技术领域technical field
本发明涉及一种光电化学电池电极的制备方法，尤其涉及一种通过在半导体材料上复合共催化剂制备光电化学电池纳米结构光电极的方法。The invention relates to a method for preparing a photoelectrochemical battery electrode, in particular to a method for preparing a photoelectrochemical battery nanostructure photoelectrode by compounding a co-catalyst on a semiconductor material.
背景技术Background technique
氢能，是热值很高的能源，其热值是相同质量汽油的2.7倍，而且氢气完全燃烧的产物是水，不会对环境有任何污染。因而开发低能耗高效的氢气生产方法，已成为国内外纵多科学家共同关注的问题。现在高效常见的制氢方式主要是电解水，还有其他如生物制氢等手段。但是这却需要额外的能量，限制了其发展。太阳能是一种取之不尽、用之不竭的自然资源，能否利用太阳能来直接分解水制氢成为制氢领域中的研究热点。而现在利用半导体材料组装光电化学电池利用太阳光来分解水产生氢气为制氢提供了新的可能途径。Hydrogen energy is an energy source with a high calorific value, its calorific value is 2.7 times that of gasoline of the same quality, and the product of complete combustion of hydrogen is water, which will not cause any pollution to the environment. Therefore, the development of low-energy and high-efficiency hydrogen production methods has become a common concern of many scientists at home and abroad. Nowadays, the most efficient and common hydrogen production method is mainly electrolysis of water, and there are other methods such as biological hydrogen production. But this requires extra energy, which limits its development. Solar energy is an inexhaustible and inexhaustible natural resource. Whether solar energy can be used to directly decompose water to produce hydrogen has become a research hotspot in the field of hydrogen production. Now, using semiconductor materials to assemble photoelectrochemical cells and using sunlight to split water to generate hydrogen provides a new possible way for hydrogen production.
自从1972年日本的Fujishima和Honda首次发现金红石型TiO2单晶电极能在进紫外光照射下能使水在常温下分解为氢气和氧气以来，大光催化分解制取氢气领域出现了大量的研究。目前光催化分解水的最大问题是效率比较低，主要由4个因素引起：(1)太阳能利用率低；(2)光量子产率低；(3)能级不匹配；(4)逆反应载流子复合。所以研究出新型、高效的光催化材料是现在众多科研者努力的目标。Since Fujishima and Honda in Japan discovered for the first time in 1972 that the rutile TiO2 single crystal electrode can decompose water into hydrogen and oxygen at room temperature under the irradiation of ultraviolet light, there has been a lot of research in the field of photocatalytic decomposition to produce hydrogen . At present, the biggest problem of photocatalytic water splitting is relatively low efficiency, which is mainly caused by 4 factors: (1) low solar energy utilization rate; (2) low photon quantum yield; (3) energy level mismatch; (4) reverse reaction carrying current Subcompound. Therefore, it is the goal of many researchers to develop new and efficient photocatalytic materials.
就提高光吸收方面，可进行的手段有主要有：(1)带隙修饰。通过本征掺杂或非本征掺杂，改变材料的带隙结构，使之光谱吸收边红移，达到吸收更多太阳光的目的；(2)染料敏化或量子点敏化。用作染料敏化或量子点敏化的材料本身能吸收额外的太阳光，因而增加了单一材料的光吸收。In terms of improving light absorption, the main methods available are: (1) Bandgap modification. Through intrinsic doping or extrinsic doping, the bandgap structure of the material is changed, and the spectral absorption edge is red-shifted to achieve the purpose of absorbing more sunlight; (2) dye sensitization or quantum dot sensitization. Materials used as dye-sensitized or quantum-dot-sensitized materials themselves absorb additional sunlight, thereby increasing the light absorption of a single material.
就改善载流子传输方面，可进行的手段有：(1)构建异质结。异质结可以利用其内建电场抑制电子空穴对的复合，加速载流子的分离；(2)共催化剂修饰。共催化剂可以加速电子或空穴与电解液中的反应物反应；(3)等离子效应。等离子材料不仅可以产生多余的热电子，还可以产生局部电磁场，加速电子空穴分离。In terms of improving carrier transport, the available means are: (1) Constructing a heterojunction. The heterojunction can use its built-in electric field to inhibit the recombination of electron-hole pairs and accelerate the separation of carriers; (2) co-catalyst modification. The co-catalyst can accelerate the reaction of electrons or holes with the reactants in the electrolyte; (3) plasma effect. Plasmonic materials can not only generate redundant thermal electrons, but also generate local electromagnetic fields to accelerate electron-hole separation.
