CN106582721A - 取代贵金属Pt片析氢的MoS2/TiO2NTs异质结光电催化剂及其制备方法 - Google Patents
取代贵金属Pt片析氢的MoS2/TiO2NTs异质结光电催化剂及其制备方法 Download PDFInfo
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- 229910052961 molybdenite Inorganic materials 0.000 title claims abstract description 39
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 39
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 34
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 25
- 239000001257 hydrogen Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229910000510 noble metal Inorganic materials 0.000 title abstract description 3
- 239000010411 electrocatalyst Substances 0.000 title abstract 6
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims abstract description 115
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 45
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000010936 titanium Substances 0.000 claims abstract description 19
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 13
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 13
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 11
- 230000003647 oxidation Effects 0.000 claims abstract description 5
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 5
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 239000003054 catalyst Substances 0.000 claims description 33
- 239000002071 nanotube Substances 0.000 claims description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 239000010970 precious metal Substances 0.000 claims description 13
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 13
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 12
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- 238000001291 vacuum drying Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- 229910052697 platinum Inorganic materials 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 3
- 239000008151 electrolyte solution Substances 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- 229910004619 Na2MoO4 Inorganic materials 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 238000005868 electrolysis reaction Methods 0.000 claims description 2
- 238000010926 purge Methods 0.000 claims description 2
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- 239000010410 layer Substances 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- 239000002344 surface layer Substances 0.000 abstract 1
- 229910015667 MoO4 Inorganic materials 0.000 description 7
- 239000011734 sodium Substances 0.000 description 7
- 238000003756 stirring Methods 0.000 description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
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- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 2
- 229920005479 Lucite® Polymers 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000005622 photoelectricity Effects 0.000 description 2
- 239000004926 polymethyl methacrylate Substances 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
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- UCVQOIPQDBZRMG-UHFFFAOYSA-N [C].COC(C=1C(C(=O)OC)=CC=CC1)=O Chemical compound [C].COC(C=1C(C(=O)OC)=CC=CC1)=O UCVQOIPQDBZRMG-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种取代贵金属Pt片析氢的MoS2/TiO2NTs异质结光电催化剂及其制备方法,本发明的光电催化剂,采用二步法合成,首先阳极氧化金属Ti片形成高比表面积、有间距的TiO2NTs,以二甘醇和HF体系作为溶剂,采用Ti片为钛源,阳极氧化法制得;其次,将MoS2负载在制备好的TiO2NTs上,分别以钼酸钠和硫代乙酰胺为Mo源和S源在二甘醇为溶剂釜热得到。TiO2表面层状结构利用MoS2层的比表面积可以增加对H2O分子的吸附,同时MoS2自身优异的传到电子能力及边带效应,增加反应活性位点;光电催化协同能有效地分离电子和空穴,从而提高光催化活性,所以本发明的催化剂能快速高效分解产氢。
Description
技术领域
本发明涉及一种光电催化剂,具体为用原位负载方法合成的取代贵金属Pt片析氢的MoS2/TiO2 NTs异质结光电催化剂及其制备方法。
背景技术
随着世界人口和经济的增长,环境和能源问题成为制约人类发展的两大因素。光电催化剂在光电协同分解水制氢中独特的优势。与传统制氢相比,光电催化具有独特的优点:反应条件温和、能耗低、二次污染少、取代贵金属Pt等,在环境和能源方面具有非常重要的发展应用前景。近年来对其研究越来越多,众所周知,Pt由于高活性,无毒,稳定等优点被广泛的用作光电催析氢。但是受其高价格的限制,很难广泛应用于工业生产中,只能用于实验研究。
异质结MoS2/TiO2 NTs光电催化在外加偏压的基础上能够有效分离半导体的电子和空穴,有利于光电催化性能的提高。阳极纳米管阵列利用光的多重反射提高对光的利用率,阴极MoS2/TiO2 NTs迅速转移电子及MoS2自身边带析氢效应,进而提高光电析氢反应活性。
发明内容
本发明的目的在于针对现有贵金属析氢催化剂所存在的缺陷和为实际应用,提供一种MoS2/TiO2 NTs异质结光电催化剂,以及简单易行、产率高的制备方法。
本发明的技术方案是:
一种取代贵金属Pt片析氢的MoS2/TiO2 NTs异质结光电催化剂的制备方法,包括如下步骤:
(1)将钛片剪裁、按压使之平整,依次用丙酮、乙醇、超纯去离子水分别进行超声清洗,浸没在超纯去离子水中封存待用;
(2)配制HF的二甘醇(DEG)新鲜混合溶液,将钛片取出烘干,作为阳极将其浸入配制好的电解溶液;
