure primer thickness.

2.2 Application Procedure

The primer was applied in several coats rather than in

a one or two pass build up of primer thickness. The Brinks Wren

B (air brush) was set up for best spray pattern using 20-25

rsi line pressure and the primer was applied in 10 to 15

passes at a distance of 8 inches (20 cm). The Brinks Model 15

(spray gun) was adjusted for the best pattern at 30-35 psi lineu

pressure and the prirler was applied in a criss-cross ;pattern

of 4-5 passes in each direction at a distance of 12 inches .3U cm,

Thickness measurements were taken with the Lern,)tron D-9

inrstrum-Ient several ti!eOs J.arin1 t I co arse of t.:. [riner au.'l ica-tion until the dusired primer tl~celss hjU beer:, ittacncdd. The

: I

SJ

. . . ..

ccor of the primed surface was noted and the remainder of the

panels were sprayed to visual color equivalence. All primed

surfaces were inspected with the Dermitron D-9 Instrument to

insure that the primer layer was within the desired limits.

Any primed surfaces with visibly obvious defects/blemishes

were also rejected.

2.3 Cure Cycle (both primers)

Air dry for 30 minutes at 72'F (22'C)

100 percent check of primer thickness (manufacturersspeci fication)

Force dry for 60 minutes at 250OF (1220 C)

Spot check for primer thickness

2.4 Storage

The primed adherends were covered with Kimwipes and

stored at 721F (22 0 C), 50 percent relative humidity until bonding.

2.5 Bonding

The panels were bonded within 24 hours of priming using

the manufacturers recommeiided cure cycle.

71

APPENDIX III

PANEL LAY-UP AND BONDING PROCEDURES

The various types of panels prepared during this procgram

are illustrated in Figures 1, 3, and 4. The film adhesives

were stored in a closed plastic wrapper at 00 F (-180C) prior to

use. The adhesive was warmed to room temperature before removal

from the wrapper to prevent moisture condensation on the adhe-

sive. Adhesive pieces were cut to the required size with a

razor knife. These sizes were 5/8" x 9-1/4" for the lap-shear

and stress-durability panels, 3" x 8" for the peel panels, and

6" x 12" for the crack growth panels.

The etched and primed adherend panels, along with the

adhesive, were assembled in the stacking sequence iilustrated in

Figure IIi-I. The assembled lay-up stack was placed in a pre-

heated press and the curing schedule appropriate for each adhesive

was carried out (see Table III-1).

The only exception to the above procedure was for t~he

LRI00-172, a 2-part paste adhesive stored at room temperature.

With this system, appropriate amounts of each component werf.

hand blended on a clean flat surface with a steel spatula until

color homocapnPity was achieved. It was then trowelled onto the

bond area by hand to an approximate thickness of 0.010-0.015

inches (0.254-0.381 mm) and the lay-up stack assembled as

shown in Figure III-1.

After curing of the bonded panels the panels were inspected

for proper alignment (no slippage during cure), and thie glue

line thickness was measured on the lap shear panels to insure

that they were within the acceptable limits of 0.004-0.007 inches

(0.10-0.18 ram)

59

F G Gi ___ _....__<

H

(a) Lap-Shear and Stress-Durability Specimen Layup 'Iodel

Er 1E

(b) floating Roller Peel and DCa Crack Growth Sp,.,cimen LayupModel

A[ ' SB

Specimen Layup (a or b above)

D

(cL ]Bc) L ayu- Stack Common to Both Type Specimen Layut:'s

A - Upper or Lower FlattenD - 1/8" Aluminum Cauls

( - 1/3" Silicone Rubber Sheet- 5 mil Teflon Release Sheet

E - Panel AdherendF - 5 mil Teflon ShimG- Siacor (Thickness of ianel Aaherenc)H - AdCesive (Film or Paste)

V1::uj U il--: . Bonded Panel Layup. Models.

'.) I)

|-

TA H 1, F I - 1.

b*:AJl'• U f ACT U l; I: T H U [ L:4C/ L:C :1".L N D.ED1

ADLHES CURE 3CIIEDULES

Scure cycle :

ldlho0 iV, Lu.1 re T' in-'l 2 mT it.', ra turc.-1'reo s u 2,'ott'Y

R7114 47 + 5 minutes at 280 +_ ',F (138 C) 3 ,

aKCd 4o ' u ) s (276 -•5 69 _

XA-I [ 4 + 5 minutes at 280 + 5°[F (138 + 3Ct1_____ ard 43 * tO psgi (276 + 69 [Pa ____

iAg01NWV.5 W 5 minutes at 25j + I ) OF (121 + 3(-) 2and 4.) L 10 )si (276 + 69 KPa _

LK1,3o-252 4V *_ 5 ;inutus at 250 + 5'F 121 + 3'C) 2and 40 + 10 r.'si (276 + 69 Xp a

I R382-7 1+ 5 vili)uitus a 5L . £0- 121 -1 3"C______ -4'o + 2 276 + 6 O)

x -42, 6!; + 1 5 untut:Os at 253 + 5°' 121 + 11c) 3___ _and '0 + IO si (-27t 69 KPa _____

j : ,'1c -]7. "ilx l0O parts uy oeig(4 t of part A with 18 4

:parts by wcs 'Ih of iart U., +ti; Li S Utci at 185 1 K.f 3 3 )

[ ~ ~a;id i. _ , si ( 7 1 3b .i a,

cu(ur. C'.'c(le Nutegs;

[-. :euir*.a Lure Cycic teXci pt a~; IIotC!.d above).

aa. .re--eat press tLo 250 + 5 0 F (121 + 3°C)].. 2-l¼eeonding Lxturc and p.art into press

at contact prossureC. Aliov 3 to 5 minutes dwell timed. A: pIy 40 4 10 C si (276 + 69 KI a) rcssure

cand increase ,ross tcm;urature to 28 +

F (138 -t 3 C)-c. Cure for 45 4 s minutesf. RCI:,OVe bLorIding fixture and part from press

g ool Lohdiny fixture arid part for S minutes at 1,.T.ii. "ccov. ;art from bonding fixture

i. Ceo). lyart

2. ' a Ilal'- as abovu cxccle t for stue (d}, thic temp.ratut.rcma lied at 2 SC0 + S P (121 - 3 0c') t irouj. t)ut thucur: -c-'u].u

."fl sair• a±-. ] abovo exccept for step (di, tle temuoratUr'-

r. aiurod at 25u 30!" (121 + 320 ) throughmout tI,"

euro, i-cl., and :.te). (,, f"-, curL time, ,ite, wasur rcr-ascu to 6.) 4 5- IlinLrtcs.

"j i r.om ,.: LUd zurc cycole. jor luc-172

P. 1'lai. n boidir g fJxtLu a.d pa i t. j, to a ,r C- I . atCd

yr.:. [ {.P' D i-" 02 + 3,:'1I........... ... ' ¾;, + - , ( 1 2 • 31.~ 12 ,

S ur, f - , -0 M :Ut

d. '( ] [,, ]. i:,j xi11 ur, ýI;d art tc I,-'• VP•t) at 204, S ,., (172• V 3" Pa)

4 a

B i-Vt -, i IU 1; x" _urt I I ni r I idf ri"rt

61

- .- -:' :• •--

APPENDIX IV

SPECIMEN MACHINING PROCEDURES

Mlahined Lap-Shear Specimens

There were two types of machined lap shear specimens Aemployed in this program: those used in the static lap

shear tesLs and illustrated in FiQure 1 (page 5) , and ithose

used in the stress-durability tests and illustrated in Figure 5

(page 12). The only difference between These two types of

specinen is that the stress-durability specimens are 2 inches

(5.1 cm) longer and have a hole in each end. BothL were layed

up in panel form as illustrated in Figure 1-a with five

specimens obtained from each panel. All five speci.nens

were finish-cut simultaneously from a panel on a gang milL

usinc circular mill blades s-)aced one inch apart. During the

milling operation the panels were clamped firmly in; place

in a special fixture to support the bondline during cutting

and eliminate vibration damage. The clamping fixture is

slotted to accornmodaee tne mill olades. After nilling, the

hole position on the stress durability specimen was located

4b, hand measuremeit a-nd drilled to accommnodate the gripping

bolt in the spring fixture.

Preslotted (Finger) Lap-Shear Specmrnens

The finger specimens were obtain2d from a panel illustrated

in Figure 1-b (page 6). The panel was cut into individual test

specimens (five per panel ) by bandsawing through the small

webs connecting the specimens together.

Floating Rolloi Peel and DCB Crack Extension Specimens

The panels from which these types of specimens are

obtained are illust'7ated in Figures 3 (page 10) and 7 (page 13)Four specimetns were obtained from each peel panel and livespecimens from eaca, DCB panel. The DCB panels were 5 inzhes

(15.24 cmw %iae as fabricated. Each of these two types of

AINA

panel was cut into slightly oversized strips on a bandsaw

then dry-milled to their respective final dimensions. The

hole position in the DCB bpecimen was then located by hand

measurement, drilled, and tapped.

63-

APPENDIX V

ADHESIVE PROPERTY

DATA FROM MANUFACTURERS' LITERATURE

Hyso! LRIOO-172

2024-T3 Clad, FPL etch, no primerCure Cycle: 2.5 hours at 165oF (74 0 C), psi not specified

StrengthLap Shear: Exposure Cond. Test Temp. psi MPa

None R.T. 4500 31.0None 200 0 F(930 C) 2000 13.8

14 days @ 200*F(930 C 200 0 F(93*C) 3000 20.795-100% R.H.

Hysol LA 9601 NW

2024-T3 Clad, chromic acid etched, no primer,0.063 inch (0.16 cm) adherendCure cycle: 60 minutes at 250'F (121C) , 25-40 psi

(172-276 KPa) Strength

Lap Shear: Exposure Cond. Test Temp. psi MPa

None -67 0 F(-55 0 C) 5000 34.5None 77 0 F(370 C) 5300 36.5

None 180*F(920 C) 4300 29.61 0 min 1 250'F(1210 C) 250 0 F(121 0 C) 2200 15%1

Reliabond R 382-7

Aluminum, etch and primer not specifiedCure cycle: 60 minutes at 250'F (1210C), 25 psi (172 KPa) ji ~Strength

Lap Shear: Exposuxe Cond. Test Temp. psi MPa

None -67 0 F(-550 C) 4500 31.0None R.T. 5120 35.3None 200 0 F(930 C) 2800 19.3

Reliabind R 7114

Aluminum, etch and primer not specifiedCure cycle: 45 minutes @ 28-°-' (141'C) , 25-50 psi

(172-345 KPa)

I ,StrengthLap Shear: Exposure Cond. Test Temp. psi MPa

None -67 0 F(-550 C) 5990 41.3None I R.T. 6140 42.3None 200 0 F(930 C) 4560 31.4

14 days @ 200OF(93 0 C) 200 0 F(930 C) 2195 15.1% R.H. not specified i__

64

4¢

=. •. -I

Hysol LRI00-252 (EA 9652) - 0.085 lb/ft 2 (0.415 Yg/m2) film

2024-T3 Clad, FPL etch, corrosion inhibiting primer,0.063 inch (0.16 cm) adherend

Cure cycle: 45 minutes at 250QF (1210C), 40 psi (276 KPa)

StrengthLap Shear: Exosure Cond. Test Temnp. psi MPa

None -67 0 F(-55(C) 5040 34.7None 72 0 F(220 C) 4540 31.3None 200 0 F(93 0 C) 4040 27.8

14 days @ 200 0 F(93 0 C) 200 0 F(930 C) 2370 16.3and 95% R.H.

3M AF-180

2024-T3 Clad, etch and primer not specifiedCure cycle: 90 minutes at 235OF (1130C) , 35 psi (241 KPa)


None -67 0 F(-55-C) 4500 31.0None R.T. 5500 37.9None 180OF(82 0 C) 3000 20.7

McCann MA 429

Aluminum, etch and primer not specifiedCure cycle: 60 minutes at 250OF (121'C), 10-50 psi

(69 to 345 KPa)


None -67'F(-550 C) 5030 34.7None R.T. 5400 37.2None 1800 F(820 C) 4520 31.1

65

- __ I

APPENDIX VI

INDIVIDUAL SPECIMEN LAP SHEAR TEST DATA

The data presented here are for the tests and results

discussed in paragraphs 2.3.1 and 3.1.

66

INDIVIDUAL LAP SH]AA TEST RESULTS FOR R382-7 ACHESI'.:VE

O4 MACHINED SPECIMENS PREPAJ.ED WITH STANDARD FPL ETCH

Test Temp. 72*F (22*C) Dry. 200"o (93-C) After Aqing I

dh.hr.1 I SStrength Failure 2 .Sec. S tren ten I Failure-'.oy r er .Ps. a 14ode i. psi. 9a Mode1 I

1H34 1-1 2192 15.1 40-60 3-2 1437 9.9 100-0I-3 '36o 6.3 5C-50 1,7 a.5 90-i-4

!-'.a 40-61 I 4-1 1353 9.3 90-102-2 2396 16.5 50-50 4-3 1387 9.6 9C-'-

2-5 2544 17.5 40-60 4-5 1244 8 .6 90-10

Ave. 2416 16.7 40-63 Ave. 1340 9.2 90-10S.D. $.D 79 .0.

