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I MATERIALS AND INTERFACES LAB J E MCGRATH ET AL.

k AD-Ai4 624 ELASTOMERS AND OTHER ORGANIC COMPOSITES(U) VIRGINIA i/i POLYTECHNIC INST AND STATE UNIV BLACKSBURG POLYMER I MATERIALS AND INTERFACES LAB J E MCGRATH ET AL. UNCASSFIE 25OCT 84 ARO-i76i7.33-CH
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k AD-Ai4 624 ELASTOMERS AND OTHER ORGANIC COMPOSITES(U) VIRGINIA i/i POLYTECHNIC INST AND STATE UNIV BLACKSBURG POLYMER I MATERIALS AND INTERFACES LAB J E MCGRATH ET AL. UNCASSFIE 25OCT 84 ARO-i76i7.33-CH DAAG29-88 K 8893 F/G N L2.8M 25 1o 1111 U.02 UU I I MICROCOPY RESOLUTION TEST CHART NATO UO TNMW6- (0 N I- A a /%I,,7.33.4,' ELASTOMERS AND OTHER ORGANIC COMPOSITES FINAL REPORT J. E. MCGRATH, G. L. WILKES, D. G. BAIRD, T. C. WARD, D. W. DWIGHT OCTOBER 15, 1984 U.S. ARMY RESEARCH OFFICE O T IC CONTRACT NUMBER: DAAG29-80-K W A VIRGINIA POLYTECHNIC INSTITUTE AND STATE UNIVERSITY -POLYMER MATERIALS AND INTERFACES LABORATORY 404 DAVIDSON HALL BLACKSBURG, VIRGINIA DISTRIBUTION APPROVED FOR PUBLIC RELEASE; UNLIMITED D' 11 s 085 SECURITY CLASSIFICATION OF THIS PAGE (Wien Date Entero MATER COPY - FOR REPRODUCTION PURPOSES H.RPR UMBER REPOR DOCUMENTATION PAGE READ INSTRUCTIONS 2.GOVT ACCESSION NO. S. RECIPIENT'S CATALOG NUMBER [ _N/A N/A 14. TITLE (d Sabdtl.) S. TYPE OF REPORT & PERIOD COVERED Elastomers and Other Organic Composites Final Report 9/30/80-6t29/84 S. PERFORMING ORG. REPORT NUMBER 7. AUjTNORE') S. CONTRACT Olt GRANT NUNSERt(a) J. E. McGrath, G. 1. Wilkes, T. C. Ward, D. G. Baird, D. W. Dwight DAAG29-8OK PERFORMNG14 ORGANIZATION NAME AND ADDRESS 10. PROGRAM ELEMENT PROJECT. TASK AREA A WORK UNIT NUMBERS Virginia Polytechnic Institute and State Univ. Polymer Materials and Interfaces Laboratory 404 Davidson Hall, Blacksburg, VA It. CONTROLLING OFFICE NAME AND ADDRESS 12. REPORT DATE U. S. Army Research Office October 25, 1984 Post Office Box IS. NUMBER OF PAGES M1N. UP0ING GNYAMO I hen ConteoIhoa 0Office) 1S. SECURITY CLASS. (of di. tepees) Unclassified IS&. DECJIASSIFICATION/ DOWNGRADING SCHEDULE IS. DISTRIBUTION STATEMENT (of tis Repot) Approved for public release; distribution unlimited. 17- DISTRIBUTION STATEMENT (of the absaoetaere~td In Block 20. i dtewent from Report MA IS. SUPPLEMENTARY NOTES The view, opinions, and/or findings contained in this report are those of the author(s) and should not be construed as an official Department of the Army position, policy, or decision, unless so Apee InntPA hy nrhor dn',etnt4n it. KEY WORDS (Centhww, en reverse side I ecessary mi IdenuUI by. block member) Elastomers, Composites, Anionic Polymerization, Siloxanes, Butadlene, Liquid. Crystals, Blends, Ion-Containing Polymers, Morphology, Rheology, Inverse Chromatography, NMR, Surface Science. A4 AcrAC t(ndu M.oet abb 0.enow mi euaty by Wleek nmber),-=the objective of this program was to bring together five investigators whosk expertise was in the area of polymer synthesis, characterization, rheology and processing, solid state morphology and mechanical behavior and surface science. This abstract will describe some highlights of research findings and'potential applications. In addition, in an appendix we have included statistics on publications, preprints and theses. JIM 1 3 'YSO NO SSOLT UNCLASSIFIED SECURITY CLASSIFICATION, OF THIS PAGE (8ken Date Entered) !