CN116173987A - CdIn2S4/CeO2异质结光催化剂及其制备方法和应用 - Google Patents
CdIn2S4/CeO2异质结光催化剂及其制备方法和应用 Download PDFInfo
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Abstract
本发明涉及一种硫化铟镉/氧化铈异质结光催化剂的制备及其在光催化分解水产氢方面的应用。该催化剂首先通过水热法和煅烧法两步反应合成了氧化铈，再将一定质量百分比的氧化铈加入到水热合成硫化铟镉的反应过程中，制得了硫化铟镉/氧化铈异质结光催化剂。该方法制备的异质结光催化剂拓宽了材料的光响应范围，提高了光吸收强度和太阳能利用率，有效的抑制了光生载流子的复合，且该制备过程成本低，简便可控，绿色环保。将所述催化剂进行光催化分解水产氢研究具有高效的催化活性，在光催化领域具有较高的应用前景。
Description
技术领域
本发明属于复合材料光催化分解水制氢领域，具体涉及一种硫化铟镉/氧化铈光催化分解水制氢功能的光催化剂；还涉及所述催化剂的制备及在光催化制氢方面的应用。
背景技术
社会工业化给我们带来经济效益的同时，也引发了一系列能源枯竭和环境污染问题，这就需要我们建设一个可持续发展的生态文明系统，将能源布局向新能源倾斜。光催化制氢技术利用太阳能作为驱动力来分解水制氢，将取之不尽用之不竭的太阳能转化为清洁、无污染、易储藏和运输的氢能，被认为是解决能源危机的理想方案。近年来，科学家们一直致力于研究稳定、高效率的光催化剂。
二氧化铈(CeO2)是稀土元素氧化物中最活跃的一种，它具有丰富的氧缺陷以及较高的储氧释放能力，最重要的是铈的氧化态可以在Ce3+和Ce4+之间转换，这有利于的电子的转移，从而使其成为热门的光催化材料。然而纯相的CeO2因其带隙比较宽，光吸收能力有限，载流子的复合效率高导致其在在实际应用中的光催化效率并不高。为了解决这些问题，需要设计将其与它材料复合，制备异质结复合材料可加快电荷传输，有效抑制光生电子和空穴对复合，拓宽光响应范围从而提高光催化活性。
硫化铟镉(CdIn2S4)属于三元硫化物，是一种n型半导体，因其带隙合适(2.1eV)被广泛应用于光催化降解有机污染物和分解水制氢领域。CdIn2S4可以吸收可见光，稳定性好，且它的比表面积较大可以提供更多的活性位点。然而，光生空穴与电子的高复合速率和光腐蚀限制了其在光催化中的发展。目前已经构建了多种策略来提高CdIn2S4的光催化性能，如：构建异质结、形貌调控以及掺杂等策略。
为了设计制备新型稳定具有高可见光响应的光催化剂，本发明首先以硝酸铈和氢氧化钠为原料利用水热法和煅烧法制备氧化铈微米花光催化剂，再以硝酸镉、硝酸铟和硫代乙酰胺为原料利用水热法制备硫化铟镉光催化剂，最后在制备硫化铟镉的过程中加入一定量的制备好的氧化铈微米花来获得CdIn2S4/CeO2异质结光催化剂。目前采用此方法制备CdIn2S4/CeO2异质结光催化剂及该催化剂用于光催化分解水产氢的研究还未见报道。该方法制备的所述光催化剂不仅拓宽了光吸收范围，而且有效抑制了光生电子和空穴的复合，在光催化过程中表现出显著提高的光催化分解水产氢活性。对解决能源危机的问题具有很重要的理论指导和实际意义。
发明内容
