负膨胀材料Zr_2P_2MO_(12)的制备及性能研究
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摘要
负膨胀材料,在一定的温度范围内,其平均热膨胀系数为负值,即具有“热缩冷胀”的特性。由于这类材料在电子,光学,航天航空等领域具有广阔的应用空间和巨大的应用价值,所以从被发现以来,已经引起大家的广泛关注。作为其中的重要成员,正交相的A2(MO4)3系列材料具有很大的各向异性负膨胀系数,且灵活多变,不仅三价离子A3+可以被不同元素替代,还可以用五价离子替代六价的M,Zr2P2MO12(M为W或Mo)材料就是用P替换其中的部分W或Mo而得到的一类材料。
Zr2P2MO12可以在很大的温度范围内保持正交相和负膨胀性能,且不吸水,具有很高的稳定性。但对这类材料的制备方法和性能研究尚处于起步阶段。为此,我们用快速烧结合成法对Zr2P2WxMo1-xO12(0≤x≤1)和Zr2PVMoO12的制备进行了研究,运用XRD和拉曼光谱技术研究其性能,并对这些材料的拉曼光谱进行了分析。作为Zr2P2MO12材料的功能化应用,Zr2P2WO12与ZrW2O8的复合陶瓷可以用来做光纤布拉格光栅的绝热衬底,在本文中用高温快速烧结法制备出Zr2P2WO12与ZrW2O8的复合陶瓷。研究的主要结果和结论如下：
1利用快速烧结合成法在较短的时间内制备出高纯度的Zr2P2WxMo1-xO12(0 2对于Zr2P2WO12、Zr2P2MoO12和Zr2P2WxMo1-xO12(0开放式框架结构并具有各向异性的负膨胀性能。通过测试这些材料的变温拉曼光谱发现,他们在20-600℃之间没有发生相变和放水,即始终保持了负膨胀特性。
3通过对Zr2P2WxMo1-xO12(O≤x≤1)的拉曼光谱分析发现,相对于A2(M04)3材料的拉曼光谱,其在1200-1060cm-1和760-460cm-1之间多出了几个拉曼峰,这是由于PO4的存在引起的。对Zr2P2WxMo1-xO12 (0≤x≤1)的拉曼光谱比较后进而发现,随着x的变化,拉曼谱发生了相应改变,据此,对Zr2P2WxMo1-xO12(0≤x≤1)的拉曼峰进行了具体指认。
4利用快速烧结合成法制备出高纯度的Zr2P2WO12与ZrW2O8的复合陶瓷以及新材料Zr2PVMO12。通过XRD分析发现,在运用了快速冷却技术后,在Zr2P2WO12与ZrW2O8的复合陶瓷中避免了ZrW2O8的分解。
Negative thermal expansion (NTE) materials have been receiving increasing attention for their potential applications in engineering materials with controlled coefficients of thermal expansion (CTE) by compositing them with positive thermal expansion materials. A large family of such materials is tungstates and molybdates with the formula A2M3O12, this type of compounds shows negative thermal expansion behavior only in orthorhombic structure. An interesting feature of these structures is the large chemical flexibility. The A3+ cation can not only be a transition metal or rare earth that occupies an octahedral position, but also be substituted by a mixture of tetravalent and bivalent cations, or by a tetravalent cation with partial replacing of M6+ by quinquevalent cations. Zr2P2MO12 (M=W or Mo) have been reported to maintain orthorhombic structure in a wide temperature range.
Zr2P2MO12 display anisotropic volume NTE in a wide range of temperature (60-300K,122-400K respectively).In this work, a range of Zr2P2WxMo1-xO12(0≤x≤1) and Zr2PVMo12 samples were prepared by the solid state reaction. The structure changes and properties of Zr2P2WxMo1-xO12 were studied by X-ray diffraction and Raman spectroscopy. The ceramic of Zr2P2WO12 and ZrW2O8 were synthetized which can find use as substrates for athermalization of fiber Bragg gratings.The main results obtained are as follows.
