CN109052988B - Preparation method of zinc indium sulfide nanosheet array film - Google Patents

Preparation method of zinc indium sulfide nanosheet array film Download PDF

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CN109052988B
CN109052988B CN201811222709.0A CN201811222709A CN109052988B CN 109052988 B CN109052988 B CN 109052988B CN 201811222709 A CN201811222709 A CN 201811222709A CN 109052988 B CN109052988 B CN 109052988B
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znin
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CN109052988A (en
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何丹农
卢静
涂兴龙
白仕亨
李砚瑞
金彩虹
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Shanghai National Engineering Research Center for Nanotechnology Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
    • C03C17/3429—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating
    • C03C17/3464—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating comprising a chalcogenide
    • C03C17/347—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating comprising a chalcogenide comprising a sulfide or oxysulfide
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/40—Coatings comprising at least one inhomogeneous layer
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/70—Properties of coatings
    • C03C2217/71—Photocatalytic coatings
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/90—Other aspects of coatings
    • C03C2217/94—Transparent conductive oxide layers [TCO] being part of a multilayer coating
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00—Methods for coating glass
    • C03C2218/10—Deposition methods
    • C03C2218/11—Deposition methods from solutions or suspensions
    • C03C2218/111—Deposition methods from solutions or suspensions by dipping, immersion

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Abstract

The invention discloses a ZnIn2S4The preparation method of the nano-sheet array film comprises the steps of firstly using a chemical method to sink on FTO conductive glassDepositing a layer of In2S3Sputtering a layer of zinc on the surface of the nano film, finally taking an indium source and a sulfur source as precursors, and controlling the temperature and time of the solvothermal reaction to prepare ZnIn2S4A nanosheet array. The invention prepares ZnIn2S4The nano sheet is of an ultrathin structure, the thickness of the nano sheet is 5-6 nm, and the nano sheet has the excellent characteristics of high crystallinity, good light trapping performance, reusability and the like. In addition, the method has the advantages of simple preparation, easily controlled process, low cost, no toxicity and environmental protection, and has huge application prospect in the fields of photocatalytic hydrogen production, photocatalytic degradation of organic pollutants, artificial photosynthesis and the like.