/CT.ARR T WTV SCCUNTY CLASIICATION OF THIS PAGE(Ufm Daated AM10 Butadiene-isoprene copolymers and their hydrogenated derivatives were examined. It was demonstrated that the block copolymers could be designed to provide a balance of chain scission and crosslink degradation behavior. This may be important in a variety of applications including vehicle treads. The block isoprene copolymers were also hydrogenated to yield interesting semi,-crystalline thermoplastic elastomers. Fundamental aspects of anionic polymeriiations have been studied which allow the control of molecular weight, molecular weight distribution and functional end groups. Such intermediates have promise for the synthesis of new elastomer components including possibly hybrid polyurethane cast pads that would have selective surface structure. Soluble difunctional initiators which can be used as intermediates to elastomers andpoyos have alsp been studied. Liquid crystalline copolymers are of great current interest and have already been demonstrated to be important reinforcing fibers for both elastomers and composites. This study has principally dwelt upon the relationships between chemical structure, rheology, morphology, and mechanical behavior. In addition, thermotropic polyesters and their blends with conventional PET have also been examined and show promise as advanced materials. Inverse gas chromotography (IGC) has been used to probe polymer coatings with a variety of organic liquids as the mobile phase. Depending upon the relative retention times, important thermodynamic behavior can be derived. This has applications in the swelling of polymers and elastomers and also in the transport of agents through solid polymeric films. A second important technique that has been studied and further developed by this research is solid state NMR. This method has the ability to identify and define chemical structure and possibly molecular motion in elastomers, glasses and various network structures. Polyisobutylene ion containing copolymers containing sulfonate end groups were investigated. Trifunctionality allowed for excellent mechanical properties as a combined result of ionic associations and strain induced crystallization. The ionic reinforcing phase could lead to new elastomeric materials with interesting transport properties that could possibly catalyze the decomposition of liquid agents. Copolymerization of dimethyl and trifluoropropyl methyl siloxane elastomersystems shows promise for producing a low glass transition temperature (-60 C) that can be designed to show low swelling in hydrocarbons. Cycloaliphatic linked urea copolymers were synthesized which were transparent candidates for light stable elastomeric coatings. Additional work has been done in identifying and developing chemistry for matrix resins. A dielectric unit has been constructed which will be suitable for monitoring the cure or network formation for a variety of thermosets. These would include polyimides, epoxys, and elastomer networks. Finally, extensive research has been conducted in the area of surface science which has included ESCA, SEM, and EDAX type techniques. There has been extensive instrumentation development and currently a Kratos-unit is operative. Information on the composition of surfaces versus bulk in elastomers and composites has been generated. This information has wide applicability with respect