使用木糖醇合成纳米ZrB2粉末的研究

doi:10.15541/jim20150481

无机材料学报 ›› 2016, Vol. 31 ›› Issue (6): 597-601.DOI: 10.15541/jim20150481

使用木糖醇合成纳米ZrB₂粉末的研究

赵月¹, 李军平², 汪庭语¹, 李锐星¹, 冯志海², 才鸿年³

(1. 北京航空航天大学材料科学与工程学院空天材料与服役教育部重点实验室, 北京100191; 2. 航天材料及工艺研究所, 北京100076; 3. 中国兵器装备集团公司, 北京100089)

收稿日期:2015-10-18 修回日期:2016-01-11 出版日期:2016-06-20 网络出版日期:2016-05-19
作者简介:赵月(1991–), 女, 硕士研究生. E-mail: 412174292@qq.com
基金资助:
国家自然科学基金(51372006);国家人力资源和社会保障部 2010年度高层次留学人才回国工作资助(人社厅函2010, No.411)

Synthesis of ZrB₂ Nanoparticles by Using Xylitol

ZHAO Yue¹, LI Jun-Ping², WANG Ting-Yu¹, LI Rui-Xing¹, FENG Zhi-Hai², CAI Hong-Nian³

(1. Key Laboratory of Aerospace Materials and Performance (Ministry of Education), School of Materials Science and Engineering, Beihang University, Beijing 100191, China; 2. Aerospace Research Institute of Materials & Processing Technology, Beijing 100076, China; 3. China South Industries Group Corporation, Beijing 100089, China)

Received:2015-10-18 Revised:2016-01-11 Published:2016-06-20 Online:2016-05-19
About author:ZHAO Yue. E-mail: 412174292@qq.com
Supported by:
National Natural Science Foundation of China (51372006);Scientific Research Starting Foundation for Returned Overseas Chinese Scholars, Ministry of Education, Start-Up Fund for High-End Returned Overseas Talents (2010, No.411)

摘要/Abstract

摘要：

以正丙醇锆、乙酸、硼酸和木糖醇为原料, 采用溶胶-凝胶法, 通过碳热还原反应制备了纳米ZrB₂粉末。在反应体系中, 木糖醇既提供反应所需的碳, 又与硼酸形成了配位化合物。通过对凝胶前驱体粉末进行傅里叶红外光谱以及热重分析, 探讨了溶胶-凝胶反应过程对碳热还原反应温度以及凝胶陈化时间的影响。结果表明, 引入木糖醇促进了反应过程的进行, 湿凝胶无需陈化处理, 并且降低了碳热还原温度。当木糖醇与正丙醇锆的摩尔配比为1.4时, 使用未经陈化的凝胶前驱体, 经1450℃碳热还原即可获得平均直径约50 nm的等轴状ZrB₂纳米颗粒, 粉体氧含量为1.36wt%。

关键词: 纳米, 木糖醇, ZrB2, 溶胶-凝胶, 合成

Abstract:

ZrB₂ nanoparticles were synthesized synergistically by Sol-Gel method and carbothermal reduction reaction using zirconium n-propoxide, acetic acid, boric acid and xylitol as starting materials. In the reaction system, xylitol acted as a carbon source for the carbothermal reduction reaction and chelated boron, leading to the formation of coordination compound through its polyhydroxy reaction with boric acid. According to the Fourier Transform infrared spectra and thermal analysis of gel precursor, the effects of sol and gel reaction processes on the carbothermal reduction reaction temperature and gelation time were discussed. The results show that the polyhydroxy compound of xylitol is beneficial to initiate reactions and gelation, which makes the threshold throughout the whole chemical processes easy to overcome. The gel does not need aging treatment and the reaction temperature is lowered. Besides, a single phase of equiaxed ZrB₂ nanoparticles could be obtained from nascent state gel calcined at 1450℃ with n(xylitol)/n(zirconium n-propoxide) of 1.4. The average diameter and oxygen content of ZrB₂ nanoparticles are ca. 50 nm and 1.36wt%, respectively.

Key words: nanoparticles, xylitol, ZrB2, Sol-Gel, synthesis

中图分类号:

TQ174

赵月, 李军平, 汪庭语, 李锐星, 冯志海, 才鸿年. 使用木糖醇合成纳米ZrB₂粉末的研究[J]. 无机材料学报, 2016, 31(6): 597-601.

ZHAO Yue, LI Jun-Ping, WANG Ting-Yu, LI Rui-Xing, FENG Zhi-Hai, CAI Hong-Nian. Synthesis of ZrB₂ Nanoparticles by Using Xylitol[J]. Journal of Inorganic Materials, 2016, 31(6): 597-601.

图/表 7

图1 合成ZrB2粉末的工艺流程图

Fig. 1 General flow chart for synthesis of ZrB2 powder

图2 (a)硼酸和(b)n(木糖醇)/n(正丙醇锆)=1.4时得到的前驱体粉末傅里叶红外光谱图

Fig. 2 FTIR spectra of (a) boric acid and (b) ZrB2 precursor powder prepared with n(Xylitol)/n(Zr(OPr)4)=1.4

图3 (a)木糖醇和(b)n(木糖醇)/n(正丙醇锆)=1.4时得到的前驱体粉末(条件: 氩气, 10℃/min)的热分析TG-DSC曲线

Fig. 3 TG-DSC curves of (a) xylitol and (b) ZrB2 precursor powder prepared with n(Xylitol)/n(Zr(OPr)4)=1.4 under argon flow at a heating rate of 10℃/min

图4 n(木糖醇)/n(正丙醇锆)=1.4时得到的前驱体粉末在(a) 1200℃、(b)1300℃、(c)1400℃和(d)1450℃下煅烧产物的XRD图谱

Fig. 4 XRD patterns of the products calcined from precursors at (a) 1200℃, (b) 1300℃, (c) 1400℃ and (d) 1450℃ for 2 h with n(Xylitol)/n(Zr(OPr)4)=1.4

图5 n(X)/n(Zr)分别为(a)1、(b)1.2和(c)1.4制备的前驱体粉末在1450℃保温2 h产物的XRD图谱

Fig. 5 XRD patterns of the products calcined from precursors at 1450℃ for 2 h with n(X)/n(Zr) of (a) 1, (b) 1.2 and (c) 1.4

图6 n(X)/n(Zr)=1.4时, (a)未陈化与(b)陈化6d的凝胶前驱体粉末在1450℃下煅烧产物的XRD图谱

Fig. 6 XRD patterns of the products calcined from precursors at 1450℃ for 2 h using (a) nascent state gel and (b) 6 d-aged gel with n(X)/n(Zr) of 1.4

图7 n(X)/n(Zr)为1.4, 未经陈化的前驱体粉末在1450℃保温2 h得到的ZrB2粉末的SEM照片

Fig. 7 SEM images of single-phase ZrB2 powder calcined from precursors at 1450℃ for 2 h with n(X)/n(Zr)=1.4

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使用木糖醇合成纳米ZrB₂粉末的研究

Synthesis of ZrB₂ Nanoparticles by Using Xylitol

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