WO2018133197A1 - 一种具有多层BiVO4的电极、其制备方法及其在光电催化中的用途 - Google Patents

一种具有多层BiVO4的电极、其制备方法及其在光电催化中的用途 Download PDF

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WO2018133197A1
WO2018133197A1 PCT/CN2017/077880 CN2017077880W WO2018133197A1 WO 2018133197 A1 WO2018133197 A1 WO 2018133197A1 CN 2017077880 W CN2017077880 W CN 2017077880W WO 2018133197 A1 WO2018133197 A1 WO 2018133197A1
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bivo
electrode
layers
photoelectrode
layer
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邹吉军
武金梦
潘伦
张香文
王莅
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Tianjin University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/8647—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites
    • H01M4/8657—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites layered
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88—Processes of manufacture
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88—Processes of manufacture
    • H01M4/8825—Methods for deposition of the catalytic active composition
    • H01M4/8853—Electrodeposition
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/90—Selection of catalytic material
    • H01M4/92—Metals of platinum group
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

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  • the invention belongs to the field of catalysts, and in particular relates to an electrode with a plurality of layers of BiVO 4 , a preparation method thereof and application thereof in photoelectrocatalysis.
  • the research on the photoelectric activity of BiVO 4 mainly focuses on doping and constructing heterojunctions (including Z-scheme and pn junctions), but even so, the photocurrent density is only about 2 mA/cm 2 , which is relatively lower than the theoretical value. .
  • Kim and Choi used the electrochemical deposition method to grow BiOI in situ on FTO conductive glass, and obtained high-temperature calcination to obtain BiVO 4 after introduction of V source. Adding Na 2 SO 3 as an electrolyte in a phosphate buffer solution, the photocurrent density was measured at 1.1 V (vs RHE) of about 4 mA/cm 2 (Kim TW, Choi K S. Science, 2014, 343 (6174) :990-994.). However, this method has a large difference in repeatability in subsequent studies. For example, Gan et al.
  • Lee et al. used electrochemical deposition to synthesize BiOI, which was then converted to BiVO 4 , and the photocurrent was only 0.14 mA/cm 2 at 1.1 V (vs RHE). It is modified by a synthetic pn junction, which reports the formation and activity of four pn junctions, including TiO 2 -BiVO 4 junctions, Fe 2 O 3 -BiVO 4 junctions, SnO 2 -BiVO 4 junctions, and WO 3 -BiVO 4 knot, wherein WO 3 -BiVO 4 has the best performance and a current of 0.8 mA/cm 2 . (Lee M G, et al. Nano Energy, 2016, 28: 250-260.)
  • the present invention synthesizes a highly active multilayer BiVO 4 photoelectrode based on an electrochemical deposition method.
  • the invention utilizes electrochemical deposition to form a layer of BiOI in situ on the FTO conductive glass, and then synthesizes a layer of high activity BiVO 4 by simple calcination; repeats the electrochemical deposition and calcination steps to obtain a multilayer BiVO 4 photoelectrode;
  • the photocurrent is 4.3 mA/cm 2 at a voltage of 1.1 V (vs RHE), the solar energy utilization efficiency is as high as 56.6%, and the activity is 2 to 3 times higher than that reported in other literatures.
  • a first aspect of the invention relates to a multilayer BiVO 4 photoelectrode, the electrode body being an FTO conductive glass on which a plurality of layers of BiVO 4 are deposited, the plurality of layers being three or more layers, each layer being independently of thickness 0.90 to 3.50 ⁇ m.
  • the plurality of layers are six layers, and the thickness of each layer outward along the FTO conductive glass is 0.970 ⁇ m, 1.090 ⁇ m, 1.272 ⁇ m, 1.516 ⁇ m, 1.879 ⁇ m, and 3.333 ⁇ m, respectively.
  • a second aspect of the invention relates to a method for preparing the multilayer BiVO 4 photoelectrode, comprising the following steps:
  • step (1) dissolving p-benzoquinone in absolute ethanol, and then adding the cerium salt solution of step (1), mixing for 20 to 40 minutes to obtain a mixed solution;