(3)阴极使用铂片电极,接入直流电源,采用恒压直流电解方法,阳极氧化过程结束后,关闭电源,将表面生长TiO2纳米管阵列的钛片取出放入超纯去离子水中清洗,烘干,煅烧,最后得到结构完整有序结晶良好的有间距TiO2纳米管阵列;
(4)将钼酸钠(Na2MoO4)和硫代乙酰胺(TAA)溶于DEG中,放入制备好的间距TiO2纳米管阵列,200℃烘箱中保温24h,最后得到的黑色电极用水和乙醇清洗,然后真空干燥,得到催化剂MoS2/TiO2纳米管阵列。
优选地,步骤(1)中钛片剪裁规格大小为33×20×0.3mm,超声清洗时间分别为20min。
优选地,步骤(2)中HF的二甘醇新鲜混合溶液的质量浓度为1%,钛片浸没有效电解面积为20×20mm。
优选地,步骤(3)中铂片电极的规格为20×20×0.1mm,电解电压大小为60V,电解时间为120h。
优选地,步骤(3)中煅烧条件为:在马弗炉中以2℃/min的升温速率至450℃煅烧2h。
优选地,步骤(4)中真空干燥温度为80℃。
上述方法制备的取代贵金属Pt片析氢的MoS2/TiO2 NTs异质结光电催化剂为MoS2负载在制备好的TiO2 NTs上,所述TiO2 NTs其纳米管阵列长度3um左右,孔径10nm,间距20-50nm。
本发明的MoS2/TiO2 NTs异质结光电催化剂,采用二步法合成,首先阳极氧化金属Ti片形成高比表面积、有间距的TiO2 NTs,以二甘醇和HF体系作为溶剂,采用Ti片为钛源,阳极氧化法制得;其次,将MoS2负载在制备好的TiO2 NTs上,分别以钼酸钠和硫代乙酰胺为Mo源和S源在二甘醇为溶剂釜热从而得到MoS2/TiO2 NTs异质结光电催化剂。TiO2表面层状结构利用MoS2层的比表面积可以增加对H2O分子的吸附,同时MoS2自身优异的传到电子能力及边带效应,增加反应活性位点;光电催化协同能有效地分离电子和空穴,从而提高光催化活性。所以该催化剂能快速高效分解产氢。
本发明的光催化剂性能测试在液相中完成,模拟CO2光电催化转化成单一产物碳酸二甲酯(DMC)。
本发明制备的产品通过以下手段进行结构表征:采用在日本理学Rigaku D/Max-RB型X射线衍射仪上测量的X射线衍射进行样品的结构分析;采用日本JEOL JSM-6380LV型扫描电镜获得的扫描电镜照片;采用日本电子光学公司生产的JEM 2010型透射电子显微镜,进行催化剂样品形貌分析;采用Perkin Elmer公司出产的PHI 5000C型X射线光电子能谱仪进行催化剂材料的XPS测试。
本发明与现有技术相比,具有以下优点及突出效果:本发明所使用的化学试剂均为常用试剂、廉价易得,方法工艺简单,合成光电催化剂产氢活性达到128.44umol·h-1·cm-1,远远大于贵金属Pt片的活性。
附图说明
图1为所制得MoS2/TiO2 NTs异质结光电催化剂样品的XRD图谱;
图2为所制得MoS2/TiO2 NTs异质结光电催化剂样品的高分辨扫描电镜图;
图3为所制得的MoS2/TiO2 NTs异质结光电催化剂样品的透射电子显微镜图;
图4为所制得的MoS2/TiO2 NTs异质结光电催化剂样品元素分析的XPS能谱图;(a)为元素Mo3d谱图(b)为为元素S2p谱图
图5为所制得的MoS2/TiO2 NTs异质结光电催化剂样品的产氢活性图。
具体实施方式
下面结合具体实施例对本发明是如何实现的做进一步详细、清楚、完整地说明,所列实施例仅对本发明予以进一步的说明,并不因此而限制本发明:
实施例1
将工业钛片剪裁规格大小为33×20×0.3mm,按压使之平整,依次用丙酮、乙醇、超纯去离子水分别进行超声清洗20min,浸没在超纯去离子水中封存待用。制备前配制浓度为1%HF的二甘醇(DEG)新鲜混合溶液,将预处理好的钛片取出烘干,作为阳极将其浸入配制好的电解溶液,浸没有效电解面积20×20mm。阴极使用20×20×0.1mm的铂片电极,接入直流电源,采用恒压直流电解方法,调节电压大小为60V,控制电解时间为120h。阳极氧化过程结束后,关闭电源,将表面生长TiO2纳米管阵列的钛片取出放入超纯去离子水中清洗,烘干,放入马弗炉中以2℃/min的升温速率至450℃煅烧2h,最后得到结构完整有序结晶良好的有间距TiO2纳米管阵列。
实施例2
称取10mg的钼酸钠(Na2MoO4)和20mg硫代乙酰胺(TAA)溶于20ml DEG中,搅拌20min,放入制备好的间距TiO2纳米管阵列,将其放到200℃的烘箱中保温24h,最后得到的黑色电极用水和乙醇各洗三次,然后80℃真空干燥,得到催化剂MoS2/TiO2纳米管阵列。
实施例3
称取10mg的钼酸钠(Na2MoO4)和30mg硫代乙酰胺(TAA)溶于20ml DEG中,搅拌20min,放入制备好的间距TiO2纳米管阵列,将其放到200℃的烘箱中保温24h,最后得到的黑色电极用水和乙醇各洗三次,然后80℃真空干燥,得到催化剂MoS2/TiO2纳米管阵列。
