CN106384673A - 一种制备钨酸铜光阳极薄膜方法 - Google Patents
一种制备钨酸铜光阳极薄膜方法 Download PDFInfo
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- OQFRENMCLHGPRB-UHFFFAOYSA-N copper;dioxido(dioxo)tungsten Chemical compound [Cu+2].[O-][W]([O-])(=O)=O OQFRENMCLHGPRB-UHFFFAOYSA-N 0.000 title abstract 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 44
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052802 copper Inorganic materials 0.000 claims abstract description 16
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 6
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910001887 tin oxide Inorganic materials 0.000 claims abstract description 5
- SXTLQDJHRPXDSB-UHFFFAOYSA-N copper;dinitrate;trihydrate Chemical compound O.O.O.[Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O SXTLQDJHRPXDSB-UHFFFAOYSA-N 0.000 claims abstract description 4
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- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims abstract 2
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 claims description 29
- 239000010408 film Substances 0.000 claims description 20
- 239000010409 thin film Substances 0.000 claims description 16
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- 239000012467 final product Substances 0.000 claims description 6
- 235000011150 stannous chloride Nutrition 0.000 claims description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 abstract 2
- 238000004090 dissolution Methods 0.000 abstract 2
- 229910052731 fluorine Inorganic materials 0.000 abstract 2
- 239000011737 fluorine Substances 0.000 abstract 2
- FWPIDFUJEMBDLS-UHFFFAOYSA-L tin(II) chloride dihydrate Chemical compound O.O.Cl[Sn]Cl FWPIDFUJEMBDLS-UHFFFAOYSA-L 0.000 abstract 2
- 238000006243 chemical reaction Methods 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
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- 230000005622 photoelectricity Effects 0.000 description 3
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- 239000000203 mixture Substances 0.000 description 2
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- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
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- 238000004519 manufacturing process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
