CN111495365A - 一种新型n-Cu2O/CuO半导体光催化剂的制备方法 - Google Patents
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Abstract
本发明涉及一种新型n‑Cu2O/CuO半导体光催化剂的制备方法,属于无机金属功能材料领域。首先采用水热法合成了Cu2O/CuO复合材料,在反应结束后放入马弗炉内进行了退火处理。Cu2O/CuO复合材料中Cu2O的含量可以通过改变乙醇的量来实现合理调控。通过本发明,以高纯度Cu(NO3)·3H2O(≥99.5%),NH3和无水乙醇为原料,采用水热法,通过对原料称量、搅拌,水热制备,干燥等步骤,最终制备得到一种新型n‑Cu2O/CuO半导体光催化剂,制备方法简单周期短,合成成本低廉且易于大量生产。
Description
技术领域
本发明涉及一种新型n-Cu2O/CuO半导体光催化剂的制备方法,属于无机金属功能材料领域。
背景技术
由于化石燃料污染严重且其资源有限,开发新能源已经迫在眉睫。氢气作为一种可再生且绿色环保的运输和便携式能源载体,已经受到了广泛的关注。然而找到可靠且可持续的制氢方法目前仍然是一个巨大的挑战。各项研究工作都致力于开发一种高效的制氢工艺,而在众多的研究方法中,光电化学(PEC)裂解水被认为是最可持续和最有前途的方法。PEC装置只需要半导体电极、水和太阳光即可,将太阳能转化为化学能不仅可以减少碳排放,还可以提高能源供应的安全性。在PEC器件中,半导体光电极材料是关键所在,因为它的作用是吸收太阳光并产生电子-空穴对。而一般来说,合理的能带排布和有效的载流子分离是选择电极材料的主要标准。考虑到价格和可持续性等因素,最好使用低成本的过渡金属来改善PEC性能。在这些过渡金属半导体材料中,铜氧化物由于其制造成本低、光学带隙和电导率适中,被认为是最具前景的一种PEC裂解水光催化剂,并且目前也有许多报道证实了铜在PEC水裂解方面确实比贵金属有优势。氧化铜(CuO)和氧化亚铜(Cu2O)是铜氧化物的两种主要类型,这两种相均可用于PEC水裂解。Cu2O和CuO是非常常见的p型半导体材料,带隙分别为2.1eV和1.7eV。但有趣的是,Cu2O在p型和n型之间可以表现出可调谐的半导体特性,p型特性是由铜空位引起,其受主能级在0.45-0.55eV之间,而n型特性则是由氧空位引起,施主能级为0.38eV。特别是铜的价态可以在Cu2O和CuO之间发生热力学变化,为Cu2O/CuO二元结构的组装提供了可能,从而使形成的异质结具有更高的催化性能。半导体异质结是提高PEC性能的一种有效方法,因为其特殊的能带排布可以有效地减少载流子的复合。然而,由于合成方法的限制,制备这种Cu2O/CuO纳米结构的研究很少,且已报道的方法往往都比较复杂,如自旋镀膜、电化学沉积、溅射沉积以及改变退火温度或气氛。Yang等人采用重复双电位脉冲计时安培(r-DPPC)方法合成Cu2O/CuO双层复合材料来作为光电阴极,而在另一项研究中通过调整300~400℃的不同退火温度,在ITO基体上对Cu进行热氧化使之在ITO基体上形成纳米结构的Cu2O/CuO络合物薄膜,然而目前报道的方法大多都难以实现合理的调控。此外,目前广泛报道的CuxO复合材料为p-Cu2O/CuO异质结,采用n-Cu2O/CuO异质结来作为光电阴极用于PEC水裂解的研究却很少。
