CN109012700B - 一种硫化铜-49氧化18钨-石墨烯纳米复合材料的制备方法 - Google Patents
一种硫化铜-49氧化18钨-石墨烯纳米复合材料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种CuS‑W18O49‑rGO纳米复合材料的制备方法。以分散在WCl6前驱反应液中的CuS和氧化石墨烯为载体,在溶剂热条件下,氧化石墨烯被还原,同时在溶剂热过程中,W18O49直接在CuS和石墨烯上生长,最终得到CuS‑W18O49‑rGO的复合材料。本发明方法能够通过改变反应液中WCl6的浓度控制W18O49在复合物中的含量。复合材料的光电和光催化性能均优于纯CuS材料,并且随W18O49在复合物中含量的改变而发生变化。所制备的CuS‑W18O49‑rGO纳米复合材料能够用于光电和光催化领域。
Description
技术领域
本发明属于光催化半导体技术领域,具体涉及一种CuS-W18O49-rGO纳米复合材料的制备方法。
背景技术
对于应用于光催化领域的半导体材料,要实现良好的光催化性能,除了需要具有合适的带隙,对光有较高的吸收利用率之外,其载荷子迁移率要较大,光生电子和空穴能够快速传输到反应位点。采用单一的半导体材料应用于光催化领域时,由于光生电子和空穴随时会发生复合而消失,因此其性能常常不尽如人意。构建半导体异质结,产生内建电场是有效分离电子和空穴的方法。
非化学计量氧化钨(W18O49)为n型半导体,文献报道的纳米W18O49的带隙范围在1.6-2.9eV左右,具有较高的吸光系数。此外,W18O49中存在大量氧空位,这些氧空位能够降低带隙,使材料的吸收边红移,同时氧空位还能提供活性位点从而增强光催化活性。CuS为p型导电材料,CuS纳米材料的带隙可调范围很宽,有文献报道的数据在0-2eV,其空穴的传输速度很快,在4.7K温度下,空穴迁移率高达1440cm2•V-1•s-1。将CuS应用于催化领域,可实现较好的光谱吸收和快速的空穴传输。二维石墨烯具有高比表面积和优异的电子传输性,应用于光催化领域,不仅能提高反应物的接触面积,并且能将光生电子快速的从产生的位置传输到反应位点。
将W18O49与CuS和石墨烯复合不仅能拓宽材料的吸光范围,并且能构建分离电子和空穴的异质结,同时,由于CuS和石墨烯分别具有很高的空穴和电子迁移率,分离的电子和空穴能快速的传输到反应位点,能使材料的光催化性能得到提升,在光催化领域具有巨大的应用潜力。
本发明首先采用水热法合成纳米CuS,改良hummer法制备氧化石墨烯,随后在制备W18O49的前驱反应液中加入事先合成的纳米CuS和氧化石墨烯,在溶剂热条件下,氧化石墨烯被还原为石墨烯(rGO),同时W18O49直接在CuS和石墨烯上生长,得到CuS-W18O49-rGO复合材料。可通过改变反应液中钨源的浓度来控制复合物中W18O49的含量,从而得到性能不同的复合材料。这一制备CuS-W18O49-rGO纳米复合材料的方法还未见报道。
发明内容
本发明的目的是提供一种CuS-W18O49-rGO纳米复合材料的制备方法。
本发明的思路:以分散在WCl6前驱反应液中的CuS和氧化石墨烯为载体,在溶剂热条件下,氧化石墨烯被还原,同时W18O49直接在CuS和石墨烯上生长,最终得到CuS-W18O49-rGO的复合材料。
具体步骤为:
(1)将硝酸铜加入乙二醇溶液中充分溶解后加入硫脲并在常温下搅拌30min,将得到的混合溶液转移到水热反应釜中,在180℃的恒温烘箱中反应72小时。自然降温至室温后,用水和乙醇离心清洗得到的CuS黑色沉淀物,在80℃下真空干燥过夜。
(2)氧化石墨烯采用改良hummer法制备,并分散于乙醇中得到分散液。
