CN109052988A - A kind of preparation method of zinc indium sulphur nano-chip arrays film - Google Patents
A kind of preparation method of zinc indium sulphur nano-chip arrays film Download PDFInfo
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- CN109052988A CN109052988A CN201811222709.0A CN201811222709A CN109052988A CN 109052988 A CN109052988 A CN 109052988A CN 201811222709 A CN201811222709 A CN 201811222709A CN 109052988 A CN109052988 A CN 109052988A
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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
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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
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
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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
- C03C2217/00—Coatings on glass
- C03C2217/40—Coatings comprising at least one inhomogeneous layer
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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
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
- C03C2217/71—Photocatalytic coatings
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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
- C03C2217/00—Coatings on glass
- C03C2217/90—Other aspects of coatings
- C03C2217/94—Transparent conductive oxide layers [TCO] being part of a multilayer coating
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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
- 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
Abstract
The invention discloses a kind of ZnIn2S4The preparation method of nano-chip arrays film first deposits one layer of In with chemical method on FTO electro-conductive glass2S3Then nano thin-film sputters one layer of zinc on its surface, finally using indium source, sulphur source as presoma, by controlling the temperature and time of solvent thermal reaction, to prepare ZnIn2S4Nano-chip arrays.The present invention prepares ZnIn2S4Nanometer sheet is a kind of superthin structure, and thickness has crystallinity high in 5 ~ 6 nm, and it is good and being capable of the excellent characteristics such as Reusability to fall into optical property.In addition, this method preparation is simple, process is easily-controllable, low in cost, asepsis environment-protecting, and in photocatalysis hydrogen production, the fields such as photocatalysis degradation organic contaminant and artificial photosynthesis have huge application prospect.
Description
Technical field
The invention belongs to nano film material preparation and photocatalytic applications field more particularly to a kind of zinc indium sulphur nanometer sheet battle arrays
The preparation method of column film.
Background technique
With countries in the world rapid economic development, demand of the mankind to the energy is higher and higher, to the cry of environmental protection
It grows to even greater heights.But traditional fossil energy is a kind of non-renewable energy resources, is faced with increasingly depleted trend, and fossil energy
Source generates CO in burning2、SO2Equal pernicious gases have huge destruction to environment.So solving energy crisis and environmental pollution
Problem becomes two major subjects that the world today faces, and countries in the world are all environmentally protective, sustainable development new establishing
Significant development strategy of the energy system as country.Photocatalitic Technique of Semiconductor is a kind of environmental-friendly type ring efficiently, safe
Border purification and production hydrogen technology, have huge application potential on solving environmental pollution and problem of energy crisis, urge at present in light
Change hydrogen manufacturing, photocatalysis degradation organic contaminant, artificial photosynthesis, photo-catalyst, the fields such as solar battery suffer from extensively
General application.
In recent years, ternary chalcogenide ABmCn(A=Cu, Ag, Zn, Cd etc.;B=Al, Ga, In;C S, Se, Te)
Semiconductor material has been a great concern, because they show unique optically and electrically characteristic.In these materials,
With ZnIn layered2S4The research of a large number of scientific researchers is attracted, because it is in charge storage, electrochemical recording and light
There is huge application prospect in the fields such as catalysis.And ZnIn2S4Band gap and photoelectronic energy it is very close, it is a kind of potential
Energy converslon materials.Since the physicochemical properties and his pattern, size, structure etc. of material have very big relationship, because
This global researcher, which is competing always, synthesizes new ZnIn2S4Nanostructure and the potential application for exploring them.
Up to the present, the ZnIn of various patterns2S4 (such as nanometer rods, nanotube, nanoparticle) all can pass through
Different method synthesizes.For example Gou etc. [J. Am. Chem. Soc. 2006,128 (22), 7222-7229] passes through solvent
The method of heat, has synthesized nano wire, nanobelt isostructural ZnIn under conditions of having adjuvant2S4；Hu [2] etc. passes through microwave
The method of auxiliary has synthesized ZnIn2S4Porous microsphere (Crystal Growth & Design, 2016,7 (12), 2444-
2448).But the nano material overwhelming majority of these synthesis is all powdered samples, recycles difficulty greatly, it is straight in conductive substrates
It is bonded into ZnIn2S4Nano material is still a huge challenge；It on the other hand is that these materials are substantially 1-dimention nano
Material, two-dimentional ZnIn2S4The potentiality of nano material (such as nanometer sheet, nanobelt) in terms of photocatalysis are still huge.And Peng
Deng one-step synthesis direct by way of being activated to FTO substrate ZnIn2S4The method of nano-chip arrays, have cost compared with
Height, process is complicated and the problem of than relatively hazardous (need to use chloroazotic acid), and the ZnIn of preparation2S4Morphology controllable is poor, can not carry out big
Large-scale production.The present invention on FTO by first synthesizing In2S3Then nano-chip arrays are further generated as template
ZnIn2S4Nano-chip arrays film, technical solution is simple, and reaction process is easily-controllable, low in cost, and asepsis environment-protecting can effectively solve the problem that
ZnIn2S4Nano-chip arrays can not large-scale application problem, can for its engineering fields such as photocatalysis further application establish
Fixed good basis.
