Skip to main content
Log in

Synthesis, Morphology, and Viscoelastic Properties of Polyhedral Oligomeric Silsesquioxane Nanocomposites with Epoxy and Cyanate Ester Matrices

  • Published:
Journal of Inorganic and Organometallic Polymers and Materials Aims and scope Submit manuscript

Octaaminophenyl(T8)POSS [1, (C6H4NH2)8(SiO1.5)8] and dodecaaminophenyl(T12)POSS [2, (C6H4NH2)12(SiO1.5)12] were synthesized, characterized and then incorporated into two types of thermoset resins: (1) the bisphenol-F-based cyanate ester resin, PT-15, and (2) epoxy (Epon 828, Shell Chemical Corp.)/4,4′-diaminodiphenylmethane (DDM) resin, respectively, to make two series of nanocomposites. The sum of amino groups in both DDM and POSS were held in a 1:1 mole ratio to the epoxy groups. EPON-828/1/DDM and EPON-828/2/DDM composites (78.63/0/21.37, 77.48/5/17.52, 76.34/10/13.66, 74.05/20/5.95 and 72.28/27.72/0 wt/wt/wt compositions for both series) were prepared. PT-15/1 and PT-15/2 composites (99/1, 97/3 and 95/5 wt/wt compositions for both types) were also prepared. These nanocomposites were characterized by transmission electron microscopy (TEM), dynamic mechanical analysis (DMA), solvent extraction and FT-IR. In all systems, POSS 1 and 2 were chemically bound into the resin matrix and phase-separated POSS particle domains were not observed. Incorporation of both 1 and 2 can dramatically elevate the high temperature bending storage moduli, E′, of epoxy resins.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Scheme 1
Scheme 2
Scheme 3
Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6
Fig. 7
Fig. 8

Similar content being viewed by others

References

  1. Giannelis E. P. (1996). Adv. Mater. 8: 29

    Article  CAS  Google Scholar 

  2. Jog J. P., Hambir S., Bulakh N. (2002). Polym. Eng. Sci. 42: 1800

    Article  Google Scholar 

  3. Kim D. S., Lee K. M. (2003). J. Appl. Polym. Sci. 90: 2629

    Article  CAS  Google Scholar 

  4. Liu Z. J., Chen K. Q., Yan D. Y. (2003). Eur. Polym. J. 39: 2359

    Article  CAS  Google Scholar 

  5. Priya L., Jog J. P. (2002). J. Polym. Sci. Part B: Polym. Phys. 40: 1682

    Article  CAS  Google Scholar 

  6. Wang Y. Z., Zhang L. Q., Tang C. H., Yu D. S. (2000). J. Appl. Polym. Sci. 78: 1879

    Article  CAS  Google Scholar 

  7. Bureau M. N., Denault J., Cole K. C., Enright G. D. (2002). Polym. Eng. Sci. 42: 1897

    Article  CAS  Google Scholar 

  8. Wan C. Y., Qiao X. Y., Zhang Y., Zhang X. Y. (2003). Polym. Test. 22: 453

    Article  CAS  Google Scholar 

  9. Wu S. H., Wang F. Y., Ma C. C. M., Chang W. C., Kuo C. T., Kuan H. C., Chen W. J. (2001). Mater. Lett. 49: 327

    Article  CAS  Google Scholar 

  10. Burnside S. D., Giannelis E. P. (1995). Chem. Mater. 7: 1597

    Article  CAS  Google Scholar 

  11. Agag T., Koga T., Takeichi T. (2001). Polymer 42: 3399

    Article  CAS  Google Scholar 

  12. Kodgire P., Kalgaonkar R., Hambir S., Bulakh N., Jog J. P. (2001). J. Appl. Polym. Sci. 81: 1786

    Article  CAS  Google Scholar 

  13. Chen Z., Gong K. (2002). J. Appl. Polym. Sci. 84: 1499

    Article  CAS  Google Scholar 

  14. Gilman J. W. (1999). Appl. Clay. Sci. 15: 31

    Article  CAS  Google Scholar 

  15. Lepoittevin B., Devalckenaere M., Pantoustier N., Alexandre M., Kubies D., Calberg C., Jerome R., Dubois P. (2002). Polymer 43: 4017

