CN114192163A - 一种外切36面{110}晶面K离子掺杂SrTiO3纳米光催化剂及其制备方法 - Google Patents
一种外切36面{110}晶面K离子掺杂SrTiO3纳米光催化剂及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种外切36面{110}晶面K离子掺杂SrTiO3纳米光催化剂及其制备方法，属于光催化纳米材料的形貌调控领域，本发明纳米光催化剂为暴露出36面{110}晶面的K离子掺杂SrTiO3，并担载RhCrOx作为析氢助催化剂，CoOOH为析氧助催化剂，K摩尔占比为1%~10%，助催化剂担载量为0.1wt%‑0.5wt%的不同的RhCrOx/K‑SrTiO3/CoOOH复合纳米光催化材料；所述催化剂具有特殊形貌，能实现在紫外—可见光下的光催化反应，在光催化反应中具有很好的催化活性和稳定性，且制备工艺操作简单，反应条件温和，所用试剂价格低廉。
Description
技术领域
本发明属于光催化纳米材料的形貌调控领域，尤其涉及一种外切36面{110}晶面K离子掺杂SrTiO3纳米光催化剂及其制备方法。
背景技术
半导体光催化在温和条件下能促成多类困难的化学反应有利进行，例如光催化降解有机物、光催化合成氨、甲醇及其它高附加值的化工原料，光催化分解水等，这被认为是一种将光子能量转化为化学能的关键技术。由于氢具有较高的燃烧热值和环境友好性，被认为是一种清洁的替代能源，2 mol的水分解可生成2 mol的氢气和1 mol氧气，在以光能源的利用为前提转化成可存储的氢能时，光催化纯水分解技术就以很高的水准可能替代化石燃料的纯粹消耗机制，因而成为研究热门。但是水分解反应是一个热力学上的“爬坡”过程，分解水占用的大比重能耗致使水分解产氢的策略无法大面积投入实际生产。
自从1972年Fujishima和Honda利用金红石型TiO2阳极和铂阴极进行光电化学的水分解以来，人们一直致力于构建高效的多相光催化的研究。到目前为止，已经有大量的半导体光催化剂被研究出来，如硫化物(CdS)、氮化物(Ta3N5)和金属氧化物(TiO2)等。SrTiO3具有简单的立方钙钛矿结构，还原后为n型半导体，禁带宽度为3.2 eV。在研究早期，SrTiO3已经被一些尝试证明可以作为光电极电解水产氢。截至目前，SrTiO3基半导体材料又被证实可在无偏压下转化太阳能进行纯水分解。然而如何促进光生载流子的激发，以及载流子的分离和迁移效率的进一步提高，都是目前该领域研究是重中之重。
因为光催化反应都在材料的表面进行，所以光催化材料的表面结构就直接影响着反应物分子的吸附、光生载流子的转移以及产物分子的脱附，最终影响着光催化材料的催化活性，因此针对光催化材料的晶面调控，特别是合成具有高能晶面暴露的光催化材料成为近年来研究的热点。研究表明，Domen等人合成了无规则的Al-SrTiO3纳米颗粒，暴露出{110}晶面，显著提高了光生电子与空穴的分离效率。但是，其{110}晶面暴露数量有限。
发明内容
本发明提供了一种外切36面{110}晶面K离子掺杂SrTiO3纳米光催化剂及其制备方法，所述催化剂具有特殊形貌，并暴露出36面{110}晶面，能实现在紫外—可见光下的光催化反应，在光催化反应中具有很好的催化活性和稳定性，且制备工艺操作简单，反应条件温和，所用试剂价格低廉。
为实现以上目的，本发明采用以下技术方案：
一种外切36面{110}晶面K离子掺杂SrTiO3纳米光催化剂，所述光催化剂为K离子掺杂SrTiO3，所述K相对于SrTiO3的摩尔占比为1%~10%，且催化剂颗粒形貌共暴露36面{110}晶面，并担载RhCrOx作为析氢助催化剂、CoOOH为析氧助催化剂，所述RhCrOx和CoOOH的担载量为K-SrTiO3的0.5wt%；所述K离子掺杂的SrTiO3纳米立方体的8个顶角和12条棱同时被剪切，暴露出36面{110}晶面。
一种外切36面{110}晶面K离子掺杂SrTiO3纳米光催化剂的制备方法，包括以下步骤：
（1）将定量摩尔比K: Ti为0-0.06的含钾化合物与SrTiO3纳米颗粒均匀球磨混合1~24小时；
（2）将步骤(1)中球磨混合好的含钾化合物和SrTiO3与过量SrCl2均匀混合后，于800-1300℃保温4-12小时；
