CN107175124A - 一种硫化隔锌固溶体/石墨烯/g‑C3N4复合型光催化剂的制备方法 - Google Patents
一种硫化隔锌固溶体/石墨烯/g‑C3N4复合型光催化剂的制备方法 Download PDFInfo
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Abstract
本发明公开了一种硫化隔锌固溶体/石墨烯/g‑C3N4复合型光催化剂的制备方法,属于无机环保光催化材料的合成技术领域。本发明的技术方案要点为:一种硫化隔锌固溶体/石墨烯/g‑C3N4复合型光催化剂的制备方法,是通过将Zn0.5Cd0.5S和石墨烯负载在g‑C3N4而形成的,其中g‑C3N4与Zn0.5Cd0.5S的质量比为1:0.01‑0.1,g‑C3N4与石墨烯的质量比为1:0.01‑0.1。本发明将Zn0.5Cd0.5S和石墨烯负载在g‑C3N4上能有效降低光生电子和空穴的复合率,极大提高了g‑C3N4的量子效率和光解水制氢效率,具有操作条件温和、所制备的产品团聚程度低、分散性好及光催化活性高等优点。
Description
技术领域
本发明属于无机环保光催化材料的合成技术领域,具体涉及一种硫化隔锌固溶体/石墨烯/g-C3N4复合型光催化剂的制备方法。
背景技术
近年来,随着人口的增长和社会的进步,对化石燃料的需求越来越大,但是化石燃料是不可再生资源且会造成温室效应,所以人类面临着两大挑战:能源短缺和环境污染,解决这些挑战的关键方法是寻求更好的方式来探索清洁能源。太阳能被认为是取之不尽的可再生资源,而半导体可将太阳能转化为化学能将水分解成氢气和氧气,这被认为是一种突破性的方法,既解决了能源短缺的问题又不造成环境污染。
g-C3N4具有类石墨状结构,具有良好的热稳定性和光催化性能,且具有较窄的禁带宽度(2.7eV),其导带电势比EH2/H+更负,满足光解水制氢的条件。但纯的g-C3N4在反应的过程中光生电子和空穴很容易复合,导致其光解水产氢效率很低,大大阻碍了其工业化的发展。研究发现,将g-C3N4半导体材料与另外一种具有合适能级结构半导体进行复合能有效改善光生载流子的复合,进而提高其光催化活性。石墨烯被称为“黑金”,是“新材料之王”,具有超高的导电特性,可以作为两种半导体之间的桥梁,能够快速的转移电子,抑制电子跟空穴的复合,有效的降低光生电子和空穴的复合率,大大提高光催化性能。为提高g-C3N4量子点的光催化活性,将其与具有合适带隙结构的Zn0.5Cd0.5S和具有超强电子传导能力的石墨烯相复合,利用两种半导体的能级差使光生载流子在两者的导带和价带之间互相迁移,同时利用石墨烯的超强导电性,极大提升了g-C3N4半导体材料光生载流子的分离和量子效率,进而提高其光分解水制氢的催化性能。
发明内容
本发明解决的技术问题是提供了一种操作简单且易于实现的硫化隔锌固溶体/石墨烯/g-C3N4复合型光催化剂的制备方法,该方法制备的硫化隔锌固溶体/石墨烯/g-C3N4复合型光催化剂太阳能利用率高且光解水制氢性能好。
本发明为解决上述技术问题采用如下技术方案,一种硫化隔锌固溶体/石墨烯/g-C3N4复合型光催化剂的制备方法,其特征在于具体步骤为:
(1)将尿素置于氧化铝坩埚中,再将氧化铝坩埚置于马弗炉中于500℃煅烧2h得到块状的氮化碳,该块状的氮化碳经超声分散、洗涤、干燥得到片状的g-C3N4;
(2)将1.25×10-4mol醋酸镉和1.25×10-4mol醋酸锌与去离子水混合均匀得到混合溶液,在搅拌状态下向混合溶液中加入0.15-1.5g步骤(1)得到的g-C3N4和0.015g石墨烯,搅拌10min后再向混合溶液中加入3.75×10-4mol硫化钠,继续搅拌2h后将混合溶液转移至反应釜中,然后将反应釜放入微波消解仪中于160-180℃微波反应5-30min;
(3)待反应结束后将反应釜冷却至常温,经离心、洗涤、干燥得到Zn0.5Cd0.5S/石墨烯/g-C3N4复合型光催化剂。
进一步优选,步骤(2)中将1.25×10-4mol醋酸镉和1.25×10-4mol醋酸锌与去离子水混合均匀得到混合溶液中醋酸镉的摩尔浓度为0.001-0.01 mol/L。
本发明与现有技术相比具有以下有益效果:
1、采用适宜的合成工艺制备出能带结构相匹配的Zn0.5Cd0.5S/石墨烯/g-C3N4复合型光催化剂,利用两种半导体之间的能级差能使光生截流子由一种半导体微粒的能级注入到另一种半导体微粒的能级上,同时利用石墨烯的超强导电性,从而极大提高光生电荷的分离效率和g-C3N4光催化剂的制氢性能;
2、根据微波水热法加热速率快和溶液受热均匀等特点,采用微波水热法制备出晶粒粒度小且团聚程度低的高活性Zn0.5Cd0.5S纳米粉体,进而有效的提高了Zn0.5Cd0.5S/石墨烯/g-C3N4复合型光催化剂的活性。
附图说明
