水热合成不同形态氧化钇的制备工艺及生长机制

Preparation of Yttrium Oxide in Different Forms with Hydrothermal Synthesis and Growth Mechanism

以六水硝酸钇（Y（NO3）3·6H2O）为原料，通过调整沉淀剂（NH3·H2O或CO（NH2）2）、分散剂（C2H6O）或模板剂（C3H8O3），采用水热法制备了3种不同形态的微米级氧化钇颗粒，分析了3种形态氧化钇的生长机制。利用扫描电子显微镜（SEM）、X射线衍射仪（XRD）、能谱（EDS）、透射电子显微镜（TEM）分别对制备过程中的含钇化合物以及含钇氧化物的形态、尺寸与相结构进行表征。实验结果表明：氨水作为沉淀剂与硝酸钇溶液水热反应后生成了棒状Y2NO3（OH）5·1．5H2O，加入丙三醇（C3H8O3）后生成杨桃状Y2（OH）514（NO3）0.86·H2O；以尿素为沉淀剂与硝酸钇和乙醇反应后生成球状Y（OH）CO3。经过煅烧后，3种水热反应产物均转变成为体心立方型Y2O3，其形态分别继承了水热反应产物的棒状、杨桃状和球状形态；Y2O3的晶粒尺寸小，颗粒分布均匀；晶体生长所需能量满足二维生长趋势时形成棒状Y2O3；加入H原子成角度分布的模板剂丙三醇（C3H8O3）形成畅桃状Y2O3；分散剂乙醇（C2H6O）使晶体各个方向均匀生长，形成球状Y2O3。

Using six water yttrium nitrate （Y （NO3 ）3 ·6H2 O） as raw material, three ditterent forms of micron yttrium oxide particles were researched with hydrothermal method by adjusting precipitant （ NH3 · H2O or CO（ NH2 ）2 ）, dispcrsant （ C2H60） or template （ C3 H8O3 ） and growth mechanism on the three forms of yttrium oxide was analyzed. The forms, sizes and phase structures of yttrium compounds and yttrium oxide in the process were investigated by using scanning electron microscopy （SEM）, X-ray diffraction （XRD）, energy spectrum （EDS）, transmission electron microscopy （TEM）. The experimental results showed that yttrium nitrate and ammonia, which acted as precipitant, generated rod like Y2 NO3 （OH）s· 1.5H2O. When adding glycerol, yttrium nitrate and ammonia generated carambola like Y2 （OH）5 .14 （NO3）0.86· H2O. When using urea as precipitating agent, yttrium nitrate and ethanol produced spherical Y （OH）CO3. After calcination, three hydrothermal reaction products were transformed into body centered cubic Y2O3 and the morphology of samples were still rod-like, carambola and the sphere. The grain size of Y2O3 was small and particle distribution was uniform. When the required energy of mystal growth could meet the growth trend of two-dimensional, it formed bar-like Y2O3. When adding template glycerol, in which H atoms distributed in diferent angles, it generated carambola like Y2O3. The dispersant, ethanol （C2H6O） , could make the growth of each side uniform and Y2O3 finally came into being spherical like.