CN113952964B - Preparation method and application of 2D/3D structured molybdenum disulfide/indium oxide nanocomposite - Google Patents
Preparation method and application of 2D/3D structured molybdenum disulfide/indium oxide nanocomposite Download PDFInfo
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- 239000002114 nanocomposite Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229910003437 indium oxide Inorganic materials 0.000 title claims abstract description 11
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 title claims abstract description 11
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 25
- 239000001257 hydrogen Substances 0.000 claims abstract description 25
- 230000001699 photocatalysis Effects 0.000 claims abstract description 24
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 21
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000004202 carbamide Substances 0.000 claims abstract description 18
- VBXWCGWXDOBUQZ-UHFFFAOYSA-K diacetyloxyindiganyl acetate Chemical compound [In+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VBXWCGWXDOBUQZ-UHFFFAOYSA-K 0.000 claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 claims abstract description 18
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229940043267 rhodamine b Drugs 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 12
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 10
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 10
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 10
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 10
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- 239000012153 distilled water Substances 0.000 claims description 28
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
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- 229910052799 carbon Inorganic materials 0.000 description 6
- 238000010586 diagram Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 238000013032 photocatalytic reaction Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
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- 239000003403 water pollutant Substances 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033558 biomineral tissue development Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
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- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
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- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
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Abstract
Description
技术领域Technical field
本发明属于纳米材料合成技术领域，利用简单的水热方法合成2D/3D结构的二硫化钼(MoS2)/氧化铟(In2O3)纳米复合材料，可用于高效光催化分解水制氢耦合光催化降解罗丹明B。The invention belongs to the technical field of nanomaterial synthesis. It uses a simple hydrothermal method to synthesize 2D/3D structured molybdenum disulfide (MoS 2 )/indium oxide (In 2 O 3 ) nanocomposite materials, which can be used for efficient photocatalytic water decomposition to produce hydrogen. Coupled photocatalytic degradation of rhodamine B.
背景技术Background technique
全球能源危机和环境污染是当今世界所面临的两大难题。目前，光催化技术具有节能、清洁、无污染等优点，在解决能源和环境问题方面受到了广泛关注。一般在光催化分解水制氢过程中，需要加入甲醇、三乙醇胺、乳酸等牺牲剂来加速光生空穴的消耗，从而实现光生电子高效参与制氢反应。然而，这些不可再生的牺牲剂是重要的化工原料，利用它们作为牺牲剂进行光催化制氢反应不符合可持续发展的要求。另一方面，以罗丹明B为代表的有机染料废水对生态***和人类健康造成了严重危害。因此，如果光催化制氢和光催化降解罗丹明B可以在一个光催化***中进行，就很有可能解决社会发展所引起的能源与环境问题。The global energy crisis and environmental pollution are two major problems facing the world today. At present, photocatalytic technology has the advantages of energy saving, cleanliness, and no pollution, and has received widespread attention in solving energy and environmental problems. Generally, in the process of photocatalytic water splitting to produce hydrogen, sacrificial agents such as methanol, triethanolamine, and lactic acid need to be added to accelerate the consumption of photogenerated holes, so that photogenerated electrons can efficiently participate in the hydrogen production reaction. However, these non-renewable sacrificial agents are important chemical raw materials, and using them as sacrificial agents for photocatalytic hydrogen production reactions does not meet the requirements of sustainable development. On the other hand, organic dye wastewater represented by rhodamine B has caused serious harm to the ecosystem and human health. Therefore, if photocatalytic hydrogen production and photocatalytic degradation of rhodamine B can be carried out in a photocatalytic system, it is very likely to solve the energy and environmental problems caused by social development.
氧化铟(In2O3)是一种典型的n型半导体材料，其带隙能约为2.8eV，由于具有优良的光化学稳定性、适宜的光吸收和无毒无害等优点，已被广泛应用于光催化分解水制氢、光催化剂降解有机污染物、光催化二氧化碳还原等反应。然而，由于其光生电子-空穴的分离、迁移速率较慢，单一的In2O3材料在光催化反应中通常展现出较低的光催化活性。二硫化钼(MoS2)是一种类似于石墨烯二维结构的过渡金属二卤族化合物，作为可替代贵金属的助催化剂，在光催化反应中受到了极大关注。例如：MoS2与TiO2构建复合材料能够显著提高光催化制氢性能；MoS2与Cu2O构建复合材料能够明显加速光催化降解染料性能。然而，目前2D/3D结构的MoS2/In2O3纳米复合材料构建及其用于光催化分解水制氢耦合光催化降解罗丹明B的相关研究还未见报道。Indium oxide (In 2 O 3 ) is a typical n-type semiconductor material with a band gap energy of approximately 2.8 eV. It has been widely used due to its excellent photochemical stability, suitable light absorption, and non-toxic and harmless properties. It can be used in photocatalytic water splitting to produce hydrogen, photocatalytic degradation of organic pollutants, photocatalytic carbon dioxide reduction and other reactions. However, due to its slow separation and migration rate of photogenerated electrons and holes, a single In 2 O 3 material usually exhibits low photocatalytic activity in photocatalytic reactions. Molybdenum disulfide (MoS 2 ) is a transition metal dihalogen compound with a two-dimensional structure similar to graphene. As a cocatalyst that can replace noble metals, it has received great attention in photocatalytic reactions. For example: composite materials constructed of MoS 2 and TiO 2 can significantly improve the photocatalytic hydrogen production performance; composite materials constructed of MoS 2 and Cu 2 O can significantly accelerate the photocatalytic degradation of dyes. However, the construction of 2D/3D structured MoS 2 /In 2 O 3 nanocomposites and their use in photocatalytic water splitting for hydrogen production coupled with photocatalytic degradation of rhodamine B have not yet been reported.