1 Zr2P2WxMo1-xO12(0≤x≤1) solid solutions were synthesized by the solid state reaction. The starting compounds of Zr2P2WO12 were sintered at 1200-1400℃for not less than 20min. The starting compounds of Zr2P2MoO12 and Zr2P2WxMo1-xO12 (0 2 The XRD analyses show that all samples maintain orthorhombic structure and contain a network of corner-sharing AO6 octahedra and MO4/PO4 tetrahedra. Raman spectroscopic studies of the samples at different temperatures reveal that there is no phase transition between 20-600℃
3 There are more Raman bands between 1200-1060cm-1 and 760-460cm-1 in the Raman spectra of Zr2P2WxMo1-xO12 compared with the Raman spectra of A2(MO4)3. Raman spectra on the vibrational properties of three kinds of tetrahedra (MoO4, WO4 and PO4 tetrahedra) are discussed by analyzing the difference of the spectra of Zr2P2WxMo1-xO12.
4 Zr2PVMO12 and ceramic composites of Zr2P2WO12 and ZrW2O8 were synthesized by the solid state reactions. The XRD analyses show that the ceramic composites can be prepared by rapid cooling to prevent ZrW2O8 from decomposing into ZrO2 and WO3.
Zr2P2MO12可以在很大的温度范围内保持正交相和负膨胀性能,且不吸水,具有很高的稳定性。但对这类材料的制备方法和性能研究尚处于起步阶段。为此,我们用快速烧结合成法对Zr2P2WxMo1-xO12(0≤x≤1)和Zr2PVMoO12的制备进行了研究,运用XRD和拉曼光谱技术研究其性能,并对这些材料的拉曼光谱进行了分析。作为Zr2P2MO12材料的功能化应用,Zr2P2WO12与ZrW2O8的复合陶瓷可以用来做光纤布拉格光栅的绝热衬底,在本文中用高温快速烧结法制备出Zr2P2WO12与ZrW2O8的复合陶瓷。研究的主要结果和结论如下：
1利用快速烧结合成法在较短的时间内制备出高纯度的Zr2P2WxMo1-xO12(0
3通过对Zr2P2WxMo1-xO12(O≤x≤1)的拉曼光谱分析发现,相对于A2(M04)3材料的拉曼光谱,其在1200-1060cm-1和760-460cm-1之间多出了几个拉曼峰,这是由于PO4的存在引起的。对Zr2P2WxMo1-xO12 (0≤x≤1)的拉曼光谱比较后进而发现,随着x的变化,拉曼谱发生了相应改变,据此,对Zr2P2WxMo1-xO12(0≤x≤1)的拉曼峰进行了具体指认。
4利用快速烧结合成法制备出高纯度的Zr2P2WO12与ZrW2O8的复合陶瓷以及新材料Zr2PVMO12。通过XRD分析发现,在运用了快速冷却技术后,在Zr2P2WO12与ZrW2O8的复合陶瓷中避免了ZrW2O8的分解。
Negative thermal expansion (NTE) materials have been receiving increasing attention for their potential applications in engineering materials with controlled coefficients of thermal expansion (CTE) by compositing them with positive thermal expansion materials. A large family of such materials is tungstates and molybdates with the formula A2M3O12, this type of compounds shows negative thermal expansion behavior only in orthorhombic structure. An interesting feature of these structures is the large chemical flexibility. The A3+ cation can not only be a transition metal or rare earth that occupies an octahedral position, but also be substituted by a mixture of tetravalent and bivalent cations, or by a tetravalent cation with partial replacing of M6+ by quinquevalent cations. Zr2P2MO12 (M=W or Mo) have been reported to maintain orthorhombic structure in a wide temperature range.
Zr2P2MO12 display anisotropic volume NTE in a wide range of temperature (60-300K,122-400K respectively).In this work, a range of Zr2P2WxMo1-xO12(0≤x≤1) and Zr2PVMo12 samples were prepared by the solid state reaction. The structure changes and properties of Zr2P2WxMo1-xO12 were studied by X-ray diffraction and Raman spectroscopy. The ceramic of Zr2P2WO12 and ZrW2O8 were synthetized which can find use as substrates for athermalization of fiber Bragg gratings.The main results obtained are as follows.
1 Zr2P2WxMo1-xO12(0≤x≤1) solid solutions were synthesized by the solid state reaction. The starting compounds of Zr2P2WO12 were sintered at 1200-1400℃for not less than 20min. The starting compounds of Zr2P2MoO12 and Zr2P2WxMo1-xO12 (0
3 There are more Raman bands between 1200-1060cm-1 and 760-460cm-1 in the Raman spectra of Zr2P2WxMo1-xO12 compared with the Raman spectra of A2(MO4)3. Raman spectra on the vibrational properties of three kinds of tetrahedra (MoO4, WO4 and PO4 tetrahedra) are discussed by analyzing the difference of the spectra of Zr2P2WxMo1-xO12.