(3)将WCl6超声溶解于乙醇,得到黄色溶液,随后将一定量CuS和石墨烯的乙醇分散液超声分散在这一WCl6的乙醇溶液中,放入水热反应釜中,在150℃的恒温烘箱中保温10小时。自然降温后,用水和乙醇多次清洗产物,最后干燥得到复合物。
附图说明
图1是本发明实施例1所制备的CuS和CuS-W18O49-rGO纳米复合材料的XRD图谱与CuS和W18O49标准卡片的对比图。
图2(a)和(b)分别是本发明实施例2制得的纯CuS和CuS-W18O49-rGO纳米复合材料的SEM图。
图3是本发明实施例1、2、3和4 制得的CuS和W18O49含量不同的CuS-W18O49-rGO纳米复合材料的光电响应曲线。
图4是本发明实施例1、2、3和4制得的CuS和W18O49含量不同的CuS-W18O49-rGO纳米复合材料光催化分解亚甲基蓝曲线图。
具体实施方式:
实施例1:
(1)将241.6mg硝酸铜加入60ml乙二醇中充分溶解后再加入152.24mg硫脲并在常温下搅拌30min,将得到的混合溶液转移到100ml水热反应釜中,在180℃下反应72小时。自然降温至室温后,将产物离心,用水和乙醇清洗数次,将得到的黑色沉淀物CuS在80℃下真空干燥过夜。
(2)氧化石墨烯采用改良hummer法制备,随后将其分散在乙醇中得到浓度0.0185g/ml的分散液。
(3)将0.0223g WCl6加入到12ml乙醇中超声溶解得到金黄色溶液,然后加入0.0161g (1)中制备的CuS粉末和1ml(2)中制备的氧化石墨烯乙醇分散液,随后超声2min-3min后放入水热反应釜中在150℃下恒温反应10小时。反应结束后,在室温下自然冷却,离心产物用水和乙醇清洗三次,在真空箱内60℃下真空干燥。将此实施例制备的样品命名为CWG1。
附图1为本实施例制得的CuS和水热反应制得的CuS-W18O49-rGO复合材料样品的xrd图谱。测试结果表明,CuS样品在27.67°,29.27°,31.78°,32.85°,47.91°,52.72°,58.64°和59.32°出现衍射峰,分别对应于六方晶型CuS的(101),(102),(103),(006),(110),(108),(203)和(116)晶面。复合物样品除了CuS的衍射峰之外出现了新的衍射峰,这些新的衍射峰与W18O49的衍射峰数据相符,说明形成了W18O49和CuS的复合物。由于石墨烯的衍射峰信号较弱,被CuS和W18O49的衍射信号掩盖,因此没有观察到石墨烯的衍射峰。附图3的光电测试结果表明,纳米CuS样品和CWG1样品都显示了光响应性,在100mW/cm-2光强下,偏压0.2V时,复合材料样品的响应电流为9.74µA cm-2,高于CuS样品在同样条件下1.74µA cm-2的响应电流值。附图4的光催化亚甲基蓝测试结果表明,经过48分钟的光照后,CWG1对亚甲基蓝的降解率达到85%,高于纯CuS 62.7%的降解率。
实施例2:
将实施例1中步骤(3)中氯化钨的加入量改为0.0667 g,其余均同实施例1,得到的样品记为CWG2。
从图2的SEM图(a)可看出制备的纯硫化铜为粒径为100nm左右的颗粒,经过在氯化钨溶液中的溶剂热反应复合后得到的CWG2样品其粒径增大到200-400nm(图2(b)),并且在颗粒表面附着大量丝状物质,可以推断为W18O49纳米线附着在CuS颗粒上。附图3的光电测试结果表明,CWG2样品显示了光响应性,在100mW/cm-2光强下,电压0.2V时,CWG2样品的响应电流为16.88 µA cm-2,高于CWG1样品在同样条件下9.74µA cm-2的响应电流。附图4的光催化亚甲基蓝测试结果表明,经过48分钟的光照后,CWG2对亚甲基蓝的降解率达到91%,高于CWG1 85%的降解率。
实施例3:
(1)与实施案例1中的步骤(1)相同
(2)与实施案例1中的步骤(2)相同。
