CN114105188A - In2S3Preparation method of nano-flake array material - Google Patents
In2S3Preparation method of nano-flake array material Download PDFInfo
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- CN114105188A CN114105188A CN202111459945.6A CN202111459945A CN114105188A CN 114105188 A CN114105188 A CN 114105188A CN 202111459945 A CN202111459945 A CN 202111459945A CN 114105188 A CN114105188 A CN 114105188A
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- C01G15/00—Compounds of gallium, indium or thallium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C01P2004/00—Particle morphology
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- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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Abstract
The invention discloses an In2S3Dissolving a sulfur source in deionized water, stirring to prepare a solution, then adding zinc salt and indium salt, and stirring to prepare a mixed solution; putting a substrate into a polytetrafluoroethylene kettle, transferring the mixed solution into the polytetrafluoroethylene kettle with the substrate, putting the polytetrafluoroethylene kettle into an oven, heating to 180-210 ℃, preserving heat for 0.5-4 hours, and naturally cooling the reaction kettle to room temperature after the reaction is finished; taking out the substrate, repeatedly washing with ethanol and deionized water, and oven drying to obtain In2S3A nanoflake array material. According to the invention, a hydrothermal method and water are used as a solvent, so that the method is simple, environment-friendly and easy to operate; inert atmosphere protection is not needed, and the conditions are simple; the obtained nano material hasLarge specific surface area, visible light response and photoelectrochemical performance, and uniform appearance.
Description
Technical Field
The invention relates to a preparation method of an array structure material, In particular to2S3A preparation method of a nano flake array material.
Background
Hydrogen energy is considered as one of the green energy sources with the most development potential in the 21 st century, high-efficiency hydrogen production is realized by utilizing sunlight to catalytically decompose water through artificial simulation of photosynthesis, and one of the most direct ways of realizing artificial photosynthesis is to construct an effective Photoelectrochemical (PEC) water decomposition system. Photoelectrochemical (PEC) water splitting has attracted considerable interest in recent years because of its renewable, clean and environmentally friendly advantages. In order to utilize and convert solar energy efficiently, a suitable semiconductor photoelectric electrode needs to be designed and prepared.
In2S3Is a typical III-VI sulfide semiconductor material, and has a forbidden band width of about 2.00 eV. Due to stable physical and chemical properties, narrower forbidden band width and better visible light absorption characteristics, the material has good application prospect in the fields of photocatalysis, photoconduction, photoelectricity and the like, and is a photoelectric material with good application potential. To date, In having various two-dimensional morphologies has been successfully synthesized by different methods2S3Such as nanoparticles, nanosheets, nanorods, nanosheets and microspheres composed of nanosheets. The unique physical and chemical properties of indium sulfide are not only related to the indium sulfide, but also depend on the shape and the organization structure of the indium sulfide to a great extent. For In2S3The morphology control of the organic electroluminescent device to simultaneously enhance the specific surface area and the charge mobility of the organic electroluminescent device has become a research hotspot. Due to the large specific surface area, good stability, light scattering-promoting light absorption properties, and direct electron transport paths of ordered nano-array structures, the design and synthesis of nano-array structures have attracted much attention.
Up to now, In was prepared using a conventional hydrothermal method2S3Nanoarrays are difficult and are susceptible to photo-erosion and peeling from the substrate under illumination. In the reported article, In is involved2S3The preparation of nanoarrays mostly uses solvothermal methods.
Disclosure of Invention
In view of the problems of the prior art, the present invention provides an In2S3A method for preparing a nano-flake array material,in is caused to be2S3The material can be effectively excited by visible light, has good stability and the like, and avoids the environmental pollution caused by the use of a large amount of organic solvents.
In order to achieve the purpose, the invention provides the following technical scheme: in2S3The preparation method of the nano flake array material comprises the following steps:
a. dissolving a sulfur source in deionized water, stirring to prepare a solution, then adding a zinc salt and an indium salt, and stirring at a constant speed for 20-30 min to prepare a mixed solution, wherein the mass ratio of the sulfur source to the indium salt is 1.5: 1-2: 1, and preferably 1.9: 1;
b. putting transparent conductive glass, copper foil or stainless steel into a polytetrafluoroethylene kettle as a substrate, transferring the mixed solution obtained in the step a into the polytetrafluoroethylene kettle with the substrate, putting the polytetrafluoroethylene kettle into an oven, heating to 180-210 ℃, preserving heat for 0.5-4 hours, and naturally cooling the reaction kettle to room temperature after the reaction is finished;
c. taking out the substrate, repeatedly washing the substrate with ethanol and deionized water, and drying the substrate In a drying oven at the temperature of 60-80 ℃ to obtain In2S3A nanoflake array material.
