CN107829108A - 一种FeOOH/CdS/Ti:Fe2O3复合光电极及其制备方法 - Google Patents
一种FeOOH/CdS/Ti:Fe2O3复合光电极及其制备方法 Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000010936 titanium Substances 0.000 claims abstract description 61
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 44
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 16
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 11
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 9
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- 230000008021 deposition Effects 0.000 claims abstract description 9
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- 238000006243 chemical reaction Methods 0.000 claims description 11
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 9
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 8
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
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- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical group Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 claims description 6
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- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 abstract 1
- 229910003145 α-Fe2O3 Inorganic materials 0.000 description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 8
- 238000004140 cleaning Methods 0.000 description 5
- 229910003153 β-FeOOH Inorganic materials 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
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- 238000005516 engineering process Methods 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
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- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
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- 230000004083 survival effect Effects 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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Abstract
本发明公开了一种FeOOH/CdS/Ti:Fe2O3复合光电极及其制备方法。该方法步骤如下:(1)将FTO清洗干净;(2)将FTO浸没于氯化铁、尿素和钛源的混合水溶液后,置于密封的反应釜中,在95~120℃的烘箱中反应3~12h;(3)水热反应后的FTO置于马弗炉中于500~800℃高温煅烧,制备出Ti‑Fe2O3光电极;(4)化学浴沉积CdS;(5)溶液沉积法沉积FeOOH制备得到FeOOH/CdS/Ti:Fe2O3复合光电极。本发明的制备方法简单,可控性强,FeOOH修饰的CdS/Ti:Fe2O3光电极提高了光生电子和空穴的分离效率和稳定性,具有优异的光电催化性能。
Description
技术领域
本发明涉及纳米材料领域,具体涉及一种FeOOH/CdS/Ti:Fe2O3复合光电极及其制备方法。
背景技术
能源是人类赖以生存和发展的物质基础。近几十年来,随着煤、石油、天然气等化石能源的日渐枯竭和与之伴随的环境污染问题的日益严峻,人类社会的可持续发展受到了严重的威胁,开发清洁的可再生能源已经迫在眉睫。与此同时,因为具有清洁无污染、分布广泛、取之不尽和用之不竭的优点,太阳能越来越受到人们的重视并开始在现有的能源结构中扮演重要的角色。纳米半导体光催化剂是一种纳米尺度的半导体催化剂,通常由一些窄带隙的氧化物或硫化物通过各种物理或化学方法制备而成,其优点在于不需要额外的能量,只需要吸收太阳光就能实现光催化,分解水产生氢气以及分解废水中的有机物,有效的解决目前人类所面临的环境问题和能源问题。
α-Fe2O3纳米材料由于其禁带宽度窄 (2.0-2.2 eV),对太阳光中的紫外光和可见光均具有良好的光电化学响应,理论研究表明纳米α-Fe2O3光电极的最大光生电流密度可达12.6 mA/cm2,相应的太阳能-氢能的转换效率可达15.5 %。除此之外,纳米α-Fe2O3还具有光电催化性能稳定、来源丰富、对环境友好和价格低廉的优点。因此,α-Fe2O3纳米材料作为一种非常有前途的可见光光催化剂,已经成为半导体光电催化分解水产氢领域的研究热点之一。但是由于α-Fe2O3纳米材料的导带位置不合适、光生空穴扩散距离短、导电性差,导致其光生载流子的复合速率快、存活寿命短,从而也使其光电转化效率远低于理论值。因而,近年来人们采取了多种修饰方法对纳米α-Fe2O3进行改性以提高其光电催化分解水的活性,比如离子掺杂、形貌调控、半导体复合等。
已有研究表明,CdS敏化的Fe2O3可以提高光生电子-空穴的分离效率。本发明制备CdS敏化的Ti掺杂的Fe2O3,但CdS/Ti:Fe2O3异质结存在严重的光腐蚀。因此,为了提高CdS/Ti:Fe2O3光电极的稳定性和光电性能,本发明通过溶液沉积法在CdS表面沉积超薄的FeOOH层。FeOOH一方面可以提高光生空穴传递速率,另一方面作为保护层,阻碍CdS的光腐蚀现象产生。本发明对金属氧化物与金属硫化物进行表面修饰,成功制备出了一种高效的三元复合光电极,在光电化学应用领域有重要的意义。
发明内容
为了克服上述三氧化二铁光电极中的缺点和不足,本发明的目的在于提供一种FeOOH/CdS/Ti:Fe2O3复合光电极及其制备方法。
本发明的目的通过以下技术方案实现。
一种FeOOH/CdS/Ti:Fe2O3复合光电极的制备方法,包括如下步骤:
(1)清洗导电玻璃FTO;
(2)将FeCl3·6H2O和尿素溶于水中,得到混合溶液;
(3)在步骤(2)的混合溶液中加入钛源,得到水热溶液;
(4)将步骤(3)中的水热溶液倒入反应釜内衬中,然后将步骤(1)清洗得到的FTO垂直或倾斜放入所述反应釜内衬中;
(5)将步骤(4)的反应釜密封之后,置于90~130℃的烘箱中进行水热反应;
(6)水热反应之后,取出FTO(FTO上形成β-FeOOH膜),将FTO置于马弗炉,在550~750℃下高温煅烧,制备出Ti:Fe2O3光电极;
(7)化学浴沉积CdS,将Ti:Fe2O3光电极置入含有Cd(NO3)2·4H2O和硫代乙酰胺的溶液中,加热到40~50℃沉积,制备得到CdS/ Ti:Fe2O3光电极;
(8)溶液沉积法沉积FeOOH,将步骤(2)中配制的混合溶液加热到90~130℃,再将步骤(7)中的CdS/Ti:Fe2O3光电极浸泡在混合溶液中,制备得到FeOOH/CdS/Ti:Fe2O3复合光电极。
优选的,步骤(2)所述的FeCl3·6H2O 、尿素在水热溶液中的浓度分别为0.1~0.2M和0.1~0.2M。
优选的,步骤(3)中钛源的用量为10~20μL。
优选的,步骤(3)所述钛源为三氯化钛和四氯化钛中的至少一种。
优选的,步骤(5)所述水热反应的时间为3~12h。
优选的,步骤(6)所述高温煅烧的时间为0.5~2.5h。
