共沉淀法制备ZrW2O8及其中间产物的晶体结构
Crystal Structure of ZrW2O8 and the Intermediate Products Prepared with Coprecipitation Method
摘 要
以仲钨酸铵[(NH4)10W12O41·5H2O]和氧氯化锆(ZrOCl2·8H2O)为原料,采取共沉淀法制备具有负热膨胀系数的钨酸锆(ZrW2O8)。采用X射线衍射仪(XRD)分析合成过程的前驱体、中间体和最终产物等的晶体结构,并采用FullProfSuite程序和Material Studio程序分别对ZrW2O8晶体的XRD数据进行处理,精化修正其原子坐标参数和晶体结构参数。结果表明,前驱体结构呈无定形态;中间体的结晶度为33.66%;最终产物为立方晶系的ZrW2O8,空间群为P213(198),晶胞参数a0为0.915 98 nm,晶胞体积为0.768 52 nm3,衍射峰指标化的可靠性因子F(30)=57.1(44),峰形因子RP为0.251 9,权重因子Rwp为0.134 3。
晶体结构
X射线衍射
共沉淀法
zirconium tungstate
crystal structure
X-ray diffraction
coprecipitation methodHQ〗
Abstract
Negative thermal expansion zirconium tungstate ZrW2O8 powder was prepared from ammonium metatungstate (NH4)10W12O41·5H2O and zirconium oxychloride ZrOCl2·8H2O with coprecipitation method. The physical structure of the precursor,intermediate powder in the synthesis and final product powder were analyzed by X-ray diffraction,and XRD data of ZrW2O8 crystal structure were treated by FullProf-Suite software and Material Studio software,in which the atomic coordinate parameter and the crystal structure parameter of ZrW2O8 were refined. The results indicated that the structure of precursor was identified as amorphous,the crystallinity of the intermediate was 33.66%,and the final product was cubic phase ZrW2O8 with space group of P213(198),cell parameter of 0.915 98 nm and cell volume of 0.768 52 nm3. Through XRD data treatment it was obtained that the figure of merit for the index F(30) was 57.1(44),the peak profile simulation factor RP was 0.251 9 and the weight factor Rwp was 0.134 3.
中图分类号 TB383
所属栏目 试验与研究
基金项目 上海市高新工程专项资金资助项目(SU-06-05)
收稿日期 2008/1/11
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备注贺志强(1981-),男,硕士研究生。
引用该论文: HE Zhi-qiang,GUO Qiang,PAN Guo-liang. Crystal Structure of ZrW2O8 and the Intermediate Products Prepared with Coprecipitation Method[J]. Physical Testing and Chemical Analysis part A:Physical Testing, 2009, 45(4): 191～194
贺志强,郭 强,潘国梁. 共沉淀法制备ZrW2O8及其中间产物的晶体结构[J]. 理化检验－物理分册, 2009, 45(4): 191～194
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【3】MATSUMOTO A,KOBAYASHI K,NISHIO T,et al. Fabrication and thermal expansion of Al-ZrW2O8 composites by pulse current sintering process[J]. Materials Science Forum,2003,429: 2279-2284．
【4】YILMAZ S,DUNAND D C. Finite-element analysis of thermal expansion and thermal mismatch stresses in a Cu-60vol%ZrW2O8 composite[J]. Composites Science and Technology,2004,64(12): 1895-1898．
【5】JOSE MANUEL GALLARDO-AMORES,ULISES AMADOR,EMILIO MORA’N,et al. XRD study of ZrW2O8 versus temperature and pressure[J]. International Journal of Inorganic Materials,2000,2: 123-129．
【6】NOAILLES L D,PENG H H,STARKOVICH J,et al. Thermal expansion and phase formation of ZrW2O8 aerogels[J]. Chemistry of Materials,2004,16: 1252-1259．
【7】DE MEYER C,VANDEPERRE L,VAN DRIESSCHE I,et al. Processing effects on the microstructure observed during densification of the NTE-compound ZrW2O8[J]. Crystal Engineering,2002,5: 469-478．
【8】MANCHEVA M N,IORDANOVA R S,DIMITRIEV Y B,et al. Direct synthesis of metastable nanocrystalline ZrW2O8 by a melt-quenching method[J]. Journal of Physical Chemistry C,2007,111(41): 14945-14947．
【9】KAMESWARI U,SLEIGHT A W,EVANS J S O. Rapid synthesis of ZrW2O8 and related phases,and structure refinement of ZrWMoO8 [J]. International Journal of Inorganic Materials,2000,2: 333-337．
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