低温固相反应合成纳米级TiB2-TiC复合粉体

doi:10.15541/jim20150524

摘要/Abstract

摘要：

在Ti-B体系中引入PTFE作为反应促进剂, 实现了TiB₂-TiC粉体的低温固相合成。分别采用热分析仪、X射线衍射仪和场发射扫描电子显微镜, 测定了体系的反应温度, 表征了生成物的物相和微观形貌, 并对其反应过程和反应机理进行了分析。合成实验在氩气炉中进行, 结果表明: 当添加10wt% PTFE时, 能够在550℃通过固相反应制备出平均粒径小于400 nm的TiB₂-TiC复合陶瓷粉体。DTA测试表明固相反应合成过程主要包括两步: 首先, 在低温下PTFE和Ti发生反应并释放出大量的热, 然后, 诱发Ti和B的固相反应生成TiB₂。

关键词: TiB₂-TiC, 固相合成, PTFE, 反应机理

Abstract:

TiB₂-TiC composite powders were prepared at low temperature in the Ti-B system with the PTFE polytetrafluoroethylene (polytetrafluoroethylene) as a chemical activator. Reaction temperature, phase composition and morphology were measured via differential thermal analysis, X-ray diffraction and field emission scanning electron microscopy (FESEM) in order to explore the reaction mechanism, respectively. Actual solid-state reaction synthesis experiments were carried out for the same composition in an argon atmosphere furnace. It was found that TiB₂-TiC composite powder could be synthesized successfully at 550℃ by adding 10wt% PTFE into the initial reactant Ti-B mixture. The FESEM image showed that the average size of the product was smaller than 400 nm. According to differential thermal analysis results, the combustion synthesis mainly includes two reaction processes: firstly, the initial reaction between titanium and PTFE particles resulting in great amounts of heat release; subsequently, the released energy triggers the solid-state reaction between titanium and boron particles to form TiB₂.

Key words: TiB₂-TiC, solid-state synthesis, PTFE, reaction mechanism

中图分类号:

TQ174

鱼银虎, 汪涛, 廖秋平, 缪润杰, 潘剑锋, 张度宝. 低温固相反应合成纳米级TiB₂-TiC复合粉体[J]. 无机材料学报, 2016, 31(3): 324-328.

YU Yin-Hu, WANG Tao, LIAO Qiu-Ping, MIAO Run-Jie, PAN Jian-Feng, ZHANG Du-Bao. Low-temperature Solid-state Synthesis of Nanometer TiB₂-TiC Composite Powder[J]. Journal of Inorganic Materials, 2016, 31(3): 324-328.

图/表 5

Fig. 1 DTA curves of the Ti-B mixtures with (a) 0wt%, (b) 1wt%, (c) 3wt%, (d) 5wt%, (e) 8wt%, (f) 10wt%, and (g) 12wt% PTFE

Fig. 2 XRD patterns of the Ti-B mixtures with (a) 0wt%, (b) 1wt%, (c) 3wt%, (d) 5wt%, (e) 8wt%, (f) 10wt%, and (g) 12wt% PTFE after reactions in argon atmosphere at 550℃

Fig. 3 XRD patterns of the Ti-B mixtures with (a) 0wt%, (b) 1wt%, (c) 3wt%, (d) 5wt%, (e) 8wt%, (f) 10wt%, and (g) 12wt% PTFE after reactions in argon atmosphere at 1300℃

Fig. 4 Morphologies and EDS results of the product of Ti-B system with (a) 10wt% PTFE and (b) 12wt% after reactions in argon atmosphere at 550℃

Fig. 5 DTA curves of (a) PTFE, (b) B-PTFE and (c) Ti-PTFE at a heating rate of 10℃/min in argon atmosphere