所以在这里我们报道一种新型n-Cu2O/CuO半导体光催化剂的制备方法,简便且快速的水热合成方法。与常规方法不同的是,可以通过改变溶剂中乙醇的含量来合理地调控CuxO复合材料中Cu2O的含量。乙醇作为一种软还原剂,在缓慢的反应过程中为CuO转化为Cu2O提供了可能。
发明内容
本发明的目的在于提出了一种新颖、简便的方法,合成了稳定、高效的铜氧化物复合光电阴极材料用于PEC裂解水。提供一种具有优秀稳定性能,合成成本低、制备工艺简单的一种新型n-Cu2O/CuO半导体光催化剂的制备方法。采用水热法首先合成p型CuO纳米片,然后通过调节中乙醇溶液浓度,在p型CuO纳米片上生长具有30nm左右的n-Cu2O纳米颗粒,形成p-n结。测量发现CuO、Cu2O形成的p-n结为II-型半导体异质结,在光照下增加了光生载流子的分离,形成的耗尽层延长了载流子的寿命,因此具有较高的光电流。PEC测试结果显示n-Cu2O/CuO异质结构的光电流比纯相CuO提升了两倍,最高的光电流密度达150μA。
本发明的目的是这样实现的,一种新型n-Cu2O/CuO半导体光催化剂的制备方法,其特征在于,包括如下步骤:
(1)将FTO分别放入丙酮、乙醇和去离子水中超声10min去除其表面的油污和杂质,然后对FTO干燥待用;
(2)称量1g的Cu(NO3)·3H2O,在1g的Cu(NO3)·3H2O加入30mL去离子水搅拌至完全溶解,得到拌均匀的第一溶液;
(3)用移液枪在搅拌均匀的第一溶液中加入1.5ml NH3,搅拌均匀,得到第二溶液;
(4)充分反应后将该配置好的第二溶液移入反应釜中,将干燥后的FTO倾斜放入第二溶液中,在200℃烘箱中反应6-12h;
(5)在反应釜降至室温后将FTO取出用去离子水冲洗,干燥后移入马弗炉在300℃温度下退火2h,得到一种新型n-Cu2O/CuO半导体光催化剂。
步骤(1)中,FTO的尺寸为1×1cm。
步骤(2)中,用电子天平称量1g原料Cu(NO3)·3H2O,用量筒量取30mL去离子水,量筒在使用前用超声清洗机清洗干净。
采用X射线衍射仪(XRD)对样品进行物相结构分析;采用扫描电子显微镜(SEM)观察制备化合物样品的表面形貌进行性能表征。
本发明提出了一种新颖、简便的方法,合成了稳定、高效的铜氧化物复合光电阴极材料用于PEC裂解水。该方法分为两步,首先我们采用水热法合成了Cu2O/CuO复合材料,在反应结束后放入马弗炉内进行了退火处理。值得一提的是,Cu2O/CuO复合材料中Cu2O的含量可以通过改变乙醇的量来实现合理调控。
综上,本发明公开了一种新型n-Cu2O/CuO半导体光催化剂的制备方法。以高纯度Cu(NO3)·3H2O(≥99.5%),NH3和无水乙醇为原料,采用水热法,通过对原料称量、搅拌,水热制备,干燥等步骤,最终制备得到一种新型n-Cu2O/CuO半导体光催化剂,制备方法简单周期短,合成成本低廉且易于大量生产。
附图说明
图1为本发明一种新型n-Cu2O/CuO半导体光催化剂的XRD图谱。
图2为本发明一种新型n-Cu2O/CuO半导体光催化剂的SEM图谱。
图3为本发明一种新型n-Cu2O/CuO半导体光催化剂的UV图谱。
图4为本发明一种新型n-Cu2O/CuO半导体光催化剂的光电流图谱。
具体实施方式
本实验所用原料为:Cu(NO3)·3H2O(分析纯),NH3和无水乙醇水热法制备一种新型n-Cu2O/CuO半导体光催化剂,下面结合实例对本发明作进一步的描述。
实施例1
(1)将1×1cm的FTO分别放入丙酮、乙醇和去离子水中超声10min去除其表面的油污和其他杂质;