Description

Preparation method of zinc indium sulfide nanosheet array film
Technical Field
The invention belongs to the field of nano film material preparation and photocatalytic application, and particularly relates to a preparation method of a zinc indium sulfide nanosheet array film.
Background
Along with the rapid development of the economy of all countries in the world, the demand of human beings on energy is higher and higher, and the call for environmental protection is also rising. However, the traditional fossil energy is a non-renewable energy and faces the trend of increasing exhaustion, and the fossil energy generates CO when being burned2、SO2And the harmful gases have great damage to the environment. Therefore, solving the problems of energy crisis and environmental pollution becomes two main problems facing the world at present, and all countries in the world take the establishment of a green, environment-friendly and sustainable new energy system as a national important development strategy. The semiconductor photocatalysis technology is an efficient and safe environment-friendly environment purification and hydrogen production technology, has huge application potential in solving the problems of environmental pollution and energy crisis, and has wide application in the fields of photocatalytic hydrogen production, photocatalytic degradation of organic pollutants, artificial photosynthesis, photocatalytic sterilization, solar cells and the like.
In recent years, ternary chalcogenide ABmCn (A = Cu, Ag, Zn, Cd, etc.; B = Al, Ga, In; C ¼ S, Se, Te) semiconductor materials have received great attention because they exhibit unique optical and electrical propertiesAnd (4) characteristics. Among these materials, ZnIn having a layered structure2S4Attracts a great deal of research of researchers, and has great application prospect in the fields of charge storage, electrochemical recording, photocatalysis and the like. And ZnIn2S4The band gap of (a) is very similar to the energy of photoelectrons, which is a potential energy conversion material. Because the physical and chemical properties of the material are greatly related to the shape, size, structure and the like of the material, researchers all over the world compete to synthesize new ZnIn2S4Nanostructures and explore their potential applications.
ZnIn of various morphologies to date2S4 (e.g., nanorods, nanotubes, nanoparticles, etc.) have been synthesized by various methods. Such as Gou et al [ J. Am. chem. Soc. 2006,128 (22); 7222-]ZnIn with the structure of nano wire, nano belt and the like is synthesized by a solvothermal method under the condition of having an auxiliary agent2S4；Hu[2]The ZnIn is synthesized by a microwave-assisted method2S4Porous microspheres (Crystal Growth)&Design, 2016, 7(12), 2444-2448). However, most of the synthesized nano materials are powdery samples, the recovery is difficult, and ZnIn is directly synthesized on the conductive substrate2S4Nanomaterials remain a significant challenge; on the other hand, the materials are basically one-dimensional nano materials, two-dimensional ZnIn2S4The potential of nanomaterials (such as nanosheets, nanobelts, etc.) in photocatalysis remains enormous. Peng et al directly synthesized ZnIn in one step by activating FTO substrate2S4The method of the nanosheet array has the problems of high cost, complex process and high danger (aqua regia is needed), and the prepared ZnIn2S4The shape controllability is poor, and large-scale production cannot be carried out. The invention synthesizes In on FTO2S3Nanosheet array, and further generating ZnIn by using the nanosheet array as a template2S4The nano-sheet array film has the advantages of simple technical scheme, easily controlled reaction process, low cost, no toxicity and environmental protection, and can effectively solve the problem of ZnIn2S4The nano-sheet array cannotThe difficult problem of large-scale application can lay a good foundation for further application in the engineering fields of photocatalysis and the like.
Disclosure of Invention
Aiming at the defects of the existing zinc-indium-sulfur nanosheet structure preparation technology, the invention aims to provide ZnIn2S4The preparation method of the nanosheet array film is simple in process, safe, reliable and low in cost.
The purpose of the invention can be realized by the following technical scheme:
(1) depositing a layer of In on the surface of clean FTO conductive glass by adopting a chemical method2S3And sputtering a layer of zinc on the surface of the nano film to be used as a substrate.
(2) Adding an indium source and a sulfur source with the concentration of 0.1-0.3M into a reaction kettle inner container until the molar ratio of indium salt to the sulfur source is 1: 4-1: 8, adding a solvent, and stirring or ultrasonically dissolving to prepare a uniform precursor solution.
(3) Putting the substrate and the prepared precursor into a reaction kettle, sealing, controlling the temperature to be 150-200 ℃, and reacting for 1-4 hours; after the reaction is finished, the reaction kettle is naturally cooled to room temperature, and the sample is taken out and cleaned and dried to obtain the ZnIn uniformly grown on the substrate2S4A nanosheet array film.
The clean FTO in the step (1) is ultrasonic cleaned for 10 min by acetone, absolute ethyl alcohol and deionized water in sequence.
In step (1)2S3The thickness of the nano-film is approximately 1 μm.
In step (1)2S3The thickness of the zinc sputtered on the surface of the nano film is about 50-200 nm.
The indium salt in the step (2) is indium chloride, indium nitrate, indium sulfate or indium acetate and the like, and the sulfur source is thiourea, cysteine or thioacetamide and the like.
The organic solvent in the step (2) is ethylene glycol or a mixture of ethylene glycol and ethanol.
Of the indium salt described in step (2), whichAt a concentration of to prepare In2S31/2 at concentration.
The reaction time in the step (3) is preferably 2-3h, and the reaction temperature is preferably 180-200 ℃.
Compared with the prior art, the invention has the following advantages:
1. the raw materials used in the invention are relatively easy to obtain, the preparation process is simple, safe and reliable, the cost is low, and the method has a good application prospect in the field of solar photocatalysis.
2. In the invention2S3The nano-sheet array is a self-sacrifice template to obtain high-quality ZnIn2S4A nanosheet array; compared with the traditional one-step method, the process is more controllable, and the desired morphology can be obtained.