    Article  CAS  Google Scholar 

  16. Gu A.J., Liang G.Z. (2003). Polym. Degrad. Stab. 80: 383

    Article  CAS  Google Scholar 

  17. Bourbigot S., Devaux E., Flambard X. (2002). Polym. Degrad. Stab. 75: 397

    Article  CAS  Google Scholar 

  18. Gilman J. W., Kashiwagi T., Lichtenhan J. D. (1997). SAMPE J 33: 40

    CAS  Google Scholar 

  19. Romo-Uribe A., Mather P. T., Haddad T. S., Lichtenhan J. D. (1998). J. Polym. Sci. Part B: Polym. Phys. 36: 1857

    Article  CAS  Google Scholar 

  20. Mather P. T., Jeon H. G., Romo-Uribe A., Haddad T. S., Lichtenhan J. D. (1999). Macromolecules 32: 1194

    Article  CAS  Google Scholar 

  21. Lee A., Lichtenhan J. D. (1999). J. Appl. Polym. Sci. 73: 1993

    Article  CAS  Google Scholar 

  22. Jeon H. G., Mather P. T., Haddad T. S. (2000). Polym. Int. 49: 453

    Article  CAS  Google Scholar 

  23. Fu B. X., Hsiao B. S., Pagola S., Stephens P., White H., Rafailovich M., Sokolov J., Mather P. T., Jeon H. G., Phillips S., Lichtenhan J. D., Schwab J. (2001). Polymer 42: 599