Furthermore, the molar ratio of the zinc salt to the indium salt In the step a is 3.4:100 to 10.2:100, preferably 5.5:100, and the molar ratio of the zinc salt to the indium salt is far lower than that of the indium salt, so that the main component of the obtained product is In2S3Instead of ZnIn2S4(ii) a The molar ratio of the zinc salt to the sulfur source is 2:3, so that the In of the synthesized product can be ensured2S3And the waste of indium raw materials is reduced.
Further, the sulfur source in the step a is thiourea or thioacetamide; the zinc salt is zinc chloride, zinc sulfate or zinc nitrate; the indium salt is indium nitrate, indium chloride or indium sulfate.
Further, In said step c2S3The thickness of the nano thin sheet array material is 100 nm, and the thickness of the film layer is 4.5 mu m.
Further, the hydrothermal temperature in the step b is 190 ℃.
Further, the hydrothermal time in the step b is 3 hours.
Further, the ratio of the sulfur source, the indium salt and the zinc salt added in the step a is 1.5-2: 1: 0.034-0.134, preferably 2: 1: 0.04; the proportion of adding zinc salt is particularly important, and if no or too little zinc salt is added, a nano flake array structure cannot be obtained; if an excess of zinc salt is added, ZnIn will be formed2S4Nanoarrays instead of In2S3A nanoflake array material.
Compared with the prior art, the method has the advantages that a hydrothermal method and water are used as a solvent, so that the method is simple, environment-friendly and easy to operate; inert atmosphere protection is not needed, and the conditions are simple; in2S3The band gap of the material is narrow and is about 2.0 eV, and the material has visible light response; produced In2S3The nano-flake array material is of an array structure formed by orderly arranging a plurality of nano-flakes, has larger specific surface area, visible light response and catalytic performance, is uniform in appearance and is suitable for large-area production and application; is suitable for gas-sensitive sensing, hydrogen production by photoelectric decomposition of water and photoelectric reduction of CO2And the like.
Drawings
FIG. 1 shows In of the present invention2S3Nano thin sheet array material and ZnIn2S4Comparing the appearance and the appearance of the nano array material;
FIG. 2 shows In of the present invention2S3A micro-topography of the nanoflake array material;
FIG. 3 shows In of the present invention2S3An XRD spectrum of the nano-flake array material;
FIG. 4 shows In of the present invention2S3The ultraviolet-visible light absorption spectrum of the nano-flake array material and a forbidden band width estimation result graph thereof;
FIG. 5 shows In of the present invention2S3XPS spectra of nanoplatelet array materials: (a) the total spectrum, (b) the fine spectrum of the In element, and (c) the fine spectrum of the S element.
Detailed Description
The invention will be further explained with reference to the drawings.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Dissolving 0.15g of thiourea in 20mL of deionized water, stirring at a constant speed for 20min, then adding 0.29g of indium chloride and 0.02g of zinc nitrate, stirring at a constant speed for 30min, transferring the mixed solution to a polytetrafluoroethylene kettle, and putting two pieces of transparent conductive glass with the conductive surfaces facing downwards, which are 2 multiplied by 3cm in advance, in the polytetrafluoroethylene kettle as a substrate; then putting the mixture into an oven to react for 3 hours at the temperature of 210 ℃; naturally cooling the reaction kettle to room temperature after the reaction is finished, taking out the transparent conductive glass, repeatedly washing the transparent conductive glass by using ethanol and deionized water, and drying the transparent conductive glass In a drying oven at the temperature of 60 ℃ to obtain an orange film layer, namely In2S3A nanoflake array material.
In2S3The macro topography of the nano-flake array material is shown in fig. 1b, which is an orange thin film; as shown in FIG. 1a, ZnIn without zinc salt is added2S4The material is yellow. FIG. 2a and FIG. 2b are In of the present invention, respectively2S3Surface and cross-sectional views of the micro-topography of the nanoflake array material, In can be seen In FIG. 2a2S3The nano flake array material is an ordered array consisting of a plurality of nano flakes, and as can be seen from figure 2b, the nano flake array consists of two layers, wherein the lower layer is ZnIn2S4The seed layer has a thickness of about 100 nm and an upper layer of In2S3The thickness of the film layer was 4.5. mu.m. As shown In FIG. 3, In2S3Except the peak showing FTO In the nano-flake array material, other miscellaneous peaks do not exist, and purer In is obtained2S3. As shown In FIG. 4, In2S3The visible light region of the nano flake array material has stronger absorption, and the band gap of the nano flake array material is 2.08 eV. As shown In FIG. 5, In2S3Nano thin sheet array materialThe In element In the XPS spectrum of (1) shows a valence of +3, the S element shows a valence of-2, and the hetero phase ZnIn2S4The composition of (a) is extremely small and negligible.