参考文献 28

[1]	JENSEN M S, EINARSRUD M A, GRANDE T.The effect of surface oxides during hot pressing of TiB2.J. Am. Ceram. Soc., 2009, 92(3): 623-630.
[2]	BILGI E, CAMURLU H E, AKGUN B, et al. Formation of TiB2 by volume combustion and mechanochemical process. Mater. Res. Bull., 2008, 43(4): 873-881.
[3]	KHANRA A K, GODKHINDI M M, PATHAK L C. Sintering behaviour of ultra-fine titanium diboride powder prepared by self-propagating high-temperature synthesis (SHS) technique. Mater. Sci. Eng. A, 2007, 454-455: 281-287.
[4]	CHENG Y, SHIGETA M, CHOI S, et al. Formation mechanism of titanium boride nanoparticles by RF induction thermal plasma. Chem. Eng. J., 2012, 183: 483-491.
[5]	NEKAHI A, FIROOZI S.Effect of KCl, NaCl and CaCl2 mixture on volume combustion synthesis of TiB2 nanoparticles.Mater. Res. Bull., 2011, 46(9): 1377-1383.
[6]	KANG S H, KIM D J.Synthesis of nano-titanium diboride powders by carbothermal reduction.J. Eur. Ceram. Soc., 2007, 27(2/3): 715-718.
[7]	CONTRERAS L, TURRILLAS X, VAUGHAN G B M, et al. Time-resolved XRD study of TiC-TiB2 composites obtained by SHS. Acta Mater., 2004, 52(16): 4783-4790.
[8]	CALKA A, OLESZAK D.Synthesis of TiB2 by electric discharge assisted mechanical milling.J. Alloys Compd., 2007, 440(1/2): 346-348.
[9]	AVILES M A, CHICARDI E, CORDOBA J M, et al. In situ-synthesis of ceramic composite materials in the Ti-B-C-N system by a mechanically induced self-sustaining reaction. J. Am. Ceram. Soc., 2012, 95(7): 2133-2139.
[10]	YU YIN-HU, WANG TAO, ZHANG HONG-MIN, et al. Low temperature combustion synthesis of TiC powder induced by PTFE. J. Inorg. Mater., 2015, 30(3): 272-276.
[11]	LICHERI R, ORRU R, CAO G.Chemically-activated combustion synthesis of TiC-Ti composites.Mater. Sci. Eng. A, 2004, 367(1/2): 185-197.
[12]	HAMBARTSUMYAN A A, KHACHATRYAN H L, KHARATYAN S L.Mechanically and chemically activated SHS in the Mo-Si-C system: Synthesis of MoSi2-SiC composites.Int. J. SHS, 2007, 16(2): 87-91.
[13]	ZURNACHYAN A R, KHARATYAN S L, KHACHATRYAN H L, et al. Self-propagating high temperature synthesis of SiC-Cu and SiC-Al cermets: Role of chemical activation, Int. J. Refract. Met. Hard Mater., 2011, 29(2): 250-255.
[14]	NIKZAD L, LICHERI R, VAEZI M R, et al. Chemically and mechanically activated combustion synthesis of B4C-TiB2 composites. Int. J. Refract. Met. Hard. Mater., 2012, 35: 41-48.
[15]	NERSISYAN H H, NIKOGOSOV V N, KHARATYAN S L, et al. The chemical mechanism of transformations and combustion in the Si-C-teflon system. Fiz. Goreniya Vzryva, 1991, 27(6): 77-81.
[16]	ABOVYAN L S, NERSISYAN H H, KHARATYAN S L, et al. Synthesis of alumina-silicon carbide composites by chemically activated self-propagating reactions. Ceram. Int., 2001, 27(2): 163-169.
[17]	LEE I, REED R R, BRADY V L, et al. Energy release in the reaction of metal powders with fluorine containing polymers. J. Therm. Anal. Calorim., 1997, 49(3): 1699-1705.
[18]	KUWAHARA T, MATSUO S, SHINOZAKI N.Combustion and sensitivity characteristics of Mg/TF pyrolants.Propell. Explos. Pyrotech., 1997, 22: 198-202.
[19]	BINNEWIES M, MILKE E.Thermochemical Data of Elements and Compounds, 2nd ed. Weinheim: Wiley-VCH, 2002.
[20]	NIELSON D B, TRUITT R M, ASHCROFT B N. Reactive Material Enhanced Projectiles and Related Methods. US, Patent, 20120167793A1. 2012.
[21]	SHERIDAN E W, HUGUS I V G D, BELLOMO F, et al. Thermal Enhanced Blast Warhead. US, Patent, 8250986B1. 2012.
[22]	NERONOV V A, KORCHAGIN M A, ALEKSANDROV V V, et al. Investigation of the interaction between boron and titanium. J. Less-common Met., 1981, 82: 125-129.
[23]	BHAUMIK S K, DIVAKAR C, SINGH A K, et al. Synthesis and sintering of TiB2 and TiB2-TiC composite under high pressure. Mater. Sci. Eng. A, 2000, 279: 275-281.
[24]	TARASOV A V, ALIKHANIAN A S, KIRAKOSYAN G A, et al. Chemical interaction of metallic titanium with a tetrafluoroethylene- vinylidene fluoride copolymer. Inorg. Mater., 2010, 46(12): 1308-1312.
[25]	WANG H, WU W, SUN S, et al. Characterization of the structure of TiB2/TiC nanocomposite powders fabricated by high-energy ball milling. Ceram. Int., 2011, 37(7): 2689-2693.
[26]	CARLO S R, PERRY C C, TORRES J, et al. Surface reactions of vapor phase titanium atoms with halogen and nitrogen containing polymers studied using in situ X-ray photoelectron spectroscopy and atomic force microscopy. Appl. Surf. Sci., 2002, 195(1-4): 93-106.
[27]	DUNMEAD S D, READEY D W, SEMLER C E, et al. Kinetics of combustion synthesis in the Ti-C and Ti-C-Ni systems. J. Am. Ceram. Soc., 1989, 72(12): 2318-2324.
[28]	HOLT J B, KINGMAN D D, BIANCHINI G M.Kinetics of the combustion synthesis of TiB2.Mater. Sci. Eng., 1985, 71: 321-327.

低温固相反应合成纳米级TiB₂-TiC复合粉体

Low-temperature Solid-state Synthesis of Nanometer TiB₂-TiC Composite Powder

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