简言之，利用半导体材料的光催化作用分解水制氢仍然有很多问题需要攻克，但是这种手段确实是简洁环保的制氢方法。可以预测通过众多科研工作者的努力，在突破光解水效率低等缺点和其他一些技术难题后，太阳能分解水制氢必将是未来一向重要的造福地球的产业。In short, there are still many problems to be overcome in using the photocatalysis of semiconductor materials to split water to produce hydrogen, but this method is indeed a simple and environmentally friendly method for hydrogen production. It can be predicted that through the efforts of many scientific researchers, after breaking through the shortcomings of low photolysis water efficiency and other technical problems, solar water splitting to produce hydrogen will be an important industry that will benefit the earth in the future.
有鉴于上述的内容，本设计人，积极加以研究创新，以期创设一种通过在半导体材料上复合共催化剂制备光电化学电池纳米结构光电极的方法，使其更具有产业上的利用价值。In view of the above-mentioned content, the designer is actively researching and innovating in order to create a method for preparing a nanostructured photoelectrode of a photoelectrochemical cell by compounding a co-catalyst on a semiconductor material, so that it has more industrial value.
发明内容Contents of the invention
为解决上述技术问题，本发明的目的是提供一种制备简单，能够提高光解水效率的通过在半导体材料上复合共催化剂制备光电化学电池纳米结构光电极的方法。In order to solve the above-mentioned technical problems, the object of the present invention is to provide a method for preparing a nanostructured photoelectrode of a photoelectrochemical cell by compounding a co-catalyst on a semiconductor material, which is simple to prepare and can improve the efficiency of photolysis of water.
本发明提出的一种通过在半导体材料上复合共催化剂制备光电化学电池纳米结构光电极的方法，该光电极是由氧化铁(α-Fe2O3)纳米薄膜与氢氧化镍(Ni(OH)2)两种材料复合而成的半导体纳米结构光阳极，用于分解水制备氢气，其特征在于：包括以下步骤：The present invention proposes a method for preparing a nanostructured photoelectrodeof a photoelectrochemical cell by compounding a co-catalyston a semiconductor material. )2 ) A semiconductor nanostructured photoanode formed by compounding two materials, which is used to decompose water to prepare hydrogen, and is characterized in that it includes the following steps:
步骤(1)合成α-Fe2O3纳米薄膜；Step (1) synthesizing α-Fe2 O3 nano film;
步骤(1.1)α-Fe2O3纳米薄膜通过ALD(原子层沉积系统)技术合成，将导电基底分别在酒精，丙酮和去离子水里各超声清洗15分钟；Step (1.1) The α-Fe2 O3 nano film is synthesized by ALD (atomic layer deposition system) technology, and the conductive substrate is ultrasonically cleaned in alcohol, acetone and deionized water for 15 minutes respectively;
步骤(1.2)把清洗好的导电基底放入250℃的ALD(原子层沉积系统)反应腔体中，以二茂铁和臭氧分别作为铁源和氧源，在导电基底上沉积氧化铁(α-Fe2O3)，得到前期样品；Step (1.2) Put the cleaned conductive substrate into the ALD (atomic layer deposition system) reaction chamber at 250 °C, use ferrocene and ozone as the iron source and oxygen source respectively, and deposit iron oxide (α -Fe2 O3 ), to obtain the previous sample;
步骤(1.3)然后把前期样品在马弗炉中于550℃下退火烧结2小时，得到多晶结构的α-Fe2O3纳米薄膜；Step (1.3) then annealing and sintering the previous sample in a muffle furnace at 550° C. for 2 hours to obtain a polycrystalline α-Fe2 O3 nano film;
步骤(2)制备α-Fe2O3和Ni(OH)2复合样品(α-Fe2O3/Ni(OH)2)；Step (2) preparing α-Fe2 O3 and Ni(OH)2 composite samples (α-Fe2 O3 /Ni(OH)2 );