to elastomer or composite properties and systems such as tank treads. It can identify variations in compounding and also in surface oxidation by comparing, for example, oxygen to carbon ratios before and after various experiments. The general area of applying surface science to failure mechanisms has been developed significantly in this period and several good applications UNCLASSIFIED SECURITY CLASSIFICATION OF THIS PAGE(Whm Dt 0UI.t.W 4 APPENDIX (A) Publications 1. Editor, Anionic Polymerization: Kinetics, Mechanisms and Synthesis, 592 pages, ACS Symposium Series, No. 166, November, Co-Editor, Photo, Electron and Ion Probes of Polymer Structure and Properties , ACS Symposium Series, No. 162 (1981). 3. Editor, Ring Opening Polymerization: Kinetics, Mechanisms and SynthesisN, ACS Symposium Series, in preparation, J. E. Mc:Grath, An Introduction and Overview of Block Copolymers, in *Block Copolymers*, 0. J. Meier, Editor, MHI Press (1983), p J. E. McGrath, Synthesis of Block, Graft, Segmented and Ion Containing Copolymers , Pure and Applied Chemistry, Vol. 55(10), (1983). 6. I. C. Wang, Y. Mohajer, T. C. Ward, G. L. Wilkes, and J. E. McGrath, Anionic Copolymerization of Butadiene and Isoprene with Organolithium Initiators in Hexane , ACS Symposium Series, J. E. McGrath, Editor, OAnionic Polymerization: Kinetics, Mechanisms, and Synthesis , No. 166, (1981). 7. M. K. Martin, T. C. Ward, and J. E. McGrath, The Reactivity of Polydiene Anions with Divinylbenzenew, ACS Symposium Series, J. E. McGrath, Editor, Anionic Polymerization: Kinetics, Mechanisms, and Synthesis, No. 166, (1981). 8. A. K. Banthia, D. Lunsford, D. C. Webster and J. E. McGrath, *Interfacial Synthesis Part 1: Phase-Transfer Catalyzed Synthesis of Polyhydroxy EtherN, J. Macromol. Sci.-Chem., A15(5), , (1981). 9. J. S. Riffle, R. G. Freelin, A. K. Banthia, and J. E. McGrath Interfacial Synthesis Part II: Phase-Transfer Catalyzed jacoslofl For Synthesis of Polycarbonate/Polysiloxane Block Copolymers . J. -yis &I Macromol. Sci.-Chem., A15(5), , (1981). DTIC TAB 10. T. C. Ward, D. P. Sheehy, J. S. Riffle, and 3. E. McGrath, Just utoat o Inverse Gas Chromatography of Polycarbonate-Polydimethyl Siloxane Block Copolymers, Macromolecules, 14(6), , (1981). Listribution/ 11. Y. Mohajer, G. L. Wilkes, I. C. Wang, and J. E. McGrath, Ava~labLty Cad9 a /or *Hydrogenated Linear Block Copolymers of Butadiene and Isoprene special Effects of Variation in Composition and Sequence Architecture 0 SPO 1-- Properties,N Polymer (London), 23(10, (1982). 12. S. Abouzahr, Y. MohaJer, 6. L. Wilkes, and J. E. McGrath, Chemorheology of Butadiene-Isoprene Block Copolymer Networks, Polymer (London), 23(10), (1982). 2 13. J. S. Riffle, E. Shchori, G. Freelin, T. C. Ward, and J. E. McGrath, Synthesis of Hydroxyl Terminated Polycarbonates of Controlled Molecular Weight, J. Polymer Sci. (Chemistry Edition), 20, (1982). 14. Y. Mohajer, I. C. Wang, G. L. Wilkes, and j. E. McGrath, Hydrogenated Linear Block Copolymers of Butadiene and Isoprene: Dynamic Mechanical Behavior, in Elastomers and Rubber Elasticity, J. Lal and J. E. Mark, Editors, Polymer Symposium Volume Series, p (1982) Yilgor, J. S. Riffle, G. L. Wilkes, and J. E. McGrath, Siloxane-Urea Segmented Copolymers. I. Syntheses and Characterization of Model Polymers for MDI and a,w Bis(Aminopropyl)Polydimethyl Siloxane , Polymer Bulletin, 8, , (1982). 