Phases in the ZrxTa1 –x(O,N)y system, formed by ammonolysis of Zr–Ta gels: preparation of a baddeleyite-type solid solution phase ZrxTa1 –xO1 +xN1 –x, 0≤X≤1
Phases in the ZrxTa1 –x(O,N)y system, formed by ammonolysis of Zr–Ta gels: preparation of a baddeleyite-type solid solution phase ZrxTa1 –xO1 +xN1 –x, 0≤X≤1
复制标题
ZrxTa1 –x(O,N)y 体系中的相，由 Zr–Ta 凝胶氨解形成：斜锆石型固溶体相 ZrxTa1 –xO1 +xN1 –x 的制备，0≤X≤1
DOI：
10.1039/jm9940401293
复制
发表时间：
1994
影响因子：
--
通讯作者：
G. Svensson
中科院分区：
文献类型：
--
作者：
J. Grins;P. Käll;G. Svensson
用溶胶-凝胶法制备了Zr-Ta凝胶，在700 ~ 1000 °C温度范围内，通过氨解反应研究了ZrxTa_（1-x）（O，N）_y体系的相形成。通过X射线粉末衍射（XRPD）、扫描和透射电子显微镜（SEM和TEM）以及热重（TG）分析来表征起始凝胶和观察到的相。在800 °C下制备了ZrxTa 1-xO 1 + xN 1-x（0≤x≤1）的氧氮化物相，具有斜锆石型结构。晶胞体积从TaON（x= 0）的127.8 A3线性增加到ZrO 2（x= 1）的140.9 A3。通过Rietveld精修（RF= 3.5%），使用Cu-Kα1，XRPD数据，验证组成为Zr0.4Ta0.6O1.6N0.4（x= 0.4）的结构。在ZrxTa 1-xO 1 + xN 1-x中，当温度为700 °C，x≤ 0.26 ≤ 0.90时，观察到正交相的氧氮化物相。晶胞参数和粉末X射线反射强度与正交ZrO 2型结构一致。根据X射线数据，在900 °C下对于0.26≤x≤ 0.68制备的材料中存在具有萤石相关亚晶胞的立方固溶体相。电子显微衍射结果表明，该晶体为度规单斜晶系，晶胞参数为a = 6.1 A，B= 14.1 A，c= 7.1 A，β= 125°。的Ta 3 N5，结构类型被发现纳入高达约。在900和1000 °C下的18原子% Zr。
Phase formation in the system ZrxTa1–x(O,N)y has been studied by ammonolysis of Zr-Ta gels, prepared by the sol–gel technique, at temperatures between 700 and 1000 °C. The starting gels and observed phases were characterised by X-ray powder diffraction (XRPD), scanning and transmission electron microscopy (SEM and TEM) and thermogravimetric (TG) analysis. Oxynitride phases of compositions ZrxTa1–xO1 +xN1–x, 0≤x≤1, with the baddeleyite-type structure, were prepared at 800 °C. The unit-cell volume increased linearly from 127.8 A3 for TaON (x= 0) to 140.9 A3 for ZrO2(x= 1). The structure was verified for the composition Zr0.4Ta0.6O1.6N0.4(x= 0.4) by a Rietveld refinement (RF= 3.5%) using Cu-Kα1, XRPD data. An orthorhombic oxynitride phase was observed in preparations at 700 °C for 0.26 ≤x≤ 0.90 in ZrxTa1–xO1+xN1–x. Unit-cell parameters and powder X-ray reflection intensities agree with an orthorhombic ZrO2 type structure. According to X-ray data, a cubic solid solution phase with a fluorite related subcell is present in materials prepared at 900 °C for 0.26≤x≤ 0.68. However, electron microdiffraction patterns suggest a metrically monoclinic unit cell with a = 6.1 A, b= 14.1 A, c= 7.1 A and β= 125°. The Ta3N5, type of structure was found to incorporate up to ca. 18 atom% Zr at 900 and 1000 °C.