步骤(2.1)配制包含六水合硝酸镍和六次甲基四胺的均匀混合水溶液；Step (2.1) prepares the homogeneous mixed aqueous solution that comprises nickel nitrate hexahydrate and hexamethylenetetramine;
步骤(2.2)量取10mL该水溶液放置于20mL体积的聚四氟乙烯内衬的高压釜中，把上述合成的α-Fe2O3纳米薄膜在导电面朝下且以一定角度置于该高压釜内衬中，然后将高压釜加热到80℃，并在该温度下进行反应，反应结束后，待冷却到室温后，取出后期样品；Step (2.2) Measure 10mLof this aqueous solution and place it in a polytetrafluoroethylene- lined autoclave with a volume of 20mL. Then heat the autoclave to 80°C and carry out the reaction at this temperature. After the reaction is completed, after cooling to room temperature, take out the late sample;
步骤(2.3)把后期样品分别在去离子水和酒精里洗刷，然后在真空中于60℃烘干2小时，最后得到(α-Fe2O3/Ni(OH)2)复合样品。In step (2.3), wash the late-stage samples in deionized water and alcohol, and then dry them in vacuum at 60°C for 2 hours, and finally obtain (α-Fe2 O3 /Ni(OH)2 ) composite samples.
作为本发明方法的进一步改进，步骤(1.1)所述的导电基底为FTO(氟掺杂氧化锡)导电玻璃。As a further improvement of the method of the present invention, the conductive substrate described in step (1.1) is FTO (fluorine-doped tin oxide) conductive glass.
作为本发明方法的进一步改进，步骤(1.2)中所述的氧化铁(α-Fe2O3)沉积在导电基底上的厚度为10纳米。As a further improvement of the method of the present invention, the iron oxide (α-Fe2 O3 ) described in step (1.2) is deposited on the conductive substrate with a thickness of 10 nanometers.
作为本发明方法的进一步改进，步骤(2.1)中所述水溶液中六水合硝酸镍和六次甲基四胺的摩尔浓度分别为0.05mol/L和0.15mol/L。As a further improvement of the method of the present invention, the molar concentrations of nickel nitrate hexahydrate and hexamethylenetetramine in the aqueous solution described in step (2.1) are 0.05 mol/L and 0.15 mol/L respectively.
作为本发明方法的进一步改进，步骤(2.2)中所述的反应时间为30-120分钟。As a further improvement of the method of the present invention, the reaction time described in step (2.2) is 30-120 minutes.
借由上述方案，本发明至少具有以下优点：利用α-Fe2O3这种半导体材料与Ni(OH)2这种具有催化作用的共催化剂复合得到的新型的光电化学电池电极，超薄的α-Fe2O3可以减少空穴因其迁移率低和扩散长度很小而造成的严重复合作用，表面的Ni(OH)2可以迅速将α-Fe2O3价带上的空穴传输到电解液里，加速空穴同电解液里的还原物质反应。这种复合结构比单一α-Fe2O3纳米薄膜电极的在1.23V的电压下光电流提高了0.13-0.75倍多。因此该方法可以克服单一半导体尤其是α-Fe2O3的缺点，为提高光解水效率提供了切实可行的手段。By means of the above scheme, the present invention has at least the following advantages: a novel photoelectrochemical cell electrode obtained by compounding a semiconductor material such as α-Fe2 O3 with a catalytic co-catalyst Ni(OH)2 , ultrathin α-Fe2 O3 can reduce the severe recombination of holes due to its low mobility and small diffusion length, and the Ni(OH)2 on the surface can quickly transport the holes on the valence band of α-Fe2 O3 In the electrolyte, the holes are accelerated to react with the reducing substances in the electrolyte. Compared with the single α-Fe2 O3 nanometer film electrode, the photocurrent of this composite structure is increased by 0.13-0.75 times under the voltage of 1.23V. Therefore, this method can overcome the shortcomings of a single semiconductor, especially α-Fe2 O3 , and provides a practical means for improving the efficiency of photo-splitting water.