BR1 7 M5F3C . MSFBC I-e. 193 5.1 4c-0.-0- 60 3-2 190 13.6 85-0C- iC'1 -3 ' 4 _ -2 1 6 . 4 0 -) _ -6 1 3 -4 2 3 • ý 13 o • -• i o.

6061-; _____ 11.6 4-1 245i 6 I .

1-5 I 556 176 53-30-50 l -I 583 17 8 8-0-C-2D

- 068 14.3 40-0-'-60 .- 3 2.53 . 0 - -C

I

I

1-1 2349 24.3 40-1.0-0 3 - 2 5145 67. eOO•4u

Ave. 12278 15.7 40-1-0-60 ',Ave. 2442 16.8 85-0-0-1i

S.D. L4 I S.D. 2 1.

1- 310 !459534 32 I1. '

!AXA3950 MSm ,4 5 FPC--

1-1 2646 18.2 80l-0-0-20 1 - 1.636 13 0- ,- .4-3 -516 7.9 7C-.3-0-)-30 i 3-4 165C *i.4 7,0-C-23

1-3 2401 16.c 80-o-0-20 4 1562 4 0.8 70-0-0-302-2 30 I2 13. ' I 4-3 958 i 6.6 -0-24,2-4 21 6. 4-5 4 ia

.241 16.6 -- - AV 167 11.1 6S-0-j- 33S ,D. 265 1.36 SD . 2 6 4.3

1-1 2949 3 -2 43 675 6I-4

1-3 3888 213.4 590---1 3 I c 141. 30C- I-1-3 X7051 3 2J-:7-2 4-1 1846 11. 5 4i-l-0I79

2- )6 2 01C4-3 958 6.6 30-2--

2-2 3263 21.2 10-90-0 4-5 2 13 7.7 90-i0

2-4 3282 239. 60-9--0 [ A4e 1346 13 i. r-'7[-52

Ave. 299C 2.6 i2 A-3

SD. ill D.8 . S-D 398 1 2.7; i

BRI27 .46FBC 6 F 31-1 3229 22.3 5---03 i 223)3 15.4 1 0-0- )-o•

i4,7

1-3 3089 211.2 10-:3-90-0 3-4 1825 l•I , --Eg1-5 3400 23.4 2 -' -04-1 2371 16,3 3)-C- -'2-2 3771 26.-- 20-0-433-0 4-3 2152 14,8 .a 7¢ ,3S

2-4 9 20' 22.1 ic-1 - 9 20- 0 4-I I 2. 56 14.[ -149-0-.-.Ave. S340 Z3.- - Av9. 12 -S.D. 265 1.8 1$-. . 2,4 1.4 I

"' i~mw -

XA3•50i MTFMC .16 FMC1-I .92? 1 0 2 8 -i--2 - 9 3 1 . 40- 3 -•1-1 288a !1 . 90-0-C0-10 3-3 2c85 14.4 --- '1-5 "7.0 13,6 60-a- -0 3--% 17-6 1 1.8 140-0 - 0-oi2-2 321 1 22.2 70-0- -}-30 4-2 22C4 1 3.8 30-0--- 7.2 - 4 3 1 2 9 1 2 0 . 9 •C -0 - 4 0 4 - 4 j ) 2 4 1 3 . 3 1 ( - -0 5 -

Ave, 2?14 2 .4 ec-¢ :> L Ave. i 42 " . 3 - -'- "S.D. i89 ý .3 • S D 41 ] ,

SNC7L 1 - Tested ? 200=? (93*C), after 14 da:.s 1 200•*F j9"• 5-lC0% R -.4.

S2. See Figure 9, page 18.

S~67

- -t

INDIVIDC3•L LAP SHEAR TEST RESULTS FOR iUnl NW AH.SI " -VE

ON MACHINED SPECLIMt-NS PREPA.R-. WITH STA230AIy3.2 FPL ETCH

Test Temp. 72"F (220C) Dry I 209F 932C' After Aging

SprT. T Strength Failure- SP. SP trength FailureI -- =I't1oy ?rimer: No. psi IP a mode .Jo4 s Ma I Md

5052- NoNE IMFNB i MSFNE I13 4 >- 3320 2-.8 98-' ]-4 33 I9 2.7 I 95-5

-3 3170 M.d 2-i 143 - - -4- I ] 2¢ 22 2 80-2 _ 37C ,• .

5- , 2960 20.'. 70- 4-4 420 2.9 90-1.)i 6-4 3390 21.3 60- 6-i 38R0 2.6 95-5

I I[ _ __ Ae.21.3 1 7-.-I AVG. 3J90 21.3 5 7 --=5 Ave. 1 3 r, 2.6 i 95-5S.D. 10u S-0 29

CR127 II, B I I•SF882-4 ;0 19.6 lOu-0-- 1-4 75C0 10O-C--

4-i 3300 20. 7 00-1)-0-3 4-2 757 5.2 100-00--

5-5 2600 17.9 100-0-- 6-1 670 4.6 1000--0

6-5 317, 21.8 100-0-1-1 6-4 670 4.b 100-0-3-0

Ave. 2950 20.3 100-0.-c Ave. 700 4.8 I -- :.-.6:

S.D. 292 1.9 S.D. 54

X.A39 s0 .4 5 FAB M5FsriB2-j 3339 Z•2.3 S C---B 2-2 S30 3.7 100-o-0-0

2-5 3390 21.3 00o-- 4-2 46C 3.2 Oc-'-4- i 3230 I 22.3 -5 4- .46 -0-.-

' .i 3 10O- 5-3 6_ 4.4 I-3'->:-'- 3. j7 5-, 5 6-5 490 3.4

Ave. 300 i 21.4 350 Ave. 530 3.6 100-c-c-:

S.D. 130 .. 4 S.. 70 0.1.,

4,ýC 1- M6 I

T6861- NO4E 20ENS I'

1-2 4860 33.5 40-60 1-4 420 2.9 90-10

2-3 427,0 29.4 90-13 2-5 430 3.0 90-10

3-2 4080 28.1 80-2C 4-1 I 420 2.9 90-10

4-_ 4130 28.5 9C-_ IC 5-2 I 340 2.3 90-ic

6-1 39_, _ _ -_ 6__ I 45IE 3.1 93-,

Ave. 4250 29.3 715-2. Ave. 41950 2.6 90-10S.D. 360 2.5 S.D. 40 0.3

TIIM0I184.

BR327 I3M6"0-,F, -

2-2 42O 3 .3 10-0 -'-1 2-3 12? 4u00

I 3-3 4)40 . 34.1 3- - 3-4 9 " 6.5I 28.3 ioo 4-5 I000 6.4 2 ) 6 0-04-,

} = 5 40 •7. ,9 :-DO .- :'-,5 I 6-1 115C . O -3<

I AV 440 29,9 Avve.. 11c 72 1•.5 -5-.

S..•. 340 2.4 SAv. 1I C. 8

N3O: 3840 26.5 Ia -4 . 4-d 3-30 2.6 95-1-50Re F r 3 pe 14-c 3, 5-C-50-I "-2 3420 23.16 l 3 0-6O - I'.! 'i 5- 520 I 3 9 6 - - -1 6-4 3C•• 34 ,3 -ý-O_-!• j : -3 4 5' 0 3.1 60-v:-4 -.

I . . o . li . . o ..Ave. 3 f4;0 24.4 3 5_O 4 _0 2 iI Ave. 5,), 3 5 6,D ,9 40,-,

NOaTE: . Tetd@20? (3 ),after 34 days .•200*F (93*C), 95-1O0% R.,h. -•

68SI-

INDIVIDUAL LAP SHEAR TEST RESULTS FOR R 7114 ADHESVWE

ON MACHINED SPEC.IJENS PREPUJ•ED WITH STANDARD FPL ETCH

Test Temp. 121F (22/C) Dry 2001F (93*C) After Aging'

Aohe ,r. Spe. Strength Failure' Spec. Streng•eh a;.lure2Alo rmr No. ____ ____ mod _____ mode

1 50ý51 NONE m5l.iO c M~r'NN I" 27.7, 10-90 I 1-2 54 3.7

1-3 3930 27.1. 20-80 1 530 3.7 1,30-O

1-5 4280 29.5 b0-SO0 2-13 8 012-2 -450 30.7 9C-10 2-3 380 2.6 IcC-O

2-4 4t10 31.8 80-20 -5 290 2.0 10O-0

Ave. 4260 29.4 50-i0 Ave 420 2.9 i3O-CS.2. 2.0 2.0-S.D 110 .3

B1~i2 7 MSF8D msnr59 0-:-1.

1-3 438o 30.2 80-0-0-20 1-i 4 a 070.0 o-C-0-1o1-5 4210 29.0 80-C-3-20 2-1 750) -0 o , , ^- ,

22 37 260 8 0-0-0-0 2-3 640 4,4 0 - - -0132-4 .41i60 28.7 30-0-30 2-5 68I 4.7 0-c--Ave. 4_70 26.7 80-0-0-2C 0 5Ave. 7-5 !

I j S.C. 350 1.7 S.D. ncI f -YZ

!XA3950 M5Fý-' 71 I-1- 45CC 30, - - i C- a.C 2 - 7.

1-3 4630 3i.9 0-0-a-- 2 I 1-4 I920 6. 3 7s

- 444 3 .6 i - -- 2-1 6Z-2 4730 32.6 0-c0-43-50 2-3 s00 -,--.

2-4 4430 31.4 2zI 900 20-)- -O

S 31.3 5-)-7j-25 Ave. 0--05.0. 130 . .9 I• S,. -C .3

6C6- N"O:N .4 6FNI I L6l6,6- M -i 5540' 38.2 0-100 I.G - 2 360:- 5490 1 37.8 5-9; 1 -4 310 2.1 i3C-C

-5 540C 37.2 5-.5 -i 340 i ~ -2- l i 64 ID-- 2-3K 2 ,1

- -4 566C 3.C, io-gc 2-5 220

"" 32 5-95 Ave.I _____ $.0. lu~ 270 .D

13, I' 6r I6. 41- 539, -- 37.1 N :OT A-.AIL.ABL-- 3-2 5 ." 5 ?> :

3 C)O - Z ] 3-4 z••2 ? 5 '3 -,'

-3 4 ' 46 i 3.,

4-4 4951 34.1 4 - 4 ,

Ave. Ave. 5 '

2 I

IXA3950 i6FK Z

II$

sýc 38. 7,- -*

S.C. t? . i. 4I

3. ),-ested P c•.3°- aft-r I; I2. See Figure 9, page 18.

69

IIUMMDtV!D L LAP SKEMA TEST RESULTS FOR AX-18C ACESIVE

ON KACHINED SPECIMIENS LPAREPD WITH STAND~ARD rPL ET.H

STest Temp. 72*F (22*C) Dry 200r (931C) After Aging

dLher.j Spec. Strength Failure 2

Spec. Stren5 th Failure 2,lloy Primer NO. pal ,P Mods No. psi MPa Mode

5052 NONE M5FNE M5FNEH34 1-1 4280 29.5 20-80 1-2 2160 14.9 90-10

1-3 4350 30.0 20-80 1-4 2040 14.1 95-51-5 4410 30.4 1C-90 2-. 1900 13.1 90-102-2 4450 30.7 IC-90 2-3 1970 13.6 90-102-4 4580 31.6 10-90 2-5 1910 13.2 95-5

Ave. 4420 30.5 15-85 Ave. 2000 13.8 90-10JS.D. 110 .8 1S.D- 110 0.8

88127 0.8 10 0. 5F

i-1 3340 23.0 30-0-0-70 1 2180 o 15.0 4C-0-0-6@1-3 3(30 25.0 23-0-40-40 3-3 2320 16.3 50--0--5c

3020 20.8 3C-0-1-63 3- 2210 15.2 50-3-0-502-2 3460 23.8 3-0-C-20-5C 4-2 2360 16.3 53-0-0-50

1-4 3140 21.6 30-0-10-60 4-4 40 16.5 40-0-0-6'

Ave. 3320 22.9 30-0-15-55 229C 15.8 45-0-0-5-SS.D. 240 1.SD 0.7

XA3950 .M•SFR, M 5 F.T,,.1 -1 361,:- :4. ) 1 - --1--93 1 1-2 13223 8.4 40-7- 0-'

I83 200107 123 88 -- 1502-5 355C 4,5 I¢-0-10-80 I- 1280 8.8I

2-2 3650 25.2 0-o-1l0•-0 2-3 1360 9.4 53-D-50--2-4 384 . 2-5 1280 8.8 60-2-4u-5

3760 23.. IC-0-•-S8 Ave. 120 8.9 55-1-45-:

,S . . 2 4 0 1 .S . 0 .3

6G61 CN'E M6FNE J 16 M6'T61-1 4850 33.4 10-90 1: -2 1880 13.0 90-10

1-3 5.31: 34.- 10 1c 1-4 12.21-5 490, 33. ! I0-90 .6 20 11.2-2 5240 36.1 - 3 1 1 2.2 -2-4 52 2 " 36.0 -C g - 70 1.7 l: ,

I 1Ave. %:4,c 34.1 :1-90 t Ave. i'5 .i 5-

1 .M . 1.'2 2 32,- 16-..

4 7 3 . 4 234.---5 4641", 33.4 -; - - - . -- 2-5ý 5 5 *- -3-O •3-- 472".' 3 .3 3 -- •-?•,- 236,• -6.3 57 '.•'

" 3"3.- 4--

Ave. 4,:-" 2.ý 3 Ave. 232. i , -.S.D

XA3950 M6F.3 " Ei

- 4 4 . 1?'