发明内容Contents of the invention
本发明的目的是提供具有2D/3D结构的MoS2/In2O3纳米复合材料的制备方法，并将2D/3D结构的MoS2/In2O3纳米复合材料用于光催化分解水制氢耦合光催化降解罗丹明B反应。该MoS2/In2O3纳米复合材料催化活性高，实现制取氢气的同时达到去除水体污染物的目的。The purpose of the present invention is to provide a preparation method of MoS 2 /In 2 O 3 nanocomposite material with 2D/3D structure, and to use the 2D/3D structure MoS 2 /In 2 O 3 nanocomposite material for photocatalytic water splitting. Hydrogen-coupled photocatalytic degradation of rhodamine B. The MoS 2 /In 2 O 3 nanocomposite material has high catalytic activity and can achieve the purpose of producing hydrogen while removing water pollutants.
本发明的技术方案Technical solution of the present invention
一种2D/3D结构MoS2/In2O3纳米复合材料的制备方法，包括以下步骤：A method for preparing 2D/3D structure MoS 2 /In 2 O 3 nanocomposite materials, including the following steps:
步骤1：称取一定量的醋酸铟和尿素分别置于15mL和20mL蒸馏水中，在室温下搅拌使二者完全溶解后，用吸管将尿素溶液逐滴滴入醋酸铟溶液，形成均匀的混合液。Step 1: Weigh a certain amount of indium acetate and urea and place them in 15 mL and 20 mL of distilled water respectively. Stir at room temperature to completely dissolve the two. Then use a pipette to drop the urea solution into the indium acetate solution drop by drop to form a uniform mixture. .
所述醋酸铟与尿素的摩尔量比为1:12.8。The molar ratio of indium acetate to urea is 1:12.8.
步骤2：将混合液转移到一定体积的聚四氟乙烯内衬的高压釜中，在一定温度下加热一定时间，进行水热反应，待高压釜冷却至室温后，离心收集白色产物，再分别用蒸馏水和乙醇洗涤3次，于80℃烘箱内干燥，得到前驱体。Step 2: Transfer the mixed solution to a certain volume of polytetrafluoroethylene-lined autoclave, heat it at a certain temperature for a certain time, and perform a hydrothermal reaction. After the autoclave cools to room temperature, centrifuge to collect the white product, and then separate Wash three times with distilled water and ethanol, and dry in an oven at 80°C to obtain the precursor.
所述高压釜体积为50mL；水热反应温度为130℃、时间为12h。The volume of the autoclave is 50 mL; the hydrothermal reaction temperature is 130°C and the time is 12 hours.
步骤3：在室温下将前驱体置于马弗炉中，调控一定的升温速率进行加热反应，待反应结束且马弗炉冷却至室温后，得到3D结构的In2O3纳米立方体。Step 3: Place the precursor in a muffle furnace at room temperature, and adjust a certain heating rate to perform a heating reaction. After the reaction is completed and the muffle furnace cools to room temperature, In 2 O 3 nanocubes with a 3D structure are obtained.
所述升温速率为2℃/min；加热反应温度为600℃、时间为2h。The heating rate is 2°C/min; the heating reaction temperature is 600°C and the time is 2h.
步骤4：称取一定量的In2O3超声分散在一定容积的蒸馏水中，然后加入一定量的钼酸钠和硫代乙酰胺，经超声、搅拌直至物料完全分散后，形成均匀的悬浮液。Step 4: Weigh a certain amount of In 2 O 3 and ultrasonically disperse it into a certain volume of distilled water. Then add a certain amount of sodium molybdate and thioacetamide. Ultrasonic and stir until the material is completely dispersed to form a uniform suspension. .
所述In2O3质量为300mg；钼酸钠和硫代乙酰胺的摩尔量比为1:5。The mass of In 2 O 3 is 300 mg; the molar ratio of sodium molybdate and thioacetamide is 1:5.