16. D. Tyagi, I. Yilgor, G. L. Wilkes, and.j. E. McGrath, Siloxane- Urea Segmented Copolymers. II. Mechanical Behavior, Polymer Bulletin, 8, , (1982). 17. D.J.T. Hill, J. H. O'Donnell, P. W. O'Sullivan, J. E. McGrath, I. C. Wang and T. C. Ward Anionic Copolymerization of Butadiene and Isoprene: Applicability of the Terminal Model to High Conversion, Polymer Bulletin, 9(6/7), (1983). 18. J. E. McGrath, J. S. Riffle, 1. Yilgor, A. K. Banthia and G. L. Wilkes, An Overview of the Polymerization of Cyclosiloxanes, Initiation of Polymerization, ACS Symposium Series, No. 212, (1983). 19. R. E. Jerman and D. G. Baird, Rheological Properties of Copolyester Liquid Crystalline Melts. Part I. Capillary Rheometry, J. Rheol., 25:2, (1981). 20. D. G. Baird and G. L. Wilkes, Thermotropic Liquid Crystalline Copolyesters - Rheological Properties, ACS Preprints, 22:2, 357 (1981). 21. E. Joseph, G. L. Wilkes and D. G. Baird, Morphological Studies of Thermotropic Liquid Crystalline Polyesters Based on Polyethyleneterephthalate and Parahydroxy Benzoic Acid,* ACS Preprints, 22:2, 239 (1981). 22. D. G. Baird, Rheological Properties of Thermotropic Liquid Crystalline Copolyesters, Proceedings from the Second World Congress of Chemical Engineers, Vol. VI, Montreal Canada, October 4-9, D. G. Baird and G. L. Wilkes, Sandwich Injection Molding of Thermotropic Copolyesters and Filled Polyester, NATEC Papers, Society of Plastics Engineers, Bal Harbor, Florida, October L 1 I ' I I ... -, T -.. ',,... i,,..1.. 3 24. D. G. Baird and C. D. Nguyen, Mold Filling Studies on Thermotropic Liquid Crystalline Copolyesters, Soc. Plast. Engr. Tech. Papers, May D. G. Baird and G. L. Wilkes, Sandwich Injection Molding of Thermotropic Copolyesters and Filled Polyester, Polym. Engr. & Sci., 23:11 (1983). 26. D. G. Baird, A. Gotsis, G. Viola, Transient Shear Flow Behavior of Thermotropic Liquid Crystalline Copolyesters, ACS Preprints, Washington, D.C. Meeting, August A. Gotsis and 0. G. Baird, Rheological Properties of Copolyester Liquid Crystalline Melts. Part II. Comparison of Steady Shear and Dynamic Oscillatory Behavior, Submitted to Journal of Rheology. 28. G. Viola and 0. G. Baird, Comparison of the Predictions of Ericksen's Transversely Isotropic Fluid Theory with Transient Flow Properties of Thermotropic Liquid Crystalline Copolyesters, Submitted to the Journal of non-newtonian Fluid Mechanics. 29. D. G. Baird and G. L. Wilkes, Sandwich Injection Molding of Thermotropic Copolyesters and Filled Polyester , Polym. Engr. & Sci., 23:11 (1983). 30. Y. Mahajer, 0. Tyagi, G. L. Wilkes, R. F. Storey and J. P. Kennedy, New Polyisobutylene Based Model Ionomers, 3. Further Mechanical and Structural Studies , Polym. Bull., 8, 47 (1982). 31. S. Bagrodia, Y. Mahajer, G. L. Wilkes, R. F. Storey and J. P. Kennedy, New Polyisobutylene Based Model Ionomers, 4. Strain Induced Crystallization of Low Molecular Weight Model Ionomers , 32. Ibid, 8, 281 (1982). 33. S. Bagrodia, Y. Mohajer, G. L. Wilkes, R. F. Storey, and J. P. Kennedy, New Polyisobutylene Based Model Ionomers, 5. The Effect of Molecular Weight on the Mechanical Properties of Tri-arm-star Polyisobutylene Base Model Ionomers , Ibid, 9, 1974 (1983). 34. Y. Mohajer, S. Bagrodia, G. L. Wilkes, R. F. Storey, and J. P. Kennedy, New Polyisobutylene Based Model Elastomeric Ionomers, 6. The Effect of Excess Neutralizing Agents on Solid State Mechanical Properties , J. Appl. Polym. Sci., in press. 