CN111533462A - Chemical method for rapidly synthesizing silver sulfide film at normal temperature - Google Patents
Chemical method for rapidly synthesizing silver sulfide film at normal temperature Download PDFInfo
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- CN111533462A CN111533462A CN202010262158.1A CN202010262158A CN111533462A CN 111533462 A CN111533462 A CN 111533462A CN 202010262158 A CN202010262158 A CN 202010262158A CN 111533462 A CN111533462 A CN 111533462A
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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
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/20—Metallic material, boron or silicon on organic substrates
- C23C14/205—Metallic material, boron or silicon on organic substrates by cathodic sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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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
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/28—Other inorganic materials
- C03C2217/287—Chalcogenides
- C03C2217/288—Sulfides
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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
- C03C2218/15—Deposition methods from the vapour phase
- C03C2218/154—Deposition methods from the vapour phase by sputtering
- C03C2218/156—Deposition methods from the vapour phase by sputtering by magnetron sputtering
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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
- C03C2218/30—Aspects of methods for coating glass not covered above
- C03C2218/32—After-treatment
Abstract
The invention relates to a chemical method for rapidly synthesizing a silver sulfide film at normal temperature. The method comprises the following steps: and reacting the substrate deposited with the simple substance silver film with an ammonium polysulfide aqueous solution at normal temperature and normal pressure, thus obtaining the silver sulfide semiconductor film material in situ on the surface of the substrate material. The method has the advantages that the ammonium polysulfide and the simple substance silver film are reacted under the conditions of normal temperature and normal pressure, the reaction speed is high, the preparation of the silver sulfide film can be quickly realized under the condition that the reaction time is less than 1min, and the obtained silver sulfide film has high compactness and good stability. The thickness of the silver sulfide film can reach 300-1000 nm.
Description
Technical Field
The invention belongs to the technical field of material chemistry, and particularly relates to a chemical method for rapidly synthesizing a silver sulfide film at normal temperature.
Background
Silver sulfide is a narrow band gap n-type semiconductor material, has a forbidden band width of about 0.9eV, and can absorb sunlight in a near infrared region. At present, the material has been widely applied to the research field of photoelectric conversion, such as: thin film solar cell devices, photodetectors, photocatalysis, photoluminescence, and the like.
At present, there are patent publications and related reports on the preparation of silver sulfide thin film materials. For example, the patent (201010111402.0) before the subject group discloses a chemical method for in-situ synthesis of a flaky silver sulfide nanocrystalline photoelectric thin film at low temperature: firstly, adding sulfur powder and an organic solvent into a clean container, then placing a silver film at the bottom of the solvent, and reacting for 4-184 hours at the temperature of 20-60 ℃ to obtain the silver sulfide film material. Patent (201510348950.8) discloses a method for preparing a vermicular nano silver sulfide film: adding silver nitrate and thiourea serving as reactants into a container filled with a substrate material according to a molar ratio of 2:1, standing the device at room temperature for 3 days, and taking out the deposited silver sulfide film material after the solution is completely clarified. Chunlei Guo professor topic group of national emphasis laboratory for optical applications of Changchun reports a preparation method of a silver sulfide film, which comprises the steps of utilizing a hot injection method to react Ag-TOP (Ag-tri-n-octyl phosphorus oxide) with sulfur simple substance for 5min at 160 ℃ to prepare a small amount of silver sulfide quantum dots, then carrying out centrifugal cleaning and purification, and finally carrying out spin coating to obtain the silver sulfide film. YongZhai et al, university of Henan, reported that a silver sulfide thin film material was prepared by a precursor thermal decomposition method, in which silver oxalate and thiourea were dissolved in a mixed solution of n-butylamine and propionic acid, and then spin-coated on the surface of a substrate to form a precursor, which was heated at 150 ℃ for 10min, and this operation was repeated several times to obtain a silver sulfide thin film material. The professor C.D. Lokhand of Hewaji university in India prepares the silver sulfide film material by utilizing a continuous ion layer exchange method, firstly, a substrate material is soaked in a silver nitrate aqueous solution for 12s, then soaked in deionized water for 10s, then the substrate material with silver ions adsorbed on the surface is soaked in a thiourea aqueous solution for 10s, then soaked in the deionized water for 10s and cleaned, and the operation is repeated for 30min to prepare the silver sulfide film.