步骤5：将悬浮液完全转移到一定体积的聚四氟乙烯内衬的高压釜中，在一定温度下加热一定时间，进行水热反应，待反应的高压釜冷却至室温后，离心收集样品，再分别用蒸馏水和乙醇洗涤3次，于80℃烘箱内干燥，最终得到2D/3D结构的MoS2/In2O3纳米复合材料。Step 5: Completely transfer the suspension to a certain volume of polytetrafluoroethylene-lined autoclave, heat it at a certain temperature for a certain time, and perform a hydrothermal reaction. After the reaction autoclave is cooled to room temperature, centrifuge to collect the sample. Then they were washed three times with distilled water and ethanol, and dried in an oven at 80°C to finally obtain a 2D/3D structured MoS 2 /In 2 O 3 nanocomposite.
所述高压釜体积为50mL；水热反应温度为210℃、时间为24h。The volume of the autoclave is 50 mL; the hydrothermal reaction temperature is 210°C and the time is 24 hours.
本发明的有益效果Beneficial effects of the invention
1、本发明利用2D层状结构的MoS2纳米片材料能够有效加速光生电子-空穴分离/迁移速率的优势，来代替传统贵金属Pt基助催化剂，成功构建廉价、高催化活性的2D/3D结构MoS2/In2O3纳米复合材料。1. The present invention takes advantage of the 2D layered structure of MoS 2 nanosheet materials that can effectively accelerate the separation/migration rate of photogenerated electrons and holes to replace the traditional precious metal Pt-based cocatalyst, and successfully constructs a cheap, high catalytic activity 2D/3D Structure of MoS 2 /In 2 O 3 nanocomposites.
2、本发明利用In2O3材料能带结构的特点(导带产生的电子能够还原水制氢且价带生成的空穴能够氧化污染物)，将光催化分解水制氢反应与光催化降解罗丹明B反应进行协同耦合，实现制取氢气的同时达到去除水体污染物的目的。2. The present invention utilizes the characteristics of the energy band structure of the In 2 O 3 material (the electrons generated in the conduction band can reduce water to produce hydrogen and the holes generated in the valence band can oxidize pollutants) to combine the photocatalytic water splitting reaction and photocatalytic hydrogen production reaction. The degradation reaction of rhodamine B is synergistically coupled to achieve the purpose of producing hydrogen and removing water pollutants at the same time.
3、本发明原料具有价格便宜、制备简单等优点，减少了能耗和反应成本，便于批量生产且无毒无害，符合节能环保与可持续发展的要求。3. The raw materials of the present invention have the advantages of low price and simple preparation, reduce energy consumption and reaction costs, are convenient for mass production, are non-toxic and harmless, and meet the requirements of energy conservation, environmental protection and sustainable development.
附图说明Description of the drawings
此处的附图被并入说明书中并构成本说明书的一部分，示出了符合本发明的实施例，并与说明书一起用于解释本发明的原理。The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and together with the description serve to explain the principles of the invention.
图1A为本发明实施例1所制备In2O3纳米立方体的X-射线衍射图(XRD)。Figure 1A is an X-ray diffraction pattern (XRD) of In 2 O 3 nanocubes prepared in Example 1 of the present invention.
图1B为本发明实施例2所制备MoS2纳米片的XRD图。Figure 1B is an XRD pattern of MoS 2 nanosheets prepared in Example 2 of the present invention.
图1C为本发明实施例3-6所制备MoS2/In2O3纳米复合材料的XRD图。Figure 1C is the XRD pattern of the MoS 2 /In 2 O 3 nanocomposite prepared in Examples 3-6 of the present invention.
图2A为本发明实施例1所制备In2O3纳米立方体的扫描电子显微镜(SEM)图。Figure 2A is a scanning electron microscope (SEM) image of In 2 O 3 nanocubes prepared in Example 1 of the present invention.
图2B为本发明实施例2所制备MoS2纳米片的透射电子显微镜(TEM)图。Figure 2B is a transmission electron microscope (TEM) image of MoS 2 nanosheets prepared in Example 2 of the present invention.
图2C和图2D为本发明实施例5所制备10％MoS2/In2O3纳米复合材料的TEM图。Figure 2C and Figure 2D are TEM images of the 10% MoS 2 /In 2 O 3 nanocomposite material prepared in Example 5 of the present invention.
图3A为本发明实施例1和实施例5所制备In2O3纳米立方体和10％MoS2/In2O3纳米复合材料的光电流图。Figure 3A is the photocurrent diagram of In 2 O 3 nanocubes and 10% MoS 2 /In 2 O 3 nanocomposite materials prepared in Example 1 and Example 5 of the present invention.
图3B为本发明实施例1和实施例5所制备In2O3纳米立方体和10％MoS2/In2O3纳米复合材料的电化学阻抗图。Figure 3B is an electrochemical impedance diagram of In 2 O 3 nanocubes and 10% MoS 2 /In 2 O 3 nanocomposite materials prepared in Example 1 and Example 5 of the present invention.
