DEVELOPMENT OF DESIGN ALLOWABLES DATA FOR ADHESIVES FOR ATTACHING REUSABLE SURFACE INSULATION FINAL TECHNICAL

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1 DEVELPMENT F DESIGN ALLWABLES DATA FR ADESIVES FR ATTAING REUSABLE SURFAE INSULATIN FINAL TENIAL REPRT tber 972 R U.S. GVERNMENT AGENIES AND IblR NTRATRS NLY Prepred Under ntrt N. MAS GENERAL DYNAMIS nvir Aerspe Divis Frt Wrth, Texs fr NATINAL AERNAUTIS AND SPAE ADMINISTATIN MANNED SPAERAFT ENTER ustn, Texs

2 Pge Inttlly Left Blnk

3 DEVELPMENT F DESIGN ALLWABLES DATA FR ADESIVES FR ATTAING REUSABLE SURFAE INSULATIN. P. w ' M. T. rrll.-: nvir Aerspe Divis f Gerl Dynis Frt Wrth pert FINAL TENIAL REPRT NTRAT N. NAS9-292 tber 972 NATINAL AERNAUTIS AND SPAE ADMINISTRATIN MANNED SPAERAFT ENTER USTN, TEXAS

4 FREWRD This fl reprt ws prepred by Gerl Dynis' nvir Aerspe Divis t Frt Wrth fr Ntl Aernutis nd Spe Adistrt, Mnned Sperft ter (NASA,MS) under ntrt NAS9-292 ludg A N., "Develpt f Design Allwbles Dt fr Adhesives fr Atthg Reusble Surfe Insult." Wrk reprted here ws perfred under the diret f the Mterils Tehnlgy Brnh f the Strutures nd Mehnis Divis with I. K. Spiker s the ntrtg ffier's tehnil nitr. Develpt wrk reprted here ws nduted betwe 7 Jnury 972 nd Septeber 972. The uthrs wish t knwledge the ntributs f the fllwg dividuls wh were diretly respnsible fr perfrg the prgr tsks nd preprg this fl reprt: J. E. lkis, E. W. Turns, J. D. Reynlds, nd. J. Weltn (Engeerg Test Lbrtries), R. V. Wlff nd M. S. weth (Strutures nd Mterils) nd E. W. Gez (Stress Anlysis).

5 T A B L E F N T E N T S Set Pge INTRDUTIN AND SUMMARY 2 TEST MATERIALS AND METDS 5 2. Speified Adhesives ' Selet f Adherds nd Priers Adherds (Substrtes) Priers 2 2. Pressg 2.. Mixg.nd ndlg hrteristis 2..2 Unifrity f Lts Vdr Qulity ntrl ertifites Selet f RTV Sile fr Mdifit Selet f Mirblln Fillers Selet f lsed-ell Sile Rubber Spnge 8 DEVELPMENT F REDUED MDULUS AND LWER DENSITY ADESIVE SYSTEM 9. Mdifit f Dw g's 77-7 RTV Sile Mteril 2.2 Mdifit f GE RTV-56 Usg Mirbllns s Fillers 2. Rybests-Mnhttn's lsed-ell Sile Rubber Spnge, RL-97, Bnded Betwe GE RTV Effet f Redued Pressure n RL-97 Spnge Selet f RL-97/GE RTV-56 s the Furth Adhesive Syste the Prgr 28.4 Dsity f Adhesives iii

6 TABLE F NTENTS (ntued) Set Pge 4 MEANIAL PRPERTIES 4. Adhes Ts Test Methd Results nd Disuss Dt Anlysis Adhes Sher Test Methd Results nd Disuss Dt Anlysis Tsile Mdulus nd Pissn's Rti Test Methd Results nd Disuss Sher Mdulus Test Methd Results nd Disuss press Mdulus Test Methd Results nd Disuss Pissn's Rti Results Disuss nstnt StStress Relxt Test Methd Results nd Disuss 27 iv

7 TABLE F NTENTS (ntued) Set Pge 5 TERMAL PRPERTIES 5. Therl Expns Test Methd Results nd Disuss Therl ndutivity Test Methd Results nd Disuss Speifi et Test Methd Results nd Disuss Therl ylg Bnd-Shped Speis Trsl Sher Speis Sher Strgth t Filure Tsile (Spl) Speis 6 6 BEAVIR F SILINE RUBBER ADESIVES AT AND BELW TEIR GLASS TRANSITIN TEMPERA- TURES bservt f Speis t nd Belw Glss-Trnsit Teperture Literture Survey Regrdg Lw Teperture Prperties f Sile Rubber Stress Relxt f Plyers t Lw Teperture 68 7 NLUSINS AND REMMENDATINS 7 7. nluss Redts 7

8 TABLE F NTENTS (ntued Set APPENDIX I APPENDIX II i APPENDIX III APPENDIX IV APPENDIX V APPENDIX VI REFERENES Qulity ntrl Duts Reeived fr Test ndidte Mterils Sury f Regress Anlysis nd Tlerne Liit Tehniques Used Dt Redut pilt f Stress-Str lults Sury f Str nfide Liits fr Best Fittg Regress Equt t Stress-Str Dt Sury f Strgth nfide Liits fr Best Fittg Regress Equt t Strgth-Teperture Dt Tsile Mdulus, Piss's Rti Lest Squre putts Pge vi

