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CN105967722A - 一种Bi4Si3O12多孔材料的制备方法 - Google Patents

一种Bi4Si3O12多孔材料的制备方法 Download PDF

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CN105967722A
CN105967722A CN201610292815.0A CN201610292815A CN105967722A CN 105967722 A CN105967722 A CN 105967722A CN 201610292815 A CN201610292815 A CN 201610292815A CN 105967722 A CN105967722 A CN 105967722A
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伍媛婷
栗梦龙
司楠
王秀峰
刘玲
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Shaanxi University of Science and Technology
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Abstract

本发明公开了一种Bi4Si3O12多孔材料的制备方法，以将硝酸铋、正硅酸乙酯和多种分散剂(乙二胺四乙酸、柠檬酸、二乙烯三胺五羧酸、酒石酸、乙二醇、聚乙二醇等)溶于无水乙醇和去离子水的混合溶液中，使离子均匀存在于分散体系中，再经凝胶化、干燥、干压和热处理过程获得Bi4Si3O12多孔材料；该方法工艺步骤少、设备工艺简单、成本低，所得多孔材料中孔隙分布均匀。

Description

一种Bi4Si3O12多孔材料的制备方法
技术领域
本发明属于材料技术领域，特别涉及一种Bi4Si3O12多孔材料的制备方法。
背景技术
目前在Bi2O3-SiO2系统中发现和研究的化合物晶相主要包括有Bi4Si3O12晶体、Bi12SiO20晶体和Bi2SiO5晶体各相,其中前两种为稳定化合物，后一种为亚稳化合物，其中Bi4Si3O12晶体具有电光、闪烁等性能。多孔材料以其特殊的结构特点，在克服了纳米粉体团聚的问题的同时，使材料本身具有更优越的性能。目前制备多孔材料的方法主要是利用水热法、溶胶-凝胶法、沉淀法等合成粉体后，再利用发泡剂、粘结剂等与粉体进行复配，经成形后制备出多孔块体材料，这些方法的制备周期长且复杂，本专利即针对目前制备多孔材料制备方法的弊端，发明了一种制备周期短而有效的Bi4Si3O12多孔材料制备方法。
发明内容
为了克服上述现有技术的缺点，本发明的目的在于提供一种Bi4Si3O12多孔材料的制备方法，具有生产工艺简单、设备要求简单、周期短的特点。
为了实现上述目的，本发明采用的技术方案是：
一种Bi4Si3O12多孔材料的制备方法，包括如下步骤：
(1)将柠檬酸溶于氨水中搅拌溶解得到柠檬酸溶液，量取1/2的柠檬酸溶液，将正硅酸乙酯溶于其中形成溶液A备用，将硝酸铋溶于剩余柠檬酸溶液中形成溶液B；
(2)将分散剂加至溶液B中，加入无水乙醇搅拌溶解，在不断搅拌下加入溶液A，之后调节pH值至7～9获得溶胶C；
(3)将溶胶C于80～85℃下水浴1～3h至凝胶化，再在140～160℃下干燥形成干凝胶，室温下自然晾干后进行研磨过筛得到干凝胶粉体；
(4)将过筛后的干粉直接干压成型，形成块状坯体材料，最后将块状坯体材料进行热处理得到Bi4Si3O12多孔材料。
所述步骤(1)中，氨水的量以能溶解柠檬酸为准。
所述步骤(1)中，所述正硅酸乙酯和硝酸铋的用量满足Si与Bi的摩尔比为(1:1)～(2:1)，且Si离子与Bi离子之和与柠檬酸的摩尔比为1：(0.5～0.8)。
所述分散剂由乙二胺四乙酸、柠檬酸、二乙烯三胺五羧酸、酒石酸、乙二醇和聚乙二醇组成。
所述分散剂加至溶液B后，分散剂各组份的浓度范围均为0～0.6mol/L。
所述无水乙醇的体积是氨水体积的1～3/2。
所述步骤(4)中，所述热处理是在ZnO粉体中进行埋烧，温度为700℃～800℃。
