纳米颗粒包覆ZrW<sub>2</sub>O<sub>8</sub>空心结构的制备和性能

doi:10.11901/1005.3093.2014.587

材料研究学报

2015, Vol. 29

Issue (10): 773-778 DOI: 10.11901/1005.3093.2014.587

本期目录 | 过刊浏览

纳米颗粒包覆ZrW₂O₈空心结构的制备和性能

张琳达¹,王浩伟¹,齐军²,吴一¹(

),彭思平³

1. 上海交通大学特种材料研究所上海 200240
2. 上海紫竹新兴产业技术研究院上海 200240
3. 上海无线电设备研究所上海 200090

Preparation and Properties of ZrW₂O₈Hollow Structures Coated with Colloidal Carbon Spheres

Linda ZHANG¹,Haowei WANG¹,Jun QI²,Yi WU^1,^**(

),Siping PENG³

1. Research Center of Special Materials, Shanghai Jiao Tong University, Shanghai 200240, China
2. Advanced Industrial Technology Research Institute (AITRI), Shanghai 200240, China
3. Shanghai Radio Equipment Institute, Shanghai 200090, China

引用本文:

张琳达,王浩伟,齐军,吴一,彭思平. 纳米颗粒包覆ZrW₂O₈空心结构的制备和性能[J]. 材料研究学报, 2015, 29(10): 773-778.
Linda ZHANG, Haowei WANG, Jun QI, Yi WU, Siping PENG. Preparation and Properties of ZrW₂O₈Hollow Structures Coated with Colloidal Carbon Spheres[J]. Chinese Journal of Materials Research, 2015, 29(10): 773-778.

全文: PDF(2238 KB) HTML

摘要:

采用包覆法制备单一相钨酸锆(ZrW₂O₈)空心球。研究选择以水热合成法制备的胶体碳球作为制备空心球的模板, 通过溶胶—凝胶法制备了具有网状结构的钨酸锆前驱体凝胶, 经过后续简单的包覆过程得到胶体碳球—钨酸锆凝胶形成的壳核结构, 并对该壳核结构进行煅烧(610℃保温10 h)后除去碳球模板得到ZrW₂O₈空心球。实验所得ZrW₂O₈空心球平均粒径约3 μm, 球壳平均厚度为1.5 μm, 构成壳层结构的纳米级ZrW₂O₈颗粒为棒状无规则多面体, 尺寸约500 nm×50 nm×50 nm。FTIR和TG-DTA分析证明, 产物为立方相ZrW₂O₈空心球, 密度为2.8 g/cm³, 比理论值降低了45%; 产物空心球具有良好的负热膨胀特性, 在室温至200℃的温度区间内, 负膨胀系数略低于理论值, 平均热膨胀系数为-11.4×10^-6K^-1。

关键词 ：无机非金属材料, 胶体碳球, 纳米颗粒包覆, 负膨胀, ZrW₂O₈

Abstract：

Colloidal carbon microspheres were prepared from aqueous glucose solutions by hydrothermal synthesis procedure, and then submicron core/shell structured precursors of carbon spheres/ZrW₂O₈ were prepared by sol-gel method with colloidal carbon microspheres as templates to provide reactive surfaces for facilitating the deposition of nano-sized ZrW₂O₈ particles. Finally, hollow spheres of ZrW₂O₈ can be produced by calcinating the precursors at 610℃ for 10h to remove the colloidal carbon sphere templates. The final spheres ZrW₂O₈ with an average size about 3μm were proved to be composed of single phase nano-sized ZrW₂O₈ particles. Their density was measured to be 2.8 g/cm³, ca 45% lower than that of ZrW₂O₈. Along with the density, FTIR and TG-DTA results also indicate the existence of hollow structure of the spheres ZrW₂O₈, of which the thermal expansion coefficient was -11.4×10^-6K^-1 in the temperature range from room temperature to 200℃, a little higher than the theoretical value.

Key words： inorganic non-metallic materials colloidal carbon spheres nano-layered structures NTE ZrW₂O₈

收稿日期: 2014-10-15

基金资助:* 航天科技创新基金USCAST2012-08, CASC201106资助项目。

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图1 胶体碳球的SEM像

图2 用溶胶-凝胶法制备的ZrW2O8空心球的SEM像

图3 胶体碳球、胶体碳球–ZrW2O8前驱体以及ZrW2O8空心球的红外光谱

图4 ZrW2O8空心球粉体的XRD谱

图5 胶体碳球–ZrW2O8前驱体壳核结构的TG-DTA曲线

图6 以胶体碳球为模板合成ZrW2O8空心球的过程

图7 ZrW2O8空心球粉体在不同温度下的衍射谱

图8 ZrW2O8粉体的晶胞参数与温度关系曲线

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