在很宽的温度范围内，立方ZrW2O8类型化合物为各向同性的热收缩化合物，在许多领域中都有极大的应用前景，但由于其在约430K处存在α相到β相的相变，在一定程度上限制了其应用范围。ZrW2O8化合物的改性可通过掺入其它离子，形成固溶体,其中包括同价离子的取代固溶体和异价离子的取代固溶体。本文合成和表征了Zr1-xDyxW2O8-x/2固溶体，并对合成Zr1-xCexW2O8-y固溶体，进行了初步尝试。(1)用高温固相法合成了Zr1-xDyxW2O8-x/2固溶体，用常温XRD对固溶体进行了表征，证明固溶体在常温下和-ZrW2O8具有相同的立方晶胞结构，空间群为P 213，稀土离子的掺杂没有破坏ZrW2O8特有的晶胞结构，但是导致了结构的畸变，这一点可以从超结构衍射峰310峰的变化中观察到。根据固溶体的相变温度与固溶体浓度的关系，分别运用热机械分析(TMA)测定的升温与降温的相变温度与浓度的关系和晶胞参数与固溶体浓度的关系，确定固溶度分别在(1.84±0.02)mol%，(1.79±0.05)mol%和1.85mol%，三种方法测定的固溶度的结果基本一致。通过X射线衍射(XRD)得出掺杂Dy元素的量和310峰强度呈反比关系，定义了常温饱和有序参数//，来解释固溶体的无序化过程。用SEM和EDX研究了陶瓷体的显微结构和块体中的元素分布，对晶相和第二相进行了详细元素分析及讨论。最后对固溶体的热行为和荧光性质进行了简单的分析。(2) 用燃烧法，酸蒸气水热法和高温固相法合成Zr1-xCexW2O8-y固溶体，对三种合成方法的优劣进行了讨论。并用燃烧法合成样品进行表征，运用差式扫描量热分析方法(DSC)，通过固溶体的相变温度降低不超过10℃，结果证明ZrW2O8晶格中只能掺进很少量的Ce元素。附录里对合成过程的细节进行了叙述，对样品应力的消除做了简单探索。

Cubic ZrW2O8 has been shown to display a character of isotropic negative thermal expansion over a wide temperature range. It has a huge applied prospect. However, the compound has a fundamental demerit for the practical use, because ZrW2O8 undergoes an α-βphase transition. In order to control the phase transition temperature, the solid solution can be made. The Zr of ZrW2O8 can be substituted by the element with the same valence or the different valence.In this paper, Zr1-xDyxW2O8-x/2 solid solutions have been synthesized and characterized. I have also tried to synthesize and characterize Zr1-xCexW2O8-y solid solutions and made a simple characterization.(1) Zr1-xDyxW2O8-x/2 solid solutions have been synthesized by solid-state reaction. The XRD patterns of these solid solutions were indexed using -ZrW2O8 as structural model with its space group P 213. Zr1-xDyxW2O8-x/2 solid solutions substituted by rare earth ion have been kept its original structure, but some structure distortion which can be observed by observing variation of superlattice diffraction peak 310. Phase transition temperature of solid solutions fall measuring by thermo-mechanical analysis (TMA). The broken line of the composition dependence of the phase transition temperature determines the solid solubility which is (1.84±0.02)mol%和(1.79±0.05)mol%. The structure of the solid solutions has been characterized by X-ray diffraction (XRD), then cell parameter calculated determines the solid solubility which keeping consistent with front result according to Vegards law. The amount of Dy element is inverse proportion with intensity of 310 peak, According to it, room temperature saturated order degree  has been defined which can be used to explan disordering of the solid solution. The element distribution block and micro-structure of ceramic body have been made by SEM and EDX. This study explores crystal grain and grain boundary and makes detailed discussion. In the last, the thermal behavior and fluorescence of the solid solution have been simply studied.(2) Zr1-xCexW2O8-y solid solutions have been synthesized by solid-state reaction、combustion method and acid steam hydro-thermal method. The merit and demerit of the three methods have been discussed. Phase transition temperature of the sample synthesized by combustion method fall not exceeding 10℃ measuring by thermo-mechanical analysis (TMA). According to it, we think the solid solubility is very small.The detail of synthetic process and the stress of the sample have been simply studied in the appendix.