Influence of temperature on the properties of polycarbosilane

被引:21
作者
Cheng, XZ [1 ]
Xie, ZF [1 ]
Xiao, JY [1 ]
Song, YC [1 ]
机构
[1] Natl Def Univ, Coll Aerosp & Mat Engn, State Key Lab Novel Ceram Fibers & Ceram Matrix C, Changsha 410073, Hunan, Peoples R China
关键词
liquid polysilane; polycarbosilane; SiC fibers;
D O I
10.1007/s10904-004-5542-9
中图分类号
O63 [高分子化学(高聚物)];
学科分类号
070305 ; 080501 ; 081704 ;
摘要
A polycarbosilane precursor of SiC fiber was synthesized at high temperature under high pressure from liquid polysilane (LPS), which was obtained by thermal decomposition of poly(dimethylsilane). The effect of reaction temperature on the Si-H bond content, degree of linearity, Si-Si bond content, molecular weight, molecular weight distribution, elemental composition, softening point, and yield of the polycarbosilane (PCS) was studied spectroscopically ( FTIR, UV, H-1-NMR, and Si-29-NMR) and by gel permeation chromatography (GPC). The results showed that the molecular weight, yield and softening point of the PCS increased, the molecular weight distribution broadened, and the Si-Si bond content and degree of linearity decreased when the reaction temperature increased. The Si-H bond content increased when the thermolysis reaction temperature was less than 450 degrees C and decreased when the temperature was over 460 degrees C. Increasing of the reaction temperature affected the composition with a general decrease in the amount of carbon, hydrogen and oxygen in the product. A middle molecular weight region of PCS in the GPC appears when the reaction temperature approaches 450 degrees C; and, the as-synthesized PCS was stable with low Si - Si bond content. Synthetically, the conversion process is initially the formation of PCS by thermal decomposition of LPS, which is followed by an increase in molecular weight via condensation of PCS molecules.
引用
收藏
页码:253 / 259
页数:7
相关论文
共 11 条
[1]   COMPREHENSIVE CHEMISTRY OF POLYCARBOSILANES, POLYSILAZANES, AND POLYCARBOSILAZANES AS PRECURSORS OF CERAMICS [J].
BIROT, M ;
PILLOT, JP ;
DUNOGUES, J .
CHEMICAL REVIEWS, 1995, 95 (05) :1443-1477
[2]  
FAN XL, 1999, THESIS NAT U DEFENSE
[3]  
FENG C, 2002, THESIS NATL U DEFENS
[4]   SYNTHESIS OF CONTINUOUS SILICON-CARBIDE FIBER .4. THE STRUCTURE OF POLYCARBOSILANE AS THE PRECURSOR [J].
HASEGAWA, Y ;
OKAMURA, K .
JOURNAL OF MATERIALS SCIENCE, 1986, 21 (01) :321-328
[5]   PRECERAMIC POLYMER ROUTES TO SILICON-CARBIDE [J].
LAINE, RM ;
BABONNEAU, F .
CHEMISTRY OF MATERIALS, 1993, 5 (03) :260-279
[6]   Conversion of polycarbosilane (PCS) to SiC-based ceramic - Part 1. Characterisation of PCS and curing products [J].
Ly, HQ ;
Taylor, R ;
Day, RJ ;
Heatley, F .
JOURNAL OF MATERIALS SCIENCE, 2001, 36 (16) :4037-4043
[7]  
SCHILLING CL, 1983, AM CERAM SOC BULL, V62, P912
[8]  
YAHIMA S, 1978, J MATER SCI, V13, P2569
[9]  
YONGCAI S, 1997, POLYM MAT SCI ENG, V13, P30
[10]  
YONGCAI S, 1995, ACTA POLYMERICA SIN, V12, P753