Effect of Calcination Conditions on Synthesis of Ultrafine ZrB2 Powder by Sol-Gel Method
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摘要: ZrB2基陶瓷材料在超高温领域具有广阔的应用前景,为研究煅烧条件对ZrB2粉体的影响,本研究分别以正丙醇锆、蔗糖和硼酸为Zr源、C源和B源,采用溶胶-凝胶法制备ZrB2粉体,研究了煅烧温度、保温时间及氩气流量对ZrB2粉体合成的影响。结果表明,随着煅烧温度的升高,生成物中的杂质相含量逐渐降低,ZrB2相含量逐渐增加。B∶Zr∶C摩尔比为2.85∶1∶7的前驱体粉体在氩气气氛、1 550 ℃下分别保温30、60和120 min后均得到了纯ZrB2粉体。由Scherrer公式计算得到的ZrB2平均晶粒尺寸远小于SEM观测的粒径,表明制得的ZrB2粉体由小晶粒组成。煅烧过程中通入的氩气流量会影响B2O3的挥发程度,进而影响产物的物相组成。Abstract: ZrB2-based ceramics have broad application prospects in the field of ultra-high temperature. ZrB2 powders are prepared by sol-gel method with zirconium propanol, sucrose and boric acid as Zr, C and B sources, respectively, and the effects of calcination temperature, holding time and argon flow rate on the synthesis of ZrB2 powder are studied. The results show that with the increase of calcination temperature, the content of impurity phase in the product decreases gradually, and that the content of ZrB2 phase increases gradually. Pure ZrB2 powders are obtained by holding the precursor powders with a molar ratio of 2.85∶1∶7 of B∶Zr∶C in argon atmosphere at 1 550 ℃ for 30, 60 and 120 minutes. The average grain size of ZrB2 powders calculated by Scherrer formula is much smaller than that observed by SEM, indicating that the ZrB2 powders are composed of small grains. The argon flow rate during calcination process will affect the volatilization degree of B2O3, and then affect the phase composition of the product.
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Keywords:
- ZrB2 /
- sol-gel method /
- calcination temperature /
- microstructure /
- volatilization of B2O3
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