Ave. .66.': t3-.C . . ...i• - Ave. 2:,•• 3 40°.- 2.- 4.,S.C. =,. ) .4 [ .Z. .

2 . S e e F i g u r e 9 , p a g e 3.7

70 ,

• ='" - ---- - - - -• -- -• - - • = . . . . . .. . .. . =* - -

._.•_• •m•,•!i e .... ----

MAI

INDIVIDUAL LAP SHEAR TEST RESULTS FOR LR10-172 AH-SIV'.'E

ON MACHINED SPECIM'CNS PREPARED WITH STAN.DARD FFL ETCH

Test temp. I 72*F (223C) Dry '1 20i 0P (93WC) After Aging'dher. Spec. Strength F&IluIe2 Spec. S 2

Rilyv Primer ,N. N s,. Kra Mode Iao. psi M .a " ode11 4

505.- NONE MSr-NA IM.5F!; IH34 4-1 2750( 19.0 i00- 4-2 1 206C 13.8 0

4-3 2710 is.7 1Q3-0 4-4 32 16 I(-.09-5 .2850 0-6 0- .1 2820 19.4

?-2 38870 26.7 100-,0 7.3 28900 1 --4 2970 20.5 100-0 7.5 251 .2 1

Ave. 3030 20.9 ICC-) Ave 251- 17.S.D. i 4_80 3.3,_ 2.CI

-3 25; 1.3 100---- I- 2080 j 14.3

-, .-.- 1.3 I -1- - Ai 2783c 19.2 1 J-

7'-2 2-. i .

7-4 37170 26.0 0--0 .2460Av . .. 11.

Ave. 3180 21.9 100-0-Q-¢ Ave. 2558 17S.D. 633 4.3 S_ _ . 330C 2.'

XA3950 MS F.XA i0 5 F'M.ALA

1-3 2383 '-4 ------ ,- . ') O ..- O

1-5 3400 23.4 Ic--0- 4-2 19 13.6 I-4-3 2730 18. , I1 -c -9C -. - '890 13.3 a0-,-20--

SA90 e 1-,- -. 0 136I .D 320 2. ,.7

606-- N NE M6FJA x 6 A A

T6 1 -2 3350 23. 10 - - 81¢ 19.4 10,-02-3 3360 22.3 200-80-,Ave 3312 0 1 22.9 1,-0-0- - 4-A 301 21C.7 10

i S-4 . 580 17.3 100-0 I-i 3.23 2-.3

6-5 .15 21. 7 '-U-2 2194- 20.-0 i1A5 21.7 ICt -O Ave 2940 2-.3 '0

,,- 295.. 330 2.3 10S.D. ' j l -

X6F3A :-!C "SAl-, 3361 23.2 9 - 5- - -2.2

34480 23.2 10- -7 -4 2.9-!-23010 '' 1' 0-3 --

4-3) 2720 -8.- 7 01-c-c.-0 4- 4 -35) 1E.2'-'-5- 4 30190 -"1.3 1 0 •-" 5-5 - • ' 6 3 I 3 ->6-3 279*0 i9.2 !CZ 3 2- - 195- 13.4 IZ - - -:Ave. 31-56- 21 2. 1-' - . .' -

S.D. 330 2.2 ' Ave 23D. 7 210

iXA3950 M6 FY-A ,.A

:I

- 2 -C 23. 35-2-7- 15.95 j4-3 . 3,41--.6.6

6- 73 1921233- i ~ 1.

Ave. 3 5-,)2-2b85 3-5- Ave.I A

I..

S,• 0 '21 ;, a 1-ter i .2 2 C, :1 R..!!

2. See Figure 9, page 16,

I 21.5

IND:VZUgAL LAP SK 1 \ TST RESULTS PCR t.-? AL1ES:•-E

CN FINGER SPEC:ŽMENS P?.PAR-ED eITH iT1It FPL 77T!.

?6st Temp. 722F (22zc; :r-' After Ag:rgi ?.s I•'=•e I -. f2'' 9 • fe g n )!

' e.. Spec. Strength Fa ' ,ire" zepec" ' t re -t~ i FaUl-re

1-3 -- '.,Mode - I 7ode , •5 o p.6

:--•~ ~~ ~~ _•o -• - 20 4.3 -0A-e :- c6-. 3

3-4 0)" ; .... ... .5

1-, )2' •- • -------

o' i .. . 0C-

- -• 3 . • 2- o 6.3 6-C

p . .. . .. . . ..

.- 4 3 5:1C 2 '4.4 .- -4 '-6" 2-=- 7 • 5 3 3-.%-:, -,Ave. 7 Ave.

, . -I : + . 1 .3 . •1.iS.D. 13 ' 180.

XA3950 ' -5]•2ii: ' C--- 2 :44-

4-'407 '3 22 L '- -, 11 -3 ' ; ) 1 -o- --. .

2- 4 'I -, '.- -: i " 3 1 .- 2 1"

Ave. Ave. i

,7 .,- 4 - 6.,

u'-' •" 'i'. • i :-•6 J :--.62-. IS3 7 j 2-4 1- -

I- I (.?I 24 5 3 - -I 1 "' .I'-•

I -i 3 '7- t 2-3 !I. - -t4 3664 -5.

Ave. I0 70 i . Ave.-I. 1 3 - 7' . I.e 1. 44

'.4 2' f. - .

Ave i i I Av .- :

I- )) ' . .-'•-+ .T -' . .. I "- 1 - ' - "

I "

3 .I-. .D. I -iv . "' iC - -

I- 4 4 ! ? -' - - i ' - ' -4 4. " 1 2 - . ..

2, See FIgure 9, page 18.

-..

:NDtV!DCAL "S-. SKNAA TEST PESULTS oFop 9601 :ir2 CI H-SIVE

ON4 FINZQ SPECUJiS PREPA.RD WITH QVU-. MIED FRL ETC4

Test res,,p. 71 (22) DrY 2I OrF (93*C) After Aging

r e Stren1th Failure snec. I Strer thMP a Mode i .0. Mcde

Ave. : 1- -- .Faeue

_ _ _ _• _ _ _ i _ _ _ _ _ _ _

3.,:

I -"I 4 - I 1''0 i ec9-::

' ' A-3e7 1. 10 2

ý.D D I.S'-•ve AV

, i

Ave.-:=

F. I ;B

- I ,.-., I

I; I I v•-" ' i-. -. 2- " C

I I.I

S I

• i-4 ' .t ., e .- • -

I AI . ;ve . .. .

ID

, 3

I I

I_ :-_ _ _ -- _ _ _ __.-_ _ _ _ __,-

I .*'\*- .'fl -2 •:• :w; I

I . - J : .I -.- . - , 0LI .. : - -i. -

: IA~e.'f""et, .'-.-t:s-' Ave. ,' -3-.t5 < . : -. 2 -

2. See Fi.gure 9, page 19.

-n

.-

9

INDI'flUAL LAP SI4SA.R TEST RESULTS FOR R 7314 ALKHSIVE

C4 MACHINED SPEC.'N.'4 PrPAZC WITH 0't'TIxzzL Fp. F-TCH

Test Tenp. 7 (22W) Cry "2007F (930*) After Ai.ng

dher Spec. Strength F rL re Sre.e¢ , tren ,.,gtIm•d.rSre.I.aMde ; p.• 'a Mode

N,'E 1SON • ,

1-3 I-i :3 6.1 40-60

1-3 43C .j.. !-4 180 7.2 40-61

2-2 ..86 2- a'-6-O 4. 50-50

S.D. 260 8 S.O. 150 .

-. ., 420 ,..I

48700"44 II1 -3 8-", 33.6 .. ."3- 960 6.6 C-0-1,3-I00

Ii-5 484C 32.1 .. .2,-1 611) 4.. - - - S

2-2 413- 31.9 0-0-30-70 '2-3 5508 -,- 10

.43 2.12- 29CJi

. 422 29.20- -- 4-3--7

XA3e5 M57 35. 0 YV-60

0-. 4330 33.1 .3-C- 2390 440 3.0

1-3 I -4 'I ý 8

2- • 3 33.- 3- -4-ED ,-3 8,-' 5-.5 3-6-O- - c09SOJMOMD 3-

- 4970 70-0- 30- 650 4.5 0-0--C

4810 33.1 1-0-25-60 IiAve. 590 4.1 2-0-0-100

S. 130 0.7 S.D. 160 .1 i

6361- .N E 6D6 . IT6 4-.3 070-30 960 6.6 40-60

-3 5690 39.2 60 -40 1-4 SrO 5.9 50-50)

39.0 a - __ 3 - 1I 570 3. 3C-70

-3 45782 33, 0-090-80 555 3.9 5 -

1430 32,4 --- 90 2-5 620 4.3 4C-60

Ave. 5569 39. 5 35-65 AVe. 820 5. 40-6aI s o - .0S.D. 1180 1.2

IIBY6-!5 .,:c 36 .0 - -Lo - 9 -- 2 5 7 C 3 -3 NOT A A L;

i-3 482D 33.2 0-0- 20-80 -1-4 555 3.9

2-2 5500o 3ý.-) 0-0-:--80 2-3 6 9 4.8 '!I.1-4 5590 38.5 - - -80-5 89C 6.1I I...

Ave. 5210 36.D 0-C-10-9g Ave. 680 4.7 410T AVAILAHqS.D. i s 3.c s0 132 C ~

XA395I M6CY I

K-.3 37 Zh 0- 70-:•- '-2 r40 5.31-- .

*-3 5 -- ? 5.' -}.4.

I- ,'0 ; ] . -'-2 ' I' -I VC 3.. -S O - C

IIi -I Ave. •. ' 7 -. ], 7} i" Ave. ;30.' - -l

NOT2ES: 1. Tested . 2'Q0i I33' , aftar , Di.':) t.u " (92., . ":-1."J' i.. .

2. See Figuro 9, page 18.ji. Adherend Failure. 74

74I

S.......... i. -. _....- .. ----U-

IlNDIVIDUAL LAP SHZAR TEST RESULTS FOR AF-180 ADHESIVE fcON FINGER SPECi.M4S PREPAPED WITHOPTIMIZED FPL ETCHI

letTm.72'F (12'C)_Dry_____ _ 1 2;30.F_(931C) After Aqinq1

Ahr * Sp.c. Strength a&.lure 2 Spec. Strength FPLure 2

. .. .loy Primer 140. pal, Ma Mods i0. I psi., a Mode-52 Nu%ý F 5ONE F iN5052 FSO I ]H34 1-_2 ] 2080 14.3 10-90 1 -1 1050 7.2 ")1-90 ="

1-4 2320 16.0 10-90 1-3 1110 7.6 10-902-1 2120 14.6 10-90 1-5 1090 7.5 10-91-2-3 2020 13.9 10-90 2-2 950 6.5 10-902-5 2170 15.0 10-90 2-4 1100 1 7.6 10-90

Ave. 2140 14.1• 0-90 Ave. 1060 7. 3 10a,,, 20 C..q S. D - .

I I22 15.3 0-0-0-100 1-1 1080 7.4 0-0-0-103-20 15.3 0-0-0--1.X I1-3 1110 7.6 -0-¢-1,0

2 21r. 15.3 0-C-C-iO C 1 .- 1190 -0--5-1

2-5 154 16. 0-.- J • 5 }! 2-4 1140 7.8 O t ,-t

Ave . 4 - Ave . 1 2 0 97 C- 0- - 100:,. . 10.. ' -.D . 9 0 iS.. 70 S. , 0 O

ZA3950 F50K• T F5OME

-1- 263 18 . 1-- - "-1 370.- 247.- 7 ; * v 3 .% b : - - ., 1 . .' I' ' •

2-2 2142' 16. - 1.90 a.:2-4 245-) 16.9 -- 2-4 1270 8.7 0-0-0-100

I-

A~~e.~ I--3-c C- -

. 2490 .- Av . 1 .)20 1 9. 0-

5 - . i) ,.*LJ 3~'~

3.D. 19? .5 ]. . 90 .

F6C•II

S1-4 J-22ý 2-ý.2 10- 4"0 1 -3 1490 10.3 3 - 730l 2- -33 ), 2-,. " 1 C - 9: - 39• i . ,-AO3- 3 27 2:.- IL-90 139. .-5-,

2(-' IsAv e. 3 '' .4 1 - . A. • ' 1 .4 0,- 703S .D. 0 I '"i ' " , 1 , 3.

II - . Z ; 3 q' 1 - 7 "-..3; . j l i : l ' ' . 7 A ' - [ I - - i :

Av- -4 Av'F6-X.F m

A' Ave

2 . 4 ýe li u r , p a e . 6 . . . - ,• - • . . 6 . .

