| 549 | 10 | 70 |
| 下载次数 | 被引频次 | 阅读次数 |
通过二甲基胺硼烷(dimethylamine borane,DMAB)与低分子量聚碳硅烷(low-molecular mass polycarbosilane,LPCS)反应合成硼溶胶,将硼溶胶与高分子量聚碳硅烷(high-molecular mass polycarbosilane,HPCS)共混制备含硼聚碳硅烷先驱体,经熔融纺丝、氧化交联、热解以及1 800℃烧结制备含硼碳化硅纤维(SiC-B),研究了硼溶胶的形成过程以及SiC-B纤维的组成与性能,结果表明:由于Si—H键和B—H键的相互作用,LPCS与DMAB发生反应,实现LPCS的化学交联,从而形成高分散、高稳定的硼溶胶;硼的引入有效抑制了高温烧结过程中SiC晶粒长大,显著提高了纤维的致密度和力学性能;经1 800℃烧结后,SiC-B纤维表面光滑、断面致密,纤维平均拉伸强度为0.8 GPa。X射线衍射结果显示:SiC-B纤维的主要晶相为β-SiC和少量α-SiC,β-SiC的平均晶粒尺寸约为17.8 nm。
Abstract：Dimethylamine borane(DMAB) was reacted with low-molecular mass polycarbosilane(LPCS) to form a boron-containing colloid.The colloid was then added into a high-molecular mass polycarbosilane(HPCS) to form a boron-containing polycarbosilane precursor.The precursor was melt-spun,oxidation cured,pyrolyzed and sintered at 1 800 ℃ to obtain boron-containing silicon carbide(SiC-B) fibers.Formation of the colloid as well as the composition and performance of SiC-B fibers were studied.Results show that the interaction between Si—H bond and B—H bond is responsible for the reaction of DMAB and LPCS,resulting in the chemical cross-linking of LPCS,and hence forming well-dispersed and highly-stable boron-containing colloids.Introduction of boron could effectively inhibit a rapid growth of SiC grains during sintering,improving fiber density and tensile strength.Surface of SiC-B fibers sintered at 1 800 ℃ is smooth and fracture surface is dense.Average tensile strength of SiC-B fibers is 0.8 GPa.Results by X-ray diffrac-tion indicate that SiC-B fibers consist of mainly β-SiC crystals and a small amount of α-SiC.The average grain size of β-SiC is 17.8 nm.
[1]YAJIMA S.Development of ceramics,especially silicon carbide fibres,from organosilicon polymers by heat treatment[J].Philos Trans R SocLondon,Ser A:Math Phys Sci,1980,294:419–426.
[2]LAINE R M,BABONNEAU F.Preceramic polymer routes to siliconcarbide[J].Chem Mater,1993,5:260–279.
[3]李文华,王军,王浩,等.先驱体转化法含硼连续SiC纤维研究进展[J].宇航材料工艺,2007,4:5–7.LI Wenhua,WANG Jun,WANG Hao,et al.Aerosp Mater Technol(inChinese),2007,4:5–7.
[4]余煜玺,李效东,曹峰,等.先驱体法制备含异质元素SiC陶瓷纤维的现状与进展[J].硅酸盐学报,2003,31(4):371–374.YU Yuxi,LI Xiaodong,CAO Feng,et al.J Chin Ceram Soc(in Chi-nese),2003,31(4):371–374.
[5]崔之开.陶瓷纤维[M].北京:化学工业出版社,2004:18–21.CUI Zhikai.Ceramic Fibers(in Chinese).Beijing:Chemical IndustryPress,2004:18–21.
[6]王曙中,王庆端,刘兆峰.高科技纤维概论[M].上海:中国纺织大学出版社,1999:434–436.WANG Shuzhong,WANG Qingduan,LIU Zhaofeng.An Introductionof High Performance Fibers(in Chinese).Shanghai:China TextileUniversity Press,1999:434–436.
[7]YAJIMA S,HAYASHI J,OMORI M,et al.Development of a siliconcarbide fiber with high tensile strength[J].Nature,1976,261:683–685.
[8]YAJIMA S,HAYASHI J,OMORI M.Continuous silicon carbide fiberof high tensile strength[J].Chem Lett,1975,9:931–934.
[9]MAH T,HECHT N L,CULLUM D E,et al.Thermal stability of SiCfibres(Nicalon)[J].J Mater Sci,1984,19(4):1191–1201.
[10]BUNSELL A R,PIANT A.A review of the development of threegenerations of small diameter silicon carbide fibres[J].J Mater Sci,2006,41(3):823–839.
[11]VAHALAS C,MONTHIOUX M.On the thermal degradation of Lox-MTyranno fibres[J].J Eur Ceram Soc,1995,15:445–453.