    Article  CAS  Google Scholar 

  24. Gonzalez R. I., Phillips S. H., Hoflund G. B. (2000). J. Spacecraft Rockets 37: 463

    Article  CAS  Google Scholar 

  25. Lichtenhan J. D., Otonari Y. A., Carr M. J. (1995). Macromolecules 28: 8435

    Article  CAS  Google Scholar 

  26. Haddad T. S., Lichtenhan J. D. (1996). Macromolecules 29: 7302

    Article  CAS  Google Scholar 

  27. Simon S. L., Gillham J. K. (1993). J. Appl. Polym. Sci. 47: 461

    Article  CAS  Google Scholar 

  28. Yeh J. M., Chin C. P. (2003). J. Appl. Polym. Sci. 88: 1072

    Article  CAS  Google Scholar 

  29. Wang Z., Pinnavaia T. J. (1998). Chem. Mater. 10: 1820

    Article  CAS  Google Scholar 

  30. Alexandre M., Dubois P. (2000). Mater. Sci. Eng. Rep. 28: 1

    Article  Google Scholar 

  31. Gangun S., Dean D. (2003). Polymer 44: 1315

    Article  Google Scholar 

  32. Ganquli S., Dean D., Vaia R. (2002). Polym. Mater. Sci. Eng. 87: 94

    CAS  Google Scholar 

  33. Dufresne A., Paillet M., Putaux J. L., Canet R., Carmona F., Delhaes P. (2002). J. Mater. Sci. 37: 3915

    Article  CAS  Google Scholar 

  34. Penumadu D., Dutta A., Pharr G. M., Files B. (2003). J. Mater. Res. 18: 1849

    Article  CAS  Google Scholar 

  35. Thostenson E. T., Chou T. W. (2002). J. Phys. D: Appl. Phys. 35: L77

    Article  CAS  Google Scholar 

  36. Bai J. B., Allaoui A. (2003). Compos. A 34: 689

    Article  CAS  Google Scholar 

  37. Kuriger R. J., Alam M. K., Anderson D. P., Jacobsen R. L. (2002). Compos. A 33: 53

    Article  Google Scholar 

  38. Shofner M. L., Rodriguez-Macias F. J., Vaidyanathan R., Barrera E. V. (2003). Compos. A 34: 1207

    Article  CAS  Google Scholar 

  39. Kuriger R. J., Alam M. K. (2001). Polym. Compos. 22: 604

    Article  CAS  Google Scholar 

  40. Gordeyev S. A., Ferreira J. A., Bernardo C. A., Ward I. M. (2001). Mater. Lett. 51: 32

    Article  CAS  Google Scholar 

  41. Lakshminarayanan P. V., Toghiani H., Pittman C. U. Jr. (2004). Carbon 42: 2433

    Article  CAS  Google Scholar 

  42. Patton R. D., Pittman C. U. Jr., Wang L. (1997). Int. SAMPE Technol. Conf. 29: 77

    CAS  Google Scholar 

  43. Patton R. D., Pittman C. U. Jr., Wang L., Hill J. R., Day A. (2001). Compos. A 33: 243

    Article  Google Scholar 

  44. Yamamoto K., Otsuka H., Takahara A., Wada S. I. (2002). J. Adhes. 78: 591

    Article  CAS  Google Scholar 

  45. Xu H. Y., Kong H., Yang Z. B. (2003). Chin. J. Mater. Res. 17: 127

    CAS  Google Scholar 

  46. Lee A., Lichtenhan J. D. (1998). Macromolecules 31: 4970

    Article  PubMed  CAS  Google Scholar 

  47. Lichtenhan J. D., Schwab J. J. (2000). Int. SAMPE Technol. Conf. 32: 185

    CAS  Google Scholar 

  48. Mather P. T., Jeon H. G., Haddad T. S. (2000). Polym. Prepr. 41: 528

    CAS  Google Scholar 

  49. Haddad T. S., Choe E., Lichtenhan J. D. (1996). Mater. Res. Soc. Symp. Proc. 435: 25

    CAS  Google Scholar 

  50. Haddad T. S., Stapleton R., Jeon H. G., Mather P. T., Lichtenhan J. D., Phillips S. H. (1999). Polym. Prepr. 40: 496

    CAS  Google Scholar 

  51. S. H. Phillips, R. L. Blanski, S. A. Svejda, T. S. Haddad, A. Lee, J. D. Lichtenhan, F. J. Feher, P. T. Mather, and B. S. Hsiao, Mater. Res. Soc. Symp. Proc. 628, CC4.6.1 (2000)

  52. Blanski R. L., Phillips S. H., Chaffee K., Lichtenhan J. D., Lee A., Geng H. P. (2000). Polym. Prepr. 41: 585

    CAS  Google Scholar 

  53. Haddad T. S., Lee A., Mather P. T., Phillips S. H. (2000). Polym. Prepr. 41: 584

    CAS  Google Scholar 

  54. Lu S., Martin G. C. (2003). Conf. Proc./Annu. Tech. Conf. 2: 1893

    Google Scholar 

  55. Constable G. S., Coughlin E. B., Lesser A. J. (2003). Conf. Proc./Annu. Tech. Conf. 2: 1663

    Google Scholar 

  56. Li G., Wang L., Toghiani H., Pittman Jr. C. U., Daulton T. L., Koyama K. (2001). Macromolecules 34: 8686

    Article  CAS  Google Scholar 

  57. Li G., Wang L., Toghiani H., Daulton T. L., Pittman Jr. C. U. (2002). Polymer 43: 4167

    Article  CAS  Google Scholar 

  58. Gupta S. K., Schwab J. J., Lee A., Fu B., Hsiao B. S. (2002). Int. SAMPE Symp. Exhib. 47: 1517

    CAS  Google Scholar 

  59. Feher F. J., Lucke S., Schwab J. J., Lichtenhan J. D., Phillips S. H., Lee A. (2000). Polym. Prepr. 41: 526

    CAS  Google Scholar 

  60. Haddad T. S., Mather P. T., Jeon H. G., Romo-Uribe A., Farris A. R., Lichtenhan J. D. (1998). Mater. Res. Soc. Symp. Proc. 519: 381