优选的,步骤(7)所述含有Cd(NO3)2·4H2O和硫代乙酰胺的溶液中Cd(NO3)2·4H2O的浓度为5~25mM,硫代乙酰胺的浓度为5~25mM。
优选的,步骤(7)所述沉积的时间为5~15min。
优选的,步骤(8)所述浸泡的时间为5~25min。
优选的,步骤(8)所述水热溶液的用量为50~100mL。
由以上所述的制备方法制得的一种FeOOH/CdS/Ti:Fe2O3复合光电极。本发明通过溶液沉积法在CdS/Ti:Fe2O3表面沉积FeOOH,使其光电催化性能得到了进一步地提高。
与现有技术相比,本发明具有以下优点及有益效果:
(1)本发明采用廉价易得的原料制备,制备条件容易实现,制备周期短。
(2)本发明采用光辅助电化学沉积羟基氧化铁助催化剂的方法对CdS/Ti:Fe2O3光电极进行了改性处理,实现了光生电子-空穴的有效分离,光电流可达2.5mA/cm2,制备得到的FeOOH/CdS/Ti:Fe2O3光电极具有优异的光电催化性能。
附图说明
图1是实施例1中所得到的FeOOH/CdS/Ti:Fe2O3复合光电极的扫描电镜图。
具体实施方式
下面结合实施例对本发明作进一步详细的描述,但本发明的实施方式并不限于此。
实施例1
(1)依次用丙酮、无水乙醇和去离子水超声清洗导电玻璃FTO,置于60℃烘箱中干燥;配制60ml含有0.1M FeCl3·6H2O和0.1M尿素的水热溶液,加入10μL的三氯化钛。将溶液转移到反应釜内衬,然后,将清洗得到的FTO垂直放入内衬中;将反应釜密封之后,置于90℃的烘箱中反应12h;水热反应之后,在FTO上形成β-FeOOH膜,冲洗后在550℃高温煅烧2.5h,制备出Ti:Fe2O3光电极。
(2)化学浴沉积CdS,将步骤(1)的Ti:Fe2O3光电极置入含有25mM Cd(NO3)2·4H2O和25mM 硫代乙酰胺的水溶液中,加热到50℃沉积5min,制备得到CdS敏化掺钛的α-Fe2O3光电极;
(3)溶液沉积法沉积FeOOH,量取50mL步骤(1)中配制的水热溶液,加热到90℃,将步骤(7)中的CdS敏化掺钛的α-Fe2O3光电极浸入水热溶液5min,制备得到FeOOH/CdS/Ti:Fe2O3复合光电极,扫描电镜图如图1所示。
(4)在1M氢氧化钠和0.1M硫化钠电解质溶液中,在AM 1.5G模拟太阳光的照射下,对制备得到FeOOH/CdS/Ti:Fe2O3复合光电极进行电化学测试。
测试结果:光电流起始电位为-0.45V vs. RHE,在电势为1.23V vs. RHE下,光电流密度为1.2mA/cm2。
实施例2
(1)依次用丙酮、无水乙醇和去离子水超声清洗导电玻璃FTO,置于60℃烘箱中干燥;配制60ml含有0.15M FeCl3·6H2O和0.15M尿素的水热溶液,加入10μL的三氯化钛。将溶液转移到反应釜内衬,然后,将清洗得到的FTO垂直放入内衬中;将反应釜密封之后,置于110℃的烘箱中反应7.5h;水热反应之后,在FTO上形成β-FeOOH膜,冲洗后在650℃高温煅烧1.5h,制备出Ti:Fe2O3光电极。
(2)化学浴沉积CdS,将步骤(1)的Ti:Fe2O3光电极置入含有15mM Cd(NO3)2·4H2O和15mM 硫代乙酰胺的水溶液中,加热到45℃沉积10min,制备得到CdS敏化掺钛的α-Fe2O3光电极;
(3)溶液沉积法沉积FeOOH,量取50mL步骤(1)中配制的水热溶液,加热到110℃,将步骤(7)中的CdS敏化掺钛的α-Fe2O3光电极浸入水热溶液25min,制备得到FeOOH/CdS/Ti:Fe2O3复合光电极。
(4)在1M氢氧化钠和0.1M硫化钠电解质溶液中,在AM 1.5G模拟太阳光的照射下,对制备得到FeOOH/CdS/Ti:Fe2O3复合光电极进行电化学测试。
测试结果:光电流起始电位为-0.50V vs. RHE,在电势为1.23V vs. RHE下,光电流密度为0.9mA/cm2。
实施例3
(1)依次用丙酮、无水乙醇和去离子水超声清洗导电玻璃FTO,置于60℃烘箱中干燥;配制60ml含有0.2M FeCl3·6H2O和0.2M尿素的水热溶液,加入10μL的三氯化钛。将溶液转移到反应釜内衬,然后,将清洗得到的FTO垂直放入内衬中;将反应釜密封之后,置于100℃的烘箱中反应6h;水热反应之后,在FTO上形成β-FeOOH膜,冲洗后在750℃高温煅烧0.5h,制备出Ti:Fe2O3光电极。
(2)化学浴沉积CdS,将步骤(1)的Ti:Fe2O3光电极置入含有5mM Cd(NO3)2·4H2O和5mM硫代乙酰胺的水溶液中,加热到40℃沉积15min,制备得到CdS敏化掺钛的α-Fe2O3光电极;