INDIVIDUAL LAP SHEAR TEST RESULTS FOR LRI00-172 ADHESIVE

ON FiNOBRR SPECL'ENS PREPARED WITH OPTIMIZED FPL ETCH

Test Temp. 72*F (22*C) Dry 2006F (93*C) After Aging 1

ddher. Spec. Strength Failure 2 Spec. Strength Failure 2

Riloy Primer No. psi MPa Mode i1o. psi We a Mode

5052- NONE F5ONA F5ONA

H34 1-1 3290 22.7 100-0 1-2 2840 19.6 100-01-3 2470 17.0 100-0 1-4 3020 20.8 100-01-5 2600 17.9 100-0 2-1 2960 20.4 100-02-2 3570 24.6 100-0 2-3 2690 18.5 100-02-4 4060 28.0 100-0 2-5 2420 16.7 100-0

Ave. 3200 22.0 100-0 Ave. 2790 19.2 100-0S.D. 670 4.9 S.D. 240 1.7

BR127 F5OBA F5CBA

1-1 3430 23.6 100-0-0-0 1-2 3150 21.7 20-0-80-01-3 3210 22.1 100-0-0-0 1-4 2890 19.9 40-0-60-0i-5 3190 22.0 100-0-0-0 2-1 2990 20.6 60-0-40-02-2 4310 29.7 ---- 3 2-3 3030 20.9 40-0-60-02-4 4360 30.0 ---- 3 2-5 3130 21.6 40-0-60-0

Ave. 3700 25.5 100-0-0-0 Ave. 3040 21.0 40-0-60-0S.D. 580 4.0 S.D. 110 .7

XA3950 F5oMA 25ozA

1-1 2550 17.6 10-0-90-0 1-2 I 2720 18.7 10-0-90-0I -, 2720 18.7 20-0-80-0 1-4 2970 20.5 10-0-90-01-5 2670 18.4 40-0-60-0 2-1 2420 16.7 40-0-60-02-2 4320 29.8 ---- 3 2-3 3020 20.8 20-0-80-02-4 4340 29.9 ---- 3 2-5 2770 19.1 50-0-50-0

Ave. 3320 22.9 25-0-75-0 Ave. 2780 19.2 20-0-80-0S.D. 920 6.4 S.D. 280 1.9

606 1-1 NONE F60NA k•N

1-1 4800 33.1 100-C 1-2 3160 21.8 100-01-3 4850 33.4 1i00-0 1-4 2960 20.4 100-01_! I-5 4900 33.4 i00-0 2 2780 19.2 100-0

Z2-2 4500 31.0 100-0) --3 2770 19.1 100-0,2-,4 4460 30.7 100-C 25 2750 l 19.0 100-0

Ave. 1700 32.4 100-0 iAve. 2880 19.8 100-0S.:). 210 1.4 S.D. ' 180 1.2

;[l••FSOBA F6BA

1-1 4100 28.3 0-0-100-0 111-4 266Cý 13.3 0-100-0-02I -3 I 4120 t 29.-1 0-0-i00-0 [-4 3330 23.0 0-i00-0-01-5 4190 2B.') 0-0-100-0 !- 3640 25.1 o-100-0-02'-2 1 4250 29.3 0-0-100-0 _-3 305C 21.0 0- 100-o-)

2-I 4400 30.3 0-0-I00-0 ---93 0.2 0 0-•'Ave. 4230 211. 1 O-Q-I00-0 ve. 312C _i5 -00-0-•

S.D. 110 .•i S.D. 38C -,.6

iXA ]950 1F6OMA F6OMA

1-1 4810 33.1 3--0 - i- 37C 3 2 00 I<-!-3 .1670 32. 2 J- -]I,- - 3160 21.8 g O 1 0 '

4. 4 ,14J• 30. J' 0-0- [,')•-0 z-1 272C'. 18.7 10-0-90-O"- 4450 3C,. - •0 l7. - 3100 21.4 o-0- i00-C}

•-; Dl:,• ] ., ,-o- 100-.-,- 3030 2 9 10-0 9 -

Ave F150 31. 1 ,-•-O - Ave. 3080 1.2 -- 5,1. . 80 S. .D. 2 0 .

'ir/[3' |ested %12r)o-r' (93-(:), after 14| Mly I 2)•? ,"5 1)• R.2. see Figura 9, pagea 18,

76

INDIVIDUAL LAP SHEAR TEST RESULTS FOR R382-7 ADHESIVE

ON FINGER SPECIMENS PREPARED WITH STANDARD FPL ETCH

Test Temp. I72*F (22*C) Dry. 200*F (930C) After Aging1

dher. pec. Strength Failure Spec. Stren th Failure 2

I rimer . psl. tPa Mode io. psi MPa Mode

SC 52- NONE F5FNC FNCH34 1-1 2525 171.4 40-60 1-2 414 2.9 90-10

1-3 1 2727 18.8 30-7u 1-4 343 2.4 90-101-5 | 2525 17.4 30-70 2-1 276 1.9 90-102-2 2590 17.2 40-60 2-3 310 2.1 80-20

2-4 2549 9.0 40-60 2-5 180 1.2 90-10

Ave. 2565 17.7 35-65 Ave. 304 2.1 90-10

S.D. 92 0.6 S.D. 86 0.6

8R127 F5FBC F5FBC

I-i 2350 16.2 40-0-0-60 1-2 1020 7.0 90-0-0-1i

1-3 21.4 70-0-0-36 1-4 940 6.5 80-U-0-20

1-5 2700 18.6 50-0-0-50 2-1 700 4.8 80-0-0-20

2-2 2600 17.? 40-0-0-60 2-3 1220 8.4 90-0-0-10

2-4 2650 18.3 50-0-0-50 2-5 850 5.9 90-0-0-10

Ave. 2680 18.5 50-0-0-50 Ave. 946 6.5 90-0-0-10

S.D. 271 1.9 S.D. 194 1.3t]XA3950 F5FMC F5FMC

1-1 260U 17.90 40-0-0-60 1-2 1280 8.8 0-0-0-100

1-3 2800 19.3 40-0-0-60 1-4 1 1320 9.1 5-0-0-95

1-5 2650 18.3 40-0-0-60 2-1 1320 9.1 10-0-0-90

2-2 2o00 18.6 30-0-0-70 1 2-3 1204 8.3 1O-0-r-O0

2-4 2700 18.6 40-0-0-60 2-5 1200 8.3 20-0-0-80

2690 16.5 40-0 Ave. 1265 8.7 10-0-0-90

S0.D. O 0.5 S.D6 60 0.4

1 601- NONE F6FNC , F6FNCT6 - 3630 25. 10-9C 1 1 544 3.8 I10-90

i4 320C 22.1 0-106 -3 41E . 95-5- 320 24. 1-5 418 2.9 80-20

S2-3 13653 25.2 30-7 22-2 694 4.8 90-10

2-5 3786 26.i £-9s - 704 100-,

Ave. 35• 24.5, 10-91 1 Ave. 555 3.8 85-15

221 i. E._. 140 1.o

BR27 F6FBC 6F BC

L-1 474( 32. -, 0-0-20-90 C-- 2040 14.1 I 20-0-0-6!-

-3 432 29 -C-20--4 199: 13.' 30-0-0-70

1-: 13Y,)-0-30- 7,; 1345 9.3 10-0-0-90

I-'2. 4ý I . -0-1 2- 1192 8.2 10-0-0-90

-4 ,3--- 2-5 1-194 8.2 10-0-0-90

Ave. 417" 2t3. 8 0-0-20-80 Ave. 1553 10.7 15-0-0-015

S.D. $ ~ 31 5 2 .4

XA3950 F6ý'MC1 47 3 1 -'io -i2 1549 30.77 40-0-0-60

4- 2.4 (j . 1 - 90 1,1 .1531 1^. 50-0-0-50i-2ý ý3 47 , 3C,0 l.0-053140.

-418. 2 .1 11T A'V'AILABLE 1-I 1260 8.9 C0-O-0-40- ,1 3i I. :--Og) I 2- 1495 10.2 50-0-0-0-

' |: 3. 10 .- F - 2-5 1569 10.8 60-0-0-47

Ave - 1 3A :, 14ui 10.2 50-0-0-50, ~~~S.D. 1 . t3.D. 31 '',

S:;o T E: I . T a Ittd q 2() 0 "F 19 3'C ) , tft et I,^ l,',,y .• 20! C " (,)3 r;) , 9 5- I00 % R .Hl.

3.0..... ......................... I 08 ______

2. see riqure, 9, page .

INDIVIDUAL LAP SHEAR TEST RESULTS FOR 9601 NW ADHESIVE

ON FINGER SPECIMENS PREPARED WITH STANDARD FPL ETCH

Test Temp. 72'F (22*C) Dry 200F (93C) Afterkdhoer. Strength- Failure2 Spec. Strength Failure 2SSpec. Srnt4.1.oy Primer No. psi Ma Mode L4o. psi Mode

5052- NONE F5FNB FSFNBH34 1-4 3380 23.3 20-80 1-3 270 1.8 100-0

2-5 3280 22.6 30-70 1-5 290 2.0 100-04-1 3440 23.7 20-80 3-1 180 1.2 100-04-3 3920 27.0 20-80 4-2 180 1.2 100-04-5 3470 23.9 20-80 4-4 220 1.5 100-0

Ave. 3500 24.1 20-80 Ave. 230 1.6 100-0S.D. 246 1.7 S.D. 54 0.4

BR127 F5FBB F5FBB1-2 2800 19.3 90-0-0-10 1-1 1140 7.9 80-0-0-201-4 3000 20.7 90-0-0-10 1-3 980 6.8 80-0-0-202-1 3280 22.5 90-0-0-10 1-5 880 6.1 60-0-0-402-3 3330 22.9 90-0-0-10 2-2 560 3.9 30-0-0-702-5 3030 20.9 80-0-0-20 2-4 580 4.0 30-0-0-70Ave. 3090 21.3 90-0-0-10 Ave. 830 5.7 55-0-0-45S.D. 219 1.5 S.D. 254 1.8

XA3950 F5FMB F5FMB1-2 3300 22.7 40-0-0-60 1-1 780 5.4 100-0-0-01-4 2800 19.3 20-0-0-80 1-3 680 4.7 100-0-0-02-1 3000 20.7 40-0-0-60 1-5 440 3.0 80-0-0-202-3 3400 23.4 5-0-0-95 2-2 600 4.1 95-0-0-52-5 3200 22.1 10-0-0-90 2-4 440 3.0 60-0-0-40

Ave. 3140 21.6 25-0-0-75 Ave. 590 4.1 90-0-0-10S.D. 241 1.7 S.D. 151 1.0

6061- NONE F6FNB F6FNBT6 2-2 4420 30.5 10-90 2-1 260 1.8 100-0

2-4 4760 32.8 10-90 2-3 330 2.3 100-03-1 4850 33.4 10-90 2-5 260 1.8 100-03-3 5030 34.7 10-90 3-2 570 3.7 100-03-5 4790 33.0 10-90 3-4 530 3.7 100-0

Ave. 4770 32.9 10-90 Ave. 390 2.7 100-0S.D. 220 1.5 S.D. 150 1.0

1BR127 F6FBB F6FBB1-2 4980 34.3 10-0-40-50 1-1 1850 12.8 30-0-0-701-4 5180 35.7 10-0-30-60 1-3 1940 13.4 40-0-0-602-3 5040 34.7 10-0-30-60 1-5 1110 7.6 10-0-0-903-1 5080 35.0 10-0-40-50 2-2 1630 11.3 50-0-0-503-5 4730 32.6 10-0-0-90 2-4 1730 11.9 60-0-0-40

Ave. 5000 34.5 10-0-33-60 Ave. 1650 11.4 25-0-0-75S.D. 162 1.2 S.D. 320 2.2

XA3950 F6FMB F6FMB2-1 4900 33.8 0-0-10-90 2-2 1660 11.4 70-0-30-02-3 5020 34.6 0-0-20-80 2-4 1790 12.3 80-0-10-102-5 4760 32.8 0-0-10-90 3-1 890 6.1 70-0-0-303-2 4960 34.2 0-0-20-80 3-3 1140 7.9 10-0-0-403-4 5020 34.6 0-0-40-60 3-5 1280 8.8 60-0-0-40

Ave. 4930 34.0 0-0-20-80 Ave. 1350 9.3 60-0-10-30

S.D. 110 0.8 S.D. 370 2.6

:JOTEs 1. Tested @ 200P (930C), after 14 days 4 200*F (930C), 95-100% R.H.2. See Figure 9, page i1.

78

INDIVIDUAL LAP SHEAR TEST RESULTS FOR R 7114 ALHESI .E

ON FINGER SPECI.MENS PREPARED WITH STANDARD FFL ETCH

I Test 7em•. 727F (221c) Dry I 2001F (331C) After Aging'

lhdher. 'Spec. Stiruent FSpe. I Strength I Fa;lure4

ýtloy Primer No. psi Mi's Mode ,Jo. ips f. MS a Mode -

0443 "9.6 .1-0--6C 1-2 4 3Ic 1.4 1' -o -C1"3 400c t 27 . 6 1ý,0-O--90j a-o' 1 .2 11-0-1--.-

1-5 50 28.7 2-30- 10-> I 2 1 1.5 I 10-3-0-C2-4. 4340 288 ¢- - -0 2-] lD i . 0 - - -

24340 9.9 20-i,-G-80 2-5C 1.5 10o-O-&-0

Ave. 4130 28.5 15-0-0-85 A 2v 0 1.4 102--0-.S.D. 18 I i S.D. I .!

