以三氯化硼和六甲基二硅氮烷为原料制备了聚硼氮烷预聚体,再经高分子化制备了可溶的氮化硼陶瓷前驱体—聚硼氮烷.该法合成工艺简单,反应温和.采用凝胶渗透色谱、核磁共振氢谱、傅里叶红外光谱、热失重分析仪、元素分析等对预聚体高分子化过程中的分子量变化、高分子化机理、聚硼氮烷的裂解过程、所得陶瓷的元素组成进行了研究.结果表明,高分子化过程中主要发生了六甲基二硅氮烷脱除和转氨基反应.所得聚硼氮烷重均分子量为7 582,氮气下1 000℃时的陶瓷产率为41.6 wt％,陶瓷化转变主要发生在400～600℃,800℃时陶瓷化转变基本进行完毕,800℃氨气下裂解得到低C含量的白色氮化硼陶瓷,进一步在1 500℃氩气中裂解可得到结晶度较高的氮化硼陶瓷.
参考文献
| [1] | Miele P;Bernard S;Cornu D.Recent developments in polymer-derived ceramic fibers (PDCFs):Preparation,properties and applications-A review[J].SOFT MATERIALS,2006(2-4):249. |
| [2] | Paciorek K J L;Harris D H;Kratzer R H .Boron nitride polymers Ⅰ mechanistic studies of borazine pyrolysis[J].Polymer Science,1986,24(01):173. |
| [3] | Fazen P J;Beck j S;Lynch A T et al.Thermally induced borazine dehydropolymerization reactions.Synthesis and ceramic conversion reactions of a new high-yield polymeric precursor to boron nitride[J].Chemistry of Materials,1990,2(02):96. |
| [4] | Fazen P J;Remsen E E;Beck J S et al.Synthesis,Properties,and ceramic conversion reactions of polyborazylene:a high-yield polymeric precursor to boron nitride[J].Chemistry of Materials,1995,7(10):1942. |
| [5] | Thomas Wideman;Larry G. Sneddon .Dipentylamine-Modified Polyborazylene: A New, Melt-Spinnable Polymeric Precursor to Boron Nitride Ceramic Fibers[J].Chemistry of Materials,1996(1):3-5. |
| [6] | Narula C K;Lindquist D A;Fan M M et al.Models and polyborazine precursors for boron nitride ceramics[J].Chemistry of Materials,1990,2(04):377. |
| [7] | Narula C K;Schaeffer R;Datye A K et al.Synthesis of boron nitride ceramics from oligomeric precursors derived from 2-(dimethylamino)-4,6-dichloroborazine[J].Chemistry of Materials,1990,2(04):384. |
| [8] | Lindquist D A;Janik J F;Datye A K et al.Boron nitride fibers processed from poly (borazinylamine) solutions[J].Chemistry of Materials,1992,4(01):17. |
| [9] | Berangere Toury;Philippe Miele;David Cornu;Henri Vincent;Jean Bouix .Boron Nitride Fibers Prepared from Symmetric and Asymmetric Alkylaminoborazines[J].Advanced functional materials,2002(3):228-234. |
| [10] | Bernard S.;Cornu D.;Miele P.;Vincent H.;Bouix J. .Pyrolysis of poly[2,4,6-tri(methylamino)borazine] and its conversion into BN fibers[J].Journal of Organometallic Chemistry,2002(1/2):91-97. |
| [11] | Duriez C.;Framery E.;Toury B.;Toutois P.;Miele P.;Vaultier M. Bonnetot B. .Boron nitride thin fibres obtained from a new copolymer borazine-tri(methylamino)borazine precursor[J].Journal of Organometallic Chemistry,2002(1/2):107-114. |
| [12] | Miele P;Toury B;Cornu D;Bernard S .Borylborazines as new precursors for boron nitride fibres[J].Journal of Organometallic Chemistry,2005(11):2809-2814. |
| [13] | D. Cornu;S. Bernard;S. Duperrier .Alkylaminoborazine-based precursors for the preparation of boron nitride fibers by the polymer-derived ceramics (PDCs) route[J].Journal of the European Ceramic Society,2005(2/3):111-121. |
| [14] | 邓橙,宋永才,王应德,李义和,雷永鹏,曹淑伟.甲胺/二甲胺共取代合成氮化硼先驱体聚硼氮烷[J].化学学报,2010(12):1217-1222. |
| [15] | 曹义苗,李书同,韩克清,赵曦,余木火.氮化硼纤维先驱体聚合物的合成及其表征[J].合成纤维,2009(01):32-35,40. |
| [16] | 沈春英,丘泰,荣华,李志顺,李晓云.BN纤维先驱体的合成[J].硅酸盐学报,2004(09):1068-1072. |
| [17] | Wideman T.;Cortez E.;Chlanda VL.;Sneddon LG.;Remsen EE. .Amine-modified polyborazylenes: Second-generation precursors to boron nitride[J].Chemistry of Materials,1998(1):412-421. |
| [18] | Paine R T;Sneddon Larry G .In Inorganic and organometallic polymers Ⅱ[J].American Chemistry Society,1994,572:358. |
| [19] | Kimura Y;Kubo Y;Hayashi N .High-performance boron-nitride fibers from poly (borazine) precermics[J].Composites Science and Technology,1994,51(02):173. |
| [20] | Brown C A;Laubengayer A W .B-Trichloroborazole1[J].Journal of the American Chemical Society,1955,77(14):3699. |
| [21] | 向阳春,陈朝辉,曾竟成,刘秀英,张光友.聚硼氮烷先驱体制备氮化硼陶瓷纤维的研究[J].高技术通讯,1998(02):38-41. |
| [22] | 曾竟成,陈朝辉,向阳春,张光友,何迎春.氮化硼纤维先驱体的合成及其热解研究[J].高分子材料科学与工程,1999(06):53-55. |
| [23] | 唐云,王军,李效东,李文华,王浩,谢征芳.新型SiBNC陶瓷先驱体--聚硼硅氮烷的合成与表征[J].化学学报,2008(11):1371-1376. |
| [24] | Paine R T;Narula C K .Synthetic Routes to Boron Nitride[J].Chemical Reviews,1990,90:73. |
上一张
下一张
上一张
下一张
计量
- 下载量()
- 访问量()
文章评分
- 您的评分：
-
10%
-
20%
-
30%
-
40%
-
50%