图4A为本发明实施例1和实施例3-6所制备In2O3纳米立方体和MoS2/In2O3纳米复合材料的光催化分解水产氢速率柱状图。Figure 4A is a histogram of the hydrogen production rate of photocatalytic water decomposition of In 2 O 3 nanocubes and MoS 2 /In 2 O 3 nanocomposites prepared in Example 1 and Examples 3-6 of the present invention.
图4B为本发明实施例1和实施例3-6所制备In2O3纳米立方体和MoS2/In2O3纳米复合材料的光催化降解罗丹明B的总有机碳去除率柱状图。Figure 4B is a histogram of the total organic carbon removal rate of the photocatalytic degradation of rhodamine B by In 2 O 3 nanocubes and MoS 2 /In 2 O 3 nanocomposites prepared in Example 1 and Examples 3-6 of the present invention.
通过上述附图，已示出本发明明确的实施例，后文中将有更详细的描述。这些附图和文字描述并不是为了通过任何方式限制本发明构思的范围，而是通过参考特定实施例为本领域技术人员说明本发明的概念。Specific embodiments of the present invention have been shown in the above-mentioned drawings and will be described in more detail below. These drawings and written description are not intended to limit the scope of the inventive concept in any way, but rather to illustrate the concept of the present invention to those skilled in the art with reference to specific embodiments.
具体实施方式Detailed ways
本发明的目的在于提出一种具有2D/3D结构MoS2/In2O3纳米复合材料的制备方法，并将所合成的纳米复合材料作为催化剂用于高效光催化分解水制氢耦合光催化降解罗丹明B反应。该方法利用醋酸铟、尿素、硫代乙酰胺和钼酸钠为原料，先经水热-煅烧法制备3D结构的In2O3纳米立方体，然后再通过简易的水热法将2D结构的MoS2纳米片负载到In2O3纳米立方体表面，构建2D/3D结构的MoS2/In2O3纳米复合材料。The purpose of the present invention is to propose a preparation method of MoS 2 /In 2 O 3 nanocomposite material with 2D/3D structure, and use the synthesized nanocomposite material as a catalyst for efficient photocatalytic water splitting and hydrogen production coupled photocatalytic degradation Rhodamine B reaction. This method uses indium acetate, urea, thioacetamide and sodium molybdate as raw materials, first prepares 3D structured In 2 O 3 nanocubes through a hydrothermal-calcination method, and then uses a simple hydrothermal method to convert the 2D structured MoS 2 nanosheets are loaded onto the surface of In 2 O 3 nanocubes to construct a 2D/3D structured MoS 2 /In 2 O 3 nanocomposite.
下面结合实施例对本发明进行详细说明，以使本领域技术人员更好地理解本发明，但本发明并不局限于以下实施例。The present invention will be described in detail below in conjunction with the examples to enable those skilled in the art to better understand the present invention, but the present invention is not limited to the following examples.
实施例1：制备In2O3纳米立方体Example 1: Preparation of In 2 O 3 nanocubes
步骤1：分别称取1.0948g醋酸铟和2.8829g尿素置于15mL和20mL蒸馏水中，在室温下搅拌15min使二者完全溶解后，用吸管将尿素溶液逐滴滴入醋酸铟溶液，形成均匀的混合液。Step 1: Weigh 1.0948g of indium acetate and 2.8829g of urea respectively and place them in 15mL and 20mL of distilled water. Stir at room temperature for 15min to completely dissolve the two. Use a pipette to drop the urea solution into the indium acetate solution drop by drop to form a uniform mixture. Mixture.
步骤2：将混合液转移到50mL的聚四氟乙烯内衬的高压釜中，在130℃下水热反应12h，待高压釜冷却至室温后，离心收集白色产物，再分别用蒸馏水和乙醇洗涤3次，于80℃烘箱内干燥，得到前驱体。Step 2: Transfer the mixture to a 50 mL polytetrafluoroethylene-lined autoclave and perform a hydrothermal reaction at 130°C for 12 hours. After the autoclave cools to room temperature, centrifuge to collect the white product, and then wash it with distilled water and ethanol for 3 seconds. times, dried in an oven at 80°C to obtain the precursor.
步骤3：在室温下将前驱体置于马弗炉中，调控升温速率为2℃/min在600℃下加热反应2h，待反应结束且马弗炉冷却至室温后，得到3D结构的In2O3纳米立方体。Step 3: Place the precursor in a muffle furnace at room temperature, adjust the heating rate to 2°C/min, and heat the reaction at 600°C for 2 hours. After the reaction is completed and the muffle furnace cools to room temperature, In 2 with a 3D structure is obtained. O 3 nanocubes.
实施例2：制备MoS2纳米片Example 2: Preparation of MoS 2 nanosheets
步骤1：称取0.3088g钼酸钠和0.5635g硫代乙酰胺置于35mL蒸馏水中，在室温下经超声、搅拌30min使二者完全分散，形成均匀的悬浮液。Step 1: Weigh 0.3088g sodium molybdate and 0.5635g thioacetamide and place them in 35 mL of distilled water. Ultrasonicate and stir for 30 minutes at room temperature to completely disperse the two to form a uniform suspension.