"- 37a 2C. 130--- -2 550 _- b--0- IC

i-3 150 24.8 100-O0-0 -4 550 3.8 -0-0-100

_i 5 23 2. - 2-1 1I 713 4.9 0-0-C-1oO

-3' 26.) 10-0-Sc-__ 2-3 6S0 4.8 b0-3-3-90"" 3. 27.4 30-2-nO 1 $ 636 4.3 10- - 9-ý'

2Ave. 5 2.• 65-3-3 - e. j 2- 3 4. 3 -

s. 26C .8 S. $ -6

XA3950'ESFMD IFMD:- 3510 24.2 !- 4'S . 1-0-0-90

7,- .4 4 -0--6¢ - ; 2.4I--

1 - 47.9 2 =.9 30-3-0-70 2-3 32DZ 2.2 1 - -- 9

, i-4 .370 :3.2 4-0-,,-6I 2-5 19 0 -0-0-

Ave. -3. 2.1. 7 3-D--70 Ave. 310 2.12 S.D. 2_0 1.6 _ _ ._. 80 .6

I-Iu I;: I ;D 6I' 1- C5 34.8 10-9' 1-2 360 2.5 0

i-3 5430 37.2 ID-90 340 2.3 100--- 440 30.4 5-9S 2-1 320 2.2 100-0

15690 . 10-9 2-3 380 2.6 170-c

* 2-4 6080 4.9 2--80 2-5 38,0 2.6 100-2

A3:e. 36. 2.4-fl'-Ave.. - Ave. 25, 2.4 0-0-S.D. 2 oC.* S.D. j 643 4.4 I _._. ___.ii EFBE

i~4 -,j.,3 [•?'[-4 44. 4 - . 4' 0-0- - it '

37. 4 3-C-6C- -3

,3 63-9 . -2 34 2.3 - 2 -

33.) -. 2-4 400 2.8 0- -'3-Ave I -0:-Bc

;ve. 5 170 37.5 23-0_-0-1S Ave. 490 3I. o -DS S.D. -9 •.. S.:- 141.

XA3950 Ir6F.1F 6 Fi R.D.in

-3 - I • 80 1 -0-.-0-' 3 . D--40-6'-51 4 10-0--0

i .3 - 55.2 20-0-.'-623 • 9 3"., - -1 - 0 I23 43 ? .3 9- - '-)

Ave. I"- 3"i.7 K-0-25-75 4.8 l- -l.-00

I se. !3).7 7: o .1.33.3. l•U i.O i] S.D. 14 .

A2E -. le~t'td 2�2�}"F 093C0 , after 14 davr'. 3 >'i 3".;, )5-i:)% R A.

2. See Figure 9, page 1i.

79

INDIVIDOAL LAP SHEAR TEST RESULTS FOR AF-180 ADHESIVE

Off FINGER SPECIMENS PREPARED WITH STANDARD FPL ETCH

Test Temp. 721F (221C) Dry. 2000F (93*C) After AgingL

%dher. Spec. Strength Failure2 Spec. Strength Failure

2}%lloh Pimr. No pstreg. FModr

5052 NONE F5FNE F5FNNE

1134 1-1 3700 25.5 20-80 1-2 1440 9.9 3G-20

1-3 3800 26.2 20-80 1-4 1580 10.9 80-20

1-5 3500 24.1 20-80 2-1 1350 9.3 20-80

2-2 3150 21.7 10-90 2-3 1480 10.2 40-60

2-4 3300 122.7 10-90 2-5 1460 I10.1 60-40

Ave. 3290 24.1 15-85 Ave. 1460 10.1 55-45

S.D. 270 1.9 S.D. 80 _0_

BR127 F5FBE F5FBE1-1 2840 19.6 30-0-20-50 1-2F | 2080 1.4.3 20-0-30-90

1-3 3140 21.6 40-0-20-40 1-4 1920 13.2 30-0-30-40

1-5 2860 1.9.7 30-0-30-40 2-1 1380 9.5 0-0-0-1002-2 2850 19.6 10-0-10-80 2-3 1570 10.G 0-6-10-90

2-4 2700 !8.6 10-0-10-80 2-5 1320 4.1 0-0-0-100

Ave. 2880 1.8 25-0-15-60 Ave. 1650 11.4 10-0-15-75

S.D. 160 1.S S.D. 330 1 2.3

XA3950 F5FME F5FFME

1-1 3210 22.8 0-0-20-80 1-2 1430 9.9 60-0-30-10

1-3 3470 23.9 0-0-20-80 1-4 1470 10.1 70-0-20-10

1-5 3430 I 23.6 0-0-20-80 2-1 1410 9.7 0-0-40-60

2-2 265C 18.3 0-0-10-90 2-3 1310 9.C 0-0-30-70

2-4 2500 17.2 0-0-0-100 2-5 1310 9.0 0-0-30-70

Ave. 3070 21.2 0-0-15-85 Ave. 1390 0.6 30-0-30-40

S.D.I 460 2S.D. 60 0.4

.t , I---.

606k NONE F6FUNE F6FNET6 0-6 1110 35.2 10-90 1-2 2270 15.o 50-5(

1-3 500') 35.1 10-90 1-4 2180 15.0 .

1-5 4820 33.2 10-00 2-1 2220 15.3 --

2-2 4150 33 10-90 2-3 2160 14.9 ?

2-4 472U 20-30 2-5 2090 14.' 4o-6U

Ave. 410 . 0-9A . 15..e 2S.n. •0 .2 s.r. i 70 0 :

FBU127 F F6FBE'(1-2 24 17. 50-0-0-5u 1-1 4670 32.2 40-0-0-60

1-4 247" 17. 0-0-0-50 1-3 5000 34.5 00-5* 2-1 j-:-i0-9Q 1-3 4700 2. 30

2- 3 C " 0-0-'-'0 2-2 412C 2'6- . -"-- 81

2- I 2. H' 20-0-0 2-4 4190 289

AVe. Ave. 4531 31.- 30-0-0-7)

S.D. 33 2. S.D. 370

XA39501 F6FME3 395 0--10-90 .- 2 2610 18.0 10-c-20-70

1-3 I 3. 1 0-0- 10-90 1-4 2560 , 7 0 0-0-10-001-4 ,o0--0-100 2-1 2430 i6. 7 2(-0-20-60

2-2 ,41 .14.0 '-0-10-90 2- 2220 i ]5.3 ,0-0- 20-6c1!.. '>• 3;.. 0•-u--0-99 I 2-o, 2300 :. ,*--2-6

14.15--"-0-20-"

Ave. 82 . _ 4 0O3. . 271) L . l b6 G 1

NOTE2!- j. Tested " 2000F (,3CI, (* P day" 20O1F (9)O* > k)5-100• R.H..

2. Sea Figure 9, page 18.

J. Adherend Failure.

80

S.... . . .. . . -1 z I• III - --

INDIVIDUAL LAP SHEAR TEST RESULTS FOR LR100-172 ADHESIVEON FINGER SPECIMENS PREPARED WITH STANDARD FPL ETCH

Test Temp. 726F (220C) Dry 2000F (930C) After AgingI

dher. Spec. Strength Failure 2 Spec. Strength Failure 2

y Primer No. psi MPa Mode :1o. psi MPa Mode

5052- NONE FSFNA F5FNAH34 1-1 2420 16.7 100-0 1-2 2870 19.0 100-0

1-3 2800 19.3 100-0 1-4 2870 19.8 100-01-5 2550 17.6 100-0 2-1 2660 17.3 100-02-2 2400 16.5 100-0 2-3 2510 14.2 100-02-4 2430 16.7 100-0 2-5 2060 14.2 100-0 1

Ave. 2520 17.4 100-0 Ave. 2590 17.9 100-0S.D. 170 1.2 S.D. 340 2.3

BRI27 F5FBA F5FBA1-1 2160 14.9 100-0-0-0 1-2 2810 19.4 100-0-0-0 41-3 2690 18.5 100-0-0-0 1-4 2990 20.6 100-0-0-01-5 2590 17.9 100-0-0-0 2-1 2540 17.5 100-0-0-02-2 2630 18.1 90-0-10-0 2-3 2650 18.3 100-0-0-02-4 3040 20.9 100-0-0-0 2-5 2750 19.0 100-0-0-0

Ave. 2620 18.1 100-0-0-0 Ave. 2750 19.0 100-0-0-0S.D. 320 2.2 S.D. 170 1.2

XA3950 F5FMA FSFMA1-7 2680 18.5 100-0-0-0 1-2 2510 17.3 100-0-0-01-3 2250 15.5 100-0-0-0 1-4 2530 17.4 100-0-0-01-5 2500 17.2 100-0-0-0 2-1 2380 16.4 100-0-0-02-2 2260 15.6 100-0-0-0 2-3 NO IEST2-4 2320 16.0 100-0-0-0 2-5 2220 15.3 100-0-0-0

Ave. 2400 16.5 100-0-0-0 Ave. 2410 16.6 100-0-0-0S.D. 180 1.2 S.D. 140 1.0

6061- NONE F6FNA F6rNAT6 1-1 4150 28.6 100-0 1-2 3260 22.5 100-0

1-3 3740 25.8 100-0 1-4 3300 22.7 100-01-5 3840 26.5 100-0 2-1 3050 21.0 100-02-2 3480 24.0 100-0 2-3 3110 21.4 100-02-4 3730 25.7 100-0 2-5 3050 21.0 100-0Ave. 3790 26.1 10-0 Ave. 3150 21.7 100-0

S.D. 240 1.7 S.D. 120 .8

BR127 F6FBA F6FBA1-1 4140 28.5 100-0-0-0 1-2 3450 23.8 70-0-30-01-3 3570 24.6 95-0-5-0 1-4 3170 21.8 80-0-20-01-5 3960 27.3 100-0-0-0 2-1 3530 24.3 100-0-0-02-2 3640 25.1 100-0-0-0 2-3 3610 24.9 75-0-25-02-4 4160 28.7 100-0-0-0 2-5 3180 21.9 70-0-30-0

Ave. 3890 26.8 100-0-0-0 Ave. 3390 23.4 80-0-20-0S.D. 280 1.9 S.D. 200 1.4

XA3950 T6FMA F6FMA1-1 3300 22.7 60-0-40-0 1-2 3200 22.1 50-0-50-01-3 5600 38.6 90-0-10-0 1-4 3330 22.9 100-0-0-01-5 3980 27.4 100-0-0-0 2-1 2530 17.4 70-0-30-02-2 4060 28.0 0-0-100-0 2-3 3140 21.6 80-0-20-02-4 4120 28.4 0-0-100-0 2-5 3100 21.4 60-0-40-0

Ave. 4210 29.0 50-0-50-0 Ave. 3060 21.1 70-0-30-0- .D. 840 5.8 S.D. 310 2.1

N='1•1 I. Tested 0 2000F (93*C), after 14 days @ 200*F (93*C), 95-100% R.H.2. Iee Figure 9, page 1.

81

4v

UNDtVIDUAL LAP SHEAP TEST RESULTS FOR P382-7 AHESZVE

OM V•ACKIND SPECIMENS PHPASD WITH OPTI•IZED rPL ZTCH

Test Tamp. 7'F (21C Dry 200-F (93-C) kf-.er Aging;

Uh:r. Spec. Strength Failure2 Spec. Stren th Failutxe 2

Icloy Primer No. p. Mp ae .:o. sa Mod eod-

5052- NONE: M5ONC MSONCH34 7-1 4040 27.8 30-70 7-2 1820 12.5 20-80

7-3 3S20 24.3 40-60 7-4 1930 13.7 20-807-5 3650 25.2 30-70 8-1 1980 13.6 30-708-2 3500 24.1 40-60 8-3 1670 11.5 40-608-4 3460 23.8 30-70 8-5 1723 11.9 30-70

Ave. 3630 25.0 35-65 Ave. 1830 12.6 30-70S.D. 236 1.6 S.D0 146 1.0

BR127 M508C M5OBC1-1 2620 16.1 0-0-40-60 3-2 1200 0.3 0-0-0-1301-2 2740 18.9 20-0-20-60 3-4 1080 7.4 0-0-0-1C,1-5 3000 20.7 10-0-20-70 4-1 1290 8.9 0-0-0-1002-2 2550 17.6 0-0-80-20 4-3 1350 9.3 0-0-3-1002-4 2830 19.6 0 -0-2C-80 4-5 1250 8.6 0-0-0-10^C

Ave. 2750 19.0 5-0-35-60 Ave. 1240 8.3 U-0-0-100S.D. 178 1.2 S.D. 105 0.7

XA3950 MS0toC MSOMC1-1 3220 22.2 90-0-0-10 3-1 1680 11.6 0-0-0-1001-3 2990 20.6 80-0-0-20 3-3 1800 12.4 0-0-0-1001-5 3270 22.1 90-0-0-10 3-5 1830 12.6 0-0-0-1!02-2 2960 20.4 70-0-0-30 4-2 2050 14.1 0-0-3-132-4 3380 23.3 60-0-0-40 4-4 1800 1,.4 0-0-0-10CC

Ave. 3160 21.8 80-0-0-20 Ave. 1830 12.6 0-0-0-i0

S.D. 182 IiJ S.D. 135 2.9

6C61- NONE M6ONC M60NCT6 1-1 4711 32.5 90-10 1-3 2240 15.4 13-90

1-3 3925 27.0 95-5 1-4 "227 15..3 40-601-5 3748 25.8 90-10 2-1 182 15.0 40-602-2 4010 27.7 90-10 2-3 2120 14.6 30-702-4 3740 25.8 95-5 2-5 2162 14.9 4C-60

Ave. 4026 27.8 90-10 Ave. 2186 15.1 30--j

S.D. 400 2.8 S.D. 49 C.3

8R27 M460)C M60801-i 3491 24.1 0-30-0-70 1-2 4065 28.0 0-0-30-7•1-3 4138 28.3 0-40-0-60 1-4 3880 26.? 0-I-%-ý1-5 3698 625.0 0-3-0-7-7 2-1 3444 23.7 0-3-33-702-2 4020 27.7 0-40-C-63 2-3 315C 21.7 0-0- 7•-a•2-4 4004 27.6 0-50-3-50 2-5 2971 20.5 0-23-8,A2-. 3864 26.6 0-40-3-60 Ave. 3502 24.1 0-0-25-75

S.D. 260 1.8 J S.D. 466 3.2

XA3950t M(6OMAC T - M60MC3-1 411, 28.6 30-0-0-?7C 3-2 2238 15.4 1,'-2-0---- 3 4158 28.6 40-0-2-60 3-4 2144 14.8 .2C-I --.- 5 4265 29.4 33-0-0-70 4-1 2038 14.0 0-0- I -")4-2 343E 23.7 . D-40-60-0 4-3 1825 2.9 1 C - 1- t%

I 4-4 3)33 27.1 3-40-6,- 3 4 i

I Ave. I -- 2? 5 20-15-25-40 Ave. 1173 136 '5-- -- "1

.3 S.D. 251 1.

