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AlPO_4-18 synthesized from colloidal precursors and its use for the preparation of thin films

机译：由胶体前体合成的AlPO_4-18及其在薄膜制备中的应用

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摘要

Nanosized AlPO_4-18 is synthesized from clear precursor solutions; a complete transformation from amorphous to crystalline colloidal particles is observed after 60, 20 and 18 h at 100, 150, and 170℃, respectively. The evaluation of the long-range ordering of nanocrystals as a function of crystallization time was followed by X-ray diffraction and dynamic light scattering. The time-dependent ~(27)Al NMR measurements in the liquid phase before and after purifications with different crystallization times show that the tetrahedrally coordinated Al is formed at RT prior to hydrothermal treatment indicating the formation of crystalline phase. The mean hydrodynamic radius of the amorphous aluminophosphate entities and the crystalline AlPO_4-18 particles does not change during the entire process of crystal growth. Further these AlPO_4-18 nanocrystals were employed for the preparation of thin films on silicon wafers via spin coating of stable AlPO_4-18/EtOH solutions, and additional crystal growth of the seeded layers at elevated temperature was carried out. The structural evolution of the thin films was studied with grazing incidence diffraction using synchrotron X-ray radiation. The orientation of growing crystals is governed by the preferred orientation of the seeded particles deposited by spin coating approach.
机译：纳米AlPO_4-18由透明的前体溶液合成；分别在100、150和170℃60、20和18 h后观察到从非晶态到结晶态胶体粒子的完全转变。通过X射线衍射和动态光散射来评估纳米晶体的长程有序性与结晶时间的关系。在具有不同结晶时间的纯化之前和之后，液相中随时间变化的〜（27）Al NMR测量表明，在水热处理之前，RT形成了四面体配位的Al，表明形成了晶相。在整个晶体生长过程中，无定形铝磷酸盐实体和结晶AlPO_4-18颗粒的平均流体动力学半径不会改变。此外，这些AlPO_4-18纳米晶体用于通过稳定的AlPO_4-18 / EtOH溶液的旋涂在硅片上制备薄膜，并在高温下对晶种层进行了额外的晶体生长。使用同步加速器X射线辐射，通过掠入射衍射研究了薄膜的结构演变。生长晶体的取向取决于通过旋涂方法沉积的种子颗粒的优选取向。

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