高活性纳米钇铝石榴石的合成及表征
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摘要
YAG多晶陶瓷具有优异的光学性能、良好的力学和热学性能，有望取代YAG单晶成为新一代固体激光基质材料，目前已成为研究的热点。YAG粉体的分散性，烧结性都对最终陶瓷的性能有重要影响，所以粉体制备技术和烧结技术就成为关键因素。目前广泛采用合成YAG的方法如沉淀法、溶胶—凝胶法等虽然可以得到纳米级的粉体，但是却不能解决颗粒的团聚问题，而超临界流体干燥技术(SCFD)能够有效地萃取前驱体中的溶剂，避免表面张力增大引起的物料收缩团聚现象，是一种具有潜力的纳米粉体干燥手段。
本实验拟以目前常用的硝酸钇、硝酸铝为无机源，尿素为沉淀剂的均匀沉淀法和醋酸钇、异丙醇铝为原料的溶胶—凝胶法分别与乙醇、CO_2超临界干燥技术相结合，以期解决YAG粉体制备中的团聚问题，提高粉体的分散性、烧结性能进而改善最终产物的物理化学性能。采用XRD、IR、TG／DSC、TEM、BET等表征手段对产物粉体的晶相组成、结构、相变过程、颗粒形貌及比表面积进行研究。结果表明均匀沉淀法制备的前驱体为结构疏松的钇铝氢氧化物，在900℃生成纯YAG晶相，并随温度升高结晶额更完善。乙醇超临界干燥后的前驱体生成AlO(OH)·xH_2O和[Y_mAl_nO_x(OH)_y·(OC_2H_5)_z]结晶体，烧结过程中发生YAM→YAP→YAG相变化。1200℃煅烧后得到纯YAG相分散性较好且颗粒大小为50-60nm左右。与此相比，CO_2超临界干燥后的前驱体既保持了原有氢氧化物的均匀性又提高了其分散性，并且在较低烧结温度(900℃)直接得到单一的YAG晶相，避免了中间相
Yttrium aluminum garnet (YAG) crystalline ceramic which has excellent optical, mechanical, thermodynamic properties has been widely studied to replace YAG single crystal to be the new solid laser material. The dispersibility and sinterability of YAG powders have important effect to performance of product ceramic, so synthesis and sinter techniques are the key factor of powder preparation. The common ways such as co-precipitaiton, sol-gel, et al. can obtain nano-scaled YAG powders, but severe aggregation is unavoidable. Otherwise, supercritical fluid technique is a potential way for drying nano powders, which can effectively extract the solvent in precursor, avoid aggregation of powders.
In this study, precursors obtained by homogenous precipitation method and sol-gel method were dried by supercritical fluid ethanol drying technology respectively to gain the well-dispersed, high actived powder, moreover improve the optical performance of product. One of YAG precursors was homogenous precipitated from a mixed solution of aluminum and yttrium nitrates using urea as precipitant, while the other precursor was obtained using Y(Ac)3 and isopropyl alcohol aluminum as raw materials. The phase transformation, composition and micro-structural features of the products were characterized by XRD, TG/DSC, BET, IR and TEM techniques. It was found that precursor
本实验拟以目前常用的硝酸钇、硝酸铝为无机源，尿素为沉淀剂的均匀沉淀法和醋酸钇、异丙醇铝为原料的溶胶—凝胶法分别与乙醇、CO_2超临界干燥技术相结合，以期解决YAG粉体制备中的团聚问题，提高粉体的分散性、烧结性能进而改善最终产物的物理化学性能。采用XRD、IR、TG／DSC、TEM、BET等表征手段对产物粉体的晶相组成、结构、相变过程、颗粒形貌及比表面积进行研究。结果表明均匀沉淀法制备的前驱体为结构疏松的钇铝氢氧化物，在900℃生成纯YAG晶相，并随温度升高结晶额更完善。乙醇超临界干燥后的前驱体生成AlO(OH)·xH_2O和[Y_mAl_nO_x(OH)_y·(OC_2H_5)_z]结晶体，烧结过程中发生YAM→YAP→YAG相变化。1200℃煅烧后得到纯YAG相分散性较好且颗粒大小为50-60nm左右。与此相比，CO_2超临界干燥后的前驱体既保持了原有氢氧化物的均匀性又提高了其分散性，并且在较低烧结温度(900℃)直接得到单一的YAG晶相，避免了中间相
Yttrium aluminum garnet (YAG) crystalline ceramic which has excellent optical, mechanical, thermodynamic properties has been widely studied to replace YAG single crystal to be the new solid laser material. The dispersibility and sinterability of YAG powders have important effect to performance of product ceramic, so synthesis and sinter techniques are the key factor of powder preparation. The common ways such as co-precipitaiton, sol-gel, et al. can obtain nano-scaled YAG powders, but severe aggregation is unavoidable. Otherwise, supercritical fluid technique is a potential way for drying nano powders, which can effectively extract the solvent in precursor, avoid aggregation of powders.
In this study, precursors obtained by homogenous precipitation method and sol-gel method were dried by supercritical fluid ethanol drying technology respectively to gain the well-dispersed, high actived powder, moreover improve the optical performance of product. One of YAG precursors was homogenous precipitated from a mixed solution of aluminum and yttrium nitrates using urea as precipitant, while the other precursor was obtained using Y(Ac)3 and isopropyl alcohol aluminum as raw materials. The phase transformation, composition and micro-structural features of the products were characterized by XRD, TG/DSC, BET, IR and TEM techniques. It was found that precursor
引文
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