实施例4
称取10mg的钼酸钠(Na2MoO4)和40mg硫代乙酰胺(TAA)溶于20ml DEG中,搅拌20min,放入制备好的间距TiO2纳米管阵列,将其放到200℃的烘箱中保温24h,最后得到的黑色电极用水和乙醇各洗三次,然后80℃真空干燥,得到催化剂MoS2/TiO2纳米管阵列。
实施例5
称取10mg的钼酸钠(Na2MoO4)和50mg硫代乙酰胺(TAA)溶于20ml DEG中,搅拌20min,放入制备好的间距TiO2纳米管阵列,将其放到200℃的烘箱中保温24h,最后得到的黑色电极用水和乙醇各洗三次,然后80℃真空干燥,得到催化剂MoS2/TiO2纳米管阵列。
实施例6
称取10mg的钼酸钠(Na2MoO4)和60mg硫代乙酰胺(TAA)溶于20ml DEG中,搅拌20min,放入制备好的间距TiO2纳米管阵列,将其放到200℃的烘箱中保温24h,最后得到的黑色电极用水和乙醇各洗三次,然后80℃真空干燥,得到催化剂MoS2/TiO2纳米管阵列。
实施例7
称取10mg的钼酸钠(Na2MoO4)和70mg硫代乙酰胺(TAA)溶于20ml DEG中,搅拌20min,放入制备好的间距TiO2纳米管阵列,将其放到200℃的烘箱中保温24h,最后得到的黑色电极用水和乙醇各洗三次,然后80℃真空干燥,得到催化剂MoS2/TiO2纳米管阵列。
实施例8
称取10mg的钼酸钠(Na2MoO4)和80mg硫代乙酰胺(TAA)溶于20ml DEG中,搅拌20min,放入制备好的间距TiO2纳米管阵列,将其放到200℃的烘箱中保温24h,最后得到的黑色电极用水和乙醇各洗三次,然后80℃真空干燥,得到催化剂MoS2/TiO2纳米管阵列。
实施例9
自制的两池中间被砂心隔离的有机玻璃反应装置。这样的反应器能够避免氢气和氧气混合,因此氢气和氧气可以分别收集。自制的装置中充满着2M乙二醇和0.5M的硫酸钠溶液。实验采用三电极体系,TiO2-NTs作为光阳极,饱和甘汞电极(SCE)作为参比电极,Pt片为对电极。
实施例10
自制的两池中间被砂心隔离的有机玻璃反应装置。这样的反应器能够避免氢气和氧气混合,因此氢气和氧气可以分别收集。自制的装置中充满着2M乙二醇和0.5M的硫酸钠溶液。实验采用三电极体系,TiO2-NTs作为光阳极,饱和甘汞电极(SCE)作为参比电极,MoS2/TiO2纳米管阵列为对电极。
Claims (7)
1.一种取代贵金属Pt片析氢的MoS2/TiO2NTs异质结光电催化剂的制备方法,其特征在于,包括如下步骤:
(1)将钛片剪裁、按压使之平整,依次用丙酮、乙醇、超纯去离子水分别进行超声清洗,浸没在超纯去离子水中封存待用;
(2)配制HF的二甘醇(DEG)新鲜混合溶液,将钛片取出烘干,作为阳极将其浸入配制好的电解溶液;
(3)阴极使用铂片电极,接入直流电源,采用恒压直流电解方法,阳极氧化过程结束后,关闭电源,将表面生长TiO2纳米管阵列的钛片取出放入超纯去离子水中清洗,烘干,煅烧,最后得到结构完整有序结晶良好的有间距TiO2纳米管阵列;
(4)将钼酸钠(Na2MoO4)和硫代乙酰胺(TAA)溶于DEG中,放入制备好的间距TiO2纳米管阵列,200℃烘箱中保温24h,最后得到的黑色电极用水和乙醇清洗,然后真空干燥,得到催化剂MoS2/TiO2纳米管阵列。
2.根据权利要求1所述的取代贵金属Pt片析氢的MoS2/TiO2NTs异质结光电催化剂的制备方法,其特征在于,步骤(1)中钛片剪裁规格大小为33×20×0.3mm,超声清洗时间分别为20min。
3.根据权利要求1所述的取代贵金属Pt片析氢的MoS2/TiO2NTs异质结光电催化剂的制备方法,其特征在于,步骤(2)中HF的二甘醇新鲜混合溶液的质量浓度为1%,钛片浸没有效电解面积为20×20mm。
4.根据权利要求1所述的取代贵金属Pt片析氢的MoS2/TiO2NTs异质结光电催化剂的制备方法,其特征在于,步骤(3)中铂片电极的规格为20×20×0.1mm,电解电压大小为60V,电解时间为120h。
5.根据权利要求1所述的取代贵金属Pt片析氢的MoS2/TiO2NTs异质结光电催化剂的制备方法,其特征在于,步骤(3)中煅烧条件为:在马弗炉中以2℃/min的升温速率至450℃煅烧2h。
6.根据权利要求1所述的取代贵金属Pt片析氢的MoS2/TiO2NTs异质结光电催化剂的制备方法,其特征在于,步骤(4)中真空干燥温度为80℃。
7.权利要求1-6任意一项所述方法制备的取代贵金属Pt片析氢的MoS2/TiO2NTs异质结光电催化剂,其特征在于,所述催化剂为MoS2负载在制备好的TiO2NTs上,所述TiO2NTs其纳米管阵列长度3um左右,孔径10nm,间距20-50nm。
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