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首页> 外文期刊>Zeitschrift fur Anorganische und Allgemeine Chemie >New phases in the lithiumnitridovanadate system - The solid solution Li7-2xMgx[VN4] with 0 <= x <= 1
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New phases in the lithiumnitridovanadate system - The solid solution Li7-2xMgx[VN4] with 0 <= x <= 1

机译：硝酸铌钒酸锂系统中的新相-固溶体Li7-2xMgx [VN4]的0 <= x <= 1

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摘要

Solid solution phases Li7-2xMgx[VN4] (0 < x less than or equal to 1) with varying Mg-content are obtained as yellow microcrystalline powders from heat treatment of mixtures of VN, Li3N and Mg3N2 or from mixtures of Li-7[VN4] and Mg3N2 at 1370 K in N-2 atmosphere at ambient pressure. At substitution parameter values of x > 0.5 a subsequent distortion from the ideal cubic unit cell to an orthorhombic unit cell is observed. The crystal structure of Li7-2xMgx[VN4] with x approximate to 1 was refined from neutron and X-ray powder diffraction data (space group Pbca, No. 61, a = 963.03(3) pm, b = 958.44(3) pm, c = 951.93(2) pm, neutron pattern 14degrees - 156degrees 2theta, step non-linear approximate to 0.0782degrees 2theta, No. of measured points 1816, R-p = 0.089, R-wp = 0.115, R-Bragg = 0.155, R-F = 0.114; X-ray pattern 10degrees - 98degrees 2theta, step 0.005degrees 2theta, No. of measured points 17600, R-p = 0.028, R-wp = 0.045, R-Bragg = 0.113, R-F = 0.133, structure variables: 45). The crystal structure resembles a Li2O type superstructure with the atomic arrangement of beta-Li-7[VN4] and with two crystallographic Li-sites each substituted by Mg with statistical occupation factors of 0.5. Chemical analyses prove the composition and XAS spectroscopy at the V K-edge support the +5 oxidation state assignment for vanadium. XAS data also support the tetrahedral coordination of vanadium by N as indicated by the structure refinements.
机译：从VN，Li3N和Mg3N2的混合物进行热处理或从Li-7 [[7] [VN4]和Mg3N2在1370 K在N-2气氛中于环境压力下。在x> 0.5的替换参数值下，观察到从理想立方晶胞到正交晶胞的后续变形。从中子和X射线粉末衍射数据（空间群Pbca，No。61，a = 963.03（3）pm，b = 958.44（3）pm，精制了x近似为1的Li7-2xMgx [VN4]的晶体结构。 ，c = 951.93（2）pm，中子模式14度-156度2θ，阶跃非线性近似于0.0782度2θ，测量点数1816，Rp = 0.089，R-wp = 0.115，R-Bragg = 0.155，RF = 0.114; X射线图10度-98度2θ，步距0.005度2θ，测量点数17600，Rp = 0.028，R-wp = 0.045，R-Bragg = 0.113，RF = 0.133，结构变量：45）。晶体结构类似于具有原子排列为β-Li-7[VN4]的Li2O型上层结构，并且具有两个晶体学Li-位，每个Li-位均被Mg取代，其统计占有因子为0.5。化学分析证明，V K边缘的成分和XAS光谱支持钒的+5氧化态分配。 XAS数据还支持钒对钒的四面体配位，如结构改进所示。

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