4 Zr2PVMO12 and ceramic composites of Zr2P2WO12 and ZrW2O8 were synthesized by the solid state reactions. The XRD analyses show that the ceramic composites can be prepared by rapid cooling to prevent ZrW2O8 from decomposing into ZrO2 and WO3.
引文
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[3]Evans J S O, Mary T A, Sleight A W.Negative thermal expansion materials[J] Physica.1998, B:241～243,311～316
[4]Sriraman A K, Tyagi A K. A new method of Fe2(WO4)3 preparation and its thermal stability[J].Thermochimica Acta.2003,406:29-33
[5]Forster P M, Sleight A W. Negative thermal expansion in Y2W3O12[J]International Journal of Inorganic Materials.1999,1:123～127
[6]G Ernst, C Broholm,G R Kowach,et al.Phonon density of states and negative thermal expansion in ZrW2O8[J].Nature.1998,396:147～149
[7]Liang E J,Huo H L, Wang J P, et al. Effect of Water Species on the Phonon Modes in rthorhombic Y2(MoO4)3 Revealed by Raman Spectroscopy[J].J. Phys. Chem.2008 Cl12:6577～6581
[8]Sikka S K.Negative thermal expansion and its relation to high pressures[J].J. Phys.:Condens. Matter,2004,16 S:1033-S1039
[9]Evans J S O,Z Hu,Jorgensen J D,et al.Compressibility,Phase Transitions,and Oxygen Migration in Zirconium Tungstate,ZrW2O8[J].Science,1997,275:61～65
[10]Khosrovani N K,Sleight A W.Structure of ZrV2O7 from-263 to 470℃[J].J Solid State Chem,1997,132:355-360
[11]Seo Dong-Kyun,Whangbo Myung-Hwan. Symmetric Stretching Vibrations of Two-Coor dinate Oxygen Bridges as a Cause for Negative Thermal Expansion in ZrVxP2-xO7 and AW2O8 (A=Zr, Hf) at High Temperature[J].J Solid State Chem,1997,129:163-160
[12]梁源,周鸿颖,梁二军等.负热膨胀材料研究进展[J].无机化学学报,2008,24：1551-1557
[13]严学华,李炳云,程晓农等.先进负热膨胀材料[J].硅酸盐学报,2009,37：653-658
[14]Liang E J, Wang S H, Wu T A,et al. Raman spectroscopic study on the structure, phase transition and restoration of zirconium tungstate blocks synthesized with a CO2 laser[J].J. Raman Spectrosc.2007,38:1186-1192
[15]Simon Allen, J S O Evans, he kinetics of low-temperature oxygen migration in ZrWMoO8[J].J.Mater.Chem.2004,141:51-156
[16]Merkel G A. Negative Thermal Expansion Materials Including Method of Preparation and Uses Therefor[P].US6187700.2001
[17]Agostini G Corvasce F G.Tire with low thermal expansion component[P]. US 2007007 4801.2007
[18]Evans J S. O, David W I F, Sleight A W.Structural investigation of the negative-thermal-expansion material ZrW2O8[J].J.Acta Cryst.1999,B55:333～340
[19]Yanase I,Miyagi M,Kobayashi H. Fabrication of zero-thermal-expansion ZrSi04/Y2W3O12 sintered body[J].Journal of the European Ceramic Society.2009,29:3129 ～ 3134
[20]Marinkovic B J, Ari M, Rizzo F J.Correlation between AO6 Polyhedral Distortion and Negative Thermal Expansion in Orthorhombic Y2Mo3O12 and Related Materials[J].Chem. Mater.2009,21 2886～2894
[21]Liang E J, Huo H L, Wang Z,et al. Rapid synthesis of A2(MoO4)3 (A= Y3+ and La3) with a CO2 laser[J]. Solid State Sciences,2009,11:139～143
[22]Evans J S O, Mary T A, Sleight A W. Negative Thermal Expansion in Sc2(WO4)3[J]. J Solid State Chem,1998,137:148～160
[23]Evans J S O, Mary T A. Structural phase transitions and negative thermal expansion in So2(MoO4)3[J]. International J Inorganic Materials,2000,2:143～151
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