高压合成新型ZnO水合物及其红外与拉曼光谱

High Pressure Synthesis of a New Zinc Oxide Hydrate and its IR and Raman Spectroscopy

在六面顶高压装置中用ZnO和水于5.5 GPa压力下合成了一种名义分子式为ZnO.3Zn（OH）2的新的ZnO水合物晶体,并确定了该水合物的单相生成条件。SEM形貌分析表明所得化合物均为长10-20μm,直径5μm左右规则的棒状单晶。用粉末X射线衍射数据确定其晶体结构,结果表明,该晶体属于单斜晶系,C2/M空间群,晶胞参数为a=0.608 7 nm,b=0.967 5nm,c=0.311 2 nm,α=90.00°,β=119.51°,γ=90.00°,V=0.159 5 nm3。通过DSC-TGA、IR和Raman光谱分析确定了其中的含水量和存在形式,实验结果显示该水合物中约含14%的结晶水,结晶水全部以[OH]^-1的形式存在。

A new kind of zinc oxide hydrate with nominal formula ZnO · 3Zn （OH）2 was synthesized under 5.5 GPa in a cubic anvil high pressure apparatus and the single phase synthesis condition was also determined. The SEM analysis found that the compound formed stick--like crystals with length of 10-20 um and average diameter of about 5 um. The crystal structure was tentatively resolved by means of powder X- ray diffraction data. This compound crystallized in a monoclinic space group C2/M with a=0. 608 7 nm, b= 0. 967 5 nm, c=0. 311 2 nm, α=90. 00°, β=119.51°, γ=90.00°, V=0. 159 5 nm^3. The amount and existing format of water in this new ZnO hydrate were analyzed using DSC--TGA, IR and Raman spectroscopy. The results indicated that 14%wt of water was contained in this material and existed only in the form of [OH-]^-1.