Summary of the invention
For the deficiency of existing zinc indium sulphur nanometer chip architecture technology of preparing, the object of the present invention is to provide one kind
ZnIn2S4The preparation method of nano-chip arrays film, process is simple, securely and reliably, low in cost.
The purpose of the present invention can be achieved through the following technical solutions:
(1) one layer of In is deposited in clean FTO conductive glass surface using chemical method2S3Nano thin-film, and sputtered on its surface
One layer of zinc is as substrate.
(2) concentration is added in reaction kettle liner for the indium source of 0.1-0.3M and sulphur source, until mole of indium salts and sulphur source
It than adding solvent for 1:4 ~ 1:8, is then stirred or ultrasonic dissolution, is made into uniform precursor solution.
(3) substrate and configured presoma are put into reaction kettle and are sealed, control 150 ~ 200 DEG C of temperature, when reaction
Between 1 ~ 4 hour；After reaction, reaction kettle cooled to room temperature is cleaned and dried after taking out sample, can be obtained in substrate
The ZnIn of homoepitaxial2S4Nano-chip arrays film.
The FTO of cleaning as described in step (1), which refers to, is successively cleaned by ultrasonic 10 by acetone, dehydrated alcohol and deionized water
min。
In In described in step (1)2S3The thickness of nano thin-film is probably at 1 μm.
In In described in step (1)2S3Nano thin-film surface sputters the thickness of zinc probably in 50-200 nm.
Indium salts described in step (2) are inidum chloride, indium nitrate, indium sulfate or indium acetate etc., and sulphur source is thiocarbamide, half Guang ammonia
Acid or thioacetamide etc..
Organic solvent described in step (2) is the mixture of ethylene glycol or ethylene glycol and ethyl alcohol.
Indium salts described in step (2), concentration is preparation In2S31/2 when concentration.
Reaction time described in step (3) is preferably 2-3h, and preferably 180 ~ 200 °C of reaction temperature.
Compared with prior art, advantage of the present invention is as follows:
1. raw material used in the present invention are relatively easily obtained, preparation process is simple, securely and reliably, low in cost, in solar energy
Photocatalysis field has a good application prospect.
2. the present invention is with In2S3Nano-chip arrays are to obtain the ZnIn of high quality from template is sacrificed2S4Nano-chip arrays；Phase
Compared with traditional one-step method, process is more controllable, can obtain desired pattern.
3. ZnIn prepared by the present invention2S4Nano-chip arrays, general 5 nm of the nanometer sheet thickness on surface, there is specific surface
Product is high, reflectivity is low, falls into the excellent characteristics such as photosensitiveness is good, defect is less, easy recycling.
Detailed description of the invention
Fig. 1 is grown in by embodiment 1 and is deposited with In2S3FTO substrate on ZnIn2S4The SEM of nano-chip arrays film
Figure；
Fig. 2 is grown in by embodiment 1 and is deposited with In2S3FTO substrate on ZnIn2S4The photoelectrocatalysis of nano-chip arrays film
Performance map.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection scope.
Embodiment 1
A kind of ZnIn2S4The preparation method of nano-chip arrays film comprising the steps of:
(1) one layer 1 μm of In is deposited in clean FTO conductive glass surface using chemical method2S3Nano thin-film, and in its table
The zinc of face sputtering 100nm.
