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用水热法并经570℃热处理6h制备了ZrW2O8粉体,对水热法制备的前驱体进行了热重–差热分析。用X射线粉末衍射、扫描电子显微镜对ZrW2O8粉体的微观结构及形貌进行表征,结果表明:ZrW2O8粉体为单一α-ZrW2O8相,粉体颗粒为规则的长方体棒状,尺寸约为1.2μm×1.2μm×10μm。原位X射线粉末衍射分析表明:所得ZrW2O8粉体具有很好的负热膨胀特性,从室温到500℃,其热膨胀系数为–6.30×10–6℃–1;在150～175℃温度范围内发生了α-ZrW2O8向β-ZrW2O8相的转变。
Abstract：ZrW2O8 powder was synthesized using hydrothermal method and heat treated at 570 ℃ for 6 h, and the negative thermal expansion property was analyzed. The precursor prepared by hydrothermal method was analyzed by thermogravimetric and differential scanning calorimeter. The microstructure and morphology of the ZrW2O8 powder were characterized by powder X-ray diffraction and scanning electron microscopy respectively. The results show that the powder is single phases of α-ZrW2O8 with a regular rectangular particle shape and an average size of 1.2 μm×1.2 μm×10 μm. The results of in situ X-ray diffraction analysis indicate that the thermal expansion coefficient of ZrW2O8 is –6.30×10–6 ℃–1 from room temperature to 500 ℃. The temperature transition of α to β phase is between 150 ℃ and 175 ℃.
[1]KORTHUIS V,KHOSROVANI N,SLEIGHT A W,et al.Negative thermal expansion and phase transition in the ZrV2–xPxO7series[J].Chem Mater,1995,7(2):412–417.
[2]MARY T A,EVANS J S O,VOGT T,et al.Negative thermal expansion from0.3–1.50Kelvin in ZrW2O8[J].Science,1996,272(5):90–92.
[3]EVANS J S O,DAVID W I F,SLEIGHT A W.Structural investigation of the negative-thermal-expansion material ZrW2O8[J].Acta Cryst B,1999,55(3):333–340.
[4]CHANG L L Y,SCROGER M G,PHILIPS B.Condensed phase relations in the systems ZrO2–WO2–WO3and HfO2–WO2–WO3[J].J Am Ceram Soc,1967,50(2):211–215.
[5]CHENG Xiaonong,SUN Xiujuan,YANG Juan,et al.Synthesis of negative thermal expansion material ZrW2O8powders using solid state reaction[J].J Jiangsu Univ(Nat Sci Ed)(in Chinese),2005,26(4):350–353.
[6]SUN Xiujuan,YANG Juan,LIU Qinqin,et al.Effect of preparation method on particle size and negative thermal expansion property of negative thermal expansion ZrW2O8powders[J].J Inorg Chem(in Chinese),2006,22(9):1635–1639.
[7]YAN Xuehua,CHENG Xiaonong,ZHANG Meifen.Effect of different treatment condition on transformation of precursor to ZrW2O8[J].J Chin Ceram Soc(in Chinese),2004,32(12):1530–1533.
[8]KAMESWARI U,SLEIGHT A W,EVANS J S O.Rapid synthesis of ZrW2O8and related phase,and structure refinement of ZrWMoO8[J].Int J Inorg Mater,2000,2(4):333–337.
[9]LIND C,WILKINSON A P.Seeding and the non-hydrolytic Sol–Gel synthesis of ZrW2O8and ZrMo2O8[J].J Sol–Gel Sci Technol,2002,25(1):51–56.
[10]WILKINSON A P,LIND C,PATTANAIK S.A new polymorph of ZrW2O8prepared using nonhydrolytic sol–gel chemistry[J].Chem Mater,1999,11(1):101–108.
[11]KOWACH G R.Growth of single crystals of ZrW2O8[J].J Cryst Growth,2000,212(1):167–172.
[12]SHI Erwei,XIA Changtai,WANG Buguo,et al.Development and application of hydrothermal method[J].J Inorg Mater(in Chinese),1999,11(2):193–206.
[13]XING Xianran,XING Qifeng,YU Ranbo,et al.Hydrothermal synthesis of ZrW2O8nanorods[J].Physica B,2006,371(1):81–84.
[14]DONG C.Powder X:Windows–95–based program for powder X-ray diffraction data procession[J].J Appl Cryst,1999,32(4):838–838.
[15]PUZDER A,WILLAMSON A J,ZAITSEVA N,et al.The effect of organic ligand binding on the growth of CdSe nanoparticles probed by ab initio calculations[J].Nano Lett,2004,4(12):2361–2365.
基本信息:
DOI：
中图分类号:O614.412
引用信息:
[1]孙秀娟,杨娟,刘芹芹等.水热法制备负热膨胀性ZrW_2O_8粉体(英文)[J].硅酸盐学报,2008,No.225(01):35-39.
基金信息:
国家自然科学基金(50372027);; 江苏省自然科学基金(BK2003404);; 江苏高校自然科学重大基础研究(06KJA43010)资助项目。