COMPATIBILITY OF TPD POLYCARBONATE BLENDS BY C-13-H-1 HETCOR IN THE SOLID-STATE

被引:20
作者
KAPLAN, S
机构
[1] Xerox Webster Research Center, Webster, New York 14580
关键词
D O I
10.1021/ma00057a028
中图分类号
O63 [高分子化学(高聚物)];
学科分类号
070305 ; 080501 ; 081704 ;
摘要
Two-dimensional heteronuclear C-13-H-1 NMR measurements in the solid state have been used to investigate the compatibility of a solvent cast blend of an aromatic diamine, N,N'-diphenyl-N,N'-bis(3-methylphenyl)-1,1'-biphenyl-4,4'-diamine (TPD) in Bisphenol A polycarbonate. Measurements of carbon-proton correlations as a function of proton spin diffusion time, inserted between the proton evolution and cross-polarization periods, are interpreted in terms of an initial fast response from both inter- and intramolecular dipolar couplings and a slower response only from intermolecular couplings. The 2-D technique is capable of observing spin diffusion between domains even though there are no resolved peaks from the individual components in the H-1 dimension. Distinction between domains is based upon the differences in aliphatic and aromatic proton populations of the individual components or on differences in proton projection line shapes for unique carbon resonances from each component. From these results it is shown that, although there is a distribution of separations of the small molecule amine from the polymer binder, inter- and intramolecular spin diffusion occur at similar rates, indicative of intimate mixing at the molecular level.
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页码:1060 / 1064
页数:5
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共 32 条
[1]   NUCLEAR-SPIN DIFFUSION BETWEEN POLYURETHANE MICROPHASES [J].
ASSINK, RA .
MACROMOLECULES, 1978, 11 (06) :1233-1237
[2]   SOLID-STATE NMR DETECTION OF MOLECULAR MIXING IN BIEUTECTIC BLENDS, D-METAL COMPLEXES, AND PHASE-SEPARATED COPOLYMERS [J].
BELFIORE, LA ;
GRAHAM, H ;
VEDA, E ;
WANG, YH .
POLYMER INTERNATIONAL, 1992, 28 (01) :81-94
[3]   SOLID-STATE 2-DIMENSIONAL C-13-H-1 CORRELATION (HETCOR) NMR-SPECTRUM OF AMORPHOUS POLY(2,6-DIMETHYL-PARA-PHENYLENE OXIDE) (PPO) [J].
BIELECKI, A ;
BURUM, DP ;
RICE, DM ;
KARASZ, FE .
MACROMOLECULES, 1991, 24 (17) :4820-4822
[4]   LOW-POWER MULTIPULSE LINE NARROWING IN SOLID-STATE NMR [J].
BURUM, DP ;
LINDER, M ;
ERNST, RR .
JOURNAL OF MAGNETIC RESONANCE, 1981, 44 (01) :173-188
[5]   AN IMPROVED EXPERIMENT FOR HETERONUCLEAR-CORRELATION 2D-NMR IN SOLIDS [J].
BURUM, DP ;
BIELECKI, A .
JOURNAL OF MAGNETIC RESONANCE, 1991, 94 (03) :645-652
[6]   OPTIMIZATION OF CHEMICAL-SHIFT-BASED POLARIZATION GRADIENTS IN H-1-NMR SPIN-DIFFUSION EXPERIMENTS ON POLYMER BLENDS WITH CHEMICALLY SIMILAR CONSTITUENTS [J].
CAMPBELL, GC ;
VANDERHART, DL .
JOURNAL OF MAGNETIC RESONANCE, 1992, 96 (01) :69-93
[7]   CHARACTERIZATION OF POLYMER BLENDS BY SELECTIVE PROTON SPIN-DIFFUSION NUCLEAR-MAGNETIC-RESONANCE MEASUREMENTS [J].
CARAVATTI, P ;
NEUENSCHWANDER, P ;
ERNST, RR .
MACROMOLECULES, 1986, 19 (07) :1889-1895
[8]   CHARACTERIZATION OF HETEROGENEOUS POLYMER BLENDS BY 2-DIMENSIONAL PROTON SPIN DIFFUSION SPECTROSCOPY [J].
CARAVATTI, P ;
NEUENSCHWANDER, P ;
ERNST, RR .
MACROMOLECULES, 1985, 18 (01) :119-122
[9]   HETERONUCLEAR SOLID-STATE CORRELATION SPECTROSCOPY [J].
CARAVATTI, P ;
BODENHAUSEN, G ;
ERNST, RR .
CHEMICAL PHYSICS LETTERS, 1982, 89 (05) :363-367
[10]   HETERONUCLEAR CORRELATION SPECTROSCOPY IN ROTATING SOLIDS [J].
CARAVATTI, P ;
BRAUNSCHWEILER, L ;
ERNST, RR .
CHEMICAL PHYSICS LETTERS, 1983, 100 (04) :305-310