9 LIST F I L L U S T R A T I N S Figure Pge Prgr verview 7 2 Tsile Spei 8 Sher Spei 8 4 Tsile Mdulus Spei 8 5 Sher Mdulus Spei 8 6 press Spei 9 7 Dsity nd Speifi et Spei 9 8 Therl Expns Spei ' 9 9 Therl ndutivity Spei 9 Bnd-Shped Spei nstnt Str Ts Adhesive Spei IQ 2 Tsile Stress-Str f Aluu t Aluu Bnded Butt Jts.64" Glue Les (pprx.) Tests t 75 F 27 Sher Stress-Str f Aluu t Aluu Bnded Sgle verlp Jts.64" Glue Les (pprx.) Tests t 75 F 27 4 Vlue hnge Vs. Tie t Vuu nd Pressure: RM RL-97 Spnge 29 5 ylder Adhes Test Setup 5 6 Tsile Strgth Vs. Teperture 8 7 Ultite Elngt Vs. Teperture 8 8 Averge Fltwise Tsile Strgth f Adhesive Mterils 45 vii

10 LIST F ILLUSTRATINS (ntued) Figure Pge 9 Tsile Strgth Vs. Teperture - RTV-56 Mteril 46 2 Tsile Strgth Vs. Teperture - SLA-56 Mteril 46 2 Tsile Strgth Vs. Teperture D 9-46 Mteril Tsile Strgth Vs. Teperture RTV 56/ RL Tsile Stress-Str RTV-56 (-27 F) Tsile Stress-Str RTV-56 (-2 F) Tsile Stress-Str RTV-56 (-75 F) Tsile Stress-Str RTV-56 (-5 F) Tsile Stress-Str RTV-56 (-65 F) Tsile Stress-Str RTV-56 (8 F) Tsile Stress-Str RTV-56 ( F) 48 Tsile Stress-Str RTV-56 (5 F) 48 Tsile Stress-Str SLA-56 (-5 F) 49 2 Tsile Stress-Str SLA-56 (-65 F) 49 Tsile Stress-Str SLA-56 (8 F) 49 4 Tsile Stress-Str SLA-56 ( F) 49 5 Tsile Stress-Str SLA-56 (5 F) 5 6 Tsile Stress-Str D-9-46 (-27 F) 5 7 Tsile Stress-Str D-9-46 (-2 F) 5 viii

11 LIST F ILLUSTRATINS (ntued) Figure Pge 8 Tsile Stress-Str D-9-46 (-75 F) 5 9 Tsile Stress-Str D-9-46 (-5 F) 5 4 Tsile Stress-Str D-9-46 (-65 F) 5 4 Tsile Stress-Str # D-9-46 (8 F) 5 42 Tsile Stress-Str #2 D-9-46 (8 F) 5 4 Tsile Stress-Str D-9-46 ( F) Tsile Stress-Str D-9-46 (5 F) Tsile Stress-Str RTV 56/RL-97 (-27 F) Tsile Stress-Str RTV 56/RL-97 (-2 F) Tsile Stress-Str RTV 56/RL-97 (-75 F) 5 48 Tsile Stress-Str RTV 56/RL-97 (-5 F) 5 49 Tsile Stress-Str RTV 56/RL-97 (-65 F) 5 5 Tsile Stress-Str RTV 56/RL-97 (8 F) 5 5 Tsile Stress-Str RTV 56/RL-97 ( F) Tsile Stress-Str RTV 56/RL-97 (5 F) 54 5 Sher Strgth Vs. Teperture Averge verlp Sher Strgth f Adhesive Mterils 6 55 Sher Strgth Vs. Teperture RTV-56 Mteril 6 56 Sher Strgth Vs. Teperture SLA-56 Mteril 6 57 Sher Strgth Vs. Teperture D 9-46 Mteril 6 IX

12 LIST F ILLUSTRATINS (ntued) Figure Pge 58 Sher Strgth Vs. Teperture RTV-56/ RL Sher Stress-Str urve RTV-56 (-75 F) 64 6 Sher Stress-Str urve RTV-56 (-5 F) 64 6 Sher Stress-Str urve RTV-56 (8 F) Sher Stress-Str urve RTV-56 ( F) 65 6 Sher Stress-Str urve RTV-56 (5 F) Sher Stress-Str urve SLA-56 (-5 F) Sher Stress-Str urve SLA-56 (-65 F) Sher Stress-Str urve SLA-56 (8 F) Sher Stress-Str urve SLA-56 ( F) Sher Stress-Str urve SLA-56 (5 F) Sher Stress-Str urve D 9-46 (-65 F) 66 7 Sher Stress-Str urve D 9-46 (8 F) 67 7 Sher Stress-Str urve D 9-46 ( F) Sher Stress-Str urve D 9-46 (5 F) 67 7 Sher Stress-Str RTV 56/RL-97 (-27 F) Sher Stress-Str RTV 56/RL-97 (-2 F) Sher Stress-Str RTV 56/RL-97 (-75 F) Sher Stress-Str RTV 56/RL-97 (-5 F) Sher Stress-Str RTV 56/RL-97 (-65 F) Sher Stress-Str RTV 56/RL-97 (8 F) 69