步骤2：将悬浮液转移到50mL的聚四氟乙烯内衬的高压釜中，在210℃下水热反应24h，待高压釜冷却至室温后，离心收集黑色产物，再分别用蒸馏水和乙醇洗涤3次，于80℃烘箱内干燥，得到2D结构的MoS2纳米片。Step 2: Transfer the suspension to a 50 mL polytetrafluoroethylene-lined autoclave and perform a hydrothermal reaction at 210°C for 24 hours. After the autoclave cools to room temperature, centrifuge to collect the black product, and then wash it with distilled water and ethanol for 3 seconds. times and dried in an oven at 80°C to obtain MoS 2 nanosheets with a 2D structure.
实施例3：制备5％MoS2/In2O3纳米复合材料Example 3: Preparation of 5% MoS 2 /In 2 O 3 nanocomposite
步骤1：分别称取1.0948g醋酸铟和2.8829g尿素置于15mL和20mL蒸馏水中，在室温下搅拌15min使二者完全溶解后，用吸管将尿素溶液逐滴滴入醋酸铟溶液，形成均匀的混合液。Step 1: Weigh 1.0948g of indium acetate and 2.8829g of urea respectively and place them in 15mL and 20mL of distilled water. Stir at room temperature for 15min to completely dissolve the two. Use a pipette to drop the urea solution into the indium acetate solution drop by drop to form a uniform mixture. Mixture.
步骤2：将混合液转移到50mL的聚四氟乙烯内衬的高压釜中，在130℃下水热反应12h，待高压釜冷却至室温后，离心收集白色产物，再分别用蒸馏水和乙醇洗涤3次，于80℃烘箱内干燥，得到前驱体。Step 2: Transfer the mixture to a 50 mL polytetrafluoroethylene-lined autoclave and perform a hydrothermal reaction at 130°C for 12 hours. After the autoclave cools to room temperature, centrifuge to collect the white product, and then wash it with distilled water and ethanol for 3 seconds. times, dried in an oven at 80°C to obtain the precursor.
步骤3：在室温下将前驱体置于马弗炉中，调控升温速率为2℃/min在600℃下加热反应2h，待反应结束且马弗炉冷却至室温后，得到3D结构的In2O3纳米立方体。Step 3: Place the precursor in a muffle furnace at room temperature, adjust the heating rate to 2°C/min, and heat the reaction at 600°C for 2 hours. After the reaction is completed and the muffle furnace cools to room temperature, In 2 with a 3D structure is obtained. O 3 nanocubes.
步骤4：称取300mg In2O3超声分散在35mL蒸馏水中，然后加入0.0193g钼酸钠和0.0352g硫代乙酰胺，经超声、搅拌直至物料完全分散后，形成均匀的悬浮液。Step 4: Weigh 300 mg of In 2 O 3 and disperse it in 35 mL of distilled water by ultrasonic, then add 0.0193 g of sodium molybdate and 0.0352 g of thioacetamide, ultrasonic and stir until the material is completely dispersed to form a uniform suspension.
步骤5：将悬浮液完全转移到50mL聚四氟乙烯内衬的高压釜中，在210℃下水热反应24h，待高压釜冷却至室温后，离心收集产物，再分别用蒸馏水和乙醇洗涤3次，于80℃烘箱内干燥，得到5％MoS2/In2O3纳米复合材料。Step 5: Completely transfer the suspension to a 50 mL polytetrafluoroethylene-lined autoclave, and perform a hydrothermal reaction at 210°C for 24 hours. After the autoclave cools to room temperature, centrifuge to collect the product, and then wash it three times with distilled water and ethanol. , dried in an oven at 80°C to obtain 5% MoS 2 /In 2 O 3 nanocomposite.
实施例4：制备7.5％MoS2/In2O3纳米复合材料Example 4: Preparation of 7.5% MoS 2 /In 2 O 3 nanocomposite
步骤1：分别称取1.0948g醋酸铟和2.8829g尿素置于15mL和20mL蒸馏水中，在室温下搅拌15min使二者完全溶解后，用吸管将尿素溶液逐滴滴入醋酸铟溶液，形成均匀的混合液。Step 1: Weigh 1.0948g of indium acetate and 2.8829g of urea respectively and place them in 15mL and 20mL of distilled water. Stir at room temperature for 15min to completely dissolve the two. Use a pipette to drop the urea solution into the indium acetate solution drop by drop to form a uniform mixture. Mixture.
步骤2：将混合液转移到50mL的聚四氟乙烯内衬的高压釜中，在130℃下水热反应12h，待高压釜冷却至室温后，离心收集白色产物，再分别用蒸馏水和乙醇洗涤3次，于80℃烘箱内干燥，得到前驱体。Step 2: Transfer the mixture to a 50 mL polytetrafluoroethylene-lined autoclave and perform a hydrothermal reaction at 130°C for 12 hours. After the autoclave cools to room temperature, centrifuge to collect the white product, and then wash it with distilled water and ethanol for 3 seconds. times, dried in an oven at 80°C to obtain the precursor.