(2) thioacetamide and inidum chloride are mixed to join in reaction kettle according to the molar ratio of 4:1, add 40 ml
Ethylene glycol, is then stirred or ultrasonic dissolution, is made into the homogeneous solution that indium salts concentration is 0.2M；
(3) substrate and configured presoma are put into reaction kettle and are sealed, control 180 DEG C of temperature, the reaction time 2 hours；
After reaction, reaction kettle cooled to room temperature is cleaned and dried after taking out sample, the homoepitaxial in substrate can be obtained
ZnIn2S4Nano-chip arrays film.
Fig. 1 is the ZnIn that the present embodiment obtains2S4The SEM of film schemes；As shown in Figure 1, ZnIn2S4Film is received by vertical
Rice piece forming array, sectional view show the characteristic of growth in situ.
Fig. 2 is the ZnIn that the present embodiment obtains2S4The performance map of film, it can be seen that it has good optogalvanic effect, says
The bright good sunken photosensitiveness of this array structure.It further illustrates that product of the present invention has in solar energy photocatalytic field to answer well
Use prospect.
Embodiment 2
A kind of ZnIn2S4The preparation method of nano-chip arrays film comprising the steps of:
(1) one layer 1 μm of In is deposited in clean FTO conductive glass surface using chemical method2S3Nano thin-film, and in its table
The zinc of face sputtering 200nm.
(2) thiocarbamide and inidum chloride are mixed to join in reaction kettle according to the molar ratio of 4:1, add 40 ml ethylene glycol,
Then it is stirred or ultrasonic dissolution, is made into the homogeneous solution that indium salts concentration is 0.3M；
(3) substrate and configured presoma are put into reaction kettle and are sealed, control 180 DEG C of temperature, the reaction time 4 hours；
After reaction, reaction kettle cooled to room temperature is cleaned and dried after taking out sample, the homoepitaxial in substrate can be obtained
ZnIn2S4Nano-chip arrays film.
Embodiment 3
A kind of ZnIn2S4The preparation method of nano-chip arrays film comprising the steps of:
(1) one layer 1 μm of In is deposited in clean FTO conductive glass surface using chemical method2S3Nano thin-film, and in its table
The zinc of face sputtering 50nm.
(2) cysteine and indium nitrate are mixed to join in reaction kettle according to the molar ratio of 4:1, add 40 ml second
Glycol, is then stirred or ultrasonic dissolution, is made into the homogeneous solution that indium salts concentration is 0.1M；
(3) substrate and configured presoma are put into reaction kettle and are sealed, control 200 DEG C of temperature, the reaction time 1 hour；
After reaction, reaction kettle cooled to room temperature is cleaned and dried after taking out sample, the homoepitaxial in substrate can be obtained
ZnIn2S4Nano-chip arrays film.
Embodiment 4
A kind of ZnIn2S4The preparation method of nano-chip arrays film comprising the steps of:
(1) one layer 1 μm of In is deposited in clean FTO conductive glass surface using chemical method2S3Nano thin-film, and in its table
The zinc of face sputtering 100nm.
(2) cysteine and indium acetate are mixed to join in reaction kettle according to the molar ratio of 8:1, add 40 ml second
Glycol, is then stirred or ultrasonic dissolution, is made into the homogeneous solution that indium salts concentration is 0.2M；
(3) substrate and configured presoma are put into reaction kettle and are sealed, control 200 DEG C of temperature, the reaction time 2 hours；
After reaction, reaction kettle cooled to room temperature is cleaned and dried after taking out sample, the homoepitaxial in substrate can be obtained
ZnIn2S4Nano-chip arrays film.
Embodiment 5
A kind of ZnIn2S4The preparation method of nano-chip arrays film comprising the steps of:
(1) one layer 1 μm of In is deposited in clean FTO conductive glass surface using chemical method2S3Nano thin-film, and in its table
The zinc of face sputtering 100nm.
(2) thioacetamide and indium sulfate are mixed to join in reaction kettle according to the molar ratio of 6:1, add 40 ml
Ethylene glycol, is then stirred or ultrasonic dissolution, is made into the homogeneous solution that indium salts concentration is 0.3M；
(3) substrate and configured presoma are put into reaction kettle and are sealed, control 150 DEG C of temperature, the reaction time 3 hours；
After reaction, reaction kettle cooled to room temperature is cleaned and dried after taking out sample, the homoepitaxial in substrate can be obtained
ZnIn2S4Nano-chip arrays film.
Embodiment 6
A kind of ZnIn2S4The preparation method of nano-chip arrays film, control temperature, 200 DEG C, the reaction time 3 hours, indium salts concentration
For 0.3M；The ZnIn of the homoepitaxial in substrate can be obtained with case study on implementation 1 in other conditions2S4Nano-chip arrays film.