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- 238000003860 storage Methods 0.000 description 1
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- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
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- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
- H01G9/2045—Light-sensitive devices comprising a semiconductor electrode comprising elements of the fourth group of the Periodic Table with or without impurities, e.g. doping materials
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E10/542—Dye sensitized solar cells
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Abstract
本发明涉及一种制备钨酸铜光阳极薄膜的方法，包括如下步骤：1)首先配制含有铜、锡元素的有机溶液，分别为三水合硝酸铜溶于乙二醇甲醚，浓度为0.04‑0.08mol/L；二水合氯化亚锡溶于乙二醇甲醚，浓度为0.04‑0.08mol/L；2)分别取(5‑X)ml和Xml的步骤1)中配置的铜与锡溶液，混合至均匀；3)再加入等摩尔量的偏钨酸铵，再加入0.1‑0.7ml的浓硝酸以及10‑100mg硝酸铵，搅拌溶液至澄清，即得前驱体溶液；4)利用移液器移取一定量的步骤3)中制备好的前驱体溶液，滴加在氟掺杂的氧化锡导电衬底上，在70℃的加热板上加热20min，去除有机溶剂；5)将步骤4)中覆有薄膜前驱体的氟掺杂氧化锡导电衬底置于550±50℃的马弗炉中煅烧1‑4h，取出自然冷却至室温，即得相应的锡元素掺杂的钨酸铜薄膜。
Description
技术领域
本发明涉及到一种制备钨酸铜薄膜并利用锡元素掺杂提升载流子浓度的方法。
背景技术
随着现代社会对能源消耗的需求日益加剧，传统化石能源的缺点也被日益放大，其有限的总量和使用过程产生的环境污染问题亟待解决，寻找传统化石能源的替代品一事也早已被很多国家提上日程。利用光电化学电池直接将高度分散的、波动性大的以及难以存储运输的太阳能转化为高能量密度和稳定的清洁氢能，有希望解决目前的能源问题。然而目前的光电化学电池分解水系统的转换效率受限于光阳极材料较低的光电流密度以及较高的开启电位。金属氧化物光阳极材料因为具有低廉的制造成本和良好的光电化学稳定性等特点得到了研究者的广泛关注。但是其光电流密度受材料的导电性制约，研究者通常利用元素掺杂来提升材料的多数载流子浓度或者载流子迁移率，改善材料的电荷传输能力，提升其分解水性能。
钨酸铜能够吸收到550nm附近的可见光，其理论太阳能到氢能转换效率可达到10％，但是实际的太阳能到氢能转换效率非常低。
发明内容：
本发明目的是，提出一种制备锡元素掺杂的钨酸铜光阳极薄膜的方法，并利用锡元素掺杂提升载流子浓度的方法，能用于提高太阳电池的氢能转换效率。
本发明的技术方案是，一种制备锡元素掺杂的钨酸铜光阳极薄膜的方法，其特征是包括如下步骤：
(1)首先配制含有铜、锡元素的有机溶液，分别为三水合硝酸铜溶于乙二醇甲醚，浓度为0.04-0.08mol/L；二水合氯化亚锡溶于乙二醇甲醚，浓度为0.04-0.08mol/L；
(2)分别取(5-X)ml和X ml的步骤(1)中配置的铜与锡溶液，混合至均匀，X取0.1-0.5；
(3)再加入等摩尔量的偏钨酸铵，再加入0.1-0.7ml的浓硝酸以及10-100mg硝酸铵，搅拌溶液至澄清，即得前驱体溶液；
(4)利用移液器移取一定量的步骤(3)中制备好的前驱体溶液，滴加在氟掺杂的氧化锡导电衬底上，在70℃的加热板上加热20min，去除有机溶剂；
(5)将步骤(4)中覆有薄膜前驱体的氟掺杂氧化锡导电衬底置于550±50℃的马弗炉中煅烧1-4h，取出自然冷却至室温，即得相应的锡元素掺杂的钨酸铜薄膜。
本发明的有益效果：采用本方法制备的锡掺杂钨酸铜光阳极薄膜材料，其性能相较于未掺杂的钨酸铜光阳极材料有大幅度提高，在模拟太阳光下(AM 1.5G，100mW cm-2)的饱和光电流密度达到1.05mA cm-2。实现了太阳能向化学能的转换。
附图说明
图1是未掺杂与3％的锡元素掺杂比例的钨酸铜薄膜样品的X射线衍射图谱；
图2是未掺杂与3％的锡元素掺杂比例的钨酸铜薄膜样品的光吸收图谱；
图3是未掺杂与3％的锡元素掺杂比例的钨酸铜薄膜样品在不同偏压下的量子转换效率；图4是未掺杂与3％的锡元素掺杂比例的钨酸铜薄膜样品的电镜照片；图4中a、c给出了3％的锡元素掺杂比例的钨酸铜薄膜样品的电镜照片(分别是表面与截面)，图4中b、d给出了未掺杂钨酸铜薄膜样品的电镜照片(分别是表面与截面)；