13 LIST F ILLUSTRATINS (ntued) Figure Pge 79 Sher Stress-Str RTV 56/RL-97 ( F) 69 8 Sher Stress-Str RTV 56/RL-97 (5 F) 69 8 Pissn's Rti fr GE's RTV 56 t R Teperture Veritrn er Munted n RE/2K Stt Tester 7 8 Tsile Mdulus Setup 7 84 Tsile Mdulus Vs. Teperture RTV-56,.4 In./In./M Str Rte Tsile Mdulus f RTV-56 Vs. Str Rte Tsile Mdulus Vs. Teperture D 9-46,.4 In./In./M Str Rte 8 87 Tsile Mdulus f D 9-46 Vs. Str Rte 8 88 Tsile Mdulus Vs. Teperture SLA-56.4 In./In./M Str Rte Tsile Mdulus f SLA-56 Vs. Str Rte 82 9 Tsile Mdulus Vs. Teperture RTV-56/ RL Tsile Mdulus f RTV-56/RL-97 Vs. Str Rte Sher Mdulus Test Setup 86 9 Sher Mdulus f GE-56 t Vrius Str Rtes, Bndle Thiknesses nd Tepertures Sher Mdulus f D 9-46 t Vrius Str Rtes, Bndle Thiknesses nd Tepertures Sher Mdulus f SLA-56 t Vrius Str Rtes } Bndle Thiknesses nd Tepertures xi

14 LIST F ILLUSTRATINS (ntued) Figure Pge 96 Sher Mdulus f GE 56/RL-97 t Vrius Str Rtes, Bndle Thikness nd Tepertures 97 press Mdulus Test Setup 98 Effet f -2 F n D 9-46 press Speis 5 99 Effet f 55 nd 6 F n press Speis 5 press Mdulus f GE RTV-56 Vs. Teperture press Mdulus f D 9-46 Vs. Teperture 2 press Mdulus f SLA-56 Vs. Teperture press Mdulus f RM/RL-97 Vs. Teperture 4 nstnt Str Test Fixture 24 5 Stked Spei nstnt Str Test Setup 24 6 Stress Relxt t nstnt Str, GE RTV-56, Bnd Speis 28 7 Stress Relxt t nstnt Str, SLA-56, Bnd Speis 28 8 Stress Relxt t nstnt Str, R/M RL-97, Bnd Speis 28 9 Stress Relxt t nstnt Str, GE RTV-56, Stked Dis Speis 29 Stress Relxt t nstnt Str, SLA-56, 29 Stked Dis Speis xii

15 LIST F ILLUSTRATINS (ntued) Figure Pge Stress Relxt t nstnt Str, R/M RL-97, Stked Dis Speis 29 2 Therphysis rp. Mdel TE-L Ler Therl Expns Unit Perk Eler Differtil Snng lrieter/ Therehnil Anlyzer Unit 4 Ler Therl Expns Vs. Teperture, RTV Ler Therl Expns Vs. Teperture, D Ler Therl Expns Vs. Teperture, SLA Ler Therl Expns Vs. Teperture, RM/RL Ler Therl Expns Vs. Teperture 4 9 Liquid Nitrg Beg Flwed Thrugh ASTM-- 77 Therl ndutivity Tester 47 2 Therl ndutivity Vs. M Teperture, RTV Therl ndutivity Vs. M Teperture, D Therl ndutivity Vs. M Teperture, SLA Therl ndutivity Vs. M Teperture, R/M RL-97 Spnge Therl ndutivity Vs. M Teperture Bnd-Shped Spei Test n RE-2K Bdix Stt Test Mhe 59 xiii

16 LIST F ILLUSTRATINS (ntued) Figure Pge 26 Test Are fr Tsile Mdulus nd Pissn's ;. Rti ; Lest Squres Elsti Mdulus nd Pissn's Rti 29 xiv

17 LIST F TABLES Tble I Adhesive Advntge nd Disdvntge Sury 4 II Adhesive Prperties f Vrius Lts f GE-56 Usg GE 44 nd 455 Priers 7 III Prperties f Dw g's RTV Sile 77-7 Frults 22 IV Dw rng Sgle verlp Sher Dt 2 V VI Dw rng X-6 Tsile nd Lp Sher Adhes Dt 24 Tsile nd Sher Strgth f Frulted GE-56 nd Rybests-Mnhttn RL-97 lsed ell Spnge Bnded Aluu t Aluu Lp nd Butt Jts 26 VII Dsity t R Teperture ASTM-D-297, 7() VIII IX Ultite Tsile Strgth nd Elngt Averge Vlues 7 Sury f Tsile Stress-Str ndits Regress Anlysis 4 X Results f Tsile Stress-Str Regress 4 XI Results f Fltwise Tsile Strgth - Teperture Regress 4 XII Sgle verlp Sher Strgth Averge 56 XIII Sury f Sher Stress-Str ndits fr Regress Anlysis 59 XIV Results f Sher Stress-Str Regress 6 XV XVI Results f Sher Strgth-Teperture Regress 62 Pissn's Rti fr GE's RTV-56 t R Teperture 72 xv