步骤3：在室温下将前驱体置于马弗炉中，调控升温速率为2℃/min在600℃下加热反应2h，待反应结束且马弗炉冷却至室温后，得到3D结构的In2O3纳米立方体。Step 3: Place the precursor in a muffle furnace at room temperature, adjust the heating rate to 2°C/min, and heat the reaction at 600°C for 2 hours. After the reaction is completed and the muffle furnace cools to room temperature, In 2 with a 3D structure is obtained. O 3 nanocubes.
步骤4：称取300mg In2O3超声分散在35mL蒸馏水中，然后加入0.0289g钼酸钠和0.0528g硫代乙酰胺，经超声、搅拌直至物料完全分散后，形成均匀的悬浮液。Step 4: Weigh 300 mg of In 2 O 3 and disperse it in 35 mL of distilled water by ultrasonic, then add 0.0289 g of sodium molybdate and 0.0528 g of thioacetamide, ultrasonic and stir until the material is completely dispersed to form a uniform suspension.
步骤5：将悬浮液完全转移到50mL聚四氟乙烯内衬的高压釜中，在210℃下水热反应24h，待高压釜冷却至室温后，离心收集产物，再分别用蒸馏水和乙醇洗涤3次，于80℃烘箱内干燥，得到7.5％MoS2/In2O3纳米复合材料。Step 5: Completely transfer the suspension to a 50 mL polytetrafluoroethylene-lined autoclave, and perform a hydrothermal reaction at 210°C for 24 hours. After the autoclave cools to room temperature, centrifuge to collect the product, and then wash it three times with distilled water and ethanol. , dried in an oven at 80°C to obtain 7.5% MoS 2 /In 2 O 3 nanocomposite.
实施例5：制备10％MoS2/In2O3纳米复合材料Example 5: Preparation of 10% MoS 2 /In 2 O 3 nanocomposite
步骤1：分别称取1.0948g醋酸铟和2.8829g尿素置于15mL和20mL蒸馏水中，在室温下搅拌15min使二者完全溶解后，用吸管将尿素溶液逐滴滴入醋酸铟溶液，形成均匀的混合液。Step 1: Weigh 1.0948g of indium acetate and 2.8829g of urea respectively and place them in 15mL and 20mL of distilled water. Stir at room temperature for 15min to completely dissolve the two. Use a pipette to drop the urea solution into the indium acetate solution drop by drop to form a uniform mixture. Mixture.
步骤2：将混合液转移到50mL的聚四氟乙烯内衬的高压釜中，在130℃下水热反应12h，待高压釜冷却至室温后，离心收集白色产物，再分别用蒸馏水和乙醇洗涤3次，于80℃烘箱内干燥，得到前驱体。Step 2: Transfer the mixture to a 50 mL polytetrafluoroethylene-lined autoclave and perform a hydrothermal reaction at 130°C for 12 hours. After the autoclave cools to room temperature, centrifuge to collect the white product, and then wash it with distilled water and ethanol for 3 seconds. times, dried in an oven at 80°C to obtain the precursor.
步骤3：在室温下将前驱体置于马弗炉中，调控升温速率为2℃/min在600℃下加热反应2h，待反应结束且马弗炉冷却至室温后，得到3D结构的In2O3纳米立方体。Step 3: Place the precursor in a muffle furnace at room temperature, adjust the heating rate to 2°C/min, and heat the reaction at 600°C for 2 hours. After the reaction is completed and the muffle furnace cools to room temperature, In 2 with a 3D structure is obtained. O 3 nanocubes.
步骤4：称取300mg In2O3超声分散在35mL蒸馏水中，然后加入0.0386g钼酸钠和0.0704g硫代乙酰胺，经超声、搅拌直至物料完全分散后，形成均匀的悬浮液。Step 4: Weigh 300 mg of In 2 O 3 and disperse it in 35 mL of distilled water by ultrasonic, then add 0.0386 g of sodium molybdate and 0.0704 g of thioacetamide, ultrasonic and stir until the material is completely dispersed to form a uniform suspension.
步骤5：将悬浮液完全转移到50mL聚四氟乙烯内衬的高压釜中，在210℃下水热反应24h，待高压釜冷却至室温后，离心收集产物，再分别用蒸馏水和乙醇洗涤3次，于80℃烘箱内干燥，得到10％MoS2/In2O3纳米复合材料。Step 5: Completely transfer the suspension to a 50 mL polytetrafluoroethylene-lined autoclave, and perform a hydrothermal reaction at 210°C for 24 hours. After the autoclave cools to room temperature, centrifuge to collect the product, and then wash it three times with distilled water and ethanol. , dried in an oven at 80°C to obtain 10% MoS 2 /In 2 O 3 nanocomposite.
