Rheological and Spectroscopic Characterizations of the Properties of a Prepolymer for High-Temperature Applications: The IP960 System

Abstract

Of the thermostable polymers on the market the American PMR-15 resin is a reference compound. Nevertheless, its defects have necessitated the development of new polymers such as IP960. The object of this work is to characterize IP960 which is soluble in the diglyme until the imide oligomer stage. HPLC and ¹H NMR analyses of the prepolymer demonstrate its polymolecularity. Several isomer forms, due to possible conformations of the nadimide endcaps, are present in equal amounts in the medium. The combined use of differential scanning calorimetry and rheological techniques have allowed us to study and to explain the evolution of properties of the prepolymer with temperature (glass transition, crosslinking etc). Using FTIR spectroscopy, we have studied the structure of the polymer network. Our results seem to confirm the validity of the crosslinking diagram of nadic structures proposed by Wong and co-workers. Thermomechanical analysis of the crosslinked compound shows that the Tg of the polymer is close to 292 °C. It also reveals on the curb of the modulus G″, namely the presence of two peaks γ and β associated with secondary mechanical relaxations within macromolecular chains (Tγ = −102 °C; Tβ =68 °C).

Get full access to this article

View all access options for this article.

References

[1] Serafini T T , Delvigs P and Lightsey G R 1992 J. Appl. Polym. Sci. 16 905-905

[2] Serafini T T and Delvigs P 1973 Appl. Polym. Symp. no 22 89-89

[3] Stenzenberger H 1988 Br. Polym. J. 20 383-383

[4] Wilson D 1988 Br. Polym. J. 20 405-405

[5] Stevens T 1990 Mater. Eng. 107 (10) 34-34

[6] Sillion B 1988 GFP Collection 7 143–170

[7] Wong A C and Ritchey W M 1980 Spectrosc. Lett. 13 503-503

[8] Wong A C and Ritchey W M 1981 Macromolecules 14 825-825

[9] Wong A C , Garroway A N and Ritchey W M 1981 Macromolecules 14 832-832

10.

[10] Sukenik C N , Malhotra V and Varde U 1984 Polym. Preprints, Am. Chem. Spc. 25 104-104

11.

[11] Sukenik C N , Ritchey W M , Malhotra V and Varde U 1987 High Temperature Polymer Matrix Composites ed E Noyes pp 77-88

12.

[12] Vijayakumar C T and Lederer K 1989 STEP I/Polyimides vol 1 ed A Abadie (Amsterdam: Elsevier) A.6/1-A.6/10

13.

[13] Grenier-Loustalot M F and Grenier P 1991 High Perform. Polym. 3 263-263

14.

[14] Hilaire B and Verdu J 1990 Annales des Composites vol 1–2 ed M F Grenier-Loustalot pp 243–248

15.

[15] Gonzales D 1993 Thèse Université de PAU et des Pays de l’Adour

16.

[16] Trillaud M 1993 Thèse Université de PAU et des Pays de l’Adour

17.

[17] Jones J F , Lubowitz H R , Burns E A and Vaughan R W 1969 Sci. Adv. Mater. Process Eng. Proc. 15 59-59

18.

[18] Lauver R W 1979 J. Polym. Sci. Polym. Chem. Ed. 17 2529-2529

19.

[19] Scola D A and Stevens M P 1981 J. Appl. Polym. Sci. 26 231-231

20.

[20] Vijayakumar C T , Lederer K and Kramer A 1989 J. Polym. Sci. Polym. Chem. Ed. 27 2723-2723

21.

[21] Hay J N , Boyle J D , Parker S F and Wilson D 1989 Polymer 30 1032-1032

22.

[22] Preston P N , Soutar I , Woodfine B and Hay J N 1989 High. Perform. Polym. 1 161-161

23.

[23] Roberts G D and Lauver R W 1987 J. Appl. Polym. Sci. 33 2893-2893

24.

[24] Grenier-Loustalot M F and Grenier P 1991 High Perform. Polym. 3 113-113

25.

[25] Grenier-Loustalot M F , Billon L and Grenier P 1996 Int. Polym. J. at press