18 LIST F TABLES (ntued) Tble. Pge XVII Tsile Mdulus f GE's RTV XVIII Tsile Mdulus f GE RTV-56 Detered fr ylder Adhes Spei 77 XIX Tsile Mdulus f D XX Tsile Mdulus f SLA-56 8 XXI Tsile Mdulus f RTV-56/RL-97 8 XXII XXIII XXIV XXV Sher Mdulus (Duble Lp Trs Test) f GE Sher Mdulus (Duble Lp Trs Test) f D Sher Mdulus (Duble Lp Trs Test) f SLA Sher Mdulus (Duble Lp Trs Test) f GE RTV-56/RL-97 Syste 95 XXVI press Mdulus f GE RTV-56 7 XXVII press Mdulus f D XXVIII press Mdulus f MM SLA-56 9 XXIX press Mdulus f RM/RL-97 XXX Pissn's Rti Ts XXXI Pissn's Rti press 4 XXXII Tsile Mdulus 5 XXXIII press Mdulus 7 XXXIV Pissn's Rti puted fr Sher nd Ts Mdulus 9 XVI

19 LIST F TABLES (ntued) Tble XXXV XXXVI XXXVII XXXVIII XXXIX XL XLI XLII XLIII Pissn's Rti puted fr Sher nd press Mdulus Sury f nstnt Str Tests n Bnd Speis Sury f nstnt Str Tests n Stked Dis Speis Sury f Ler Therl Expns Dt, RTV-56 Sury f Ler Therl Expns Dt, RTV-56 Sury f Ler Therl Expns Dt, D 9-46 Sury v f Ler Therl Expns Dt, MM SLA-56 Sury f Ler Therl Expns, RM/RL-97 Spnge Therl ndutivity Test Results, RTV-56 Pge XLIV Therl ndutivity Test Results, D XLV XLVI XLVII XLVIII Therl ndutivity Test Results, MM-SLA-56 Therl ndutivity Test Results, RL-97 Spnge Sury f Speifi et Vs. Teperture, Spe Shuttle Adhesives Ultite Sher Strgth nd Elngt After Envirntl nditg f Bnd Shped Speis xvii

20 LIST F TABLES (ntued) Tble XLIX LI LII LIU LIV LV LVI LVII LVI LIX LX LXI LXII LXIII LXIV LXV LXVI LXVII Ultite Sher Strgth nd Trsl Sher Mdulus After Envirntl nditg f Duble Lp Sher Speis Adhes Ts After Envirntl nditg f yldril Fltwise Ts Speis Tsile Stress-Str Results, -27 F Tsile Stress-Str Results, -2 F Tsile Stress-Str Results, -75 F Tsile Stress-Str Results, -5 F Tsile Stress-Str Results, -65 F Tsile Stress-Str Results, 8 F Tsile Stress-Str Results, F Tsile Stress-Str Results, 5 F Ultite Tsile Strgth nd Elngt t 55 nd 6 F Sher Stress-Str Results, -27 F Sher Stress-Str Results, -2 F Sher Stress-Str Results, -75 F Sher Stress-Str Results, -5 F Sher Stress-Str Results, -65 F Sher Stress-Str Results, 8 F Sher Stress-Str Results, F Sher Stress-Str Results, 5 F XVlll

21 LIST F TABLES (ntued) Tble LXVIII LXIX LXX LXXI LXXII Sgle verlp Sher Strgth t 55 nd 6 F Sury f Tsile Str nfide Liits t -27 F Sury f Tsile Str nfide Liits t -2 F Sury f Tsile Str nfide Liits t -75 F Sury f Tsile Str nfide Liits t -5 F Pge LXXIII Sury f Tsile Str nfide Liits t -65 F 22 LXXIV LXXV LXXVI LXXVII LXXVIII LXXIX LXXX LXXXI LXXXII Sury f Tsile Str nfide Liits t 8 F Sury f Tsile Str nfide Liits t F Sury f Tsile Str nfide Liits t 5 F Sury f Sher Str nfide Liits t -27 F Sury f Sher nfide Liits t -2 F Sury f Sher Str nfide Liits t -75 F Sury f Sher Str nfide Liits t -5 F Sury f Sher Str nfide Liits t -65 F Sury f Sher Str nfide Liits t 8 F xix

22 LIST F TABLES (ntued) Tble Pge LXXXIII Sury f Sher Str nfide Liits t F 2 LXXXIV Sury f Sher Str nfide Liits t 5 F 2 LXXXV LXXXVI Sury f Tsile Strgth nfide Liits nd Strgth Allwbles 24 Sury f Sher Strgth nfide Liits nd Strgth Allwbles 25 xx

23 SETIN' INTR D UTIN AND SUMMARY

24 SETIN INTRDUTIN AND SUMMARY The wrk perfred n NASA,MS ntrt NAS9-292, Develpt f Design Allwbles fr Adhesives fr Atthg Reusble Surfe Insult, is desribed this reprt. The verll bjetive f this prgr ws t test nd estblish design llwbles dt fr the fllwg r teperture vulnizg (RTV) sile rubber bsed dhesives, (I) Gerl Eletrie's RTV-56, (2) Dw g's 9-46, nd () Mrt Mriett's SLA-56. These dhesives re beg evluted fr tthg reusble surfe sult (RSI) t spe shuttle struture. Gerl Eletri's PD-2 dhesive syste ws riglly sheduled fr testg this prgr, but it ws deleted per A N. erly the prgr. A further bjetive ws t dify existg RTV sile dhesive frults t iprt redued dulus nd dsity s pred t the dhesives speified bve. In this prt f the prgr, develpt wrk ws nfed t difits f GE RTV-56 nd Dw g's unfilled RTV 77-7 nd develpt f n dhesive syste prised f Rybests Mnhttn's RL-97 lsed-ell sile spnge sndwihed betwe bnd les f GE RTV-56. Glss nd phli irbllns were dded t GE RTV-56 nd D-77-7 frults t redue dsity nd pssibly redue dulus. This pprh ws suessful redug dsity, but the high dulus f the irbllns used the dului f the frults t rese rther thn derese. The ddit f irbllns t the frults ls reted shelf gg nd pressg prbles. The syste prised f RL-97 spnge bnded with GE RTV- 56 prved t be quite suessful. Its dsity is less thn hlf tht f the slid dhesives tested, nd it hs very lw dulus. The syste pssesses dequte strgth t pete with the ther dhesives. Bsed n these fdgs, the RL-97/GE RTV-56 syste ws seleted fr design llwble testg lng with the three ntrt speified dhesives. The three speified dhesives nd the RL-97/GE RTV-56 develped syste were tested fr dhes ts nd sher; 2