35. I. Yilgor, J. Eberle, B. C. Johnson, E. Yilgor, W. P. Steckle, Jr., D. Tyagi, 6. L. Wilkes and J. E. McGrath, Segmented Organo Siloxane Copolymers. I. Synthesis and Characterization of Siloxane Urea Copolymers, Submitted to Polymer. 36. D. Tyagi, I. Yilgor, J. E. McGrath, and G. L. Wilkes, Segmented Organo Siloxane Copolymers. II. Thermal and Mechanical Properties of Siloxane Urea Copolymers, Submitted to Polymer. 4 37. T. C. Ward, T. S. Lin, Compatibility Studies Using Solid State NMR in Advances in Chemistry Series 206, C. D. Han ed., pp , American Chemical Society. 38. T. C. Ward, Margaret Sheridan, and D. L. Kotzev, Nondestructive Evaluation of Some Bonded Joints in Mittal, K. L. (ed.), Adhesive Joints: Formation, Characteristics and Testing, Plenum Press (1984). 39. T. C. Ward, A. W. Brinkley, Margaret Sheridan, and Paul Koning, OBlock Copolymers Adhesive Studies a Chapter in Lee, L-H (ed.) Adhesive Chemistry: Developments and Trends, Plenum Press, (1984). 40. D. G. Baird, Concepts in Rheological Studies of Polymeric Liquid Crystals , Chapter 3 in Polymeric Liquid Crystals, Plenum Press, New York (1984). 41. A. D. Gotsis and D. G. Baird, Rheological Properties of Liquid Crystalline Melts, II. Comparison of Capillary and Rotary Rheometer Results , J. Rheol. Accepted for Publication. 42. A. D. Gotsis and D. G. Baird, Normal Stresses in Liquid Crystalline Copolyesters , Submitted to Rheol. Acta. (B) Preprints 1. S. Abouzahr, G. L. Wilkes, and J. E. McGrath, Chemo-Rheological Studies of Isoprene-Butadiene Copolymers , Polymer Preprints, 22(1), (1981). 2. T. C. Ward, D. P. Sheehy, J. E. McGrath, and J. S. Riffle, Inverse Gas Chromatography Studies of Polydimethylsiloxane (PDMS) Polycarbonate (PC) Copolymers and Blends, Polymer Preprints, 22(1), (1981). 3. M. K. Martin and J. E. McGrath, Effect of Thermal History on the End-Linking of Dienyllithium Anions with Divinylbenzene, Polymer Preprints, 22(l), (1981). 4. Y. Mohajer, G. L. Wilkes, I. C. Wang, and J. E. McGrath, Hydrogeneated Tri-Block Copolymers of Isoprene-Butadlene-Isoprene: Effects of Variation of Architecture and Composition on Properties, Polymer Preprints, 22(2), (1981) Yilgor, G. L. Wilkes and J. E. McGrath, Poly(urethanesiloxane) Copolymers. I. Reaction Kinetics of Model Systems, Polymer Preprints, 23(1), (1982). 6. J. E. McGrath, J. S. Riffle, I. Yilgor, A. K. Banthia and G. L. Wilkes, An Overview of the Polymerization of Cyclosiloxanes, Org. Coatings and Plastics Preprints, 46(1), (1982). 7. I. Yilgor, E. Yilgor, J. Eberle, W. Steckle, Jr., B. C. Johnson, D. Tyagi, G. L. Wilkes and J. E. McGrath, Novel Segmented Elastomers from Amino Alkyl Terminated Dimethylsiloxane Oligomers , Polymer Preprints, 24(1), (1983). Yilgor, J. Eberle, A. Shaaban, E. Vilgor, W. P. Steckle, Jr., D. Tyati, G. L. Wilkes and J. E. McGrath, Slloxane-Urea Segmented Copolymers Structural Variations in the Polysiloxane Oligomers , Polymer Preprints, 24(l), (1983). 9. D. C. Webster, P. J. Andolino, J. S. Riffle, F. L. Keohan and * J. E. McGrath, Synthesis and Characterization of Polyester- Polydimethylsiloxane Block Copolymers , Polymer Preprints, 24(l), (1983). 10. R. D. Allen, T. L. Huang, D. K. Mohanty, S. S. Huang, H. D. Qin, and J. E. McGrath, Ion-Containing Polymers. 