本发明的目的之一是提供一种CdIn2S4/CeO2异质结光催化剂。本发明首先以硝酸铈和氢氧化钠为原料利用水热法和煅烧法制备氧化铈微米花光催化剂，再以硝酸镉、硝酸铟和硫代乙酰胺为原料利用水热法制备硫化铟镉光催化剂，最后在制备硫化铟镉的过程中加入一定量的制备好的氧化铈微米花来获得CdIn2S4/CeO2异质结光催化剂。本发明的目的之二就是提供一种CdIn2S4/CeO2异质结光催化剂的制备方法，具体包括以下步骤：
1.CeO2的制备
(1)称取1.736g Ce(NO3)3和1.8g NaOH分别溶入30ml去离子水中，磁力搅拌至充分溶解，随后将两溶液混合搅拌均匀；
(2)将(1)中混合好的溶液转移至100mL高压反应釜中100℃反应12h，反应结束后用乙醇和水反复洗涤数次，60℃真空干燥12h；
(3)将(2)中所得产物置于马弗炉中，升温至400℃煅烧4小时，得到CeO2粉末；
2.CdIn2S4的制备
(1)称取0.4～1mmol硝酸镉、0.8～2mmol硝酸铟分散到30ml去离子水中，磁力搅拌至充分溶解，得到无色透明溶液；
(2)称取3.2～8mmol硫代乙酰胺分散到溶液(1)中，磁力搅拌至完全溶解，后继续剧烈搅拌30min得无色透明溶液；
(3)将(2)的溶液转移至50mL高压反应釜中，160℃反应10小时，反应结束后用乙醇和水反复洗涤数次，60℃真空干燥箱12个小时获得CdIn2S4；
3.CdIn2S4/CeO2异质结光催化剂的制备
(1)称取0.0752～0.1504g制备好的CeO2分散到2(2)的溶液中，磁力搅拌至完全溶解；
(2)将(1)中搅拌好的溶液转移至50ml高压反应釜中160℃下反应10h,用乙醇和水反复洗涤数次，60℃真空干燥12h，得到CdIn2S4/CeO2复合异质结光催化剂,记作CISC-x，其中x表示CeO2与CdIn2S4的质量百分比。
本发明目的之三是提供一种CdIn2S4/CeO2异质结光催化剂在光催化分解水析氢方面的应用。
附图说明
图1为实施例1所得CeO2的扫描电镜图(a)；CdIn2S4的扫描电镜图(b)；CdIn2S4/CeO2的扫描电镜图(c)和高分辨透射电镜图(d)。
图2为实施例2所得CdIn2S4/CeO2异质结光催化剂的产氢速率。
具体实施方式：
为进一步理解本发明，下面以实施例对本发明作进一步说明，但并不以任何方式限制本发明。
实施例1
(a)CeO2的制备
(1)称取1.736g Ce(NO3)3和1.8g NaOH分别溶入30ml去离子水中，磁力搅拌至充分溶解，随后将两溶液混合搅拌均匀；
(2)将(1)中混合好的溶液转移至100mL高压反应釜中100℃反应12h，反应结束后用乙醇和水反复洗涤数次，60℃真空干燥12h；
(3)将(2)中所得产物置于马弗炉中，升温至400℃煅烧4小时，得到CeO2粉末，如图1(a)所示；
(b)CdIn2S4的制备
(1)称取0.4mmol硝酸镉、0.8mmol硝酸铟分散到30ml去离子水中，磁力搅拌至充分溶解，得到无色透明溶液；
(2)称取3.2mmol硫代乙酰胺分散到溶液(1)中，磁力搅拌至完全溶解，后继续剧烈搅拌30min得无色透明溶液；
(3)将(2)中的溶液转移至50ml高压反应釜中160℃反应10小时，反应结束后用乙醇和水反复洗涤数次，60℃真空干燥箱12个小时获得CdIn2S4，如图1(b)所示；
(c)CdIn2S4/CeO2异质结光催化剂的制备
(1)称取0.1128g制备好的CeO2分散到(b)中(2)的溶液，磁力搅拌至完全溶解；