[12]CHOLLON G,ALDACOURROU B,CAPES L,et al.Thermal behav-iour of a polytitanocarbosilane-derived fibre with a low oxygen content:the Tyranno Lox-E fibre[J].J Mater Sci,1998,33:901–911.
[13]ISHIKAWA T,KOHTOKU Y,KUMAGAWA K,et al.High-strengthalkali-resistant sintered SiC fibre stable to 2 200℃[J].Nature,1998,391:773–774.
[14]LIPOWITZ J,BARNARD T,BUJALSKI D,et al.Fine-diameterpoly-crystalline SiC fibers[J].Comp Sci Technol,1994,51:167–171.
[15]BALDUS P,JANSEN M,SPORN D.Ceramic fibers for matrix com-posites in high-temperature engine applications[J].Science,1999,285:699–703.
[16]楚增勇,冯春祥,宋永才,等.先驱体转化法连续SiC纤维国内外研究与开发现状[J].无机材料学报,2002,17(2):193–201.CHU Zengyong,FENG Chunxiang,SONG Yongcai,et al.J Inorg Ma-ter(in Chinese),2002,17(2):193–201.
[17]MADDRELL E R.Pressureless sintering of silicon carbide[J].J MaterSci Lett,1987,6(4):486–488.
[18]GRESKOVICH C,ROSOLOWSKI J H.Sintering of covalent solids[J].J Am Ceram Soc,1976,59(7–8):336–343.
[19]CHEN L F,ZHANG L,CAI Z H,et al.Effects of oxidation curing andsintering additives on the formation of polymer-derived near-stoichio-metricsilicon carbide fibers[J].J Am Ceram Soc,2008,91(2):428–436.
[20]彭庆勋.硼氢化合物化学[M].北京:科学出版社,1965:65–67.PENG Qingxun.Boron Hydride Chemistry(in Chinese).Beijing,Sci-ence Press,1965:65–67.
[21]BURG A B,RANDOLPH C L.The N-methyl derivatives of B2H7N[J].J Am Chem Soc,1949,71(10):3451–3455.
[22]BURG A B,RANDOLPH C L.Disproportionation reactions of thedimethylaminoboron hydrides[J].J Am Chem Soc,1951,73(3):953–957.
[23]RICE B,GALIANO R J,LEHMANN W J.Vibrational spectra andforce constants of trimethylamine-borane and trimethylamine-borane-d3[J].J Phys Chem,1957,61:1222–1226.
[24]RYSCHKEWITSCH G E,WIGGINS J W.Hydrogen elimination indimethylamine-borane[J].Inorg Chem,1970,9(2):314–317.
[25]TAYLOR R C.Vibrational frequencies,assignments,and force con-stants for some compounds containing boron-nitrogen dative bonds[C]//NIEDENZU K.Boron-Nitrogen Chemistry.Wasington,DC:American Chemical Society,1964:59–70.
[26]SU K,REMSEN E E,ZANK G A,et al.Synthesis,characterization,and ceramic conversion reactions of borazine-modified hydridopolysi-azanes:new polymeric precursors to SiNCB ceramic composites[J].Chem Mater,1993,5:547–556.
[27]施耀曾,孙祥祯,蒋燕灏,等.有机化合物光谱和化学鉴定[M].江苏:江苏科学技术出版社,1988:54–145.SHI Yaozeng,SUN Xiangzhen,JIANG Yanhao,et al.Spectroscopyand Chemical Identification of Organic Compounds(in Chinese).Jiangsu:Jiangsu Scientific and Technologic Press,1988:54–145.
[28]HASEGAWA Y,OKAMURA K.Synthesis of continuous siliconcarbide fiber:Part 3 pyrolysis process of polycarbosilane and structureof the products[J].J Mater Sci,1983,18:3633–3648.
[29]ICHIKAWA H,MACHINO F,MITSUNO S,et al.Synthesis of con-tinuous silicon carbide fiber:Part 5 factors affecting stability of poly-carbosilane to oxidation[J].Mater Sci,1986,21:4352–4358.
[30]OKAMURA K,SATO M,HASEGAWA Y.Effect of oxidation curingpolycarbosilane fiber on tensile strength of coreless silicon carbide fi-ber[J].J Mater Sci Lett,1983,2:769–771.
[31]HASEGAWA Y,IIMURA M,YAJIMA S.Synthesis of continuoussilicon carbide fiber:Part 2 conversion of polycarbosilane fiber intosilicon carbide fibers[J].J Mater Sci,1980,15:720–728.
基本信息:
DOI：10.14062/j.issn.0454-5648.2011.08.023
中图分类号:TB332
引用信息:
[1]许慜,张力,陆雪川,等.先驱体转化法制备含硼SiC纤维[J].硅酸盐学报,2011,39(08):1260-1267.DOI:10.14062/j.issn.0454-5648.2011.08.023.
基金信息:
国家自然科学基金(51072169)资助项目
2011-07-26
2011-07-26
2011-07-26