25 tsile, sher, nd press dulus lng with Pissn's rti; nstnt-str/stress-relxt; therl expns, therl ndutivity, nd speifi het; nd effets f therl ylg. Test ethds used nd dt bted re reprted here. Design llwbles urves were develped fr dhes ts nd sher t filure t tepertures bve the glss trnsit pts f the fur dhesive systes. A sury f the dvntges nd disdvntges f the fur dhesive systes is prested Tble I. Diffiulties were untered deterg the dulus f the fur dhesives t tepertures belw their glss trnsit pts. These diffiulties rse beuse the test ethds fr deterg defrt f speis under resg lds were designed t dte high elngts. As the dhesives bee stiff nd brittle t tepertures belw their glss trnsit pts, defrt under the reltively lw lds bee s sll tht ute esuret uries used extree flututs lulted vlues f dulus. Pissn's rti vlues bted n the dhesives t tepertures belw their glss-trnsit pts were ls extreely vrible fr the se resn s the dulus vlues. In ddit, it ws disvered, unexpetedly, tht speis exhibited shrkge wh itilly subjeted t ld t these lw tepertures. Initil pplible f ld prdued negtive rther thn psitive elngts. Under these lw ldg ndits, Pissn's rti uld nt be detered. Beuse f this unfrese prble t lw tepertures nd due t the ft tht vlues fr the dhesives their rubbery stte re pprxitely.5, utilizt f these dt nlysis tehniques bsed n theries f elstiity is dvisble.. Under dt 2S t this ntrt, fifth dhesive, Dw g's X-64, ws tested the se s the fur vered this reprt. In ddit, tsile dulus f X-64, lng with GE RTV-56 s ntrl, ws tested usg new predure. Mlded "dg bne" shped speis, hes lng with.5-h-dieter thrts, were fitted with 2-h Instrn extseter nd tested n virntl hber n n Instrn test he. This ethd gve signiftly higher tsile dulus vlues thn the strp speis desribed prgrph f this reprt. Detils f the test nd dt bted re prested n dddu t this reprt.

26 TABLE I ADESIVE ADVANTAGE AND DISADVANTAGE SUMMARY Adhesive Advntges Disdvntges GE RTV-56 Esy pressg Best lw teperture prperties ighest strgth t teredite teperture ighest therl ndutivity ighest dsity ighest dulus Thik sets blister ternlly t 55 F D 9-46 Sd lwest dulus Visus, diffiult t press ighest glss trnsit teperture rks n therl shk t -2 F Thik sets revert nd blister ternlly t 55 F SLA-56 Best high teperture strgth Esy pressg, esiest t degs Wek sher strgth Thik sets rk t 55 F Fresh SLA-56 hs lw dhes t ured SLA-56 RL-97/GE RTV-56 Lwest dsity Lwest dulus Lwest therl ndutivity Vlue ssitive t pressure hnge Lwest strgth Must be slied t desired thikness ptibility with bse dhesive ust be detered

27 SETIN 2 TE'ST' MATERIALS AND METDS

28 SETIN 2 TEST MATERIALS AND METDS ndidte dhesives nd tests nduted re shwn Figure, prgr verview. Tests were gerlly nduted triplite, usg idtil speis. Spei nfigurts were s shwn Figures 2 thrugh. Wh therl nditg r testg t lw r elevted teperture ws vlved, the required virnt ws ted fr five utes fllwg stbilizt f the spei t bit ndits. 2. SPEIFIED ADESIVES riglly the prgr lled fr testg f the fllwg terils:. GE RTV-56. Dw rng GE PD-2 4. Mrt MM SLA-56 The GE PD-2 ws deleted fr the prgr wh it bee iprtil fr NASA,.MS t bt fbrited speis fr GE. A further ntrt bjetive ws t ndut vestigts ledg t develpt f lwer dulus nd dsity dhesive syste. The effrt ws nt nsidered t be jr frult f dhesives but rther difit f existg dhesives. As result f this effrt the prgr, the GE RTV-56/RL-97 syste evlved s the st prisg teril, the tehnil nitr greed t lude it the prgr s the furth test dhesive syste. 2.2 SELETIN F ADERENDS AND PRIMERS Selet f these terils ws bsed n the st ret frt vilble reltive t spe shuttle tehnlgy.