通过这种方法构建的半导体光电极具有促进电子空穴对有效分离，减少复合和加速电荷与电解液的反应，降低过电势的作用，因此这种电极可以克服单一半导体载流子迁移率低，过电势高的缺点，提高传统单一半导体电极光电转化效率，提高光解水效率。这种方法工艺比较简单，具有大规模生产的潜在应用价值。The semiconductor photoelectrode constructed by this method can promote the effective separation of electron-hole pairs, reduce recombination and accelerate the reaction of charges and electrolyte, and reduce the overpotential, so this electrode can overcome the low mobility of single semiconductor carriers, The disadvantage of high overpotential improves the photoelectric conversion efficiency of traditional single semiconductor electrodes and improves the efficiency of photolysis of water. This method has a relatively simple process and has potential application value in large-scale production.
上述说明仅是本发明技术方案的概述，为了能够更清楚了解本发明的技术手段，并可依照说明书的内容予以实施，以下以本发明的较佳实施例并配合附图详细说明如后。The above description is only an overview of the technical solutions of the present invention. In order to understand the technical means of the present invention more clearly and implement them according to the contents of the description, the preferred embodiments of the present invention and accompanying drawings are described in detail below.
附图说明Description of drawings
图1为本发明所制备的复合电极材料结构的SEM(扫描电子显微镜)图；Fig. 1 is the SEM (scanning electron microscope) figure of the composite electrode material structure prepared by the present invention;
图2为本发明实施例一中复合结构电极在不同电压下的光分解水的特性曲线图。Fig. 2 is a characteristic curve of the photo-splitting water of the composite structure electrode in the first embodiment of the present invention under different voltages.
具体实施方式Detailed ways
下面结合附图和实施例，对本发明的具体实施方式作进一步详细描述。以下实施例用于说明本发明，但不用来限制本发明的范围。The specific implementation manners of the present invention will be further described in detail below in conjunction with the accompanying drawings and embodiments. The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention.
本发明提供了一种光电化学电池分解水工作电极的制备技术。所述的工作电极时通过在半导体表面复合共催化剂制备纳米复合结构的方法，制备出新型的光电化学电池电极。具体方法为先通过ALD技术在FTO导电基底上合成α-Fe2O3纳米薄膜，然后通过水热法在α-Fe2O3薄膜上生长Ni(OH)2，最后得到α-Fe2O3/Ni(OH)2复合结构。将制备的电极材料制作成电极后，用之作为光电化学电池的工作电极，Pt电极作为对电极。光照射到工作电极后，α-Fe2O3受激发产生电子空穴对，分离后，电子传到Pt电极与电解液里的H+发生还原反应2H++2e-→H2。空穴经Ni(OH)2与电解液里的还原物反应。通过这样的反应，实现了半导体材料的光催化反应，实现了对水的分解制氢。The invention provides a preparation technology of a photoelectrochemical cell splitting water working electrode. The working electrode is a novel photoelectrochemical cell electrode prepared by compounding a co-catalyst on the surface of a semiconductor to prepare a nanocomposite structure. The specific method is to synthesize α-Fe2 O3 nano film on the FTO conductive substrate by ALD technology, then grow Ni(OH)2 on the α-Fe2 O3 film by hydrothermal method, and finally obtain α-Fe2 O3 /Ni(OH)2 composite structure. After the prepared electrode material is made into an electrode, it is used as the working electrode of the photoelectrochemical cell, and the Pt electrode is used as the counter electrode. After light irradiates the working electrode, α-Fe2 O3 is excited to generate electron-hole pairs. After separation, the electrons pass to the Pt electrode and undergo a reduction reaction with H+ in the electrolyte 2H+ +2e- → H2 . The holes react with the reducing substances in the electrolyte via Ni(OH)2 . Through such a reaction, the photocatalytic reaction of the semiconductor material is realized, and the decomposition of water to produce hydrogen is realized.