与现有技术相比，本发明的有益效果是：本发明提供的Bi4Si3O12多孔材料的制备方法中，以乙二胺四乙酸、柠檬酸、二乙烯三胺五羧酸、酒石酸、乙二醇、聚乙二醇等作为分散剂，采用特定的溶胶配制过程，使离子更均匀地存在于凝胶中，凝胶化后，直接经过干燥、压块、热处理等过程获得Bi4Si3O12多孔材料。此过程中通过控制各物质的浓度，特别是各分散剂的种类和用量，配制出适合直接成型的干凝胶粉体，此方法中利用凝胶化过程使铋离子和硅离子均匀稳定地存在于凝胶粉体中，这不仅使硅离子和铋离子能够均匀地存在并按化学计量比获得纯相物质，使晶体结晶过程变得更加均匀，晶体颗粒粒径和分布更均匀，从而使多孔结构中孔隙大小及分布更加均匀，而且使晶粒形成过程和多孔结构形成过程合二为一，缩短制备周期。
具体实施方式
下面结合实施例详细说明本发明的实施方式。
实施例1
一种Bi4Si3O12多孔材料的制备方法，包括如下步骤：
(1)将柠檬酸溶于氨水(体积浓度25％～28％)中，氨水的量以能溶解柠檬酸为准，量取1/2的柠檬酸溶液，将正硅酸乙酯溶于其中形成溶液A备用；将硝酸铋溶于剩余柠檬酸溶液中形成溶液B，其中，Si：Bi(摩尔比)＝1:1，Si离子与Bi离子之和：柠檬酸(摩尔比)＝1：0.5。
(2)称量一定量的分散剂(由乙二胺四乙酸、柠檬酸、二乙烯三胺五羧酸、酒石酸、乙二醇、聚乙二醇组成，其中聚乙二醇又包括聚乙二醇400、聚乙二醇4000和聚乙二醇6000)加入溶液B中，分散剂各组份的浓度控制在0.6mol/L，再加入无水乙醇搅拌溶解(无水乙醇的体积是氨水体积的3/2)，在不断搅拌下将溶液A加入其中，之后调节pH值至7～9即获得溶胶C。
(3)将溶胶C于80℃下水浴1～3h至凝胶化。再在140℃下干燥形成干凝胶，室温下自然晾干后将粉体进行研磨过筛。
(4)将过筛后的干粉直接干压成形，形成块状坯体材料，最后将块状坯体材料在ZnO粉体中进行埋烧即获得Bi4Si3O12多孔材料，热处理温度为800℃。所得Bi4Si3O12多孔材料中为开孔结构，晶粒尺寸约为50nm～150nm，间隙尺寸为50nm～150nm。
实施例2
一种Bi4Si3O12多孔材料的制备方法，包括如下步骤：
(1)将柠檬酸溶于氨水(体积浓度25％～28％)中，氨水的量以能溶解柠檬酸为准，量取1/2的柠檬酸溶液，将正硅酸乙酯溶于其中形成溶液A备用；将硝酸铋溶于剩余柠檬酸溶液中形成溶液B，其中，Si：Bi(摩尔比)＝2:1，Si离子与Bi离子之和：柠檬酸(摩尔比)＝1：0.8。
(2)称量一定量的分散剂(由乙二胺四乙酸、柠檬酸、二乙烯三胺五羧酸、酒石酸、乙二醇、聚乙二醇组成)加入溶液B中，分散剂各组份的浓度控制在0.6mol/L，再加入无水乙醇搅拌溶解(无水乙醇的体积与氨水体积相等)，在不断搅拌下将溶液A加入其中，之后调节pH值至7～9即获得溶胶C。
(3)将溶胶C于85℃下水浴1～3h至凝胶化。再在140℃～160℃下干燥形成干凝胶，室温下自然晾干后将粉体进行研磨过筛。
(4)将过筛后的干粉直接干压成形，形成块状坯体材料，最后将块状坯体材料在ZnO粉体中进行埋烧即获得Bi4Si3O12多孔材料，热处理温度为700℃。所得Bi4Si3O12多孔材料中为开孔结构，晶粒尺寸约为50nm～150nm，间隙尺寸为50nm～150nm。
实施例3
一种Bi4Si3O12多孔材料的制备方法，包括如下步骤：
(1)将柠檬酸溶于氨水(体积浓度25％～28％)中，氨水的量以能溶解柠檬酸为准，量取1/2的柠檬酸溶液，将正硅酸乙酯溶于其中形成溶液A备用；将硝酸铋溶于剩余柠檬酸溶液中形成溶液B，其中，Si：Bi(摩尔比)＝1.5:1的比例，Si离子与Bi离子之和：柠檬酸(摩尔比)＝1：0.6。
(2)称量一定量的分散剂(由乙二胺四乙酸、柠檬酸、二乙烯三胺五羧酸、酒石酸、乙二醇、聚乙二醇组成。)加入溶液B中，分散剂各组份的浓度控制在0.01、0.1、0.1、0.5、0.5、0.6mol/L，再加入无水乙醇搅拌溶解(无水乙醇的体积是氨水体积的3/2)，在不断搅拌下将溶液A加入其中，之后调节pH值至7～9即获得溶胶C。
(3)将溶胶C于885℃下水浴1～3h至凝胶化。再在150℃下干燥形成干凝胶，室温下自然晾干后将粉体进行研磨过筛。
(4)将过筛后的干粉直接干压成形，形成块状坯体材料，最后将块状坯体材料在ZnO粉体中进行埋烧即获得Bi4Si3O12多孔材料，热处理温度为700℃℃。所得Bi4Si3O12多孔材料中为开孔结构，晶粒尺寸约为50nm～150nm，间隙尺寸为50nm～150nm。