N3'E: 1. Tested @ 200'F (93*C), after 14 days I 200'P %93*C, 96-10a R.H.2. See Figure 9, page iS.

8 2

INDIVIDUAL LAP SHEAR~ TEST RESUrLTS FOR 9C)!' ADHESIVE

ON MACHINED SP'ECI14ENS PREPARED WITH 0P'7UMIZEDEFPr. ETCH

TeSt Temp. j __ _ 72'F (22*C) nry 1[ 200*F (93*C) After Aging

e~ri Sec. St-e~nq61 Failure Spec Sie-hF.ir'.hiioy Prime No NaMd a P ode

5052- NcmE sSh 36~II

1-1 4130 28.2 5s;14 10 6.9 o233 - i21 3 2 8 . 13 40 - 60 8 5I1 0 0 7 .4 q O 0 -3 0 L A2-2 4130 28. 5 40-60 -3 1100 7.6 70-30

-- 43 0 2 R . 51 4 0 -6 -, 6 -2 1 0,5 0 .2 7 0 -3 0

Ave. 4120 28.4 45-55 Av. 1010 7.0 70-30

S.D. 1-3 S. .D. -3 .7

BRI27 m5C88 I MSOBB

1-11 4590 31.6 0-0-20-80 1-2 1140 7.) 0-0-10-90

2-2 4380 30.2 0-0-40-60 2-3 1720 11.9 0-0-20-70

4-4 443C 32.5 0-0-30-?0 5-1 1,70 9.4 10-3-10-60

5 -5 43S0 30.2 0-0-n7n0-30 I N-z 1330 9.2 03--10-90

6-3 4390 3C.3 3-3-33-7U 5 -5 1240 6.5 0-010-9C

Ave. 4430 3ý. 6 0-0-40-60 Ave. 1360 9. -0-15-85

S.C. 9.0 .6 S.D. 220 1.5

2A90 5-2 420 2.52- 0 4.

1-1 3720 25.6 'NOT AVAILABSLE 1-7 .4 NOT AVA1LABU

3-3 44 292 3-4 790 5.4

6-5 416 9.7 t71 4.92- 5 8 04 .

Ave 40U. 26.U. Ave. 76 5.

S.D. 23 1.6_____ S.D. __ 190__1.4

T6 1-1 5111 T5.3 30-70 1-5 1700 11.7 700

1-4 s033 34.7 20-80 2-1 1533 10.5 70-30

L2-2 4920 33.9 10-90 2-4 1460 10. i 70-30

14-3 4900 33:8 20-80 I4-1 420 2.; 1330-0

4-5 47,40 32.7 40-60 j4-4 440 3.31 100-0

Ave. 494C- 34.1 25-75 Ave. 1113^ 7.7 80-20S SD~ 140 laS.D. 630 4.3

BR!,-, MS3t:B I..60BB

11-1 536- 36.9 10-0-%.-301 1-2 li-o 7. 0-0-2,-801-3 539; 37.1 0 -C-3 3 1-4 i 1c0 . -- 09

-7 ? 1 41 C-O3'-C - 118C 8.1 40-0-0-602- ,,: 3. 0-ý-13-0 23 19 . ,DC6

C-08.2 0413-0-1,-6.2-49.6640038,9 2-5 02 . 30-0-0-73

AV-. 5410 37.3 0-0-60-40 Av - 130 71.8

S. 3 0 2.1 S.D.___ ----- 153 . ______

XA3950I M6CWJB M6OMS1-2 5013 34.5 0-1-10-90 1-3 1913 33.2 0-0-30--^

2-i 503 34.5 0-0-20-80 2-2 2230 15.4 0-0-4c-6,1

4-i 5340 36.8 X-ETAL FAILURE 4-- 2300 14.q --- 0

4-4 5050 1 34.81 0-0)-0- 10 4-S 10370 22.) 9 701-3

5,-4 1053 34.8 1---007 1530 1C.5 i1--07

Ae 5 )90 1 35.1 0-C-5-95 AV 1930 I13.3 0-203

NC7E; 1. Tested 200*F (93*C1, after 14 Jays 3200*F 93'3I 5 -1 R.M.I

2. $te Figure 9, page 16.

8 3

INDIVIDUAL LAP SHEAR TEST RESULTS FOR R 7114 ADHESIVE

O(t FINGER SPECIMENS PREPARED WITH OPTYMIZED FPL ETCH

Test. Temp. 72*F (22rC) Dry 200*F (93*C) After AgingL

ddher. Spec. Strength Failure2 Spec. Stren th Failure 2

iloy Primer No. MPa Mode 11o. psi MPa Mode

5052 NONE FSOND FSONDH34 1-1 2640 18.2 0-100 1-2 80 0.6 0-100

1-4 3110 21.4 0-100 1-4 80 0.6 0-1002-1 3400 23.4 0-100 2-1 90 0.6 20-802-3 2810 19.4 0-100 2-3 80 0.6 10-902-5 2820 19.4 0-100 2-5 90 0.6 20-80

Ave. 2960 20.4 0-100 Ave. 80 0.6 10-90S.D. 300 2.0 S.D. 10 0.0

BR127 F50BD F5OBD1-1 2830 19.5 0-0-0-100 1-2 110 0.8 0-0-0-1001-3 2750 18.9 0-0-0-100 1-4 90 0.6 0-0-0-1001-5 2700 18.6 0-0-0-100 2-1 90 0.6 0-0-0-1002-2 3100 21.4 0-0-0-100 2-3 110 0.8 0-0-0-1002-4 3130 21.6 0-0-0-100 2-5 90 0.6 0-0-0-100

Ave. 2900 20.0 0-0-0-100 Ave. 100 0.7 0-0-0-100S.D. 200 1.4 S.D. 10 0.1

XA3950 F5OMD FSOMD1-1 2870 19.9 0-0-0-100 1-2 90 0.6 0-0-0-1001-3 2970 20.5' 0-0-0-100 1-4 70 0.5 0-0-0-1001-5 2810 19.4 0-0-0-100 2-1 130 0.9 0-0-0-1002-2 3420 23.6 0-0-0-100 2-3 80 0.6 0-0-0-1002-4 3200 22.0 0-0-0-100 2-5 100 0.7 0-0-0-100

Ave. 3050 21.0 0-0-0-100 Ave. 90 0.6 0-0-0-100S.D. 250 1.7 S.D. 20 0.1

6061 NONE F6OND F6ONDT6 1-1 2050 14.1 0-0-0-100 1-2 100 0.7 0-0-0-100

1-3 2230 15.4 0-0-0-100 1-4 110 0.8 0-0-0-1001-5 2100 14.5 0-0-0-100 2-1 70 0.5 0-0-0-1002-2 2740 18.9 0-0-0-100 2-3 70 0.5 0-0-0-1002-4 2870 19.8 0-0-0-100 2-5 80 0.6 0-0-0-100

Ave. 2400 16.5 0-0-0-100 Ave. 90 0.6 0-0-0-100S.D. 380 2.6 S.D. 20 0.1

BR127 F6OBD F60BD1-1 3580 24.7 0-0-0-100 1-2 120 0.8 0-0-0-1001-3 3280 22.6 0-0-0-100 1-4 110 0.8 0-0-0-1001-5 3030 20.9 0-0-0-100 2-1 110 0.8 0-0-0-1002-2 3350 23.1 0-0-0-100 2-3 120 0.8 0-0-0-1002-4 3270 22.5 0-0-0-100 2-5 180 1.2 0-0-0-100

Ave. 3300 22.7 0-0-0-100 Ave. 130 0.9 0-0-0-100S.D. 200 1.4 S.D. 30 0.2

XA3950 F6OKD F60MD1-1 80 0.6 0-0-0-100 1-2 80 0.6 0-0-0-1001-3 80 0.6 0-0-0-100 1-4 80 0.6 0-0-0-1001-5 100 0.7 0-0-0-100 2-1 100 0.7 0-0-0-1002-2 120 0.8 0-0-0-100 2-3 120 0.8 0-0-0-1002-4 120 0.8 0-0-0-100 2-5 120 0.8 0-0-0-100

Ave. 100 0.7 0-0-0-100 Ave. 100 0.7 0-0-0-100

NOTU2 1. Tested 0 2000F (93*C), after 14 days 0 200*F (93*C), 95-1001 R.H.

2. see Figure 9, page 1i.

84

INDIVIDUAL LAP SHEAR TEST RESULTS FOR AF-80 ADHESIVE

ON MACHINED SPECIMENS PREPARED WITH OPTIMIZEDFPL ETCH

Test Temp. 720F (22'C) Dry 20O0F (933C) After Aging 1

oher. Spec. Strength Failure 2 Spec. Strnth Failure 2hloy Primer No. pan MPa Mode NO. psi MPa Mode

5052 NONEO M50NE 50NEH34 1-1 4560 31.4 10-90 3-2 -2700 18.6 5-95

1-3 4590 31.6 10-90 3-4 2680 18.4 5-951-5 4680 32.3 10-90 4-1 1910 13.2 10-902-2 4690 32.3 10-90 4-3 2320 16.0 10-902-4 4770 32.9 10-90 4-5 1800 12.4 10-90

Ave. 4660 32.1 10-90 Ave. 2280 15.7 10-90S.D. 80 0.6 S.D. 420 2.9

BR127 M5OBE MSOBE1-1 3730 25.7 0-0-10-90 3-2 1140 7.8 0-0-0-1001-3 3810 26.3 0-0-10-90 3-4 1230 8.5 0-0-0-1001-5 3910 27.0 0-0-10-90 4-1 1180 8.1 0-0-0-1002-2 3890 26.8 0-0-10-90 4-3 1150 7.9 0-0-0-1002-4 3870 26.7 0-0-10-90 4-5 1010 6.9 0-0-0-100

Ave. 3840 26.5 0-0-10-90 Ave. 1140 7.9 0-0-0-100S.D. 70 0.5 S.D. 80 0.6

XA3950 MSOME M5OME1-1 3960 27.3 0-0-0-100 3-2 1500 10.4 0-0-0-1001-3 4030 27.8 0-0-0-100 3-4 1370 9.4 0-0-0-1001-5 4110 28.3 0-0-0-100 4-1 1180 8.1 0-0-0-1002-2 3910 27.0 0-0-0-100 4-3 1480 10.2 0-0-0-1002-4 3900 26.9 0-0-0-100 4-5 1340 9.2 0-0-0-100

Ave. 3980 27.5 0-0-0-100 Ave. 1370 9.5 0-0-0-100S.D. 90 0.6 S.D. 130 0.9

16061 NONE M6ONE M6ONET6 1-1 5700 39.3 0-100 1-2 3400 23.4 10-90

1-5 5410 37.3 0-100 2-3 3280 22.6 10-902-2 5260 36.2 10-90 3-4 2030 14.0 20-803-3 4620 31.8 0-100 4-1 2350 16.2 40-604-4 5110 35.2 0-100 4-5 2320 16.0 40-60

Ave. 5220 36.0 0-100 Ave. 2680 18.5 25-75S.D. 400 2.8 S.D. 620 4.3

8R127 M60BE M6OBE1-1 4670 32.2 0-0-10-90 3-1 2060 14.2 10-0-0-901-3 4630 31.9 0-0-10-90 3-3 2090 14.4 10-0-0-901-5 4580 31.6 0-0-0-i00 3-5 2250 15.5 20-0-0-802-2 4860 33.5 0-0-10-90 4-2 2660 18.3 0-0-0-1002-5 4810 33.1 0-C-10-90 4-4 2420 16.7 0-0-0-100

Ave. 4710 32.4 0-0-10-90 Ave. 2290 15.8 10-0-0-90S.D. 120 0.8 S.D. 250 1.7

XA39SO M6OME M6OME1-1 4960 37.2 0-0-0-100 1-3 3000 20.7 0-0-0-1002-2 5160 35.6 0-0-0-100 2-1 2120 14.6 0-0-0-1003-1 5000 34.5 0-0-0-100 3-2 2450 16.9 10-0-0-903-3 4920 33.9 0-0-0-100 3-4 2340 16.1 20-0-0-804-1 4750 32.7 0-0-0-100 4-3 2220 15.3 10-0-0-90

Ave. 4960 34.2 0-0-0-100 Ave. 2630 18.1 10-0-0-90S.D. 150 1.0 S.D. 410 2.8

No.Zs. 1. Tested * 200"F (93C), after 14 days 0 2000F (930C), 95-100% R.H.