实施例1：将FTO(氟掺杂氧化锡)导电玻璃分别在酒精，丙酮和去离子水里各超声清洗15分钟。把上述洗好的导电玻璃基底放入250℃的ALD(原子层沉积系统)反应腔体中，以二茂铁和臭氧分别作为铁源和氧源，在基底上沉积10纳米厚的氧化铁，得到前期样品，然后把前期样品放置在马弗炉中于550℃下退火烧结2小时，得到多晶结构的α-Fe2O3纳米薄膜。配制包含0.05mol/L六水合硝酸镍和0.15mol/L六次甲基四胺的均匀混合水溶液。量取10mL该溶液于20mL体积的聚四氟乙烯内衬的高压釜中，把上述合成的α-Fe2O3纳米薄膜样品，导电面朝下且以一定角度置于该高压釜内衬中，然后将高压釜加热到80℃，并在该温度下反应30分钟。反应结束后，待冷却到室温后，取出后期样品。最后把后期样品分别在去离子水和酒精里洗刷，然后在真空中于60℃烘干2小时，最后得到α-Fe2O3/Ni(OH)2复合样品。样品形貌结构如图1所示。如图2所示，复合结构电极在1.23V的电压下光电流达到了0.369mA/cm2是α-Fe2O3的1.75倍。Example 1: FTO (fluorine-doped tin oxide) conductive glass was ultrasonically cleaned in alcohol, acetone and deionized water for 15 minutes respectively. Put the above-mentioned washed conductive glass substrate into an ALD (atomic layer deposition system) reaction chamber at 250°C, use ferrocene and ozone as iron source and oxygen source respectively, and deposit iron oxide with a thickness of 10 nanometers on the substrate. The preliminary sample was obtained, and then placed in a muffle furnace for annealing and sintering at 550° C. for 2 hours to obtain a polycrystalline α-Fe2 O3 nano film. A homogeneously mixed aqueous solution comprising 0.05 mol/L nickel nitrate hexahydrate and 0.15 mol/L hexamethylenetetramine was prepared. Measure 10mL of this solution in a polytetrafluoroethylene-lined autoclave with a volume of 20mL, and place the above-mentioned synthesized α-Fe2 O3 nanometer film sample with the conductive surface facing down and place it in the autoclave lining at a certain angle. , and then the autoclave was heated to 80° C., and reacted at this temperature for 30 minutes. After the reaction was completed, after cooling to room temperature, the later samples were taken out. Finally, wash the late-stage samples in deionized water and alcohol, and then dry them in vacuum at 60°C for 2 hours to obtain α-Fe2 O3 /Ni(OH)2 composite samples. The morphology of the sample is shown in Figure 1. As shown in Figure 2, the photocurrent of the composite structure electrode reaches 0.369mA/cm2 at a voltage of 1.23V, which is 1.75 times that of α-Fe2 O3 .
实施例2：将FTO(氟掺杂氧化锡)导电玻璃分别在酒精，丙酮和去离子水里各超声清洗15分钟。把上述洗好的导电玻璃基底放入250℃的ALD(原子层沉积系统)反应腔体中，以二茂铁和臭氧分别作为铁源和氧源，在基底上沉积10纳米厚的氧化铁，得到前期样品。然后把前期样品放置在马弗炉中于550℃下退火烧结2小时，得到多晶结构的α-Fe2O3纳米薄膜。配制包含0.05mol/L六水合硝酸镍和0.15mol/L六次甲基四胺的均匀混合水溶液。量取10mL该溶液于20mL体积的聚四氟乙烯内衬的高压釜中，把上述合成的α-Fe2O3纳米薄膜样品，导电面朝下且以一定角度置于该高压釜内衬中，然后将高压釜加热到80℃，并在该温度下反应60分钟。反应结束后，待冷却到室温后，取出后期样品。最后把后期样品分别在去离子水和酒精里洗刷，然后在真空中于60℃烘干2小时，最后得到α-Fe2O3/Ni(OH)2复合样品。这种复合结构在1.23V的电压下光电流达到了0.316mA/cm2是α-Fe2O3的1.50倍。Example 2: FTO (fluorine-doped tin oxide) conductive glass was ultrasonically cleaned in alcohol, acetone and deionized water for 15 minutes respectively. Put the above-mentioned washed conductive glass substrate into an ALD (atomic layer deposition system) reaction chamber at 250°C, use ferrocene and ozone as iron source and oxygen source respectively, and deposit iron oxide with a thickness of 10 nanometers on the substrate. Get early samples. Then the early stage sample was placed in a muffle furnace and annealed and sintered at 550° C. for 2 hours to obtain a polycrystalline α-Fe2 O3 nano film. A homogeneously mixed aqueous solution comprising 0.05 mol/L nickel nitrate hexahydrate and 0.15 mol/L hexamethylenetetramine was prepared. Measure 10mL of this solution in a polytetrafluoroethylene-lined autoclave with a volume of 20mL, and place the above-mentioned synthesized α-Fe2 O3 nanometer film sample with the conductive surface facing down and place it in the autoclave lining at a certain angle. , and then the autoclave was heated to 80° C., and reacted at this temperature for 60 minutes. After the reaction was completed, after cooling to room temperature, the later samples were taken out. Finally, wash the late-stage samples in deionized water and alcohol, and then dry them in vacuum at 60°C for 2 hours to obtain α-Fe2 O3 /Ni(OH)2 composite samples. The photocurrent of this composite structure reached 0.316mA/cm2 at a voltage of 1.23V, which is 1.50 times that of α-Fe2 O3 .