3. ZnIn prepared by the invention2S4The thickness of the nanosheet on the surface of the nanosheet array is about 5 nm, and the nanosheet array has the excellent characteristics of high specific surface area, low reflectivity, good light trapping property, few defects, easiness in recycling and the like.
Drawings
FIG. 1 shows the growth of example 1 with In deposited2S3ZnIn on FTO substrate of (2)2S4SEM image of nanosheet array film;
FIG. 2 shows the growth of example 1 with In deposited2S3ZnIn on FTO substrate2S4And (3) a photoelectrocatalysis performance diagram of the nanosheet array film.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
ZnIn2S4The preparation method of the nanosheet array film comprises the following steps:
(1) adoption and transformationDepositing a layer of 1 mu m In on the surface of clean FTO conductive glass by a chemical method2S3Nano film and sputtering zinc of 100nm on the surface.
(2) Thioacetamide and indium chloride were mixed as follows 4: 1, adding the mixture into a reaction kettle, adding 40 ml of glycol, and stirring or ultrasonically dissolving to prepare a uniform solution with indium salt concentration of 0.2M;
(3) putting the substrate and the prepared precursor into a reaction kettle, sealing, controlling the temperature at 180 ℃, and reacting for 2 hours; after the reaction is finished, the reaction kettle is naturally cooled to room temperature, and the sample is taken out and cleaned and dried to obtain the ZnIn uniformly grown on the substrate2S4A nanosheet array film.
FIG. 1 shows ZnIn obtained in this example2S4SEM image of the film; as can be seen from FIG. 1, ZnIn2S4The film is composed of an array of vertical nano sheets, and the cross section of the film shows the characteristics of in-situ growth.
FIG. 2 shows ZnIn obtained in this example2S4The film performance graph shows that the film has good photocurrent effect, which indicates that the array structure has good light trapping property. Further indicates that the product of the invention has good application prospect in the field of solar photocatalysis.
Example 2
ZnIn2S4The preparation method of the nanosheet array film comprises the following steps:
(1) depositing a layer of 1 mu m In on the surface of clean FTO conductive glass by adopting a chemical method2S3Nano film and sputtering zinc of 200nm on the surface.
(2) Mixing thiourea and indium chloride according to a ratio of 4: 1, adding the mixture into a reaction kettle, adding 40 ml of glycol, and stirring or ultrasonically dissolving to prepare a uniform solution with indium salt concentration of 0.3M;
(3) putting the substrate and the prepared precursor into a reaction kettle, sealing, controlling the temperature at 180 ℃, and reacting for 4 hours; after the reaction is finished, the reaction kettle is naturally cooled to room temperature, and a sample is taken out and then is cleaned and dried to obtain the productTo ZnIn uniformly grown on the substrate2S4A nanosheet array film.
Example 3
ZnIn2S4The preparation method of the nanosheet array film comprises the following steps:
(1) depositing a layer of 1 mu m In on the surface of clean FTO conductive glass by adopting a chemical method2S3Nano film and sputtering 50nm zinc on the surface.
(2) Cysteine and indium nitrate were mixed as follows 4: 1, adding the mixture into a reaction kettle, adding 40 ml of glycol, and stirring or ultrasonically dissolving to prepare a uniform solution with indium salt concentration of 0.1M;
(3) putting the substrate and the prepared precursor into a reaction kettle, sealing, controlling the temperature to be 200 ℃, and reacting for 1 hour; after the reaction is finished, the reaction kettle is naturally cooled to room temperature, and the sample is taken out and cleaned and dried to obtain the ZnIn uniformly grown on the substrate2S4A nanosheet array film.
Example 4
ZnIn2S4The preparation method of the nanosheet array film comprises the following steps:
(1) depositing a layer of 1 mu m In on the surface of clean FTO conductive glass by adopting a chemical method2S3Nano film and sputtering zinc of 100nm on the surface.
(2) Cysteine and indium acetate were mixed as 8: 1, adding the mixture into a reaction kettle, adding 40 ml of glycol, and stirring or ultrasonically dissolving to prepare a uniform solution with indium salt concentration of 0.2M;
(3) putting the substrate and the prepared precursor into a reaction kettle, sealing, controlling the temperature to be 200 ℃, and reacting for 2 hours; after the reaction is finished, the reaction kettle is naturally cooled to room temperature, and the sample is taken out and cleaned and dried to obtain the ZnIn uniformly grown on the substrate2S4A nanosheet array film.
Example 5
ZnIn2S4Nanosheet array filmThe preparation method comprises the following steps:
(1) depositing a layer of 1 mu m In on the surface of clean FTO conductive glass by adopting a chemical method2S3Nano film and sputtering zinc of 100nm on the surface.
(2) Thioacetamide and indium sulfate were mixed as 6: 1, adding the mixture into a reaction kettle, adding 40 ml of glycol, and stirring or ultrasonically dissolving to prepare a uniform solution with indium salt concentration of 0.3M;
(3) putting the substrate and the prepared precursor into a reaction kettle, sealing, controlling the temperature at 150 ℃, and reacting for 3 hours; after the reaction is finished, the reaction kettle is naturally cooled to room temperature, and the sample is taken out and cleaned and dried to obtain the ZnIn uniformly grown on the substrate2S4A nanosheet array film.
Example 6
ZnIn2S4The preparation method of the nanosheet array film comprises the steps of controlling the temperature at 200 ℃, reacting for 3 hours, and controlling the concentration of indium salt to be 0.3M; the ZnIn uniformly grown on the substrate can be obtained under the same other conditions as in embodiment 12S4A nanosheet array film.
Example 7
ZnIn2S4The preparation method of the nano-sheet array film comprises the steps of controlling the temperature to be 160 ℃, reacting for 3 hours, and controlling the concentration of indium salt to be 0.2M; the ZnIn uniformly grown on the substrate can be obtained under the same other conditions as in embodiment 12S4A nanosheet array film.
Example 8
ZnIn2S4The preparation method of the nano-sheet array film comprises the steps of controlling the temperature to be 150 ℃ and the reaction time to be 4 hours; the other conditions are the same as the example 1, and the three-dimensional flower-shaped ZnIn uniformly grown on the zinc sheet can be obtained2S4Micro-nanowire array films.