Embodiment 7
A kind of ZnIn2S4The preparation method of nano-chip arrays film, 160 DEG C of temperature of control, the reaction time 3 hours, indium salts concentration
For 0.2M；The ZnIn of the homoepitaxial in substrate can be obtained with case study on implementation 1 in other conditions2S4Nano-chip arrays film.
Embodiment 8
A kind of ZnIn2S4The preparation method of nano-chip arrays film controls 150 DEG C of temperature, the reaction time 4 hours；Other conditions
With embodiment 1, the three-dimensional flower piece shape ZnIn of the homoepitaxial on zinc metal sheet can be obtained2S4Micro-nano wire array film.
Claims (9)
1. a kind of preparation method of zinc indium sulphur nano-chip arrays film, zinc indium sulphur content minor is ZnIn2S4, which is characterized in that by with
Lower step preparation:
(1) one layer of In is deposited in clean FTO conductive glass surface using chemical method2S3Nano thin-film, and one layer is sputtered on surface
Zinc film is as substrate；
(2) indium salts and sulphur source that concentration is 0.1-0.3M are added in reaction kettle liner, add solvent, indium salts and sulphur source
Molar ratio is 1:4 ~ 1:8, is then stirred or ultrasonic dissolution, and uniform precursor solution is made into；
(3) substrate and configured presoma are put into reaction kettle and are sealed, control 150 ~ 200 DEG C of temperature, the reaction time 1 ~ 4
Hour；After reaction, reaction kettle cooled to room temperature is cleaned and dried after taking out sample, can be obtained in substrate uniformly
The ZnIn of growth2S4Nano-chip arrays film.
2. the preparation method of zinc indium sulphur nano-chip arrays film according to claim 1, which is characterized in that in step (1)
The clean FTO, which refers to, is successively cleaned by ultrasonic 10 min by acetone, dehydrated alcohol and deionized water.
3. the preparation method of zinc indium sulphur nano-chip arrays film according to claim 1, which is characterized in that in step (1)
It is described in In2S3Nano thin-film with a thickness of 1 μm.
4. the preparation method of zinc indium sulphur nano-chip arrays film according to claim 1, which is characterized in that in step (1)
It is described in In2S3Nano thin-film surface sputter zinc with a thickness of 50-200 nm.
5. the preparation method of zinc indium sulphur nano-chip arrays film according to claim 1, which is characterized in that the indium salts
For inidum chloride, indium nitrate, indium sulfate or indium acetate etc..
6. the preparation method of zinc indium sulphur nano-chip arrays film according to claim 1, which is characterized in that the sulphur source
For thiocarbamide, cysteine or thioacetamide.
7. the preparation method of zinc indium sulphur nano-chip arrays film according to claim 1, which is characterized in that in step (2)
Organic solvent be ethylene glycol or ethylene glycol and ethyl alcohol mixture.
8. the preparation method of zinc indium sulphur nano-chip arrays film according to claim 1, which is characterized in that in step (2)
The concentration of the indium salts is 0.1-0.3M, to prepare In2S31/2 when concentration.
9. the preparation method of zinc indium sulphur nano-chip arrays film according to claim 1, which is characterized in that in step (3)
The reaction time is preferably 2-3h, and preferably 180 ~ 200 °C of reaction temperature.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111822013A (en) * | 2020-07-06 | 2020-10-27 | 重庆大学 | Single-cell PN junction and accurate construction method thereof |
| CN114105188A (en) * | 2021-12-01 | 2022-03-01 | 徐州医科大学 | In2S3Preparation method of nano-flake array material |
| CN115125560A (en) * | 2022-06-14 | 2022-09-30 | 杭州电子科技大学 | Preparation method of beta-phase indium sulfide micron sheet array |
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| 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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2018
- 2018-10-19 CN CN201811222709.0A patent/CN109052988B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111822013A (en) * | 2020-07-06 | 2020-10-27 | 重庆大学 | Single-cell PN junction and accurate construction method thereof |
| CN114105188A (en) * | 2021-12-01 | 2022-03-01 | 徐州医科大学 | In2S3Preparation method of nano-flake array material |
| CN115125560A (en) * | 2022-06-14 | 2022-09-30 | 杭州电子科技大学 | Preparation method of beta-phase indium sulfide micron sheet array |
| 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 |
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