（3）将步骤(2)高温热处理后的样品洗涤除去多余的SrCl2，干燥后得到K-SrTiO3纳米颗粒；
（4）将步骤(3)合成的K-SrTiO3纳米颗粒与一定量的NaRhCl6和Cr(NO3)3（按各自占K-SrTiO3质量比0.1wt%~0.5wt%）均匀球磨混合1~5小时，于200-800℃保温1-5小时，制得RhCrOx/K-SrTiO3纳米颗粒；
（5）将步骤(4)合成的RhCrOx/K-SrTiO3纳米颗粒分散水中，加入占RhCrOx/K-SrTiO3质量比为0.1wt%~0.5wt%的硝酸钴，300W氙灯光照1-12小时后，过滤洗涤并烘干，制得RhCrOx/K-SrTiO3/CoOOH纳米复合光催化剂。
以上所述步骤中，步骤(1)中所述的含钾化合物为碳酸钾、醋酸钾、硝酸钾、氯化钾中的一种或多种，所述含钾化合物与SrTiO3的摩尔比为n(K): n(Ti)为0-0.06；步骤（3）中得到的K-SrTiO3纳米颗粒尺寸为200-300纳米。
有益效果：本发明提供了一种外切36面{110}晶面K离子掺杂SrTiO3纳米光催化剂及其制备方法，所述K离子掺杂SrTiO3纳米立方体具有特殊形貌，暴露了36面{110}晶面，极大地提高了光生电子与空穴的分离效率，实现在紫外—可见光下的光催化反应，在光催化反应中具有很好的催化活性和稳定性，且制备工艺操作简单，反应条件温和，所用试剂价格低廉。
附图说明
图1是本发明实施例1制得的K-SrTiO3材料的XRD图谱；
图2-3是本发明实施例2制得的K-SrTiO3扫描电镜图；
图4是本发明实施例3制得的RhCrOx/K-SrTiO3/CoOOH光催化水分解活性图；
图5为本发明制得的光催化剂纳米立方体结构示意图；
图6为本发明制得的光催化剂循环测试结果图。
具体实施方式
下面结合附图和具体实施例对本发明进行详细说明：
实施例1
一种外切36面{110}晶面K离子掺杂SrTiO3纳米光催化剂的制备方法，包括以下步骤：
分别称取0.008mol的硝酸钾和0.084mol的SrTiO3，在玛瑙研钵中混合研磨1h，将研磨后的混合物置于球磨机中，4000转速下球磨10h，再加入1mol的SrCl2继续球磨1h。将球磨后的混合物过筛分离，并置于马弗炉中，在800度下保温12小时。取出后用大量去离子水抽滤洗涤，随后将材料置于干燥箱中80度过夜干燥，即得到K-SrTiO3纳米催化剂材料，取0.5gK-SrTiO3纳米颗粒，加入2.5mg的NaRhCl6和2.5mg的Cr(NO3)3，球磨混合1小时，于空气中600度煅烧2小时后，分散于100ml水中，加入2.5mgCo(NO3)2，300W氙灯光照8小时后，过滤洗涤并烘干，制得RhCrOx/K-SrTiO3/CoOOH纳米复合光催化剂。
上述制备得到的K-SrTiO3纳米催化剂材料的XRD图如图1所示，其晶型保持了与SrTiO3相同的钙钛矿型，说明少量金属离子掺杂对其晶型改变影响不大。
实施例2
一种外切36面{110}晶面K离子掺杂SrTiO3纳米光催化剂的制备方法，包括以下步骤：
分别称取0.005mol的硝酸钾和0.09mol的SrTiO3，在玛瑙研钵中混合研磨1h，将研磨后的混合物置于球磨机中，4000转速下球磨24h，再加入1mol的SrCl2继续球磨1h。将球磨后的混合物过筛分离，并置于马弗炉中，在1000度下保温8小时。取出后用大量去离子水抽滤洗涤，随后将材料置于干燥箱中80度过夜干燥，即得到K-SrTiO3纳米催化剂材料，取0.5gK-SrTiO3纳米颗粒，加入1mg的NaRhCl6和2.5mg的Cr(NO3)3，球磨混合1小时，于空气中400度煅烧2小时后，分散于100ml水中，加入1.5mgCo(NO3)2，300W氙灯光照5小时后，过滤洗涤并烘干，制得RhCrOx/K-SrTiO3/CoOOH纳米复合光催化剂。
上述制备得到的K-SrTiO3纳米催化剂材料的扫描电镜图如图2-3所示，纳米立方体的尺寸在200-300纳米，如图5所示，立方体的8个顶角和12条棱边都被剪切，暴露出36面{110}晶面。
实施例3
一种外切36面{110}晶面K离子掺杂SrTiO3纳米光催化剂的制备方法，包括以下步骤：