图5是未掺杂与不同锡元素掺杂比例的钨酸铜薄膜样品在可见光下的光电流图；
图6是未掺杂与3％的锡元素掺杂比例的钨酸铜薄膜样品在模拟太阳光下的光电流图；
图7是未掺杂与3％的锡元素掺杂比例的钨酸铜薄膜样品的mott-schottky曲线图。
具体实施方式
下面结合实施例和附图对本发明作进一步说明。
钨酸铜光阳极的制备方法包括如下步骤：
(1)首先配制含有铜、锡元素的有机溶液，分别为三水合硝酸铜溶于乙二醇甲醚，浓度为0.05mol/L；二水合氯化亚锡溶于乙二醇甲醚，浓度为0.05mol/L；
(2)分别取(5-X)ml和X ml的步骤(1)中配置的铜与锡溶液，混合至均匀,其中X＝0.15时，锡掺杂的钨酸铜光阳极性能最优；
(3)再加入等摩尔量的偏钨酸铵，再加入0.1-0.7ml的浓硝酸以及10-100mg硝酸铵，搅拌溶液至澄清，即得前驱体溶液.其中浓硝酸体积为0.4ml，硝酸铵的质量为40mg，锡掺杂的钨酸铜光阳极性能最优；
(4)利用移液器移取一定量的步骤(3)中制备好的前驱体溶液，滴加在氟掺杂的氧化锡导电衬底上，在70℃的加热板上加热20min，去除有机溶剂。结果表明滴液量为30ulcm-2，制得的薄膜最为均匀，性能最优。
(5)将步骤(4)中覆有薄膜前驱体的氟掺杂氧化锡导电衬底置于550℃的马弗炉中煅烧2h，取出自然冷却至室温，即得相应的锡元素掺杂的钨酸铜薄膜。
图1给出了未掺杂与3at％的锡元素掺杂比例的钨酸铜薄膜样品的X射线衍射图谱，可以看出合成出的钨酸铜薄膜样品均为纯相，无杂相。
图2给出了未掺杂与3at％的锡元素掺杂比例的钨酸铜薄膜样品的光吸收图谱，可以看出两用样品的带边均在550nm附近，掺杂并没有引起带隙发生改变，而未掺杂的样品的光吸收效率要高于3at％锡元素掺杂的样品，这是因为锡元素掺杂引起了钨酸铜纳米结构的改变而导致。
图3给出了未掺杂与3at％的锡元素掺杂比例的钨酸铜薄膜样品在不同偏压下的量子转换效率，在1.23与1.63VRHE的外加偏压下，可以看出3％锡元素掺杂的钨酸铜光阳极的量子转换效率均要高于未掺杂的钨酸铜薄膜。
图4给出了未掺杂(图4b、d)与3at％的锡元素掺杂(图4a、c)比例的钨酸铜薄膜样品的电镜照片，可以看出通过该种方法合成的钨酸铜薄膜具有多孔结构，并且由于锡元素的引入导致了晶粒大小的改变，导致薄膜的厚度减薄，从1.1μm降低至700nm
图5给出了未掺杂与不同锡元素掺杂比例的钨酸铜薄膜样品在可见光下的光电流图，可以锡元素的掺杂会提升钨酸铜薄膜光阳极的光电流密度，其中3at％的掺杂比例提升最大。
图6给出了未掺杂与3at％的锡元素掺杂比例的钨酸铜薄膜样品在模拟太阳光下的光电流图，可以看出在模拟太阳光光照下(AM 1.5G，100mW cm-2)，3at％锡元素掺杂的钨酸铜薄膜光阳极的光电流密度达到1.05mA cm-2。
图7给出了未掺杂与3at％的锡元素掺杂比例的钨酸铜薄膜样品的mott-schottky曲线图，可以出来3at％的锡元素掺杂使的薄膜的载流子浓度提升了40倍。
Claims (1)
1.制备钨酸铜光阳极薄膜的方法，其特征是包括如下步骤：
1)首先配制含有铜、锡元素的有机溶液，分别为三水合硝酸铜溶于乙二醇甲醚，浓度为0.04-0.08mol/L；二水合氯化亚锡溶于乙二醇甲醚，浓度为0.04-0.08 mol/L;
2)分别取（5-X）ml和Xml的步骤1）中配置的铜与锡溶液，混合至均匀; X取0.1-0.5；
3)再加入等摩尔量的偏钨酸铵，再加入0.1-0.7 ml的浓硝酸以及10-100 mg硝酸铵，搅拌溶液至澄清，即得前驱体溶液；
4)利用移液器移取一定量的步骤3）中制备好的前驱体溶液，滴加在氟掺杂的氧化锡导电衬底上，在70 ℃的加热板上加热20 min，去除有机溶剂；
5)将步骤4）中覆有薄膜前驱体的氟掺杂氧化锡导电衬底置于550±50℃的马弗炉中煅烧1-4h，取出自然冷却至室温，即得相应的锡元素掺杂的钨酸铜薄膜。
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| CN109295474A (zh) * | 2018-10-09 | 2019-02-01 | 天津城建大学 | 一种Co掺杂的纳米棒状的CuWO4光阳极薄膜的制备方法 |
| CN109868486A (zh) * | 2019-04-02 | 2019-06-11 | 台州学院 | 一种具有可见光响应的钨酸铜/磷酸镍光阳极薄膜的制备方法 |
| CN111482150A (zh) * | 2020-04-22 | 2020-08-04 | 上海市普陀区人民医院(上海纺织第一医院) | 一种可见光响应的全铜基串联光电催化装置及其制备方法 |
| CN112695304A (zh) * | 2020-12-10 | 2021-04-23 | 华北理工大学 | 一种钨酸铜光阳极薄膜及其制备方法 |
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| CN112695304A (zh) * | 2020-12-10 | 2021-04-23 | 华北理工大学 | 一种钨酸铜光阳极薄膜及其制备方法 |
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