CN105967747A - 一种稳态Bi4Si3O12多孔材料的制备方法 - Google Patents
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Abstract
本发明公开了一种稳态Bi4Si3O12多孔材料的制备方法，首先配制柠檬酸的氨水溶液，将氧化铋溶于硝酸中，再分别将氧化铋溶液和正硅酸乙酯溶于柠檬酸的氨水溶液中，加入乙二胺四乙酸、柠檬酸、二乙烯三胺五羧酸、酒石酸、乙二醇、聚乙二醇等分散剂，制备出适合于直接压制成型的干凝胶粉体，经压制成型和热处理，即可获得稳态Bi4Si3O12多孔材料；该方法具有工艺设备简单、制备周期短、成本低等特点。
Description
技术领域
本发明属于材料技术领域，特别涉及一种稳态Bi4Si3O12多孔材料的制备方法。
背景技术
闪烁晶体Bi4Ge3O12在应用中存在价格昂贵、衰减常数较高、光产额较高的问题，而Bi4Si3O12则是Bi4Ge3O12的最佳替代品，其以价格便宜的SiO2替代昂贵的GeO2，大大降低了成本，而且与Bi4Ge3O12相比，其衰减常数(100ns)仅为Bi4Ge3O12的1/3，光产额仅为Bi4Ge3O12的20％，且具有高度的机械和化学稳定性以及优良的发光特性等优点。多孔陶瓷由于其多孔的结构，当孔隙小而分布均匀时，可使多孔陶瓷的比表面积大大增大，活性增强。相比于多孔纳米粉体材料，由于纳米粉体材料的表面断键数较多，比表面积增大，使纳米颗粒间易相互团聚，纳米颗粒越小，则表面活性越大，团聚越严重。如果多孔材料中的细孔分布均匀，则可解决这个问题，且保持了较高的比表面积和表面活性。
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稳态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：
一种稳态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得到柠檬酸溶液A，将氧化铋溶于硝酸中反应形成溶液B；
(2)量取1/2的溶液A，将正硅酸乙酯溶于其中形成溶液C；将溶液B溶于剩余柠檬酸溶液中形成溶液D；
(3)将分散剂加入溶液D中，再加入溶液C和无水乙醇搅拌溶解，之后调节pH值至1～3即获得溶胶E；
(4)将溶胶E于80～85℃下水浴1～2h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；
(5)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稳态Bi4Si3O12多孔材料。
所述步骤(1)中，氨水的量以能溶解柠檬酸为准，硝酸的量以能完全溶解氧化铋为准。
所述正硅酸乙酯和氧化铋的用量满足Bi与Si的摩尔比为(4：3)～(1:1)，且Si离子与Bi离子之和与柠檬酸的摩尔比为1：(0.8～1.5)。
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。
所述分散剂加入溶液D后，分散剂中各组份的浓度范围均为0～0.8mol/L。
所述无水乙醇的体积是氨水体积的2/3～1。
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：本发明提供的稳态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400、聚乙二醇4000、聚乙二醇6000等作为分散剂直接进行络合发泡的凝胶化过程，通过控制各物质的浓度，特别是各分散剂的用量，配制出适合直接成型的干凝胶，这不仅可以减少造粒、陈腐的过程，还可使结晶过程与烧结一步完成。结合埋烧的热处理过程，利用有机物的发泡和分解燃烧过程形成稳态Bi4Si3O12多孔材料。这种方法工艺步骤少、制备周期短、设备简单、成本低，且所得稳态Bi4Si3O12多孔材料的孔隙尺寸及分布可控性好。
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
一种稳态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形成柠檬酸溶液A，氨水的量以能溶解柠檬酸为准；将氧化铋溶于硝酸中反应形成溶液B，硝酸以能完全溶解氧化铋为准。
(2)量取1/2的溶液A，将正硅酸乙酯溶于其中形成溶液C；将溶液B溶于剩余柠檬酸溶液中形成溶液D，其中，Bi：Si(摩尔比)＝4：3，Si离子与Bi离子之和：柠檬酸(摩尔比)＝1：0.8。
(3)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，分散剂各组份的浓度控制在0.8mol/L)加入溶液D中，加入溶液C和无水乙醇搅拌溶解(无水乙醇的体积是氨水体积的2/3)，之后调节pH值至1～3即获得溶胶E。
(4)将溶胶E于80℃下水浴1～2h至凝胶化，然后在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。