2. See Figure 9, page is.

85

INDIVIDUAL LAP SHEAR TEST RESULTS FORLRIO0-17, A -KESIVE

ON MACHINED SPECLMF-NS PREPARED WITHOFTIMIlED FPL ETCHI-

Test Temnp. '72F (221C) Dry 200*F (931C) After Aggng

.FS pec Strerqct 31 E&e.. -

I-4 Pr4 4er Sp.5. 0-S rIni-3 • 1 . a- .0-a.N 1 -p mode l psi. Mode

1 -1 30 . I , 7; I

S.D.~~ i0 2.71:2[. '-

!-4 4140 :5.5 1 l..)70 -1 -3 2 4I.6

24-1 44-0 -5. -•.l :- 4-2 I 257410 1 R.• 7 ,4 -.2 -

1-4 4- 29 .6

2-1 49 8-3 .7

Ave. 411) -. 4 2--9'- Ave. .-! 1 ).,3 " -,

S. . -- . S.D. 2---'-0 1.4

1-1950 423. C00-• 1

:- 11 60 28.7 3 0-4 d-S j 3

24-2 28.4 21105 i, .e 1,&- - -O4-,3 44 .. .

- 44?0 '31b 7"--3 7-1 0 - 2.710 2...7 "S -- --

4-4 4190 3-....--5 2800 NA.3 l'--

Ave. -.3 -0- 20 -.. A

-. . C.:-. 267o. . .... I 1 7

3-- 4 -- 4 7 26" 3. -I -Av 48 • 4.-D-3 -0 . -2..8 3

3-39~b M 44 ).b ~ - - - 1 .I

4-4 '490 31.C ---- ;-5- 2E.'-

Ave. 4480 3C3, 2. 3- 0 Ave. 2 0 "I S.D. - S.D.

,X DAG0' 1B•• IM6 HI'<• E

26 3-1 4SC5• 30.1 1-0- I 3- 2 5 C1

3-z 496, 33.5 1 O.-. 23 13.4

- 5 0. - I ; 4 C- 3

Ave. 48 3 1 '1ve ". 9

S i,° D .,jS.D. 60 II.4 1.

'5. 73- 3,1' 2"32A.' 6 , - -

6-2 35-3 N-, -C 1 -- 3C - -

Ave. 1,1g 36.4 Ave. 3 1 2. .

S.D. 60 3. C5,

NOE; a etd 3 2O013P n o0) after 14 *.iays • C¢• ]CI

!.3 5 ým ,.,. 9 -!o,.,4.•

2. See 3igue 9, pege 18.3. Adhere nd F1a.2ure.

86

S-r-

INDIVIDUAL LAP SHEAR TEST RESULTS Fj3R LkNC"--252 AZKESZ'/E

CN MACHINED SPECIMENS PREPARED WITH C,,•TIIZED FPL ETCH

Test Temp. 72'F (22-C) Dry 100'F (93') After

N GI. ~ ~ ~ 3ý- C --- V

S. . 80 I 0.6 ., 20 1.4l% i6.944Xc 33. :iM*j 21 54 sc,-so-

1w ,I IB

-! -S 17.2- 47252" 302" -J'-i Av-5 3320 22.9 _ _-O__O-I

Ave. ve. 200 1 .4 53-50

I 35,3 LI 3 I i- - l

r.A3950 'CGJ- 4It 33- 1--1-90 - iC-- i-

1-4 4ý30 j9 O -1' :, -, 3-'0 2 . ,C-1G •

'-..)5 1i -i-,'1¢ - 1•" 2 .' 0-0- 0-;.cZ

-454 j 9 I 3 4 2-4 3 0 112) . -0 41 0--C- 2-.. 9-.

I

Ave. 46;0 !31.9 0-0-5-95 Ave. 3 I060 C-O-G O

Cý' 31

j 5v 34.8 30-76 7-5 22*6 -5 , c-,

2-4I6 3. I I 4--0-3 2 2 ! .4 I -- I .1i fl O-3z-9 I 33'd 34.8 1P Ii43-6 ' e 4 263 156 I 8-

Ave-Ave

3-71 Ave. [,~ % 3 . 0 7 226., 15. 75--25:. , S. D.

I-1 52•? 34.5 Ol-.- -I, i 1-2 9 S 13.4 -,-! -61-3 •0 0 34. - - -9 CO n i 4 "3 1 . t-'- 2.= R

1 20 36.4 j0-0- Ii 12.:0-0- -7

0 - i i4 , T2.2-4 5139 35. O-D . - :1- 10 6- 1•0 c, I3. -c 50 O

K ?. _ :< 3. 2-> m8 O II . "I ,; 8!. i - 2-.-0-

' 2'2t I. I ;i22>t> I C

XA3950 M6cm, ,qmDM1-1 2{ 36.2 - - -I -2 i8o0 12.4 10 C IO H

-3 "4-- 37 -. O- -1 - 01 4 " 71 . 2 2 - - 0 71- - 5 3 4 ) 3 [- -9

2-4 529 35. 1 0- -[3-c- 2-1- 3• 3- 2-. 5 £ '-I) ý36.6 1'0, 2-1 33. 2 .0

Ave. I 30 36, 9 C-11- D-95 Ave. 276,ý A ~ C 50 o60AS.D. 1M46 A

N'tES: 1. Tested @ 20,10F (93I C), after 14 days 2C003

F - 93o*, 7-1Ct P.M.

2. See Figure 9, page 18.

87

INDIVIDUAL LAP SHEAR TEST RESULTS FOR MA 429 ADHESIVE

CN MACHINED SPECIMENS PREPARED WITH OPTIMIZED FPL ETCH

Test Temp. 72*F (22*C) Dry 2006F (931C) After Aging

Sdher. pec. Strength Failure 2 Spec. Strength Failure 2

klly Primer No. psi NPa Mode 14o. psi MPa Mode

5052 NONE MSONF M50"UF

H34 1-1 4800 33.1 60-40 1-3 1460 10.1 90-101-4 4510 31.1 70-30 1-6 1630 11.2 90-101-7 4830 33.3 70-30 2-1 1230 8.5 90-102-2 4750 32.7 70-30 2-4 1180 8.1 90-102-6 4660 32.1 70-30 2-5 1250 8.6 90-10

Ave. 4710 32.5 70-30 Ave. 1350 9.3 90-10S.D. 130 0.9 S.D. 190 1.3

8R127 M5OBF M5OBr1-2 4530 31.2 90-10 1-3 2140 14.7 20-801-6 4450 30.7 90-10 1-5 2280 15.7 30-702-1 4520 31.1 90-10 1-7 2330 16.1 30-702-4 4440 30.6 90-10 2-3 2280 15.7 40-602-6 4510 31.1 90-10 2-7 2160 14.9 20-80

Ave. 4490 30.9 90-10 Ave. 2240 15.4 25-75S.D. 40 0.3 S.D. 80 0.6

XA3950 MSOMF M5OMF1-1 4620 31.8 80-20 1-3 2280 15.7 10-901-4 4630 31.9 80-20 1-6 2100 14.5 10-901-7 4440 30.6 80-20 2-1 1940 13.4 20-802-3 4450 30.7 80-20 2-4 2040 14.1 20-802-6 4470 30.8 80-20 2-7 1780 12.3 20-80

Ave. 4520 31.1 80-20 Ave. 2030 14.0 15.75 1S.D. 90 0.7 S.D. 190 1.3

6061 NONE M6ONF M6ONFT6 1-1 5290 36.5 80-20 1-2 590 4.1 100-0

1-3 5340 36.8 80-20 1-4 540 3.7 100-01-5 5060 34.9 70-30 1-6 540 3.7 100-02-2 5460 37.6 80-20 2-1 480 3.3 100-02-4 4940 34.3 70-30 2-3 590 4.1 100-02-6 5480 37.6 70-30 2-5 550 3.8 100-0Ave. 5260 36.2 75-25 Ave. 550 3.8 100-0S.D. 220 1.5 S.D. 40 0.3

8R127 M6OBF M6OBF1-1 5500 37.9 0-0-90-10 1-2 1150 7.9 10-901-3 5310 36.6 0-0-80-20 1-4 1200 8.3 20-801-5 5580 38.4 5-0-80-15 1-6 970 6.7 40-602-2 4880 33.6 0-0-70-30 2-1 760 5.2 20-802-4 5260 36.2 0-0-70-30 2-3 870 6.0 10-902-6 5100 35.1 0-0-70-30 2-5 820 5.6 20-80Ave. 5270 36.3 0-0-75-25 Ave. 960 6.6 20-80S.D. 260 1.8 S.D. 180 1.2

XA3950 M60MF .160F1-1 5490 37.8 5-0-7C-25 1-2 2230 15.4 10-901-3 5240 36.1 0-0-70-30 1-4 1750 12.1 10-901-5 5590 38.5 5-0-70-25 1-6 1680 11.6 20-802-2 5760 39.7 5-0-70-25 2-1 820 5.6 20-802-4 5p.00 39.9 5-0-60-35 2-3 730 5.0 20-802-6 A680 39.1 5-0-65-30 2-5 870 6.0 20-80

Ave. 5590 38.5 5-0-70-25 Ave. 1350 9.3 15-85

S. 210 1.4 S.D. 620 4.3

NOTEs: 1. Tested 9 200*F k93OC), after 14 days 4 200*F (93-C), 95-100% R.H.2. sse Figure 9, page 19.

. 8

S. .. . . . .. . . I I I - - . .. .-= - • - : . . . •

APPENDIX VII

INDIVIDUAL SPECIMEN FLOATING ROLLER PEEL -rEST DATA

The data presented here are for the tests and results .

discussed in Paragraphs 2.3.2 and 3.2.

F9

~1

L_ __ _ _

LNDIVIOUA.L FLOATING ROLLER PEEL TEST RESULTS

FOR LR 100-172 AnHESIVE

Test Tmp. 721F (22*C) Dry -65P (-154*C)

Adher" Spec. Strength failure 2 Spec, Stren th Failure 2Kiloy Primar 4o. Lb'in. N/i of Mods iso. 8%/in. N/ct Kof

tf width width :)f width width h _

2024- NONE 1-1 23,0 40.3 90-10 1-2 16.9 29.6 100-0

T3 1-3 26.3 46.1 90-10 1-4 17.9 31.3 100-0

2-2 27.5 48.2 100-0 2-1 24.3 42.5 90-10S2-4 25.5 44.7 1 00-0 -3 23.4 41.0 100-0

Ave. 25.5 44.8 9S-5 Ave. 20.6 36.1 95-5S.D. 1-9 3.3 I S.D. 3_ 8 6.6

BR.R27 1-2 3.5 6.1 0-2-100-C 1-1 6.2 10.9 0-0-100-13

1-4 2.9 5.1 0-0-100-0 1-3 3.8 6.7 0-0-1o0-0_2-1 4.1 7.2 0-0-100-C 2-2 3.3 5.8 0-0-100-02-3 5.4 9.5 0-0-100-0 2-4 5.7 10.0 0-0-100-0

AV,. 4.0 7.0 0-0-100-0 Ave. 4.7 8.4 0-0-100-u1.1 1.9 S.D. 1.4 2.5

6C61- NONE 1-1 14.2 24.A iO0-0 1-2 15.3 26.8 90-10

T6 1-3 13.6 23.8 100-0 1-4 15.7 27.5 90-102-2 8.0 14.0 100-0 2-1 13.2 23.1 90-10

2-4 '0.7 18.7 1OO-O 2-3 13.3 23.3 90-10

Ave. 11.6 20.4 100-0 Ave. 14.4 25.2 9C-IC

S.D. i2. 5.0 S.D. 1.3 2.3

BRI27 1-1 3.5 6.1 0-0-100-0 1-2 3.1 5.41-3 7.1i 12.4 100-0-0-0 1-4 2.9 5.1I 0-0-100-0

.. 2-1 2.8 4.9 0-0-100-0 2-1 2.0 3.5 O-0-i00-c

2-4 3.9 6.8 0-0-100-0 2-3 4.1 7.2 0-0-100-0

Ave. 4.4 7.6 25-0-75-0 Ave. 3.0 5.3 0-0-10G-0

_ S.D. 1.9 3.3 S.D. 0.9 1.5

5052- NONE 1-1 15.2 26.6 100-C I1-2 19.9 34.8 30-72

H34 1-3 17.0 29.8 100-0 1-4 17.8 31.2 30- 70

2-2 22.3 39.0 100-0 2-1 18.2 31.9 30-70

2-4 20.0 35.0 o1-0 2-3 17.9 31.3 30-770

Ave. 18.6 32.6 100-0 AVG. 18.4 32.3 30-70

S.D. 3.1 5.S 5. _. 1.0 1.7 _

BR127 1-1 3.1 5.4 0-0-100-0 1-2 3.2 5.6 0- -1 0-7

1-3 2.6 4.6 0-0-iO0-0 1-4 2.3 4,C 0-2- 0oo-2-2 3.5 6.1 O-C-100-0 2-1 3.7 6.5 0-O- -100C-C

2-4 2.8 4.9 0-0-100-0 2-3 4.3 7.5 0-- 0-00-0

NOTE, 1. Tested at -65'F (-541C) after 10 minutes at -650F (-541C).