实施例6：制备12.5％MoS2/In2O3纳米复合材料Example 6: Preparation of 12.5% MoS 2 /In 2 O 3 nanocomposite
步骤1：分别称取1.0948g醋酸铟和2.8829g尿素置于15mL和20mL蒸馏水中，在室温下搅拌15min使二者完全溶解后，用吸管将尿素溶液逐滴滴入醋酸铟溶液，形成均匀的混合液。Step 1: Weigh 1.0948g of indium acetate and 2.8829g of urea respectively and place them in 15mL and 20mL of distilled water. Stir at room temperature for 15min to completely dissolve the two. Use a pipette to drop the urea solution into the indium acetate solution drop by drop to form a uniform mixture. Mixture.
步骤2：将混合液转移到50mL的聚四氟乙烯内衬的高压釜中，在130℃下水热反应12h，待高压釜冷却至室温后，离心收集白色产物，再分别用蒸馏水和乙醇洗涤3次，于80℃烘箱内干燥，得到前驱体。Step 2: Transfer the mixture to a 50 mL polytetrafluoroethylene-lined autoclave and perform a hydrothermal reaction at 130°C for 12 hours. After the autoclave cools to room temperature, centrifuge to collect the white product, and then wash it with distilled water and ethanol for 3 seconds. times, dried in an oven at 80°C to obtain the precursor.
步骤3：在室温下将前驱体置于马弗炉中，调控升温速率为2℃/min在600℃下加热反应2h，待反应结束且马弗炉冷却至室温后，得到3D结构的In2O3纳米立方体。Step 3: Place the precursor in a muffle furnace at room temperature, adjust the heating rate to 2°C/min, and heat the reaction at 600°C for 2 hours. After the reaction is completed and the muffle furnace cools to room temperature, In 2 with a 3D structure is obtained. O 3 nanocubes.
步骤4：称取300mg In2O3超声分散在35mL蒸馏水中，然后加入0.0483g钼酸钠和0.0880g硫代乙酰胺，经超声、搅拌直至物料完全分散后，形成均匀的悬浮液。Step 4: Weigh 300 mg of In 2 O 3 and disperse it in 35 mL of distilled water by ultrasonic, then add 0.0483 g of sodium molybdate and 0.0880 g of thioacetamide, ultrasonic and stir until the material is completely dispersed to form a uniform suspension.
步骤5：将悬浮液完全转移到50mL聚四氟乙烯内衬的高压釜中，在210℃下水热反应24h，待高压釜冷却至室温后，离心收集产物，再分别用蒸馏水和乙醇洗涤3次，于80℃烘箱内干燥，得到12.5％MoS2/In2O3纳米复合材料。Step 5: Completely transfer the suspension to a 50 mL polytetrafluoroethylene-lined autoclave, and perform a hydrothermal reaction at 210°C for 24 hours. After the autoclave cools to room temperature, centrifuge to collect the product, and then wash it three times with distilled water and ethanol. , dried in an oven at 80°C to obtain 12.5% MoS 2 /In 2 O 3 nanocomposite.
本发明中催化剂的晶相结构由X射线衍射(XRD)确定。图1A、图1B和图1C的XRD谱图可以看出：In2O3纳米立方体与MoS2纳米片材料的特征衍射峰都与标准卡片JCPDS No.71-2194和JCPDS No.37-1492相符合，表明纯相In2O3和MoS2均已被成功制备；而在MoS2/In2O3纳米复合材料中，由于MoS2负载含量相对较低，所有纳米复合材料都展现出In2O3的特征XRD衍射峰，未观察到MoS2的特征峰。The crystal phase structure of the catalyst in the present invention is determined by X-ray diffraction (XRD). It can be seen from the XRD spectra of Figure 1A, Figure 1B and Figure 1C that the characteristic diffraction peaks of In 2 O 3 nanocubes and MoS 2 nanosheet materials are consistent with the standard cards JCPDS No. 71-2194 and JCPDS No. 37-1492 is consistent, indicating that both pure phases In 2 O 3 and MoS 2 have been successfully prepared; and in MoS 2 /In 2 O 3 nanocomposites, due to the relatively low loading content of MoS 2 , all nanocomposites exhibit In 2 Characteristic XRD diffraction peaks of O 3 and no characteristic peaks of MoS 2 were observed.