29 Develpt f' Lwer Mdulus nd Dsity Adhesive Mterils GE RTV-56 Dw rng 9-46 Mrt Adhesive - MM SLA-56 GE RTV-56/RL 97 Envirntl Test ndits F Tests Tsile Stress-Str Sher Stress-Str I Pissn's Rti ( Str Rtes) Sher Mdulus Tsile Mdulus press Dsity (RT) Therl Expns Speifi et Therl ndutivity Therl ylg nstnt Str/Stress Relxt Figure Prgr verview

30 B i-l > D. <u J-l 6 i-l.,- ) X l T (- t <u Xi l 6 - i, ) I-l - w ) J-l b i-l i-t. i i TD E-i M l 8

31 t «Q. X w J > (U /i T-l l-l 4J U r >j (LI N tu,

32 rl t ) 8 f - nj d) u U - J-l W (U 4: T < (U!-i d tj f (U (U. > t J2 I T> M )!-i d

33 2.2. Adherds (Substrtes) Bre luu lly sheet 224T8 nd rd 224T85 were used s the substrte fr ll the dhesive systes tested. All substrtes were unifrly led by the fllwg tehnique:. All surfe sils, il, nd grese were reved by wipg with heeselth isted with ethyl ethyl ketne (MEK). 2. Spei substrtes were th vpr degresed trihlrethyle vpr degreser.. Pre-eth lg ws plished by iers fr 9 t 5 utes slut f the fllwg psit ted t r teperture: 69% Nitri Aid t 22% by Vlue Fed. Spe. (-N-5) 7 ydrfluri Aid.4 t.8% by Vlue hriu Trixide Fed. Spe. (--B) Tp Wter.5 t (Dry Wt.) Blne t ke gl. 4. Adherds were rsed l, runng tp wter t r teperture fr 6 t 2 utes. 5. Adherds were th iersed fr 9 t 5 utes slut f the fllwg psit, whih ws ted t F. (66 Be) Sulfuri Aid Fed. Spe. (-S-89A) Sdiu Bihrte Fed. Spe. (-S-595) Wter (Tp) Prts/Wt. 4 Prts/Wt. Prts/Wt. 6. Spei substrtes (dherds) were rsed l tp wter t r teperture nd th spry rsed thrughly with r teperture deerlized wter.

34 7. Dryg ws plished 6 F + F v fr utes. NTE: Durg ll degresg, lg, rsg, nd dryg perts the speis were dividully seprted luu rks t prvide idtil, unifr trett Priers Bsed n either vdrs dt nd redts, r previusly bted dt fr r teperture lp sher tests f prier, dhesive, nd dherd bts, the fllwg dhesive prier systes were seleted.*. GE RTV-56 with GE SS44 r GE SE455 prie 2. D 9-46 with D 2 prie. MM SLA-56 with D 2 prie 4. GE RTV-56/RL 97 with GE SE455 prie * ure tie fr ll speis ws 7 dys. The fundtl nsidert seletg priers ws the bility t prte dhes suffiit t prvide hesive filures f the dhesive rther thn dhesive filure t the substrte. Prtilly ll f the speis the prgr did fil hesively. In the pplit f priers it is nvir's experie nd bservt tht very th but unifr tg f priers is required. Thiker tgs f the silne-bsed priers fr lsely dherg pwders n the surfe wh they hydrlyze. Therefre, this effrt ll priers were pplied with l el's hir rtist's brush t ver the surfe pletely. The pried surfe ws th ieditely wiped with l heeselth r lt free "Ki-Wipe's" revg ll exess prie. The reg very th fil ws llwed t ir dry fr utes befre pplit f the subsequt required dhesive. Initilly, the vdr reded tht SS44 prier be used with the GE RTV-56 dhesive. Diffiulties develped with the use f this prier (prgrph 2..2.), hwever, nd the vdr 2

35 lter suggested tht SE455 be evluted fr use ple f SS44. The SE455 prier is silne-type prier, while the SS44 is sile res type. The SE455 prests fewer prbles pplit; i.e., it kes re unifr tg n the luu substrtes. Als, urrt tests f lp sher nd fltwise ts dhes speis de with SE455 prier nd tested up t 6 F shw pert hesive filures the RL-97. e, there ppers t be n prble with the SE455 prier t elevted teperture. Bsed n these fdgs, GE prier SE455 ws used t prepre the reg speis under the ntrt. A new lt f GE RTV-56 ws rdered fr use A N. nd ws tested befre use preprg the required speis. 2. PRESSING The tehniques used were bsed n nvir Aerspe's previus experie with selg nd pttg punds. All pertt detils re supplied the fllwg sets. 2.. Mixg nd ndlg hrteristis Adhesive pnts were ixed s desribed belw. All ixg nd urg were perfred r with ntrlled teperture f 77+2 F nd reltive huidity f 5+5 pert Weighg Bse terils nd their rrespndg tlysts were weighed n trs blne. Bth sizes f grs r re were used t prvide dditl unifrity GE RTV-56 The weight rti f the bse t the tlyst fr this ndidte teril is :.5. The -desired quntity ws weighed ut new l ixg nter, nd the ext required quntity f tlyst ws dded t the bse. The teril th ws hnd blded with sptul fr iu f five utes. The pletely blded GE RTV-56 ws th trnsferred t new plsti Se trifugedispsg tubes. Mst f trpped ir bubbles ws expelled by