实施例3：将FTO(氟掺杂氧化锡)导电玻璃分别在酒精，丙酮和去离子水里各超声清洗15分钟。把上述洗好的导电玻璃基底放入250℃的ALD(原子层沉积系统)反应腔体中，以二茂铁和臭氧分别作为铁源和氧源，在基底上沉积10纳米厚的氧化铁，得到前期样品。然后前期把样品放置在马弗炉中于550℃下退火烧结2小时，得到多晶结构的α-Fe2O3纳米薄膜。配制包含0.05mol/L六水合硝酸镍和0.15mol/L六次甲基四胺的均匀混合水溶液。量取10mL该溶液于20mL体积的聚四氟乙烯内衬的高压釜中，把上述合成的α-Fe2O3纳米薄膜样品，导电面朝下且以一定角度置于该高压釜内衬中，然后将高压釜加热到80℃，并在该温度下反应90分钟。反应结束后，待冷却到室温后，取出后期样品。最后把后期样品分别在去离子水和酒精里洗刷，然后在真空中于60℃烘干2小时，最后得到α-Fe2O3/Ni(OH)2复合样品。这种复合结构在1.23V的电压下光电流达到了0.238mA/cm2是α-Fe2O3的1.13倍。Example 3: FTO (fluorine-doped tin oxide) conductive glass was ultrasonically cleaned in alcohol, acetone and deionized water for 15 minutes respectively. Put the above-mentioned washed conductive glass substrate into an ALD (atomic layer deposition system) reaction chamber at 250°C, use ferrocene and ozone as iron source and oxygen source respectively, and deposit iron oxide with a thickness of 10 nanometers on the substrate. Get early samples. Then the sample was placed in a muffle furnace for annealing and sintering at 550° C. for 2 hours to obtain a polycrystalline α-Fe2 O3 nano film. A homogeneously mixed aqueous solution comprising 0.05 mol/L nickel nitrate hexahydrate and 0.15 mol/L hexamethylenetetramine was prepared. Measure 10mL of this solution in a polytetrafluoroethylene-lined autoclave with a volume of 20mL, and place the above-mentioned synthesized α-Fe2 O3 nanometer film sample with the conductive surface facing down and place it in the autoclave lining at a certain angle. , and then the autoclave was heated to 80° C., and reacted at this temperature for 90 minutes. After the reaction was completed, after cooling to room temperature, the later samples were taken out. Finally, wash the late-stage samples in deionized water and alcohol, and then dry them in vacuum at 60°C for 2 hours to obtain α-Fe2 O3 /Ni(OH)2 composite samples. The photocurrent of this composite structure reached 0.238mA/cm2 at a voltage of 1.23V, which is 1.13 times that of α-Fe2 O3 .
以上所述仅是本发明的优选实施方式，并不用于限制本发明，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明技术原理的前提下，还可以做出若干改进和变型，这些改进和变型也应视为本发明的保护范围。The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention. It should be pointed out that for those of ordinary skill in the art, some improvements can be made without departing from the technical principle of the present invention. and modifications, these improvements and modifications should also be considered as the protection scope of the present invention.
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