Time-resolved, in situ X-ray diffraction studies of the hydrothermal syntheses of microporous materials
Time-resolved, in situ X-ray diffraction studies of the hydrothermal syntheses of microporous materials
复制标题
微孔材料水热合成的时间分辨原位 X 射线衍射研究
DOI：
10.1016/s1387-1811(98)00009-2
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发表时间：
1998
期刊：
影响因子：
--
通讯作者：
J. Hanson
中科院分区：
文献类型：
--
作者：
D. O′Hare;John S. O. Evans;R. J. Francis;P. Halasyamani;P. Norby;J. Hanson
在本文中，我们描述了使用能量色散衍射使用“白色”同步辐射和角色散x射线衍射与一个移动图像板探测器记录时间分辨在一些水热合成的原位衍射数据。我们研究了在水热条件下合成磷酸铝、开骨架硫化物tma - sn -1和氟磷酸镓ULM-5。考察了反应温度、反应物来源和溶液pH对合成的影响。已有证据表明，在形成结晶tma - sn -1的情况下，在进一步反应形成最终产物之前，反应通过中间无序层状相进行。在ULM-5的合成中至少观察到两个中间体。
In this paper we describe the use of energy dispersive diffraction using ‘white’ synchrotron radiation and angular dispersive X-ray diffraction with a moving image plate detector to record time-resolved in situ diffraction data on a number of hydrothermal syntheses. We have studied the synthesis of an aluminophosphate, the open framework sulfide TMA-SnS-1, and the gallium fluorophosphate ULM-5, under hydrothermal conditions. The effect of varying the temperature of reaction, reactant source and pH of solution on the syntheses has been investigated. Evidence has been obtained that in cases where crystalline TMA-SnS-1 is formed, the reaction proceeds via an intermediate disordered lamellar phase, before reacting further to form the final product. In the synthesis of ULM-5 at least two intermediates have been observed.