36 trifugg the teril t 5 RPM fr utes. The GE RTV-56 ws ieditely pistn dispsed fr the tube t the vrius types f spei lds r pplied dhesive jts. Wrk life f GE RTV-56 ws pprxitely 2 hurs D 9-46 D 9-46 is blk thixtrpi teril nd requires speil tehniques t hieve unifr blds. The weight rti f the bse t the tlyst is :. It ws ls bth size liited; i.e., wh bthes lrger thn 5 grs were ttepted redued pt life resulted nd the teril tded t gel nd bee re visus nd tky. nsequtly, t 4 gr bthes were utilized. Mixg ws plished by ne f the tw ethds listed belw:. The bse nd tlyst were prtilly ixed. The preixed teril ws th vuu degssed (28. g..) fllwed by fl ixg pneuti perted Pyles Industries ixer. With this devie, ixed teril ws hydrulilly fred t plsti Se tubes. Filled tubes were th ieditely utilized t jet the D 9-46 t the required spei lds r dhesive jts. 2. The : weighed D 9-46 ws thrughly ixed fr t lest 5 utes new thrw-wy nter. It ws th evuted (28. g..) fr 5 utes. The teril ws trnsferred t plsti Se tubes nd trifuged t 5 RPM fr utes. It ws ieditely jeted t fr the required speis. This evlved ethd ws the fl preferred ethd f ixg nd degssg se it elited the lbrius, tie nsug tsk f lg the Pyles ixer ieditely fter eh bth. The wrk life f D 9-46 ws pprxitely hur MM SLA-56 This teril is trnsprt bld f bse-tlyst rti f : by weight. Vissity is idel fr unifr ixg; hwever, ir bubble trppt ws prble. Bubbles were elited by evut (28. g..) fr 5 utes, fllwed by trifugt Se plsti tube fr utes t 5 4

37 RPM. The teril ws ieditely jeted t the required spei lds r dhesive jts. The wrk life f MM SLA-56 ws pprxitely hur GE RTV-56/RL-97 This ws psite teril psed f GE RTV-56 blded s desribed nd slies f RM/RL-97 lsed-ell sile spnge. The required thikness f spnge fr the vrius speis ws ut t spei nfigurt. The surfes f the spnge were wshed with ethyl ethyl ketne nd bltted dry with heeselth severl ties. After ute ir dry, RTV- 56 ws trwelled nt the spnge fyg surfes with sptul. After brief experitt, it ws lerned the surfe thikness f.5 t. h RTV-56 tg uld be ntrlled by srpg ff the exess levg just ugh teril t fill the surfe ells nd t ntuus, unifr surfe tg Unifrity f Lts ' Vribility f Differt Lts f GE RTV-56.. The jrity f tests f GE RTV-56 this prgr were nduted usg 5-pund shipt f lt nuber 592. A -pund shipt f lt 68 ws reeived t plete the tests. In the teri betwe use f these tw lts, nvir ws ntified by NASA,.MS tehnil nitr tht Gerl Eletri ws hvg dhes prbles with se lter lts f GE RTV-56, prtiulrly wh used t bnd sile rubber spnge t substrtes. nvir Aerspe ieditely tested lt 68 njunt with Rybests-Mnhttn's RL-97 lsed-ell sile rubber spnge. GE prier SS44 ws used the test speis. Test filures were stly dhesive filures betwe the GE RTV-56 nd the SS44 prier; with lts 592 nd 68, filures were pert hesive the RL-97 spnge. nvir Aerspe ntified Gerl Eletri Sile Divis f the prble, nd Gerl Eletri repled lt 68 with lt 69 nd suggested tht GE prier SE455 be used lieu f SS44. Lt 69 ws tested the se nner s desribed bve. 5

38 Lt 69 shws se f the se tdy s lt 68 t fil dhesively t the SS44 prier terfe; hwever, tests with SE455 prier shw 99 pert hesive filure the RL-97 spnge. Dt bted re tbulted Tble II. Bsed n these dt, the few reg GE RTV-56/RL-97 spnge speis were de usg SE 455 prier lieu f SS44 prier Vdr Qulity ntrl ertifites Vdr qulity ntrl ertifits pnyg terils used this prgr re luded Appdix I. 2.4 SELETIN F MATERIALS FR DEVELPMENT F REDUED MDULUS AND DENSITY ADESIVE Tw pprhes were seleted fr difyg vilble sile RTV dhesives t redue dulus nd dsity. ne pprh ws t fill suitble RTV sile dhesives with extreely lw dsity glss r phli irbllns. The ther pprh ws t bt lw-dsity, lw-teperture, erilly vilble sile rubber spnge tht n be slied t ny desired thikness. Seleted thiknesses n th be bnded betwe substrtes t prvide lw-dulus, lw-dsity bnd les Selet f RTV Sile fr Mdifit GE RTV-56 nd Dw rng 77-7 were seleted fr difit. Bth re plyers ntg phyl grups the plyer h t iprt lw-teperture prperties. GE RTV-56 ws seleted fr its lw vissity. It ws resned tht greter pert f lw-dsity fillers uld be rprted; he, lwer dsity f the ured dhesive bnd le wuld result, D 77-7 ws seleted beuse f its hert lw dulus nd bse f fillers. ere g it ws resned tht D 77-7 wuld ept greter vlue f lw-dsity fillers nd result nsiderbly redued dulus nd dsity dhesive Selet f Mirblln Fillers The fllwg irbllns were seleted fr use this prgr: 6