  • step (3) Put the mixed liquid of step (2) into the electrolytic cell and connect the three-electrode system, wherein the working electrode is initially FTO conductive glass, the counter electrode is a platinum electrode, the reference electrode is a silver/silver chloride electrode, and the voltage is set. a -0.1 ⁇ -0.2V, scanning rate of 5 ⁇ 15mV / min, after 1 ⁇ 11min, a layer of electrochemically deposited BiOI is obtained on the FTO conductive glass;
  • the working electrode of the step (3) is a photoelectrode having a layer of BiVO 4 , that is, having two layers of BiVO 4 photoelectrodes;
  • the onium salt is one of cerium nitrate, cerium sulfate or cerium chloride.
  • a third aspect of the invention relates to the use of a multilayer BiVO 4 photoelectrode for increasing photocurrent density in photoelectrocatalysis.
  • the present invention firstly prepares a multilayer (at least three layers) BiVO 4 photoelectrode by electrochemical deposition + high temperature roasting, and the photocurrent of the three-layer BiVO 4 photoelectrode reaches 4.3 at a voltage of 1.1 V (vs RHE).
  • vs RHE 1.1 V
  • mA/cm 2 solar energy utilization efficiency is as high as 56.6%, and the activity is 2 to 3 times higher than that reported so far.
  • the inventors have unexpectedly discovered that the number of deposited layers plays a crucial role in increasing the photocurrent density. For example, when depositing 1 layer, the photocurrent at 1.1 V (vs RHE) is only 1 mA/cm 2 ; but 3 layers are deposited. The photocurrent can reach 4.3 mA/cm 2 at the same voltage.
  • the preparation method of the invention is simple, the source of raw materials is rich, the cost is low, and the prepared multilayer BiVO 4 has good batch stability and is suitable for industrial production.
  • Figure 3 is an SEM image of a four-layer BiVO 4 of the present invention.
  • Figure 4 is a Raman spectrum of a BiVO 4 electrode having a different number of deposited layers of the present invention.
  • the working electrode is FTO conductive glass
  • the electrode is a platinum electrode
  • the reference electrode is a silver/silver chloride electrode
  • the electrochemical deposition parameter voltage is -0.1V
  • the scanning rate is 10mV/min
  • the scanning time is 60s, and a layer of electrochemically deposited BiOI is obtained
  • the vanadyl oxide is dissolved in dimethyl sulfoxide, and then dropped on the surface of the obtained electrochemically deposited BiOI, and then calcined at 450 ° C for 2 h; the black green V 2 O 5 is washed away with 1 M KOH to obtain the A layer of BiVO 4 photoelectrode.
  • the photocurrent density was 1 mA/cm 2 at a voltage of 1.1 V (vs RHE). Batch stability is good (>90%).
  • the photocurrent density was 1.23 mA/cm 2 at a voltage of 1.1 V (vs RHE). Batch stability is good (>92%).
  • the parameter voltage is -0.1V, the scanning rate is 10mV/min, and the scanning time is 300s; the vanadium acetylacetonate is dissolved in dimethyl sulfoxide and then dripped on the surface of the obtained electrochemically deposited BiOI, and then at 450 ° C Calcination for 2 h; washing the black-green V 2 O 5 with an alkali solution to obtain the three-layer BiVO 4 photoelectrode.
  • the photocurrent density can reach 4.30 mA/cm 2 at a voltage of 1.1 V (vs RHE). Batch stability is good (>91%).
  • the parameter voltage is -0.1V, the scanning rate is 10mV/min, and the scanning time is 420s; the vanadium acetylacetonate is dissolved in dimethyl sulfoxide, and then dripped on the surface of the obtained electrochemically deposited BiOI, and then calcined at 450 ° C. 2h; the black-green V 2 O 5 was washed away with 1 M KOH to obtain the four-layer BiVO 4 photoelectrode. .
  • the photocurrent density was 3.38 mA/cm 2 at a voltage of 1.1 V (vs RHE). Batch stability is good (>89%).
  • the vanadium acetylacetonate is dissolved in dimethyl sulfoxide and then dripped on the surface of the obtained electrochemically deposited BiOI, and then calcined at 450 ° C. 2h; the black-green V 2 O 5 was washed away with 1 M KOH to obtain the five-layer BiVO 4 photoelectrode.
  • the photocurrent density was 2.70 mA/cm 2 at a voltage of 1.1 V (vs RHE). Batch stability is good (>86%).
  • the vanadium acetylacetonate is dissolved in dimethyl sulfoxide and then dripped on the surface of the obtained electrochemically deposited BiOI, and then at 450 ° C. Calcination for 2 h; the black-green V 2 O 5 was washed away with 1 M KOH to obtain the six-layer BiVO 4 photoelectrode.
  • the photocurrent density was 1.43 mA/cm 2 at a voltage of 1.1 V (vs RHE). Batch stability is good (>80%).

