碳热还原法制备超细ZrB2/SiC复合陶瓷粉
Preparation of Ultra-fine ZrB2/SiC Composite Ceramic Powders by Carbothermal Reduction
摘 要
以ZrO2、硼酸、硅溶胶和炭黑为原料于1 300～1 700 ℃用碳热还原法合成了超细ZrB2/SiC复合陶瓷粉; 用XRD和SEM等研究了合成温度、反应物配比等对复合粉体物相组成、微观形貌和粒径的影响。结果表明: 当原料中硼酸过量(ZrO2与B2O3物质的量比为1∶1.5)才能保证在1 650 ℃下保温1 h时碳热还原反应完全进行, 得到高纯的ZrB2/SiC复合陶瓷粉体, 其颗粒平均尺寸为0.4 μm; 不同温度制备的复合粉体颗粒形貌不同, 随着温度的升高, 晶须和棒状颗粒减少, 而球形颗粒增多。
ZrB2
复合粉
碳热还原法
SiC
ZrB2
composite powder
carbothermal reduction
Abstract
Ultra-fine ZrB2/SiC composite ceramic powders were synthesized at temperatures from 1 300 ℃ to 1 700 ℃ by carbothermal reduction using zirconium dioxide, boric acid, silica sol and carbon black as raw materials. The influences of synthesis temperature and reactant ratio on the phase composition, micro morphology and particle size of the composite powders were investigated by XRD and SEM. The results show that the completeness of carbothermal reduction for the synthesis of high purity ZrB2/SiC composite powders was needed of over dosage of boric acid (molar ratio of ZrO2 and B2O3 was 1∶1.5) when synthesized at 1 650 ℃ for 1 h. The composite powders had an average particle size of 0.4 μm, and different particle shapes after prepared at different temperatures. With the increase of synthesis temperature, the whisker and rod particles gradually reduced while ball particles increased.
中图分类号 TB32
所属栏目
基金项目 国家自然科学基金资助项目(50972042)
收稿日期 2010/8/30
修改稿日期 2011/6/18
网络出版日期
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备注施浩良(1984-), 男, 浙江湖州人, 硕士研究生。
引用该论文: SHI Hao-liang,XIAO Han-ning,GAO Peng-zhao,HU Ji-lin,LI Qing. Preparation of Ultra-fine ZrB2/SiC Composite Ceramic Powders by Carbothermal Reduction[J]. Materials for mechancial engineering, 2011, 35(9): 93～97
施浩良,肖汉宁,高朋召,胡继林,李青. 碳热还原法制备超细ZrB2/SiC复合陶瓷粉[J]. 机械工程材料, 2011, 35(9): 93～97
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【4】KALSDOTTIR S N, HALLORAN J W. Formation of oxide films on ZrB2-15vol% SiC composites during oxidation: evolution with time and temperature[J]. J Am Ceram Soc,2009,92(6):1328-1332.
【5】CARNEY C M, MOGILVESKY P, PARTHASARATHY T A. Oxidation behavior of zirconium diboride silicon carbide produced by the spark plasma sintering method[J]. J Am Ceram Soc,2009,92(9):2046-2052.
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【8】KUSUNOSE T, SEKINO T, CHOA Y H, et al. Fabrication and micro structure of silicon nitride/boron nitride nanocomposites[J]. J Am Ceram Soc,2002,85(11):2678-2688.
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【10】江涛,金志浩,杨建锋,等.B4C/BN纳米复合粉末的制备与显微结构的研究[J].稀有金属材料与工程,2009,38(1):280-283.
【11】WANG X D, QIAO G J, JIN Z H. Fabrication of machinable silicon carbide-boron nitride ceramic nanocomposites[J]. J Am Ceram Soc,2004,87(4):565-570.
【12】WANG X D, QIAO G J, JIN Z H. Preparation of SiC/BN nanocomposites powders by chemical processing[J]. Mater Lett,2004,58:1419-1423.
【13】YAN Yong-jie, ZHANG Hui, HUANG Zheng-ren, et al. In situ synthesis of ultrafine ZrB2-SiC composite powders and the pressureless sintering behaviors[J]. J Am Ceram Soc,2008,91(4):1372-1376.
【14】LIU Xiao-kui, LUO Fa, ZHU Dong-mei.Microwave permittivity of SiC-Al2O3 composite powder prepared by sol-gel and carbothermal reduction[J]. Trans Nonferrous Met Soc,China,2006,16(2):494-497.
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【16】YAN Yong-jie, HUANG Zheng-ren, DONG Shao-ming, et al. New route to synthesize ultra-fine zirconium diboride powders using inorganic-organic hybrid precursors[J].J Am Ceram Soc,2006,89(11):3585-3588.
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【21】RAMAN V, BHATIA G, BHARDWAI S, et al. Synthesis of silicon carbide nanofibers by sol-gel and polymer blend techniques[J]. Journal of Materials Science,2005,40:1521-1527.
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