2. see rigure , pago Ic.

90

IID0VIDUOA FLOATING ROLLER PFEL RESULTS FOR R382-7 ADHESIVE

ON OPTIHIZED FPL ETCH ADILLRENDS, PRIPJ:O WITH F?127

Test !'tp. 72"F (22°C) Dry -6"or (-54°C)12,ýe~d ISe. t-qhSrmt 2

Se hFailure2 . Spec. , r-- Failure' 1oIts/in. N,/CM kbzd/-n. N/cm I;'i 7 f ', td~ o! width, ______o ____ __ _ _ •. i~h _ _ _ -,I . •0. o f I Mode

2024-T3 1-1- 13.2 23.1 0-0-60-40 1-2 3.5 6.1 0-0-80-20I 1-3 15.1 26.4 0-0-60-40 1-4 3.8 6.7 0-0-80-20

2-2 15.9 27.8 0-0-60-40 2-1 2.7 4.7 0-0-80-20I 2-4 17.2 30.1 0-0-50-30 2-3 4.1 7.2 0-0-80-20

I Ave. 15.4 26,9 0-0-60-40 Ave. 3.5 6.2 0-0-80-20S.D, 1.7 2.9 S.D. 0.6 1.1

606"-T6 1-1 22.2 38.9 10-0-70-20 1-2 7.13 13.7 0-0-90-i01-3 23.4 41.0 10-0-70-20 1-4 5.5 9.6 0-0-90-102-2 22.9 40.1 NOT AVAILABLE 2-1 7.7 13.5 0-0-90-102-4. 21.6 37.8 10-0-80-10 2-3 5.9 10.3 0-0-90-0I

A 2.e. 22.5 39.5 10 -0-75-15 Av 6.7 11.8 0-0-90-10

S. L)I 0.8 1.4 S.D. 1.2 2.1

50,2-ij 34 1i-1 26.5 46.4 10-0-50-40 1-2 19.5 34,.1 0-0-60-401-3 27.4 48.0 10-0-50-40 1-4 20.9 30.6 0-0-60-402-2 21.4 37.5 10-10-S0-30 2-1 19.8 34.7 IC-lc1,6-2-4 20.5 35.9 10-10-40-40 2-3 18.1 31.7 10-10-20-3-

Ave. 24.0 42.0 10-5-45-40 Ave. 19.6 34.3 5-5-5ý-35

INDIVIDUA. FLOATING ROLLER PEEL RE:ZjLTS FOR E;A96 ;1NW AiI FSIVEON OPTIMIZED FPL ETCH A1).-" .NDS, - V=TH DR127

2024-T3 1-1 36.7 64.3 0-0-0-100 1-2 33.2 58.1 10-0-0-901-3 39.1 68.5 0-0-0-100 1-4 32.9 51.6 10-;-r-902-2 45.0 78.8 U-0-O-100 2-1 31.4 55.0 50-0-20-30I2-4 42.4 74.2 0-0-0-100 2-3 i36.9 64.6 50-0-20- 30

Ave. 40.0 7A. 336 58 30-0-10-602ve . 71.5 0-0-0-100 Ave. 33.6 58.8 60-0-0-c0S. D. . 6.4 S.D. 1 .44.1

636 1-T6 1-1 54.7 95.8 0-0-0-100 1-2 1I.G 55.3 5j-0--0-501-3 53.2 93.2 Q-0-O-1O0 1-4 33,.1 Salo 6,)-i-(0-402-2 52.2 91.4 0-0-0-I00 2-1 33.5 587 60-0-0-,I10

2-4 47.8 83.7 0-0-0-10 2-3 24,3 42.5 80-1-r- 0

Ave. 52.0 91.0 0-0-0-.00 Ave. 3 .b 53.6 60-0-0- '10S.D. 3.0 5,2 S.D. 4.3 7.6

--052-04 1 22.9 40.1 o0-0-0-10c 1-2 21.9 3H.47 0-60-3-0-11-3 33.1 58.0 0-0-0-100 1-4 2-.1 42.2 10-50-30-1i(2-2 30.1 :4.1 40-0-0-60 2-1 0.t, 16.8 21-3,-.10 -2-4 30.0 53.9 20-0-0-80 2-3 14.7 25.7 0-50-40-l0L

Ave. 29.4 51.5 15-0-0-85 Ave. 17.6 30.8 5-,,0-35-10

S.D. 4.5 7.8 S.D. 6.7 11.7

NOTE: 1. Tested at -656F (-54"C) after 10 m4.nutes at -65*F (-54'C).2. See Fiquro 9, page 19.

91

~ . -.S. ..' '' '' ,, -•---..4••

iUD1V_1fl4.":,. F[.OhTIN'3 RIkLLLHR PELL RESiULTS F01h R )1 ADHESIVE

43': O'T"' "IZELD 7PF L TC1H Afiil 7NS PkIPQ9[7 WI TH S812

S* 22Adhr2 auc uattuCe Spec. t Failure'2

i)4T 3.2. 1 0 -0U-uG--1030 1-2? '1.4 7 72 .5 0-0-0- lc072.5~j 3---0 3- 3. 3. 8 10o-0-co. 5

2 72 I 012;-,) 22 1c. 2 j31.9 it 50'.-5-4 o

73. 0-0-U-l0tu 2-3 1b. 1 3 i.~ i0 (;-4t;-,)

AVQ . 1.5 72.7 0-0-5-95 Ave.v 24..3 42.5 1--uC

2 .2 3 .9 S. U:A . 11 . 4 29

3- . , 1- 2 21. 3__ 0_C --) -... 23....

G3.0 11 c .A 1 9t. 3Z. 170-3 0

I - 3.rý 23.t - - 7 - 12-4 71'-07 2 1 3 0 23- I 2 s.0

2. 4 2 I3L .2) 21: - 7:) 2 2 0 3

2~ ~ 0- 7- -

1-3-

o3.8 1. 3 -1. 4 .>

:4DZI\V- DL FLCA.r A F ? 01 E: R. S F,- A DHESIV

caOrTIMIZEDý C?L ETONl AD!442;3MIP .'-D VUI4TF8 3127

* 04-i11 33. 4 5%I 7 C- 9-3-0 I 1-2 :20.2 3S.4 I''AALO.

1-3 1 :.3 534S 7@-0-3C-0 23.0 403

* ~ 13.0 40-''3 213 33.3 C,;- 20

2- '1 .. 4 7'.5 SD0-050-U I 22. 3 3-)., I £ -- 10-0

3o~t7t.3-15 1 0. iXr N.'AF.A' . ii 3-2 2 4. 0 I ol'l

3-3 7 "I~ 24. 4

2~ ' C00

'12.9 2-10 434 -0-51"-25'

2- 17 3. . 2-3 123.1 4 0. 4N-

41 . ''-54 .v'Ž 21. . I

I.Z.1. Test-,-,t -65' F (-54'.C) after 10, emnutes at -'5[ (-F I

2. see Figure 9, page18

92

INDIVIDUAL FLOATING ROLLER PLEL RESULTS FOR :,!1^0-252 ADHESIVE

ON OPTIM•IZED FPL ETCH ADHERENDS, PRIM.ED W!IH BRI;7

'est Ter.p. 721F (221C) Dry Fai-ure [-54•C)-S t r ] h S t r e n ,-- t h 1 2Adherend 5Pec. trnt,, Failure I Spec. "Failure2o •

A11z1 SpQ. 1bs!/.r . ::/cr. -'-de No. I s/i:•. N•/cm ::d'.o___,_-i___-- £ w" "t _________'______L 9_t.'/L~£

2024-T3 1-1 53.2 93.2 10-)-0-90 1-2 1 2t-.41-3 49.6 A6.8 10-U-0-90 1-4 -3.9 2-2 30- 2:-2-2 43.3 75.8 5- -0-40 " 1 10.1 1 -,,. [!.5 "o- - -,"2-4 33.6 58.8 50-O- -50 3-3 8.C !.-. 901-- Io-o

AVe. 449 787 30-0-5-65 Avo. 1i.t 20.5 80-0-20-0S.D. 3.3 -.8

6 1.8-1 2' 50.4 90-1-0--10 1-2 7.7

1-73 27.7 47.5 70c- -2-2 28. 3 49.6 1,:- -O O -] 6.9 1 12 .i[ ] - -,u=-

2-4 35.0 61.3 L.C-0-o -1-3 i.: 4 I~

,ve 29.8 52.2 335-0-,-5 I Av. .-

S.D 3.5 6.2 Q._

1-1 40.1 70.2 . -0-80-20 22.7 .-7.1 G5.0 3-2-90-10 22.3 . - ,- ,

27.) 06.4 1-,- 0 --3-

II50., 6 6B. -1 . 2-3 2 1. 33.

I:N2!VIDU.•i FLC-ATINO ROLIE? P:-L 023LT PC' • ;*R-42'3 700-i IVE =00 CPT '.' 0 I i- F L Z5C. -... K .3'5 .?- I' , 4l ' "

? -- t'L S -

3124-r3 1-1. 12.i 21.2 -o-90-10 -O--2 I3.0 3.- 3 -',- .>;1-3 9.% 16.6 - - - 0 - 4.) 3..222 11. o 20.3 2 '-,-40-0. ,

2-1 27.2 43. 7 3--70-30 2-3 3.2 5

Ave. 15.3 27.1 i 0--85-15 1 ,A 3 .5 . __._5._-S.D8. 13 5 . -'-

i 6061-T6 1-1 20.4 35. 6 -- 40- 0-2 7I,) 12. .- - --26.2 0 >-0- 1 -0 1I .1 (s. 1

2-2 2317 41-5 0 ,-3-' -- ."-'4 2

A v . 2 . 4 2 . 0 1-

I S.D. 2.6 4.7 .D. ."O.

2-H - 1 33. "3o- 1-2 I'21.

S2~~-3 1J.% 3. 3 O .. O2, -j1 . " ::-•'

ý-2'3 3 3 . 3

0'T-: 1. T,:'-ted at -65'% (-540C) a, 0't r 1-) foinu!ot 5 - - (-54°L'), ]

2. S~ s "I

-, APPENDIX VIII

INDIVIDUAL SPECIMEN STRESS DURABILITY -1

TEST DATA

The data presented here are for the tests discussed

in paragraphs 2.3.3 and 3.3.

94

- --C- " _-. _- T_• •

Q C) 00000 0 00 00 0

oC 0 ID o ooo o0 0

L 41 V.I 0 Lt - -I ClCn) O

-. co ;i C ,G-W c o o00 11 00 o

c r > 00I s. 0o

- '. V0 o n "1 1 0 i

I I v I o

f' :" "/ "____

I -c- Ii.__ _ IZ

Q 0LK1 ,000 0 _i___-___

':Ij'; £:i, . . . . .. .. '? .. .. .. ..

c4 <

j45

cc _ co CI 0

r4_ _ _ _ _ _ _ _ _ _ _ InI

q IlViVc ZII~~I __ __ __ _ m_

~~hII- -------- a-!" 0 _ __ _ _

li LI o- 00 IO -

I' I "'I -I 95

00000 0 00000 00) k e m oo I 0 I 0 InI4.'J 00000 0 00000 LA

SI I I I I I I II IS00 0 0 0 0 0 0 0 00 0

w= w' v! n in

S• ' F • '' '' In (1 ,-* ýO,4 ý' 0C') C) 10 0 In el M M M; ) V N to ,- co4,-I I I 1 1

tL 0 0 0 0 00.

i in A p I 111 0

e ~ ~ ~ C 1)el "e) 4

1w 0 v' n ' 1

S to n0) m~ r- 14 to 100

ri 0 0 o3_ oa%_C_ too t_ r

6-I

'l ~~~~I IN(C (' n(1(l (

C-''.0r1I___ __ __ __ _ -- 0 0 I I I I0

P. 0 4 SI moU. 4 O.4 00 0 -. IT r -00,m " 0 ;AO 'to0 rIN

In Lf C LA LAC4r V- H vN.4r- 1 in m to

U) I- 1 I• 0- ..Lo I, U In 0 ,o - oo oo0 LA- - D -4 ooo In 0k O

i e•. ) ) 0c

U)II w III1_ 0 0 0 0 000 0V) 00 0 00 0j %D 0 000 0 0 0000 LA i

N 0 O 0 0('Cr. m vS0 10 0 00 0 0oL L 10 o C " o' 0'1 1~ ~00091 0 I 0 I 0 004 :3' Q In IT C I In I? '1.00 0 000 0 L0 :'3 NI0II I I I ofo 00I

1,4 0 0 C 0 00 LA -I cor Lto(It)r N r'r LA01 LA LAI C.A LAIA(

u * In V) 0 Ir *n .1 t Iu N4 11 1 N O IO A ,4I

D .1) 0N CC 0 IN r4111( C4

U). Ni -1 N Cr ()I r o.g 01 1 0A 00 00 0uI 0 1 111 0 0 0- 1(10 0 'G a,o 41~ C3NINN N rM.m't? en

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APPENDIX IX

INDIVIDUAL SPECIMEN DCB CRACK GROWTHTEST DATA

The data presented here are for the tests and results

discussed in Paragraphs 2.3.4 and 3.4.

103

S ....... .

INDIVIDUAL DClA CRACK GROWTIHI TEST RESJITz

!:Mb-7.1 ADHEIIIVE/13R127 PRIMER,

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