(2)用电子天平称量1g原料Cu(NO3)·3H2O,用量筒量取28mL去离子水和2ml无水乙醇,在Cu(NO3)·3H2O加入去离子水搅拌至完全溶解;量筒使用前用超声清洗机清洗干净;
(3)用移液枪在搅拌均匀的溶液中加入1.5ml NH3,搅拌均匀;
(4)充分反应后将该配置好的溶液移入反应釜中,将干燥后的FTO以一定角度倾斜放入溶液中,在200℃烘箱中反应6-12h;
(5)在反应釜降至室温后将FTO取出用去离子水冲洗,干燥后移入马弗炉在300℃温度下退火2h,得到一种新型n-Cu2O/CuO半导体光催化剂。
实施例2
(1)将1×1cm的FTO分别放入丙酮、乙醇和去离子水中超声10min去除其表面的油污和其他杂质;
(2)用电子天平称量1g原料Cu(NO3)·3H2O,用量筒量取25mL去离子水和5ml无水乙醇,在Cu(NO3)·3H2O加入去离子水搅拌至完全溶解;量筒使用前用超声清洗机清洗干净;
(3)用移液枪在搅拌均匀的溶液中加入1.5ml NH3,搅拌均匀;
(4)充分反应后将该配置好的溶液移入反应釜中,将干燥后的FTO以一定角度倾斜放入溶液中,在200℃烘箱中反应6-12h;
(5)在反应釜降至室温后将FTO取出用去离子水冲洗,干燥后移入马弗炉在300℃温度下退火2h,得到一种新型n-Cu2O/CuO半导体光催化剂。
实施例3
(1)将1×1cm的FTO分别放入丙酮、乙醇和去离子水中超声10min去除其表面的油污和其他杂质;
(2)用电子天平称量1g原料Cu(NO3)·3H2O,用量筒量取22mL去离子水和8ml无水乙醇,在Cu(NO3)·3H2O加入去离子水搅拌至完全溶解;量筒使用前用超声清洗机清洗干净;
(3)用移液枪在搅拌均匀的溶液中加入1.5ml NH3,搅拌均匀;
(4)充分反应后将该配置好的溶液移入反应釜中,将干燥后的FTO以一定角度倾斜放入溶液中,在200℃烘箱中反应6-12h;
(5)在反应釜降至室温后将FTO取出用去离子水冲洗,干燥后移入马弗炉在300℃温度下退火2h,得到一种新型n-Cu2O/CuO半导体光催化剂。
Claims (3)
1.一种新型n-Cu2O/CuO半导体光催化剂的制备方法,其特征在于,包括如下步骤:
(1)将FTO分别放入丙酮、乙醇和去离子水中超声10min去除其表面的油污和杂质,然后对FTO干燥待用;
(2)称量1g的Cu(NO3)·3H2O,在1g的Cu(NO3)·3H2O加入30mL去离子水搅拌至完全溶解,得到拌均匀的第一溶液;
(3)用移液枪在搅拌均匀的第一溶液中加入1.5mlNH3,搅拌均匀,得到第二溶液;
(4)充分反应后将该配置好的第二溶液移入反应釜中,将干燥后的FTO倾斜放入第二溶液中,在200℃烘箱中反应6-12h;
(5)在反应釜降至室温后将FTO取出用去离子水冲洗,干燥后移入马弗炉在300℃温度下退火2h,得到一种新型n-Cu2O/CuO半导体光催化剂。
2.根据权利要求1所述的一种新型n-Cu2O/CuO半导体光催化剂的制备方法,其特征在于,步骤(1)中,FTO的尺寸为1×1cm。
3.根据权利要求1所述的一种新型n-Cu2O/CuO半导体光催化剂的制备方法,其特征在于,步骤(2)中,用电子天平称量1g原料Cu(NO3)·3H2O,用量筒量取30mL去离子水,量筒在使用前用超声清洗机清洗干净。
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