39 TABLE II ADESIVE PRPERTIES F VARIUS LTS F GE-56 USING GE SS 44 & SE 455 PRIMERS (Lp Sher Speis,. jts, 224 T8,.64".Ld Rte."/.) Lt N. 592 Withut spnge Glue Le Pert Bndle Sher, psi hesive Thikness With RL-97 spnge (.5") Glue Le Pert Bndle Sher, psi. hesive Thikness " *With SE 455 rther tl Prier Nte: All speis de with GE SS 44 prier exept s nted n SS

40 . M's B-22A glss 2. Eersn Gug*s IG- glss. Un rbide's BJ-9 phli These three fillers were seleted fr their lw dsity (less thn.g./), vilbility, nd reltively lw st Selet f lsed-ell Sile Rubber Spnge Rybests-Mnhttn s RL-97 sile spnge ws seleted fr use the prgr beuse f its lsed-ell struture, lw dsity (.g./), nd lw-teperture prperties. nvir Aerspe uses this spnge ert F-lll irplne pplits nd it hs prved t be unifr qulity nd dsity fr lt t lt. It n be bted fr the vdr st ny thikness desired dwn t. h. 8

41 SETIN DEVELPMENT F REDUED MDULUS AND LWER DENSITY ADESI V E SYSTEM 9

42 SETIN DEVELPMENT F REDUED MDULUS AND LWER DENSITY ADESIVE SYSTEM Deresg the dulus nd dsity f the dhesive wuld effet substntil weight svgs the spe shuttle therl prtet syste (TPS). Therefre, the bjetive fr this prt f the prgr ws t dify existg dhesives t redue bth dulus nd dsity yet ret suffiit strgth prperties t prvide relible ttht f the RSI t the spe shuttle struture. Apprhes tk were:. Frult f Dw g's lw dulus sile teril 77-7 usg fillers s well s phli nd glss irbllns t ke lw-dsity syntti f. 2. Frult f GE RTV-56 with the se phli nd glss irbllns t redue dsity.. Utilizt f Rybests-Mnhttn s lsed-ell sile spnge with th glue les f GE RTV-56 n either side nd GE prier SE455 n the dherds.. MDIFIATIN F DW RNING'S 77-7 RTV SILINE MATERIAL Dw g's 77-7 ixed with pnyg tlyst ures t r ndits. Preliry tests f the teril shwed it t hve extreely lw dulus but unexpeted lw strgth prperties. Dw g's tehnil servie persnnel were ntted t disuss the need fr lw-dulus RTV sile dhesive nd the defiiies f Dw rng suggested rprtg 5 irnprtile-size Musil (Pnsylvni Snd nd Glss' grund sili) t iprve tsile strgth nd elngt. Sll bthes f 77-7, ne with nd nther with 4 prts per hundred f rubber (phr) 5-irn Musil, were prepred. Tw dditl bthes were ixed; ne hd 8 phr phli irbllns nd the ther hd 5 phr phli irbllns plus phr 5-irn Musil. Sheets f the fur bthes were st. Sll dubbell speis were ut fr these sheets nd tested fr ultite tsile strgth nd elngt. Lp sher speis usg bth D 92-9 nd 2

43 D 2 prier n.64 guge 224-T8 dherds were ls prepred. Frults nd dt bted re shwn Tble III. Anlysis f these dt dited tht re wrk ws needed t iprve the strgth, dhes, nd pressg prperties f the Refret f the 77-7 with t 4 phr f 5-irn Musil resed tsile strgth fr 8 psi t 5 psi, but its ter strgth ws still lw. Vissity f the frulted 77-7 ws lw, whih de it diffiult t nfe it bnd le. Further disusss were held with Dw rng persnnel regrdg lw strgth nd vissity f the frulted Dw rng respnded by refrultg the 77-7 t prdue re wrkble vissity teril. The new frult ws designted Explrtry tests nsistg f lp sher strgth f the t 224-T8 luu shwed the dhesive t hve exellt sher strgth fter dys ure nd it still exhibited the desirble lw dulus s shwn Tble IV. bservts durg the fbrit f these lp sher speis reveled tht the ws t visus fr esy pressg. The tests ls shw tht D 92-9 prier did nt develp full sher strgth f the Filures were pert dhesive t the luu substrtes. Fllwg further delibert with Dw rng represttives, third frult, designted X-6 nd bsed n the se plyer preursr syste, ws subitted t nvir Aerspe. Fltwise ts nd lp sher speis were prepred with the X-6. Test dt bted is shwn Tble V. The X-6 hs exellt strgth bth ts nd sher s well s high elngt nd lw dulus. Althugh X-6 shws highly desirble prperties, the bse pnt f the tw-pnt syste thiks preturely durg shelf strge. Dw rng detered tht this is due t hydrg bndg betwe ne f the fillers nd the liquid plyer. This ndit hs nw be rreted by substitut f nther filler. The furth refrult is designted X-64, but its develpt e t lte fr it t be nsidered s ndidte dhesive this ntrt wrk..2 MDIFIATIN F GE RTV-56 USING MIRBALLNS AS FILLERS Gerl Eletri's RTV-56 hs the lwest vissity f the three sile dhesives luded this prgr; therefre, it 2

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