(5)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稳态Bi4Si3O12多孔材料，热处理温度为700℃。所得稳态Bi4Si3O12多孔材料中颗粒尺寸约为100nm～200nm，间隙尺寸为50nm～180nm。
实施例2
一种稳态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形成柠檬酸溶液A，氨水的量以能溶解柠檬酸为准；将氧化铋溶于硝酸中反应形成溶液B，硝酸以能完全溶解氧化铋为准。
(2)量取1/2的溶液A，将正硅酸乙酯溶于其中形成溶液C；将溶液B溶于剩余柠檬酸溶液中形成溶液D，其中，Bi：Si(摩尔比)1：1，Si离子与Bi离子之和：柠檬酸(摩尔比)＝1：1.5。
(3)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，分散剂各组份的浓度控制在0.8mol/L。)加入溶液D中，加入溶液C和无水乙醇搅拌溶解(无水乙醇的体积与氨水体积相等)，之后调节pH值至1～3即获得溶胶E。
(4)将溶胶E于85℃下水浴1～2h至凝胶化，然后在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。
(5)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稳态Bi4Si3O12多孔材料，热处理温度为800℃。所得稳态Bi4Si3O12多孔材料中颗粒尺寸约为100nm～200nm，间隙尺寸为50nm～180nm。
实施例3
一种稳态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形成柠檬酸溶液A，氨水的量以能溶解柠檬酸为准；将氧化铋溶于硝酸中反应形成溶液B，硝酸以能完全溶解氧化铋为准。
(2)量取1/2的溶液A，将正硅酸乙酯溶于其中形成溶液C；将溶液B溶于剩余柠檬酸溶液中形成溶液D，其中，Bi：Si(摩尔比)＝4：3，Si离子与Bi离子之和：柠檬酸(摩尔比)＝1：1。
(3)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，分散剂各组份的浓度控制在0.01、0.1、0.1、0.5、0.5、0.8mol/L。)加入溶液D中，加入溶液C和无水乙醇搅拌溶解(无水乙醇的体积是氨水体积的2/3)，之后调节pH值至1～3即获得溶胶E。
(4)将溶胶E于85℃下水浴1～2h至凝胶化，然后在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。
(5)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稳态Bi4Si3O12多孔材料，热处理温度为700℃。所得稳态Bi4Si3O12多孔材料中颗粒尺寸约为100nm～200nm，间隙尺寸为50nm～180nm。
Claims (7)
1.一种稳态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得到柠檬酸溶液A，将氧化铋溶于硝酸中反应形成溶液B；
(2)量取1/2的溶液A，将正硅酸乙酯溶于其中形成溶液C；将溶液B溶于剩余柠檬酸溶液中形成溶液D；
(3)将分散剂加入溶液D中，再加入溶液C和无水乙醇搅拌溶解，之后调节pH值至1～3即获得溶胶E；
(4)将溶胶E于80～85℃下水浴1～2h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；
(5)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稳态Bi4Si3O12多孔材料。
2.根据权利要求1所述稳态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，硝酸的量以能完全溶解氧化铋为准。
3.根据权利要求1所述稳态Bi4Si3O12多孔材料的制备方法，其特征在于，所述正硅酸乙酯和氧化铋的用量满足Bi与Si的摩尔比为(4：3)～(1:1)，且Si离子与Bi离子之和与柠檬酸的摩尔比为1：(0.8～1.5)。
4.根据权利要求1所述稳态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所述稳态Bi4Si3O12多孔材料的制备方法，其特征在于，所述分散剂加入溶液D后，分散剂中各组份的浓度范围均为0～0.8mol/L。
6.根据权利要求1所述稳态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2/3～1。
7.根据权利要求1所述稳态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℃。
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