Dissolving 0.38g of thiourea in 50mL of deionized water, stirring at a constant speed for 20min, then adding 0.73g of indium nitrate and 0.02g of zinc sulfate, stirring at a constant speed for 30min, transferring the mixed solution to a polytetrafluoroethylene kettle, and putting two pieces of copper foil with the conductive surfaces facing downwards, which are 2 multiplied by 3cm in advance, in the polytetrafluoroethylene kettle as a substrate; then putting the copper foil into an oven to react for 2h at 190 ℃, taking out the copper foil after naturally cooling to room temperature, taking out the copper foil, repeatedly washing the copper foil with ethanol and deionized water, and putting the copper foil into the oven at 70 ℃ for drying to obtain orange In2S3A nanoflake array material.
Dissolving 0.38g of thioacetamide in 50mL of deionized water, stirring at a constant speed for 30min, then adding 0.73g of indium sulfate and 0.02g of zinc chloride, stirring at a constant speed for 20min, transferring the mixed solution to a polytetrafluoroethylene kettle, and putting two pieces of stainless steel with 2 x 3cm conductive surfaces facing downwards in the polytetrafluoroethylene kettle as substrates in advance; then putting the mixture into an oven, heating the mixture to 180 ℃ and reacting the mixture for 4 hours; naturally cooling the reaction kettle to room temperature after the reaction is finished, taking out the stainless steel, repeatedly washing the stainless steel by using ethanol and deionized water, and drying the stainless steel In an oven at the temperature of 80 ℃ to obtain orange In2S3A nanoflake array material.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and any minor modifications, equivalent replacements and improvements made to the above embodiment according to the technical spirit of the present invention should be included in the protection scope of the technical solution of the present invention.
Claims (7)
1. In2S3The preparation method of the nano flake array material is characterized by comprising the following steps of:
a. dissolving a sulfur source in deionized water, stirring to prepare a solution, then adding a zinc salt and an indium salt, and stirring at a constant speed for 20-30 min to prepare a mixed solution, wherein the mass ratio of the sulfur source to the indium salt is 1.5: 1-2: 1;
b. putting transparent conductive glass, copper foil or stainless steel into a polytetrafluoroethylene kettle as a substrate, transferring the mixed solution obtained in the step a into the polytetrafluoroethylene kettle with the substrate, putting the polytetrafluoroethylene kettle into an oven, heating to 180-210 ℃, preserving heat for 0.5-4 hours, and naturally cooling the reaction kettle to room temperature after the reaction is finished;
c. taking out the substrate, repeatedly washing the substrate with ethanol and deionized water, and drying the substrate In a drying oven at the temperature of 60-80 ℃ to obtain In2S3A nanoflake array material.
2. An In according to claim 12S3The preparation method of the nano-flake array material is characterized by comprising the following steps: the molar ratio of the zinc salt to the indium salt in the step a is 3.4: 100-10.2: 100; the molar ratio of zinc salt to sulfur source was 2: 3.
3. An In according to claim 12S3The preparation method of the nano-flake array material is characterized by comprising the following steps: the sulfur source in the step a is thiourea or thioacetamide; the zinc salt is zinc chloride, zinc sulfate or zinc nitrate; the indium salt is indium nitrate, indium chloride or indium sulfate.
4. An In according to claim 12S3The preparation method of the nano-flake array material is characterized by comprising the following steps: in said step c2S3The thickness of the nano thin sheet array material is 100 nm, and the thickness of the film layer is 4.5 mu m.
5. An In according to claim 12S3The preparation method of the nano-flake array material is characterized by comprising the following steps: the hydrothermal temperature in the step b is 190 ℃.
6. An In according to claim 12S3The preparation method of the nano-flake array material is characterized by comprising the following steps: the hydrothermal time in the step b is 3 hours.
7. An In according to claim 12S3The preparation method of the nano-flake array material is characterized by comprising the following steps: the ratio of the sulfur source to the indium salt to the zinc salt added in the step a is 1.5-2: 1: 0.034-0.134.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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