图1为300W氙灯照射下,本发明实施例1所制备的Zn0.5Cd0.5S/石墨烯/g-C3N4复合型光催化剂和纯g-C3N4光催化剂的光催化分解水制氢效率柱形图(操作条件:催化剂的量:0.05g;牺牲剂的浓度:0.4mol/L的Na2S和0.4mol/L的Na2SO3)。从图中可以看出,在模拟可见光的照射下,光照4h后,Zn0.5Cd0.5S/石墨烯/g-C3N4复合型光催化剂较纯的g-C3N4光催化剂表现出明显增强的光催化制氢性能。
具体实施方式
以下结合实施例进一步描述本发明。应该指出,本发明并非局限于下述各实施例。
实施例1
(1)称取10g尿素置于氧化铝坩埚中,然后将氧化铝坩埚置入马弗炉中于500℃煅烧2h得到块状的氮化碳,该块状的氮化碳经超声分散、洗涤、干燥得到片状的g-C3N4;
(2)将1.25×10-4mol醋酸镉和1.25×10-4mol醋酸锌溶于去离子水配成0.001mol/L的混合溶液,在搅拌状态下向混合溶液中加入1.5g步骤(1)得到的g-C3N4和0.015g石墨烯,搅拌10min后向混合溶液中加入3.75×10-4mol硫化钠,继续搅拌2h后将混合溶液转移至反应釜,然后将反应釜放入微波消解仪中于160℃微波反应30min;
(3)待反应结束后将反应釜冷却至常温,经离心、洗涤、干燥得到Zn0.5Cd0.5S/石墨烯/g-C3N4复合型光催化剂。
实施例2
(1)称取10g尿素置于氧化铝坩埚中,然后将氧化铝坩埚置入马弗炉中于500℃煅烧2h得到块状的氮化碳,该块状的氮化碳经超声分散、洗涤、干燥得到片状的g-C3N4;
(2)将1.25×10-4mol醋酸镉和1.25×10-4mol醋酸锌溶于去离子水配成0.005mol/L的混合溶液,在搅拌状态下向混合溶液中加入0.3g步骤(1)得到的g-C3N4和0.015g石墨烯形成混合溶液,搅拌10min后向混合溶液中加入3.75×10-4mol硫化钠,继续搅拌2h后将混合溶液转移至反应釜,然后将反应釜放入微波消解仪中于170℃微波反应20min;
(3)待反应结束后将反应釜冷却至常温,经离心、洗涤、干燥得到Zn0.5Cd0.5S/石墨烯/g-C3N4复合型光催化剂。
实施例3
(1)称取10g尿素置于氧化铝坩埚中,然后将氧化铝坩埚置入马弗炉中于500℃煅烧2h得到块状的氮化碳,该块状的氮化碳经超声分散、洗涤、干燥得到片状的g-C3N4;
(2)将1.25×10-4mol醋酸镉和1.25×10-4mol醋酸锌溶于去离子水配成0.01mol/L的混合溶液,在搅拌状态下向混合溶液中加入0.15g步骤(1)得到的g-C3N4和0.015g石墨烯形成混合溶液,搅拌10min后向混合溶液中加入3.75×10-4mol硫化钠,继续搅拌2h后将混合溶液转移至反应釜,然后将反应釜放入微波消解仪中于160℃微波反应5min;
(3)待反应结束后将反应釜冷却至常温,经离心、洗涤、干燥得到Zn0.5Cd0.5S/石墨烯/g-C3N4复合型光催化剂。
以上实施例描述了本发明的基本原理、主要特征及优点,本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明原理的范围下,本发明还会有各种变化和改进,这些变化和改进均落入本发明保护的范围内。
Claims (2)
1.一种硫化隔锌固溶体/石墨烯/g-C3N4复合型光催化剂的制备方法,其特征在于具体步骤为:
(1)将尿素置于氧化铝坩埚中,再将氧化铝坩埚置于马弗炉中于500℃煅烧2h得到块状的氮化碳,该块状的氮化碳经超声分散、洗涤、干燥得到片状的g-C3N4;
(2)将1.25×10-4mol醋酸镉和1.25×10-4mol醋酸锌与去离子水混合均匀得到混合溶液,在搅拌状态下向混合溶液中加入0.15-1.5g步骤(1)得到的g-C3N4和0.015g石墨烯,搅拌10min后再向混合溶液中加入3.75×10-4mol硫化钠,继续搅拌2h后将混合溶液转移至反应釜中,然后将反应釜放入微波消解仪中于160-180℃微波反应5-30min;
(3)待反应结束后将反应釜冷却至常温,经离心、洗涤、干燥得到Zn0.5Cd0.5S/石墨烯/g-C3N4复合型光催化剂。
2. 根据权利要求1所述的Zn0.5Cd0.5S/石墨烯/g-C3N4复合型光催化剂的制备方法,其特征在于:步骤(2)中将1.25×10-4mol醋酸镉和1.25×10-4mol醋酸锌与去离子水混合均匀得到混合溶液中醋酸镉的摩尔浓度为0.001-0.01 mol/L。
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CN110586164A (zh) * | 2019-09-29 | 2019-12-20 | 上海电力大学 | 一种g-C3N4/rGO/ZnS光催化剂的制备及在光电化学阴极保护方面的应用 |
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CN115400776B (zh) * | 2022-08-01 | 2023-05-16 | 电子科技大学长三角研究院(湖州) | 一种锌镉硫固溶体/石墨相氮化碳片片复合s型异质结光催化剂、制备及其应用 |
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