分别称取0.003mol的硝酸钾和0.095mol的SrTiO3，在玛瑙研钵中混合研磨1h，将研磨后的混合物置于球磨机中，4000转速下球磨24h，再加入1mol的SrCl2继续球磨1h。将球磨后的混合物过筛分离，并置于马弗炉中，在800度下保温8小时。取出后用大量去离子水抽滤洗涤，随后将材料置于干燥箱中80度过夜干燥，即得到K-SrTiO3纳米催化剂材料，取0.5gK-SrTiO3纳米颗粒，加入1.5mg的NaRhCl6和1.5mg的Cr(NO3)3，球磨混合1小时，于空气中500度煅烧2小时后，分散于100ml水中，加入1.5mgCo(NO3)2，300W氙灯光照4小时后，过滤洗涤并烘干，制得RhCrOx/K-SrTiO3/CoOOH纳米复合光催化剂。
将上述得到的RhCrOx/K-SrTiO3/CoOOH纳米催化剂材料用于光催化分解水，光催化水分解测试前，在紫外-可见全光谱照射纯水中测试其光催化水分解性能，催化剂用量为40mg，纯水80ml，光源为300W氙灯，如图4所示，RhCrOx/K-SrTiO3/CoOOH纳米催化剂平均析氢速率为1.94mmol/h，析氧速率为0.95mmol/h，氢氧比接近2：1，如图6所示，在6次循环后仍展现良好的催化活性。
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下还可以作出若干改进，这些改进也应视为本发明的保护范围。
Claims (9)
1.一种外切36面{110}晶面K离子掺杂SrTiO3纳米光催化剂，其特征在于，所述光催化剂为K离子掺杂SrTiO3，所述K摩尔占比为1%~10%，所述光催化剂颗粒形貌共暴露36面{110}晶面。
2.根据权利要求1所述的外切36面{110}晶面K离子掺杂的SrTiO3纳米光催化剂，其特征在于，所述光催化剂担载RhCrOx作为析氢助催化剂、CoOOH为析氧助催化剂；所述RhCrOx和CoOOH的担载量分别为0.5wt%。
3.根据权利要求1所述的外切36面{110}晶面K离子掺杂的SrTiO3纳米光催化剂，其特征在于，所述K离子掺杂的SrTiO3纳米立方体的8个顶角和12条棱同时被剪切，暴露出36面{110}晶面。
4.根据权利要求1或3所述的外切36面{110}晶面K离子掺杂的SrTiO3纳米光催化剂，其特征在于，所述K离子掺杂的SrTiO3纳米颗粒尺寸为200-300纳米。
5.一种外切36面{110}晶面K离子掺杂SrTiO3纳米光催化剂的制备方法，其特征在于，包括以下步骤：
（1）将定量摩尔比的含钾化合物与SrTiO3纳米颗粒均匀球磨混合1~24小时；
（2）将步骤(1)中球磨混合好的含钾化合物和SrTiO3与过量SrCl2均匀混合后，于800-1300℃保温4-12小时；
（3）将步骤(2)高温热处理后的样品洗涤除去多余的SrCl2，干燥后得到K-SrTiO3纳米颗粒；
（4）将步骤(3)合成的K-SrTiO3纳米颗粒与一定量的NaRhCl6和Cr(NO3)3均匀球磨混合1~5小时，于200-800℃保温1-5小时，制得RhCrOx/K-SrTiO3纳米颗粒；
（5）将步骤(4)合成的RhCrOx/K-SrTiO3纳米颗粒分散水中，加入硝酸钴，300W氙灯光照1-12小时后，过滤洗涤并烘干，制得RhCrOx/K-SrTiO3/CoOOH纳米复合光催化剂。
6.根据权利要求5所述的外切36面{110}晶面K离子掺杂SrTiO3纳米光催化剂的制备方法，其特征在于，步骤(1)中所述含钾化合物与SrTiO3的摩尔比为n(K): n(Ti)为0-0.06。
7.根据权利要求5或6所述的外切36面{110}晶面K离子掺杂SrTiO3纳米光催化剂的制备方法，其特征在于，步骤(1)中所述的含钾化合物为碳酸钾、醋酸钾、硝酸钾、氯化钾中的一种或多种。
8.根据权利要求5所述的外切36面{110}晶面K离子掺杂SrTiO3纳米光催化剂的制备方法，其特征在于，步骤(4)中所述NaRhCl6和Cr(NO3)3各自占K-SrTiO3质量比0.1wt%~0.5wt%。
9.根据权利要求5所述的外切36面{110}晶面K离子掺杂SrTiO3纳米光催化剂的制备方法，其特征在于，步骤(5)中所述硝酸钴占RhCrOx/K-SrTiO3质量比为0.1wt%~0.5wt%的硝酸钴。
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