(3)将0.1778g WCl6加入到24ml乙醇中超声溶解得到金黄色溶液,然后加入0.0322g CuS粉末和2ml 0.0185g/ml的氧化石墨烯乙醇分散液,随后超声2min-3min后放入水热反应釜中在150℃下恒温反应10小时。反应结束后,在室温下自然冷却,离心产物用水和乙醇清洗三次,在真空箱内60℃下真空干燥。将此实施例制备的样品命名为CWG3。
附图3的光电测试结果表明,附图3的光电测试结果表明,CWG3样品显示了光响应性,在100mW/cm-2光强下,电压0.2V时,CWG3的响应电流为27.12µA cm-2,高于CWG2的响应电流值。附图4的光催化亚甲基蓝测试结果表明,经过48分钟的光照后,CWG3对亚甲基蓝的降解率达到95%,高于CWG2 91%的降解率。
实施例4:
(1)同实施案例1中的步骤(1)
(2)同实施案例1中的步骤(2)。
(3) 将0.3336g WCl6加入到36ml乙醇中超声溶解得到金黄色溶液,然后加入0.0483g CuS粉末和3ml 0.0185g/ml的氧化石墨烯乙醇分散液,随后超声2min-3min后放入水热反应釜中在150℃下恒温反应10小时。反应结束后,在室温下自然冷却,离心产物用水和乙醇清洗三次,在真空箱内60℃下真空干燥。将此实施例制备的样品命名为CWG4。
附图3的光电测试结果表明,附图3的光电测试结果表明,CWG4样品显示了光响应性,在100mW/cm-2光强下,电压0.2V时,CWG4的响应电流为4.78µA cm-2,低于CWG3 27.12µAcm-2的电流值,但仍高于CuS样品在同样条件下1.74µA cm-2的响应电流。附图4的光催化亚甲基蓝测试结果表明,经过48分钟的光照后,CWG4对亚甲基蓝的降解率达到90%,低于CWG395%的降解率,但仍高于纯CuS 62.7%的降解率。CWG4的光电和光催化性能较CWG3下降的原因,可能是复合物中W18O49层过厚,导致光生载荷子的迁移距离增大,在迁移过程中电子和空穴复合的几率增加。
Claims (5)
1.一种CuS-W18O49-rGO纳米复合材料的制备方法,其特征在于其具体的步骤为:
(1)将硝酸铜加入乙二醇中充分溶解,随后加入硫脲并在常温下搅拌30min,将得到的混合溶液转移到水热反应釜中,在180℃下反应72小时,自然降温至室温后,用水和乙醇离心清洗得到的黑色沉淀物,在80℃下真空干燥过夜;
(2)氧化石墨烯采用改良hummer法制备,并分散到乙醇溶液中;
(3)取WCl6分散到乙醇中超声溶解得到黄色溶液,后加入(1)中所制备的CuS粉末和(2)中所制备的氧化石墨烯乙醇溶液,超声分散2-3min后将混合液放入水热反应釜中,在150℃温度下保温10小时,自然降温后,用水和乙醇离心清洗产物,在真空箱中干燥,即制得CuS-W18O49-rGO纳米复合材料。
2.根据权利要求1所述的一种CuS-W18O49-rGO纳米复合材料的制备方法,其特征在于,所述步骤(1)中硝酸铜的乙二醇溶液浓度为0.017mol/L,硝酸铜与硫脲的摩尔比为1:2。
3.根据权利要求1所述的一种CuS-W18O49-rGO纳米复合材料的制备方法,其特征在于,所述步骤(2)中制得的氧化石墨烯的乙醇分散液浓度为0.014g/mL 。
4.根据权利要求1所述的一种CuS-W18O49-rGO纳米复合材料的制备方法,其特征在于,所述步骤(3)中氯化钨乙醇溶液浓度为:0,0047mol/L-0.0234mol/L ,氯化钨和硫化铜的摩尔比为:0.33:1-1.67:1,氯化钨乙醇溶液与氧化石墨烯分散液的体积比为:5:1。
5.根据权利要求1所述的一种CuS-W18O49-rGO纳米复合材料的制备方法,其特征在于,所述步骤(3)中,在溶剂热条件下,氧化石墨烯被还原为石墨烯,同时生成W18O49。
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