为了合成性能较好的 ZrB2空心球粉体，以氧氯化锆（ZrClO2·8H2 O）、硼酸（H3 BO3）、葡萄糖（C6 H12 O6）为原料，先采用水热碳化工艺制备了碳微球，再以预合成的碳微球为模板，采用溶胶－凝胶法、硼热－碳热还原工艺合成了 ZrB2超细空心球粉体，研究了反应温度（1200、1300、1400和1500℃）及碳微球的含量（n（C） n（ZrO2＋B2 O3）分别为5．0、5．5、6．0和6．5）对 ZrB2空心球粉体合成的影响。结果表明：水热碳化工艺制备的碳微球表面较为光滑，具有良好的空心结构；过量的碳微球和较高的反应温度均能在一定程度上有助于 ZrB2空心球粉体的合成；合成 ZrB2空心球粉体的最佳反应温度为1500℃，最佳碳微球含量为 n（C）n（ZrO2＋B2 O3）＝6．5。
Carbon microspheres were firstly prepared using zirconium oxychloride (ZrClO2 ·8H2 O),boric acid (H3 BO3 )and glucose (C6 H 12 O6 )as the starting materials by hydrothermal carbonization.Then hollow ZrB2 spheres were successfully synthesized using a combined sol-gel and boro /carbothermal reduction method,and the prepared carbon microspheres as the template.The effects of the reaction temperatures (1 200,1 300,1 400 and 1 500 ℃,respectively)and contents of carbon microspheres (n(C) n(ZrO2 +B2 O3 )is 5.0,5.5,6.0 and 6.5,respectively)on the synthesis of hollow ZrB2 spheres were studied.The prepared carbon microspheres have smooth surface and good hollow structure by hydrothermal nitrida-tion.Increase of reaction temperature and excessive carbon microspheres can greatly promote the forma-tion of hollow ZrB2 spheres.The optimized reaction temperature and molar ratio of n(C)/n(ZrO2 +B2 O3 ) were 1 500 ℃ and 6.5,respectively.
参考文献
| [1] | Xiong Wen (David) Lou;Lynden A. Archer;Zichao Yang.Hollow Micro-/Nanostructures: Synthesis and Applications[J].Advanced Materials,200821(21):3987-4019. |
| [2] | 杨玉娇;王啸;王刚;林红.水热法制备大比表面积二氧化钛纳米片空心微球[J].硅酸盐学报,2014(10):1219-1224. |
| [3] | Wen ZH;Wang Q;Zhang Q;Li JH.Hollow carbon spheres with wide size distribution as anode catalyst support for direct methanol fuel cells[J].Electrochemistry communications,20078(8):1867-1872. |
| [4] | Yaohui Qu;Zhian Zhang;Xiwen Wang.A simple SDS-assisted self-assembly method for the synthesis of hollow carbon nanospheres to encapsulate sulfur for advanced lithium-sulfur batteries[J].Journal of Materials Chemistry, A. Materials for energy and sustainability,201345(45):14306-14310. |
| [5] | 甘治平;官建国.硬模法制备无机空心球的研究进展[J].材料导报,2007(5):105-108. |
| [6] | 江峰;李洒;彭志坚;汪长安.利用碳模板制备ZrO2亚微米空心球[J].硅酸盐学报,2014(9):1087-1091. |
| [7] | Jianke Ye;Shaowei Zhang;William E. Lee.Novel low temperature synthesis and characterisation of hollow silicon carbide spheres[J].Microporous and mesoporous materials: The offical journal of the International Zeolite Association,2012:25-30. |
| [8] | 陈丰;陈志刚;李霞章;陆晓旺;赵晓兵.以碳球为模板合成氧化铈纳米空心球[J].硅酸盐学报,2011(3):397-402. |
| [9] | Zhenghong Dong;Xiaoyong Lai;Jonathan E. Halpert;Nailiang Yang;Luoxin Yi;Jin Zhai;Dan Wang;Zhiyong Tang;Lei Jiang.Accurate Control of Multishelled ZnO Hollow Microspheres for Dye-Sensitized Solar Cells with High Efficiency[J].Advanced Materials,20128(8):1046-1049. |
| [10] | Zhang, Y.;Li, R.;Jiang, Y.;Zhao, B.;Duan, H.;Li, J.;Feng, Z..Morphology evolution of ZrB_2 nanoparticles synthesized by solgel method[J].Journal of Solid State Chemistry,20118(8):2047-2052. |
| [11] | 曹迎楠;杜爽;张海军;李发亮;鲁礼林;张少伟.溶胶-凝胶碳热还原法制备硼化锆超细粉体[J].硅酸盐学报,2014(10):1229-1234. |
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