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Abstract

本发明公开了一种多层BiVO4光电电极，所述电极本体为FTO导电玻璃，其上沉积有多层BiVO4，所述多层为三层以上，每层的厚度各自独立地为0.90～3.50μm。本发明还公开了所述多层BiVO4光电电极的制备方法及用途。

Description

一种具有多层BiVO4的电极、其制备方法及其在光电催化中的用途 技术领域
本发明属于催化剂领域，具体涉及一种具有多层BiVO4的电极、其制备方法及其在光电催化应用。
背景技术
研究光电阳极催化剂性能时，合成方法的确定以及合理的形貌调控对于评价材料性能起着重要作用。自1998年Kudo等人第一次报道BiVO4可以作为一种有效的光催化剂后，由于其具有无毒、高化学稳定性和原材料便宜易得等特征而被广泛研究。目前报道方法合成BiVO4的光电流为1～2mA/cm2，离其理论最大光电流(7.6mA/cm2)相差较远。目前对BiVO4光电活性的研究主要集中在掺杂、构建异质结(包括Z-scheme和p-n结等)，但即使如此，光电流密度也只在2mA/cm2左右，相对理论值较低。
2014年，Kim和Choi利用电化学沉积法在FTO导电玻璃上原位生长BiOI，在引入V源后高温煅烧得到BiVO4。在磷酸盐缓冲溶液中加入Na2SO3作为电解液，测其光电流密度在1.1V(vs RHE)处约为4mA/cm2(Kim T W,Choi K S.Science,2014,343(6174):990-994.)。但是该方法在后续研究中重复性差异较大。例如，Gan等人在FTO玻璃上利用同样的电化学沉积的方式原位生长BiOI，引入V源后高温煅烧，但光电流密度在1.0V(vs RHE)处仅有2mA/cm2，再利用Au进行修饰后光电流密度有一定增长，但Au作为贵金属之一，严重制约了其工业应用。(Gan J,et al.Nanotechnology,2016,27(23):235401.)
Lee等人利用电化学沉积的方式合成BiOI，再转化为BiVO4，在1.1V(vs RHE)处光电流仅有0.14mA/cm2。利用合成p-n结对其进行改性，该文献报道了四种p-n结的形成及活性，包括TiO2-BiVO4结、Fe2O3-BiVO4结、SnO2-BiVO4结及WO3-BiVO4结，其中WO3-BiVO4性能最好，电流为0.8mA/cm2。(Lee M G,et al.Nano Energy,2016,28:250-260.)
以上报道的研究内容均为探究合成BiVO4的常用方法，但是存在批次差异性大、活性低、光电流密度低，对于太阳光的利用效率不高等缺点。
发明内容
为克服上述缺点，本发明基于电化学沉积法合成了高活性多层BiVO4光电电极。本发明利用电化学沉积的方式在FTO导电玻璃上原位生长一层BiOI后再通过简单煅烧方式合成一层高活性BiVO4；重复电化学沉积和煅烧步骤，即得到多层BiVO4光电电极；其光电流在电压1.1V(vs RHE)时可达4.3mA/cm2，太阳能利用效率高达56.6％，活性是其他文献报道的2～3倍以上。
本发明第一方面涉及一种多层BiVO4光电电极，所述电极本体为FTO导电玻璃，其上沉积有多层BiVO4，所述多层为三层以上，每层的厚度各自独立地为0.90～3.50μm。
优选地，所述多层为六层，沿FTO导电玻璃向外的各层厚度分别为0.970μm、1.090μm、1.272μm、1.516μm、1.879μm、3.333μm。
本发明第二方面涉及所述的多层BiVO4光电电极的制备方法，包括如下步骤：
(1)将碘盐溶于水中，用酸调节pH值至1.2～2.0，加入铋盐使其溶解得到铋盐溶液；
(2)将对苯醌溶于无水乙醇，然后加入步骤(1)的铋盐溶液，混合20～40分钟后得到混合溶液；
(3)将步骤(2)的混合液放入电解池中，连接三电极体系，其中工作电极初始为FTO导电玻璃，对电极为铂电极，参比电极为银/氯化银电极，设置电压为-0.1～-0.2V，扫描速率为5～15mV/min，时间为1～11min后，FTO导电玻璃上得到一层电化学沉积的BiOI；
(4)将乙酰丙酮氧钒溶于二甲基亚砜中，然后滴在步骤(3)得到的电化学沉积的BiOI表面上，然后在450℃下煅烧2～5h；
(5)用碱溶液洗去黑绿色V2O5，即得到具有一层BiVO4光电电极。
(6)重复上述步骤(1)～(5)，其中步骤(3)的工作电极为具有一层BiVO4的光电电极，即得到具有两层BiVO4光电电极；
重复上述步骤(1)～(5)三次以上，即得到具有多层BiVO4光电电极。
在本发明第二方面的优选实施方案中，所述铋盐为硝酸铋、硫酸铋或氯化铋之一。
本发明第三方面涉及所述的一种多层BiVO4光电电极用于在光电催化中提高光电流密度的用途。
本发明的有益效果：
1、本发明首次采用电化学沉积+高温焙烧的方法制备了多层(至少三层)BiVO4光电电极，三层的BiVO4光电电极的光电流在电压1.1V(vs RHE)时可达4.3mA/cm2，太阳能利用效率高达56.6％，活性是目前所报道的2～3倍以上。发明人意外地发现，沉积层数对光电流密度的提高起着至关重要的作用，例如：沉积1层时，在1.1V(vs RHE)光电流仅1mA/cm2；但沉积3层，相同电压下光电流可达4.3mA/cm2。
