2Zr(CH2CH=CH2)2與液態(tài)聚硼硅氮烷(LPBSZ)在過(guò)氧化二異丙苯的作用下發(fā)生自由基共聚反應(yīng),制備了鋯含量大于10wt%的含鋯聚硼硅氮烷(PZC-PBSZ)。采用紅外光譜、核磁共振、光電子能譜等方法研究了PZC-PBSZ的分子結(jié)構(gòu)及合成機(jī)理。結(jié)果表明在先驅(qū)體的合成過(guò)程中,Cp2Zr(CH2CH=CH2)2除了自身發(fā)生自由基聚合反應(yīng)外,還會(huì)與LPBSZ中的Si-H發(fā)生硅氫加成和取代反應(yīng),生成Zr-C和Zr-Si。通過(guò)TG-MS和29Si MAS NMR分析表明,PZC-PBSZ先驅(qū)體中Cp、(CH3)3Si和(CH3)2SiH等官能團(tuán)的脫除主要發(fā)生在400~800℃。當(dāng)溫度升高到800~1200℃后,先驅(qū)體基本無(wú)機(jī)化,主要發(fā)生SiHN2C和SiN3C結(jié)構(gòu)向SiN4結(jié)構(gòu)的轉(zhuǎn)變。PZC-PBSZ經(jīng)1000℃以上高溫?zé)峤夂罂梢赞D(zhuǎn)化為ZrC納米顆粒分布均勻在SiBNC基體的ZrC/SiBNC納米復(fù)相陶瓷。經(jīng)1800℃高溫處理后,ZrC/SiBNC陶瓷仍保持均勻和晶粒細(xì)化的納米晶結(jié)構(gòu)。"/>

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高鋯含量改性聚硼硅氮烷的合成與表征
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國(guó)防科技大學(xué)航天科學(xué)與工程學(xué)院新型陶瓷纖維及其復(fù)合材料重點(diǎn)實(shí)驗(yàn)室,國(guó)防科技大學(xué)航天科學(xué)與工程學(xué)院新型陶瓷纖維及其復(fù)合材料重點(diǎn)實(shí)驗(yàn)室,國(guó)防科技大學(xué)航天科學(xué)與工程學(xué)院新型陶瓷纖維及其復(fù)合材料重點(diǎn)實(shí)驗(yàn)室

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國(guó)家自然科學(xué)基金資助(項(xiàng)目號(hào)51203184)、863項(xiàng)目(項(xiàng)目號(hào)2012AA03A210)、湖南省高校科技創(chuàng)新團(tuán)隊(duì)支持計(jì)劃和國(guó)防科技大學(xué)創(chuàng)新群體資助


Synthesis and characterization of high zirconium content modified polyborosilazane
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Science and Technology on Advanced Ceramic Fibers and Composites Laboratory,College of Areospace Science and Engineering,National University of Defense Technology,Science and Technology on Advanced Ceramic Fibers and Composites Laboratory,College of Areospace Science and Engineering,National University of Defense Technology,Science and Technology on Advanced Ceramic Fibers and Composites Laboratory,College of Areospace Science and Engineering,National University of Defense Technology

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    本文通過(guò)Cp2Zr(CH2CH=CH2)2與液態(tài)聚硼硅氮烷(LPBSZ)在過(guò)氧化二異丙苯的作用下發(fā)生自由基共聚反應(yīng),制備了鋯含量大于10wt%的含鋯聚硼硅氮烷(PZC-PBSZ)。采用紅外光譜、核磁共振、光電子能譜等方法研究了PZC-PBSZ的分子結(jié)構(gòu)及合成機(jī)理。結(jié)果表明在先驅(qū)體的合成過(guò)程中,Cp2Zr(CH2CH=CH2)2除了自身發(fā)生自由基聚合反應(yīng)外,還會(huì)與LPBSZ中的Si-H發(fā)生硅氫加成和取代反應(yīng),生成Zr-C和Zr-Si。通過(guò)TG-MS和29Si MAS NMR分析表明,PZC-PBSZ先驅(qū)體中Cp、(CH3)3Si和(CH3)2SiH等官能團(tuán)的脫除主要發(fā)生在400~800℃。當(dāng)溫度升高到800~1200℃后,先驅(qū)體基本無(wú)機(jī)化,主要發(fā)生SiHN2C和SiN3C結(jié)構(gòu)向SiN4結(jié)構(gòu)的轉(zhuǎn)變。PZC-PBSZ經(jīng)1000℃以上高溫?zé)峤夂罂梢赞D(zhuǎn)化為ZrC納米顆粒分布均勻在SiBNC基體的ZrC/SiBNC納米復(fù)相陶瓷。經(jīng)1800℃高溫處理后,ZrC/SiBNC陶瓷仍保持均勻和晶粒細(xì)化的納米晶結(jié)構(gòu)。

    Abstract:

    In this work, Zr-modified polyborosilazanes (PZC-PBSZ) with a high zirconium content over 10wt% were synthesized via radical reaction between Cp2Zr(CH2CH=CH2)2 and liquid polyborosilazane under the existence of dicumyl peroxide. The structure and reaction mechanism of PZC-PBSZ were studied using Fourier transforminfrared spectra, nuclear magnetic resonance and X-ray photoelectron spectroscopy. The results shown that besides the self-polymerization, Cp2Zr(CH2CH=CH2)2 can also reacted with Si-H in LPBSZ via hydrosilylation reaction and substitution reaction to form Zr-C and Zr-Si, respectively. The thermogravimetric-mass spectrometry and 29Si MAS NMR results shown that the escape of goups such as Cp, (CH3)3Si and (CH3)2SiH was ooccured at temperature range from 400 oC to 800 oC. As the temperature went up to 800~1200oC, the polymer PZC-PBSZ converted into inorganic mineral, and the evolution of SiHN2C and SiN3C structure to SiN4 structure was occurred at that temperature. After pyrolyzing at above 1000 oC, PZC-PBSZ can convert into ZrC/SiBNC ceramic nanocomposites, with ZrC nanoparticles finely dispersed in SiBNC matrix. The obtained ZrC/SiBNC ceramic nanocomposites can remain fine and nanocrystalline microstructure after annealing at 1800 oC.

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龍?chǎng)?邵長(zhǎng)偉,王軍.高鋯含量改性聚硼硅氮烷的合成與表征[J].稀有金屬材料與工程,2018,47(S2):122~128.[Xin Long, Changwei Shao, Jun Wang. Synthesis and characterization of high zirconium content modified polyborosilazane[J]. Rare Metal Materials and Engineering,2018,47(S2):122~128.]
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  • 收稿日期:2017-12-04
  • 最后修改日期:2017-12-04
  • 錄用日期:2018-02-01
  • 在線發(fā)布日期: 2018-11-01
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