    CAS  Google Scholar 

  61. Mantz R. A., Jones P. F., Chaffee K. P., Lichtenhan J. D., Ismail M. K., Burmeister M. (1996). Chem. Mater. 8: 1250

    Article  CAS  Google Scholar 

  62. Xu H.Y., Kuo S.W., Lee J.Y., Chang F.C. (2000). Polymer 43: 5117

    Article  Google Scholar 

  63. Pellice S. A., Fasce D. P., Williams R. J. J. (2003). J. Polym. Sci. Part B: Polym. Phys. 41: 1451

    Article  CAS  Google Scholar 

  64. Lee A. (1999). Mater. Res. Soc. Symp. Proc. 576: 343

    CAS  Google Scholar 

  65. Philips S. H., Gonzalez R. I., Chaffee K. P., Haddad T. S., Hoflund G. B., Hsiao B. S., Fu B. X. (2000). SAMPE 45: 1921

    Google Scholar 

  66. Huang J. C., He C. B., Xiao Y., Mya K. Y., Dai J., Siow Y. P. (2003). Polymer 44: 4491

    Article  CAS  Google Scholar 

  67. Fu B. X., Namani M., Lee A. (2003). Polymer 44: 7739

    Article  CAS  Google Scholar 

  68. Lichtenhan J.D., Otonari Y.A., Carr M.J. (1995). Macromolecules 28: 8435

    Article  CAS  Google Scholar 

  69. Haddad T. S., Lichtenhan J. D. (1996). Macromolecules 29: 7302

    Article  CAS  Google Scholar 

  70. Bharadwaj R. K., Berry R. J., Farmer B. L. (2000). Polymer 41: 7209

    Article  CAS  Google Scholar 

  71. Tsuchida A., Bolln C., Sernetz F. G., Frey H., Mulhaupt R. (1997). Macromolecules 30: 2818

    Article  CAS  Google Scholar 

  72. Lee A., Lichtenhan J. D. (1998). Macromolecules 31: 4970

    Article  PubMed  CAS  Google Scholar 

  73. Pan G., Mark J. E., Schaefer D. W. (2003). J. Appl. Polym. Sci. B 41: 3314

    Article  CAS  Google Scholar 

  74. Choi J., Kim S. G., Laine R. M. (2004). Macromolecules 37: 99

    Article  CAS  Google Scholar 

  75. Liang K., Toghiani H., Pittman C. U. Jr. (2005). J. Polym. Sci. Part A 43: 3887

    Article  CAS  Google Scholar 

  76. Tamaki R., Tanaka Y., Asuncion M. Z., Choi J., Laine R. M. (2001). J. Am. Chem. Soc. 123: 12416

    Article  PubMed  CAS  Google Scholar 

  77. H. S. Cho, Mississippi State University, MS. Ph.D. dissertation research (following a modification of the procedure of R. Tamaki, Y. Tanaka, M. Z. Asuncion, J. Choi, R. M. Laine, JACS 2001, 123, 12416).

  78. Grigat E., Putter R. (1967). Angew. Chem. Int. Ed. 6: 206

    Article  CAS  Google Scholar 

  79. Shimp D. A., Christenson J. R., Ising S. J. (1991) AroCy Cyanate Ester Resins: Chemistry, Properties and Applications. Rhone-Poulenc, Louisville, KY,

    Google Scholar 

  80. Bauer J., Bauer M. (2001). Macromol. Chem. Phys. 202: 2213

    Article  CAS  Google Scholar 

  81. K. Liang, Mississippi State University, MS. Ph.D. dissertation research

  82. K. Liang, H. Toghiani, and C.U. Pittman, Jr., Macromolecules, submitted for publication.

Download references

Acknowledgments

We thank Dr. Andre Lee, Michigan State University for assistance in performing a portion of the DMA studies and helpful discussions. This work was supported by the Air Force Office of Scientific Research (grant no. F49620-02-1-026-0) and the National Science Foundation (grant no. EPS0132618).

Author information

Authors and Affiliations

Authors

Corresponding author

Correspondence to Charles U. Pittman Jr..

Rights and permissions

Reprints and permissions

About this article

Cite this article

Cho, H., Liang, K., Chatterjee, S. et al. Synthesis, Morphology, and Viscoelastic Properties of Polyhedral Oligomeric Silsesquioxane Nanocomposites with Epoxy and Cyanate Ester Matrices. J Inorg Organomet Polym 15, 541–553 (2005). https://doi.org/10.1007/s10904-006-9008-0

Download citation

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s10904-006-9008-0

Keywords

Navigation