11. Anionic Synthesis of Ion-Containing Block Copol ymers: Preparation and Hydrolysis , Polymer Preprints, 24(2), (1983). 11. P. K. Das, R. D. Allen, T. C. Ward, and J. E. McGrath, Chain Dimensions of Poly(Alkyl Methacrylates) by Variable Temperature Size Exclusion Chromattography , Polymer Preprints, 24(2), (1983). 12. D. P. Sheehy, T. C. Ward and J. E. McGrath, Applicability of the Scott Ternary Model for Interpreting the Free Energy of Mixing of Nitrocellulose Containing Blends and of Low Molecular Weight Liquids , Polymer Preprints, 24(2), (1983). 13. A. Sha'aban, S. McCartney, N. Patel, 1. Yilgor, J. S. Riffle, D. W. Dwight and J. E. McGrath, ESCA Studies on Polydimethylsiloxane-Urea Copolymers and their Blends with Segmented Polyether-Urethanes , Polymer Preprints, 24(2), (1983). 14. Y. Chujo and J. E. McGrath, Synthesis of a,w-difunctional Fluorine-Containing Polysiloxane Oligomers Via Hydrosilation Reaction , Polymer Preprints, 24(2), (1983) Yilgor,' E. Yllgor, B. Johnson, J. Eberle, G. 1. Wilkes and * J. E. McGrath, Segmented Polysiloxane-Polylmide Copolymersu, Polymer Preprints, 24(2), (1983) Yllgor, B. Lee, W. P. Steckle, Jr., J. S. Riffle, D. Tyagi, G. L. Wilkes and J. E. McGrath, Segmented Polysiloxane- Polyanide Copolymers , Polymer Preprints, 24(2), (1983). 17. I. Yllgor, K. A. Packard,, J. Eberle, E. Vilgor, R. D. Lundberg, and J. E. McGrath, Ion-Containing Polymers. I. Alkyl Acrylate- Sulfonated Styrene Copolymers by Emulsion Copolymerization%, Polymer Preprints, 24(2), (1983) Vilgor, 6. L. Wilkes and J. E. McGrath, Siloxane-Urea Segmented Copolymers IV. Synthesis of Cycloaliphatic Dilsocyanate (H-MDI) Based Copolymers , Polymer Preprints, 24(2), (1983). ~I6 19. I. C. Wang, R. j. Minton and J. E. McGrath Utilization of Antioxidants During the Chemical Hydrogenation of Polydienes wfth p-toluene Sulfonyl Hydrazide (TSH) , Polymer Preprints, 24(2), (1983) G. Baird and G. L. Wilkes, Thermotropic Liquid Crystalline Copolyesters - Rheological Properties , ACS Preprints, 22:2, 357 (1981). 21. Eugene Joseph, G. L. Wilkes, and 0. G. Baird, Morphological Studies of Thermotropic Liquid Crystalline Polyesters Based on Polyethylene Terephthalate and Parahydroxy Benzoic Acid , ACS Preprints, 22:2, 239 (1981). 22. D. 6. Baird and G. L. Wilkes, Sandwich Injection Molding of Thermotropic Copolyesters and Filled Polyester , NATEC Papers, Society of Plastics Engrs., Bal Habor, FL, October G. Baird and G. L. Wilkes, Sandwich Injection Molding of Thermotropic Copolyesters and Filled Polyester , Polym. Engr. & Sci., 23:11 (1983). 24. E. Joseph, G. L. Wilkes and D. G. Baird, Thermal Studies of Flexible and Semi-rigid Polymeric Blends , NATAS Preprints, - paper delivered in Williamsburg, VA, September 25/29, R. Pisipati, E. Joseph, D. G. Gaird and G. L. Wilkes, Thermal Studies of Flexible and Semi-rigid Polymeric Blends', NATAS Preprints, - paper delivered in Williamsburg, VA, September 24/29, D. Tyagi, I. Yilgor, E. Yilgor, G. L. Wilkes and J. E. McGrath, Thermal Analysis of Segmented Siloxane Copolymers , NATAS Preprints, paper delivered in Williamsburg, VA, September 24/29, S. Bagrodia, G. L. Wilkes, and J. Kennedy, Thermal Mechanical Analysis of Polyisobutylene Based Elastomeric Ionomers, , NATAS Preprints, paper delivered in Williamsburg, VA, September 24/29, J. P. Kennedy, R. F. Storey, Y. Mahajer, and G. L. Wilkes
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