2、本发明的制备方法简单，原料来源丰富、成本较低，且制得的多层BiVO4的具有很好的批次稳定性，适宜工业化生产。
附图说明
图1为本发明的具有不同沉积层数的BiVO4电极的X射线衍射图；
图2为本发明的单层BiVO4的SEM图；
图3为本发明的四层BiVO4的SEM图；
图4为本发明的具有不同沉积层数的BiVO4电极的拉曼光谱图。
具体实施方式
实例1
将2.82g碘盐溶于50mL超纯水中，用浓盐酸将pH调到1.2，搅拌后加入0.9702g Bi(NO3)2·5H2O充分溶解；称取0.4968g对苯醌溶于20mL无水乙醇中，溶解后将上述两种溶液混合剧烈搅拌30min；利用丙酮、无水乙醇和水洗FTO玻璃，置于空气中晾干，连接好三电极体系，其中工作电极为FTO导电玻璃，对电极为铂电极，参比电极为银/氯化银电极，设置电化学沉积参数电压为-0.1V，扫描速率10mV/min，扫描时间60s，得到具有一层电化学沉积的BiOI；将乙酰丙酮氧钒溶于二甲基亚砜中，然后滴在得到的一层电化学沉积的BiOI表面上，然后在450℃下煅烧2h；用1M KOH洗去黑绿色V2O5，即得到所述的一层BiVO4光电电极。
在电压1.1V(vs RHE)时光电流密度为1mA/cm2。批次稳定性好(>90％)。
实例2
将3.02g碘盐溶于50mL超纯水中，用浓盐酸将pH调到1.4，搅拌后加入0.9702g Bi(NO3)2·5H2O充分溶解；称取0.4968g对苯醌溶于20mL无水乙醇中，溶解后将上述两种溶液混合剧烈搅拌30min；连接好三电极体系，其中工作电极 为实施例1得到的具有一层BiVO4光电电极，对电极为铂电极，参比电极为银/氯化银电极，设置参数电压为-0.1V，扫描速率10mV/min，扫描时间180s；将乙酰丙酮氧钒溶于二甲基亚砜中，然后滴在得到的电化学沉积的BiOI表面上，然后在450℃下煅烧2h；用1M KOH洗去黑绿色V2O5，即得到所述的二层BiVO4光电电极。
在电压1.1V(vs RHE)时光电流密度为1.23mA/cm2。批次稳定性好(>92％)。
实例3
将3.12g碘盐溶于50mL超纯水中，用浓硝酸将pH调到1.6，搅拌后加入0.9702g硫酸铋充分溶解；称取0.4968g对苯醌溶于20mL无水乙醇中，溶解后将上述两种溶液混合剧烈搅拌30min；连接好三电极体系，其中工作电极为实施例2得到的具有两层BiVO4光电电极，对电极为铂电极，参比电极为银/氯化银电极，设置参数电压为-0.1V，扫描速率10mV/min，扫描时间300s；；将乙酰丙酮氧钒溶于二甲基亚砜中，然后滴在得到的电化学沉积的BiOI表面上，然后在450℃下煅烧2h；用碱溶液洗去黑绿色V2O5，即得到所述的三层BiVO4光电电极。
在电压1.1V(vs RHE)时光电流密度可达4.30mA/cm2。批次稳定性好(>91％)。
实例4
将3.22g碘盐溶于50mL超纯水中，用浓硝酸将pH调到1.7，搅拌后加入0.9702g氯化铋充分溶解；称取0.4968g对苯醌溶于20mL无水乙醇中，溶解后将上述两种溶液混合剧烈搅拌30min；连接三电极体系，其中工作电极为实施例3得到的具有三层BiVO4光电电极，对电极为铂电极，参比电极为银/氯化银电极，设置参数电压为-0.1V，扫描速率10mV/min，扫描时间420s；将乙酰丙酮氧钒溶于二甲基亚砜中，然后滴在得到的电化学沉积的BiOI表面上，然后在450℃下煅烧2h；用1M KOH洗去黑绿色V2O5，即得到所述的四层BiVO4光电电极。。
在电压1.1V(vs RHE)时光电流密度为3.38mA/cm2。批次稳定性好(>89％)。
实例5
将3.32g碘盐溶于50mL超纯水中，用浓硫酸将pH调到1.8，搅拌后加入0.9702g氯化铋充分溶解；称取0.4968g对苯醌溶于20mL无水乙醇中，溶解后将上述两种溶液混合剧烈搅拌30min；连接三电极体系，其中工作电极为实施例4得到的具有四层BiVO4光电电极，对电极为铂电极，参比电极为银/氯化银电极，设置参数电压为-0.1V，扫描速率10mV/min，扫描时间540s；将乙酰丙酮氧钒溶于二甲基亚砜中，然后滴在得到的电化学沉积的BiOI表面上，然后在450℃下煅烧2h；用1M KOH洗去黑绿色V2O5，即得到所述的五层BiVO4光电电极。
在电压1.1V(vs RHE)时光电流密度为2.70mA/cm2。批次稳定性好(>86％)。
实例6
将3.42g碘盐溶于50mL超纯水中，用浓硫酸将pH调到2.0，搅拌后加入0.9702g氯化铋充分溶解；称取0.4968g对苯醌溶于20mL无水乙醇中，溶解后将上述两种溶液混合剧烈搅拌30min；连接三电极体系，其中工作电极为实施例5得到的具有五层BiVO4光电电极，对电极为铂电极，参比电极为银/氯化银电极，设置参数电压为-0.1V，扫描速率为10mV/min，扫描时间660s；将乙酰丙酮氧钒溶于二甲基亚砜中，然后滴在得到的电化学沉积的BiOI表面上，然后在450℃下煅烧2h；用1M KOH洗去黑绿色V2O5，即得到所述的六层BiVO4光电电极。
在电压1.1V(vs RHE)时光电流密度为1.43mA/cm2。批次稳定性好(>80％)。