Claims (7)

1.一种Bi4Si3O12多孔材料的制备方法，其特征在于，包括如下步骤：
(1)将柠檬酸溶于氨水中搅拌溶解得到柠檬酸溶液，量取1/2的柠檬酸溶液，将正硅酸乙酯溶于其中形成溶液A备用，将硝酸铋溶于剩余柠檬酸溶液中形成溶液B；
(2)将分散剂加至溶液B中，加入无水乙醇搅拌溶解，在不断搅拌下加入溶液A，之后调节pH值至7～9获得溶胶C；
(3)将溶胶C于80～85℃下水浴1～3h至凝胶化，再在140～160℃下干燥形成干凝胶，室温下自然晾干后进行研磨过筛得到干凝胶粉体；
(4)将过筛后的干粉直接干压成型，形成块状坯体材料，最后将块状坯体材料进行热处理得到Bi4Si3O12多孔材料。
2.根据权利要求1所述Bi4Si3O12多孔材料的制备方法，其特征在于，所述步骤(1)中，氨水的量以能溶解柠檬酸为准。
3.根据权利要求1所述Bi4Si3O12多孔材料的制备方法，其特征在于，所述步骤(1)中，所述正硅酸乙酯和硝酸铋的用量满足Si与Bi的摩尔比为(1:1)～(2:1)，且Si离子与Bi离子之和与柠檬酸的摩尔比为1：(0.5～0.8)。
4.根据权利要求1所述Bi4Si3O12多孔材料的制备方法，其特征在于，所述分散剂由乙二胺四乙酸、柠檬酸、二乙烯三胺五羧酸、酒石酸、乙二醇和聚乙二醇组成。
5.根据权利要求4所述Bi4Si3O12多孔材料的制备方法，其特征在于，所述分散剂加至溶液B后，分散剂各组份的浓度范围均为0～0.6mol/L。
6.根据权利要求1所述Bi4Si3O12多孔材料的制备方法，其特征在于，所述无水乙醇的体积是氨水体积的1～3/2。
7.根据权利要求1所述Bi4Si3O12多孔材料的制备方法，其特征在于，所述步骤(4)中，所述热处理是在ZnO粉体中进行埋烧，温度为700℃～800℃。
CN201610292815.0A 2016-05-05 2016-05-05 一种Bi4Si3O12多孔材料的制备方法 Pending CN105967722A (zh)

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