有机合成高碳锆比碳化锆陶瓷的先驱体及其热裂解性能

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摘要以四氯化锆为锆源,苯甲醇为碳源,分别采用对二甲苯,间二甲苯和二甲苯3种不同溶剂,有机合成高碳锆比(原子比28:1)碳化锆陶瓷的先驱体苯甲醇锆(benzyl alcohol zirconium,BAZ)。采用FT-IR对先驱体的基团结构进行表征,通过热重分析(TGA)和X射线衍射分析(XRD)对BAZ的耐热性和陶瓷转化过程进行研究。结果表明,采用不同溶剂制备的碳化锆先驱体在600~700 ℃时均全部热裂解,1 500 ℃完全热解为ZrC,其中采用对二甲苯溶剂制备的先驱体在氩气气氛下1 600 ℃保温1 h后的陶瓷产率最高,为51.8%,采用二甲苯溶剂制备的先驱体热裂解温度最高,为670 ℃。

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	李一鸣
	苏哲安
	杨鑫
	黄启忠
	邵俊杰
	王宇杰
	方存谦

关键词 ：碳化锆, 高碳锆比, 先驱体, 陶瓷产率, 热裂解

Abstract：Using zirconium tetrachloride as zirconium source, and benzyl methanol as carbon source, precursor benzyl alcohol zirconium (BAZ) of high carbon zirconium ratio (28:1 atomic ratio) zirconium carbide ceramic was prepared by 3 different solvents (p-xylene solvent, m-xylene solvent and xylene solvent). The structure of the BAZ was characterized by FT-IR. The heat-resistant property was studied by TGA and the transformation of ceramic was studied by XRD. The results show that all zirconium carbide precursors prepared by different solvents are pyrolysised during 600-700 ℃ and turn to ZrC after 1 500 ℃ heat treatment. The precursor prepared by p-xylene solvent has the highest ceramic yield of 51.8% after 1 600 ℃ heat treatment with argon gas protection. The precursor prepared by xylene solvent has the highest pyrolysis temperature that is 670 ℃.

Key words： Zirconium carbide high carbon zirconium ratio precursor ceramic yield pyrolysis

收稿日期: 2018-02-28 出版日期: 2019-07-12

ZTFLH:

TB383.3

基金资助:湖南省战略新兴产业科技攻关项目(2016GK4020)

通讯作者: 黄启忠,教授,博士。电话：13607442795;E-mail: huangqz@csu.edu.cn

引用本文:

李一鸣, 苏哲安, 杨鑫, 黄启忠, 邵俊杰, 王宇杰, 方存谦. 有机合成高碳锆比碳化锆陶瓷的先驱体及其热裂解性能[J]. 粉末冶金材料科学与工程, 2019, 24(1): 89-94.
LI Yiming, SU Zhean, YANG Xin, HUANG Qizhong, SHAO Junjie, WANG Yujie, FANG Cunqian. Organic synthesis and pyrolysis properties of high carbon-zirconium ratio zirconium carbide precursor. Materials Science and Engineering of Powder Metallurgy, 2019, 24(1): 89-94.

链接本文:

http://pmbjb.csu.edu.cn/CN/ 或 http://pmbjb.csu.edu.cn/CN/Y2019/V24/I1/89

[1] 杨鑫, 黄启忠, 苏哲安, 等. C/C复合材料的高温抗氧化防护研究进展[J]. 宇航材料工艺, 2014, 44(1): 1-15.
YANG Xing, HUANG Qizhong, SU Zhean, et al.Review of recent progress on oxidation protection for C/C composites at high temperature[J]. Aerospace Materials & Technology, 2014, 44(1): 1-15.
[2] 刘春轩, 陈建勋, 苏哲安, 等. 碳化锆陶瓷先驱体裂解机理及PIP法制备C/C-ZrC复合材料[J]. 中国有色金属学报, 2014, 24(6): 1779-1784.
LIU Chunxuan, CHEN Jianxun, SU Zhean, et al.Pyrolysis mechanism of ZrC precursor and fabrication of C/C-ZrC composites by precursor infiltration and pyrolysis[J]. Transactions of Nonferrous Metals Society of China, 2014, 24(6): 1779-1784.
[3] 薛亮, 苏哲安, 杨鑫, 等. 先驱体浸渍裂解法制备三维C/C- HfC复合材料及其烧蚀性能[J]. 新型炭材料, 2017, 32(3): 265-270.
XUE Liang, SU Zhean, YANG Xin, et al.Ablation behavior of a three-dimensional C/C-HfC composite prepared by a precursor infiltration and pyrolysis method[J]. New Carbon Materials, 2017, 32(3): 265-270.
[4] 刘丹, 邱文丰, 蔡涛, 等. 碳化锆液相陶瓷前驱体的制备及陶瓷化[J]. 宇航材料工艺, 2014, 44(1): 79-83.
LIU Dan, QIU Wenfeng, CAI Tao, et al.Preparation and ceramization of liquid ZrC precursor[J]. Aerospace Materials & Technology, 2014, 44(1): 79-83.
[5] PIEON D, LUCAS R, CHEHAIDE S, et al.From trimethvlvinylane to ZrC-SiC hybrid materials[J]. Eur Ceram Soc, 2011, 31(14): 2687-2690.
[6] WANG H, GAO B, CHEN X, et al.Synthesis and pyrolysis of a novel preceramic polymer PZMS from PMS to fabricate high-temperature-resistant ZrC/SiC ceramic composite[J]. Applied Organometallic Chemistry, 2013, 27(3): 166-173.
[7] TANG Y, WANG J, LI X, LI W, et al.Synthesis and characterization of polyborosilazane as novel precursor to SiBNC ceramic[J]. Acta Chimica Sinica, 2008, 66(11): 1371-1376.
[8] LI W, WANG J, XIE Z, WANG H, et al.Synthesis and characterization of silicon-containing polyborazine to boron nitride ceramic fiber[J]. Acta Chimica Sinica, 2011, 69(16): 1936-1940.
[9] QIN Y, RAO Z, HUANG Z, et al.Preparation and performance of ceramizable heat-resistant organic adhesive for joining Al₂O₃, ceramics[J]. International Journal of Adhesion & Adhesives, 2014, 55(2): 132-138.
[10] BOUZAT F, GRAFF A R, LUCAS R, et al.Preparation of C/SiC ceramics using a preceramic polycarbosilane synthesized via, hydrosilylation[J]. Journal of the European Ceramic Society, 2016, 36(12): 2913-2921.
[11] ARISH D, SHIJU C, JOSEYPHUS R S, et al.Synthesis of ZrB₂-SiC ceramic composites from a single-source precursor[J]. Materials Chemistry & Physics, 2017, 194: 308-312.
[12] PATRA N, NASIRI N A, JAYASEELAN D D, et al.Synthesis, characterization and use of synthesized fine zirconium diboride as an additive for densification of commercial zirconium diboride powder[J]. Ceramics International, 2016, 42(8): 9565-9570.
[13] WANG T, YU Q, KONG J, et al.Synthesis and heat-insulating properties of yttria-stabilized ZrO₂, hollow fibers derived from a ceiba template[J]. Ceramics International, 2017.
[14] 董占能, 赵兵, 郭玉忠. 金属醇盐的合成(Ⅰ)[J]. 云南化工, 1997(3): 58-60.
DONG Zhanneng, ZHAO Bing, GUO Yuzhong.Progress in the Synthesis of metal alkoxises[J]. Yunnan Chemical Technology, 1997(3): 58-60.
[15] 徐碇皓, 高晓梅, 周权. 含锆耐高温陶瓷化先驱体的合成和性能研究[J]. 功能材料, 2015, 46(8): 8042-8045.
XU Dinghao, GAO Xiaomei, ZHOU Quan.Synthesis and properties of the ceramic precursor containing zirconium and alkyne[J]. Journal of Functional Materials, 2015, 46(8): 8042-8045.
[16] 董占能, 赵兵, 郭玉忠. 金属醇盐的物化特性[J]. 昆明理工大学学报: 自然科学版, 2000, 25(2): 58-61.
DONG Zhanneng, ZHAO Bing, GUO Yuzhong.The pilot study of application of compound fertilizer made of waste mud to paddy[J]. Journal of Kunming University Offence & Technology, 2000, 25(2): 58-61.