(2)将(1)中搅拌好的溶液转移至50ml高压反应釜中160℃下反应10h,用乙醇和水反复洗涤数次，60℃真空干燥12h，得到CdIn2S4/CeO2异质结光催化剂,记作CISC-60，如图1(c)和1(d)所示；
实施例2
(a)CeO2的制备
按照实施例1中步骤(a)的方法和条件制备；
(b)CdIn2S4的制备
按照实施例1中步骤(b)的方法和条件制备；
(c)CdIn2S4/CeO2异质结光催化剂的制备
按照实施例1中步骤(c)的方法和条件制备；
(d)光催化制氢应用评价
光催化剂制氢性能测试用光催化活性评价系统测试，具体实验步骤如下所述：
10mg CdIn2S4/CeO2异质结光催化剂分散于100mL含有15％三乙醇胺作为牺牲剂的蒸馏水中，超声、搅拌，使反应器底部的催化剂完全分散均匀，反应器两端连接至恒温循环水泵以测试过程中反应温度始终保持在6℃左右。使用装有420nm截止滤光片的300W Xe灯提供照射光源。光催化反应开始前，打开循环氩气和气相色谱，将反应器接入在线分析系统，随后打开真空泵，将反应体系抽真空直到溶液中没有大的气泡冒出，然后打开氙灯。在氙灯照射下催化反应5小时，每隔一个小时，气相色谱仪自动分析并记录氢气的峰面积，根据峰面积和产氢时间计算氢气析出速率，如图2所示。
Claims (4)
1.一种硫化铟镉/氧化铈异质结光催化剂的制备，其特征在于该催化剂首先通过水热法和煅烧法两步制备了氧化铈，再将不同质量百分比的氧化铈加入到硫化铟镉的合成过程中，实现了将两种材料复合形成异质结催化剂。
所述的异质结光催化剂的制备方法，其特征在于：步骤如下：
(a)CeO2的制备
(1)称取1.736g Ce(NO3)3和1.8g NaOH分别溶于30ml去离子水中，磁力搅拌至充分溶解，随后将两溶液混合搅拌均匀；
(2)将(1)中混合好的溶液转移至100mL高压反应釜中100℃反应12h，反应结束后用乙醇和水反复洗涤数次，60℃真空干燥12h；
(3)将(2)中所得固体至于马弗炉中，升温至400℃煅烧4小时，得到CeO2；
(b)CdIn2S4的制备
(1)称取0.4～1mmol硝酸镉、0.8～2mmol硝酸铟分散到30ml去离子水中，磁力搅拌至充分溶解，得到无色透明溶液；
(2)称取3.2～8mmol硫代乙酰胺分散到溶液(1)中，磁力搅拌至完全溶解，后继续剧烈搅拌30min得无色透明溶液；
(3)将(2)的溶液转移至50mL高压反应釜中，160℃反应10小时，反应结束后用乙醇和水反复洗涤数次，60℃真空干燥箱12个小时获得CdIn2S4；
(c)CdIn2S4/CeO2异质结光催化剂的制备
(1)称取0.0752～0.1504g制备好的CeO2分散到b(2)的溶液中，磁力搅拌至完全溶解；
(2)将(1)中搅拌好的溶液转移至50ml高压反应釜中160℃下反应10h,用乙醇和水反复洗涤数次，60℃真空干燥12h，得到CdIn2S4/CeO2异质结光催化剂。
2.根据权利要求1中所述的制备方法，其特征在于步骤(b)中硝酸镉的用量为0.4mmol；硝酸铟的用量为0.8mmol，硫代乙酰胺的用量为3.2mmol。
3.根据权利要求1中所述的制备方法，其特征在于步骤(c)中CeO2的用量为0.1128g。
4.根据权利要求1所述的制备方法得到的CdIn2S4/CeO2异质结光催化剂，其特征在于所述催化剂用于光催化产氢，表现出显著提高的光催化产氢活性。
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