本发明中催化剂的表面形貌和微观结构由扫描电子显微镜(SEM)和透射电子显微镜(TEM)确定。图2A的SEM图可以看出：制备的纯相In2O3材料具有明显的3D立方体结构；图2B的TEM图可以看出：制备的纯相MoS2材料具有明显的2D纳米片结构；图2C和图2D的TEM图可以看出：当质量比10％的MoS2负载在In2O3表面后，所制备的10％MoS2/In2O3纳米复合材料仍表现出与纯相In2O3相似的纳米立方体结构，但在其表面均匀分布着二维层状结构的MoS2纳米片。这一结果表明独特2D/3D结构的MoS2/In2O3纳米复合材料已被成功合成。The surface morphology and microstructure of the catalyst in the present invention are determined by scanning electron microscope (SEM) and transmission electron microscope (TEM). The SEM image in Figure 2A shows that the prepared pure phase In 2 O 3 material has an obvious 3D cubic structure; the TEM image in Figure 2B shows that the prepared pure phase MoS 2 material has an obvious 2D nanosheet structure; Figure It can be seen from the TEM images in Figure 2C and Figure 2D that when MoS 2 with a mass ratio of 10% is loaded on the In 2 O 3 surface, the prepared 10% MoS 2 /In 2 O 3 nanocomposite still exhibits the same performance as pure phase In. 2 O 3 has a similar nanocube structure, but MoS 2 nanosheets with a two-dimensional layered structure are evenly distributed on its surface. This result shows that the unique 2D/3D structured MoS 2 /In 2 O 3 nanocomposite has been successfully synthesized.
本发明中催化剂的光生电子-空穴分离/迁移速率由光电流响应和电化学阻抗确定。图3A的光电流响应图可以看出：与纯相In2O3材料相比，所制备的10％MoS2/In2O3纳米复合材料具有明显提高的光电流密度；图3B的电化学阻抗图可以看出：与纯相In2O3材料相比，所制备的10％MoS2/In2O3纳米复合材料具有显著减小的阻抗半圆。这一结果表明MoS2作为助催化剂能够大幅提高In2O3材料的光生电子-空穴分离/迁移速率。The photogenerated electron-hole separation/migration rate of the catalyst in the present invention is determined by the photocurrent response and electrochemical impedance. It can be seen from the photocurrent response diagram in Figure 3A that: compared with the pure phase In 2 O 3 material, the prepared 10% MoS 2 /In 2 O 3 nanocomposite material has a significantly improved photocurrent density; the electrochemistry in Figure 3B It can be seen from the impedance diagram that the prepared 10% MoS 2 /In 2 O 3 nanocomposite has a significantly reduced impedance semicircle compared with the pure phase In 2 O 3 material. This result shows that MoS 2 as a cocatalyst can significantly improve the photogenerated electron-hole separation/migration rate of In 2 O 3 materials.
本发明中催化剂的光催化性能由光催化分解水制氢耦合光催化降罗丹明B确定。图4A的制氢速率柱状图可以看出：纯相In2O3材料展现出非常低的光催化制氢活性，而制备的MoS2/In2O3纳米复合材料均能够显著提高光催化制氢活性。其中，10％MoS2/In2O3纳米复合材料展现出最高的制氢活性(15.5μmol/g/h)，比纯相In2O3材料高出77.5倍。图4B的罗丹明B总有机碳去除率柱状图可以看出：纯相In2O3材料具有最低的总有机碳去除率，而合成的MoS2/In2O3纳米复合材料总有机碳去除率均有大幅度提高。其中，10％MoS2/In2O3纳米复合材料具有最高的总有机碳去除率(63.1％)，约是纯相In2O3材料的12倍。此外，通过图4A和图4B可以看出，催化剂的制氢速率与罗丹明B的总有机碳去除率二者成正比关系。这一结果表明所制备的MoS2/In2O3纳米复合材料在明显提高光催化分解水制氢反应的同时还能显著加速罗丹明B分子的降解、矿化过程。The photocatalytic performance of the catalyst in the present invention is determined by photocatalytic water splitting and hydrogen production coupled with photocatalytic rhodamine B reduction. It can be seen from the hydrogen production rate histogram in Figure 4A that the pure phase In 2 O 3 material exhibits very low photocatalytic hydrogen production activity, while the prepared MoS 2 /In 2 O 3 nanocomposite materials can significantly improve the photocatalytic hydrogen production activity. Hydrogen activity. Among them, the 10% MoS 2 /In 2 O 3 nanocomposite material exhibits the highest hydrogen production activity (15.5 μmol/g/h), which is 77.5 times higher than the pure phase In 2 O 3 material. The histogram of the total organic carbon removal rate of Rhodamine B in Figure 4B shows that the pure phase In 2 O 3 material has the lowest total organic carbon removal rate, while the synthesized MoS 2 /In 2 O 3 nanocomposite has the lowest total organic carbon removal rate. The rates have increased significantly. Among them, the 10% MoS 2 /In 2 O 3 nanocomposite material has the highest total organic carbon removal rate (63.1%), which is approximately 12 times that of the pure phase In 2 O 3 material. In addition, it can be seen from Figure 4A and Figure 4B that the hydrogen production rate of the catalyst is directly proportional to the total organic carbon removal rate of Rhodamine B. This result shows that the prepared MoS 2 /In 2 O 3 nanocomposite material can significantly improve the photocatalytic water splitting reaction and hydrogen production reaction, and can also significantly accelerate the degradation and mineralization process of rhodamine B molecules.
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