Claims (5)

  1. 一种多层BiVO4光电电极，其特征在于，所述电极本体为FTO导电玻璃，其上沉积有多层BiVO4，所述多层为三层以上，每层的厚度各自独立地为0.90～3.50μm。
  2. 根据权利要求1所述的多层BiVO4光电电极，其特征在于，所述多层为六层，沿FTO导电玻璃向外的各层厚度分别为0.970μm、1.090μm、1.272μm、1.516μm、1.879μm、3.333μm。
  3. 一种根据权利要求1所述的多层BiVO4光电电极的制备方法，其特征在于，包括如下步骤：
    (1)将碘盐溶于水中，用酸调节pH值至1.2～2.0，加入铋盐使其溶解得到铋盐溶液；
    (2)将对苯醌溶于无水乙醇，然后加入步骤(1)的铋盐溶液，混合20～40分钟后得到混合溶液；
    (3)将步骤(2)的混合液放入电解池中，连接三电极体系，其中工作电极初始为FTO导电玻璃，对电极为铂电极，参比电极为银/氯化银电极，设置电压为-0.1～-0.2V，扫描速率为5～15mV/min，时间为1～11min后，FTO导电玻璃上得到一层电化学沉积的BiOI；
    (4)将乙酰丙酮氧钒溶于二甲基亚砜中，然后滴在步骤(3)得到的电化学沉积的BiOI表面上，然后在450℃下煅烧2～5h；
    (5)用碱溶液洗去黑绿色V2O5，即得到具有一层BiVO4光电电极。
    (6)重复上述步骤(1)～(5)，其中步骤(3)的工作电极为具有一层BiVO4的光电电极，即得到具有两层BiVO4光电电极；
    重复上述步骤(1)～(5)三次以上，即得到具有多层BiVO4光电电极。
  4. 根据权利要求3所述的制备方法，其特征在于，所述铋盐为硝酸铋、硫酸铋或氯化铋之一。
  5. 根据权利要求1所述的一种多层BiVO4光电电极用于在光电催化中提高光电流密度的用途。
PCT/CN2017/077880 2017-01-22 2017-03-23 一种具有多层BiVO4的电极、其制备方法及其在光电催化中的用途 Ceased WO2018133197A1 (zh)

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