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Preparation of highly oriented thin films of organo-LDH(layered double hydroxide) hybrids

有机-LDH（层状双氢氧化物）杂化物高取向薄膜的制备

基本信息

批准号：
18550185
负责人：
NOBUO Iyi
金额：
$ 1.96万
依托单位：
National Institute for Materials Science
依托单位国家：
日本
项目类别：
Grant-in-Aid for Scientific Research (C)
财政年份：
2006
资助国家：
日本
起止时间：
2006 至 2007
项目状态：
已结题

项目摘要

The aim of this study is to develop new synthetic routes to the highly oriented thin films of organic-LDH (layered double hydroxide) hybrids. In the FY 2006, the oriented LDH films with anion-exchangeability were prepared from the starting CO_3^<2->LDH (a) by casting a CO_3^<2->LDH water suspension onto a glass slide, followed by decarbonation in an HC1/NaC1 solution and anion-exchange to C1O_4LDH, and (b) by casting delaminated C1O_4LDH in formamide (FA) onto a glass slide. These C1O_4LDH films formed on glass substrates were further anion-exchanged by p-toluenesulfonate anions (Tos) to produce organic-LDH hybrid films with retention of their orientation and transparency. The direct delamination of TosLDH in FA was also successfully conducted, and a highly-oriented TosLDH hybrid film was obtained by casting the colloidal TosLDH solution on a glass slide. These three procedures offered well-oriented organic-LDH films, and especially, the process involving the delamination treatments gave more dense and transparent films.In the FY 2007, we elaborated the elemental techniques necessary for LDH-film preparation (1) preparation of highly crystalline homogeneous LDH crystals, (2) refinement of decarbonation method, and (3) development of new methods for LDH delamination. As for (1), it became possible to control the size of LDH crystals by controlling the amount of hexamethylenetetramine in the homogeneous preparation method. As for (2), by using acetate buffer/NaC1 mixed solution instead of HC1/NaC1 solution, the decarbonation of LDHs could be conducted in milder conditions, and decarbonation took place in more homogeneous way. As for the nano-sheet preparation, nobel LDH hybrids which delaminate in water were synthesized, and because of the affinity of the LDH colloidal suspensions to the substrates such as glass, the oriented thin films could be obtained more easily. And furthermore, self standing film of the LDH hybrids could be obtained successfully.

本研究的目的是开发新的合成路线，以高度取向的有机-LDH（层状双氢氧化物）杂化薄膜。在2006财年，以CO_3^ LDH为起始原料<2->，通过（a）将CO_3 ^<2->LDH水悬浮液浇铸到载玻片上，然后在HCl/NaCl溶液中脱碳酸并阴离子交换为ClO_4 LDH，以及（B）将脱层的ClO_4 LDH在甲酰胺（FA）中浇铸到载玻片上，制备了具有阴离子交换的定向LDH膜。在玻璃基片上形成的C1O_4LDH膜进一步用对甲苯磺酸阴离子（Tos）进行阴离子交换，得到了保持取向性和透明性的有机-LDH杂化膜。TosLDH在FA中的直接分层也成功地进行，并且通过将胶体TosLDH溶液浇铸在载玻片上获得高度取向的TosLDH杂化膜。这三个步骤提供了良好的定向有机LDH膜，特别是，涉及分层处理的过程中，得到了更致密和透明的膜。在2007财年，我们详细阐述了LDH膜制备所需的基本技术（1）制备高度结晶的均质LDH晶体，（2）改进脱碳方法，（3）开发新的LDH分层方法。对于（1），在均相制备方法中，通过控制六亚甲基四胺的量可以控制LDH晶体的尺寸。对于（2），用醋酸盐缓冲液/NaCl混合溶液代替HCl/NaCl溶液，可以使LDH的脱碳酸反应在较温和的条件下进行，且脱碳酸反应更均匀。在纳米片的制备方面，合成了在水中分层的nobel LDH杂化物，并且由于LDH胶体悬浮液对玻璃等基底的亲和性，可以更容易地获得取向薄膜。并成功地获得了LDH杂化物的自支撑膜。