Claims (4)

1. Preparation method of zinc-indium-sulfur nanosheet array film, wherein zinc-indium-sulfur molecular formula is ZnIn2S4Characterized in that the preparation method comprises the following steps：
(1) Depositing a layer of In on the surface of clean FTO conductive glass by adopting a chemical method2S3A nano film, and sputtering a layer of zinc film on the surface as a substrate;
(2) adding indium salt with the concentration of 0.1-0.3M and a sulfur source into a reaction kettle inner container, adding a solvent, wherein the molar ratio of the indium salt to the sulfur source is 1: 4-1: 8, and then stirring or ultrasonically dissolving to prepare a uniform precursor solution;
(3) putting the substrate and the prepared precursor solution into a reaction kettle, sealing, controlling the temperature to be 150-200 ℃, and reacting for 1-4 hours; after the reaction is finished, the reaction kettle is naturally cooled to room temperature, and the sample is taken out and cleaned and dried to obtain the ZnIn uniformly grown on the substrate2S4A nanosheet array film; wherein the content of the first and second substances,
the clean FTO conductive glass in the step (1) is prepared by sequentially ultrasonically cleaning for 10 min by acetone, absolute ethyl alcohol and deionized water;
in step (1)2S3The thickness of the nano film is 1 mu m;
in step (1)2S3The thickness of the zinc sputtered on the surface of the nano film is 50-200 nm;
the solvent in the step (2) is ethylene glycol or a mixture of ethylene glycol and ethanol;
the concentration of the indium salt In the step (2) is 0.1-0.3M, and In is prepared2S31/2 at concentration.
2. The preparation method of the zinc indium sulfide nanosheet array film according to claim 1, wherein the reaction time in the step (3) is 2-3h, and the reaction temperature is 180-200 ℃.
3. The method for preparing a zinc indium sulfide nanosheet array thin film according to claim 1, wherein the indium salt is indium chloride, indium nitrate, indium sulfate or indium acetate.
4. The method for preparing the zinc indium sulfur nanosheet array film of claim 1, wherein the sulfur source is thiourea, cysteine or thioacetamide.
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CN111822013B (en) * 2020-07-06 2022-11-18 重庆大学 Single-cell PN junction and accurate construction method thereof
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CN115125560B (en) * 2022-06-14 2023-10-17 杭州电子科技大学 Preparation method of beta-phase indium sulfide micro-sheet array

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009066529A (en) * 2007-09-13 2009-04-02 Tokyo Univ Of Science Photocatalyst, its manufacturing method, and method for generating hydrogen gas
CN101805136A (en) * 2010-03-11 2010-08-18 许昌学院 Chemical method for preparing nano mesh-like sulfur-indium-zinc ternary compound optoelectronic film on ITO conductive glass in situ
CN107282070A (en) * 2017-05-26 2017-10-24 上海纳米技术及应用国家工程研究中心有限公司 A kind of three-dimensional flower piece shape sulfur-indium-zinc micro-nano nanowire arrays and its preparation method and application
CN108409157A (en) * 2018-03-19 2018-08-17 中国矿业大学 A kind of ZnIn2S4 nanometer wafer arrays structure and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009066529A (en) * 2007-09-13 2009-04-02 Tokyo Univ Of Science Photocatalyst, its manufacturing method, and method for generating hydrogen gas
CN101805136A (en) * 2010-03-11 2010-08-18 许昌学院 Chemical method for preparing nano mesh-like sulfur-indium-zinc ternary compound optoelectronic film on ITO conductive glass in situ
CN107282070A (en) * 2017-05-26 2017-10-24 上海纳米技术及应用国家工程研究中心有限公司 A kind of three-dimensional flower piece shape sulfur-indium-zinc micro-nano nanowire arrays and its preparation method and application
CN108409157A (en) * 2018-03-19 2018-08-17 中国矿业大学 A kind of ZnIn2S4 nanometer wafer arrays structure and preparation method thereof

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