(3)溶液沉积法沉积FeOOH,量取100mL步骤(1)中配制的水热溶液,加热到130℃,将步骤(7)中的CdS敏化掺钛的α-Fe2O3光电极浸入水热溶液15min,制备得到FeOOH/CdS/Ti:Fe2O3复合光电极。
(4)在1M氢氧化钠和0.1M硫化钠电解质溶液中,在AM 1.5G模拟太阳光的照射下,对制备得到FeOOH/CdS/Ti:Fe2O3复合光电极进行电化学测试。
测试结果:光电流起始电位为-0.48V vs. RHE,在电势为1.23V vs. RHE下,光电流密度为1.0mA/cm2。
实施例4
(1)依次用丙酮、无水乙醇和去离子水超声清洗导电玻璃FTO,置于60℃烘箱中干燥;配制60ml含有0.15M FeCl3·6H2O和0.15M尿素的水热溶液,加入10μL的三氯化钛。将溶液转移到反应釜内衬,然后,将清洗得到的FTO垂直放入内衬中;将反应釜密封之后,置于110℃的烘箱中反应7.5h;水热反应之后,在FTO上形成β-FeOOH膜,冲洗后在750℃高温煅烧0.5h,制备出Ti:Fe2O3光电极。
(2)化学浴沉积CdS,将步骤(1)的Ti:Fe2O3光电极置入含有10mM Cd(NO3)2·4H2O和10mM 硫代乙酰胺的水溶液中,加热到40℃沉积10min,制备得到CdS敏化掺钛的α-Fe2O3光电极;
(3)溶液沉积法沉积FeOOH,量取75mL步骤(1)中配制的水热溶液,加热到100℃,将步骤(7)中的CdS敏化掺钛的α-Fe2O3光电极浸入水热溶液15min,制备得到FeOOH/CdS/Ti:Fe2O3复合光电极。
(4)在1M氢氧化钠和0.1M硫化钠电解质溶液中,在AM 1.5G模拟太阳光的照射下,对制备得到FeOOH/CdS/Ti:Fe2O3复合光电极进行电化学测试。
测试结果:光电流起始电位为-0.40 V vs. RHE,在电势为1.23V vs. RHE 下,光电流密度为2.5mA/cm2。
可见,本发明采用光辅助电化学沉积羟基氧化铁助催化剂的方法对CdS/Ti:Fe2O3光电极进行了改性处理,实现了光生电子-空穴的有效分离,光电流可达2.5mA/cm2,制备得到的FeOOH/CdS/Ti:Fe2O3光电极具有优异的光电催化性能。
Claims (10)
1.一种FeOOH/CdS/Ti:Fe2O3复合光电极的制备方法,其特征在于,包括如下步骤:
(1)清洗导电玻璃FTO;
(2)将FeCl3·6H2O和尿素溶于水中,得到混合溶液;
(3)在步骤(2)的混合溶液中加入钛源,得到水热溶液;
(4)将步骤(3)中的水热溶液倒入反应釜内衬中,然后将步骤(1)清洗得到的FTO垂直或倾斜放入所述反应釜内衬中;
(5)将步骤(4)的反应釜密封之后,置于90~130 ℃的烘箱中进行水热反应;
(6)水热反应之后,取出FTO,将FTO置于马弗炉,在550~750℃下高温煅烧,制备出Ti:Fe2O3光电极;
(7)将Ti:Fe2O3光电极放入含有Cd(NO3)2·4H2O和硫代乙酰胺的溶液中,加热到40~50℃沉积,制备得到CdS/ Ti:Fe2O3光电极;
(8)将步骤(2)中配制的混合溶液加热到90~130℃,再将步骤(7)中的CdS/ Ti:Fe2O3光电极浸泡在混合溶液中,制备得到FeOOH/CdS/Ti:Fe2O3复合光电极。
2.根据权利要求1所述的制备方法,其特征在于,步骤(2)所述的FeCl3·6H2O 、尿素在水热溶液中的浓度分别为0.1~0.2M和0.1~0.2M。
3.根据权利要求1所述的制备方法,其特征在于,步骤(3)中钛源的用量为10~20μL。
4.根据权利要求1所述的制备方法,其特征在于,步骤(3)所述钛源为三氯化钛和四氯化钛中的至少一种。
5.根据权利要求1所述的制备方法,其特征在于,步骤(5)所述水热反应的时间为3~12h。
6.根据权利要求1所述的制备方法,其特征在于,步骤(6)所述高温煅烧的时间为0.5~2.5h。
7.根据权利要求1所述的制备方法,其特征在于,步骤(7)所述含有Cd(NO3)2·4H2O和硫代乙酰胺的溶液中Cd(NO3)2·4H2O的浓度为5~25mM,硫代乙酰胺的浓度为5~25mM。
8.根据权利要求1所述的制备方法,其特征在于,步骤(7)所述沉积的时间为5~15min。
9.根据权利要求1所述的制备方法,其特征在于,步骤(8)所述浸泡的时间为5~25min。
10.由权利要求1-9任一项所述的制备方法制得的一种FeOOH/CdS/Ti:Fe2O3复合光电极。
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