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Rapid synthesis of quasi-spherical (Ba,Sr)TiO3 nanocrystals via a microwave-activated glycothermal approach

机译:微波活化糖热法快速合成准球形(Ba,Sr)TiO3纳米晶体

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摘要

Barium strontium titanate (BST) nanocrystals with quasi-spherical shapes and average particle-sizes ranging from 20 to 80 nm were synthesized without contamination from mineralizers through a microwave-activated glycothermal (MG) approach. The synthesized BST nanocrystals under different MG conditions were structurally characterized by XRD, FESEM, Raman spectroscopy, TEM and HRTEM and investigated with emphasis on the effects of key factors including the microwave irradiation time, 1,4-butanediol/water volume ratio and Ba/(Ba + Sr) molar ratio of the reaction system on the compositions, particle-sizes and morphologies of the BST nanocrystals. It has been found that the nanosized BST crystallites could be rapidly formed under the microwave-glycothermal conditions within an extremely short time (~1 min) via an in situ reaction mechanism, with which the highly dispersed amorphous TiO2 · xH2O colloidal particles might readily be activated to react with the Ba~(2+) and Sr~(2+) ions or their hydrated species and it would be followed by the merging and Ostwald ripening of primarily-formed BST crystallites. The particle size, morphology, composition and crystal structure of as-synthesized BST nanocrystals may be effectively and steadily influenced and, thereby, tailored by the irradiation time, 1,4-butanediol/water volume ratio and Ba/(Ba + Sr) molar ratio of the reaction system through their effects on in situ microwave-powered activation, solubility of reactive species and pH value of reaction medium.
机译:通过微波活化糖热法(MG)合成了具有准球形形状且平均粒径范围为20至80 nm的钛酸锶钡(BST)纳米晶体。用XRD,FESEM,拉曼光谱,TEM和HRTEM对不同MG条件下合成的BST纳米晶体进行了结构表征,并重点研究了微波辐射时间,1,4-丁二醇/水体积比和Ba /反应体系的(Ba + Sr)摩尔比对BST纳米晶体的组成,粒度和形貌的影响。已经发现,通过微波原位反应机理,可以在极短的时间内(约1分钟)内在微波糖热条件下快速形成纳米级BST微晶,从而可以很容易地形成高度分散的非晶TiO2·xH2O胶体颗粒。活化后会与Ba〜(2+)和Sr〜(2+)离子或它们的水合物种发生反应,随后初始形成的BST微晶会合并并发生Ostwald成熟。合成后的BST纳米晶体的粒径,形貌,组成和晶体结构可能受到有效和稳定的影响,并因此受到照射时间,1,4-丁二醇/水体积比和Ba /(Ba + Sr)摩尔的影响反应体系对微波活化的影响,反应物种的溶解度和反应介质的pH值对反应体系的比率的影响。

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