In summary, the preparation method of the silver sulfide semiconductor thin film material still has many problems, such as long preparation time, complex preparation method, organic solvent pollution and the like, and can not meet the requirements of actual industrial production. Therefore, it is required to develop a method which is simple in operation, green and environment-friendly and can realize the preparation of large-area silver sulfide thin film materials in a short time.
The invention content is as follows:
the invention aims to solve the problems that: aiming at the problem that the large-area and high-quality film is difficult to be rapidly prepared under the normal temperature condition in the silver sulfide film preparation method reported in the prior art, the chemical method for rapidly preparing the silver sulfide semiconductor film material in the large area is provided.
The technical scheme adopted by the invention for solving the problems is as follows:
a chemical method for rapidly synthesizing silver sulfide film at normal temperature is characterized in that: and reacting the substrate deposited with the simple substance silver film with an ammonium polysulfide aqueous solution at normal temperature and normal pressure to prepare the silver sulfide semiconductor film material on the surface of the substrate material in situ.
In the scheme, the substrate material is ITO, FTO and polyimide;
in the scheme, the deposition method comprises magnetron sputtering, evaporation and electroplating;
in the above scheme, the thickness of the silver simple substance film is 100nm to 300nm, but is not limited to this thickness;
in the scheme, the ammonium polysulfide aqueous solution is obtained by adding sulfur powder into an ammonium sulfide aqueous solution and stirring until the sulfur powder is completely dissolved.
In the above embodiment, the amount of the sulfur powder used in the preparation of the ammonium polysulfide aqueous solution is 0.01g/mL to 0.03g/mL of the ammonium sulfide aqueous solution, but is not limited to this concentration range. The use amount of the sulfur powder is controlled, so that the silver sulfide film can not fall off in the preparation process of the silver sulfide film.
In the above embodiment, further, the concentration of the ammonium sulfide solution used in the preparation of the ammonium polysulfide aqueous solution is 40 to 48%. In the above scheme, the water used in the ammonium sulfide aqueous solution is deionized water.
In the scheme, the reaction time is less than or equal to 1 min.
According to the scheme, the silver sulfide film prepared by the method has uniform surface, 100-500nm silver sulfide crystal grains and high crystallinity.
The invention has the advantages that:
1. the method has the advantages that the ammonium polysulfide and the simple substance silver film are reacted under the conditions of normal temperature and normal pressure, the reaction speed is high, the preparation of the silver sulfide film can be quickly realized under the condition that the reaction time is less than 1min, and the obtained silver sulfide film has high compactness and good stability. The thickness of the silver sulfide film can reach 300-1000 nm.
2. The method has low cost. The ammonium sulfide aqueous solution and the elemental sulfur are used as reactants, so that the raw materials are easy to obtain and low in cost, and large-scale preparation is facilitated.
3. The method has simple post-treatment. The prepared silver sulfide film only needs to be simply cleaned by deionized water, and the processes of centrifugation, dialysis, organic solvent treatment and the like are avoided.
4. The method has large film forming area and controllable pattern. The area and the pattern of the simple substance silver film can be controlled by magnetron sputtering, and the original area and the pattern are reserved after the reaction is finished.
5. The method is environment-friendly. Deionized water is used as a solvent in the preparation process and the cleaning process, and no organic solvent is used, so that the influence of the use of organic medicines on the environment is avoided.
Drawings
FIG. 1, scanning electron micrograph of silver sulfide thin film prepared in example 1;
FIG. 2, X-ray powder diffraction pattern of silver sulfide film prepared in example 1;
FIG. 3 is a scanning electron micrograph of a silver sulfide thin film prepared in example 2;
FIG. 4, X-ray powder diffraction pattern of silver sulfide thin film prepared in example 2;
FIG. 5, SEM photograph of silver sulfide thin film prepared in example 3;
FIG. 6, X-ray powder diffraction pattern of silver sulfide thin film prepared in example 4.
The specific implementation mode is as follows:
this is further illustrated by the following examples.
Example 1
1. Preparation work: a100 nm-thick simple substance silver film is sputtered on the surface of the polyimide film by a magnetron sputtering method (in the embodiment, the film thickness is controlled by film thickness monitoring) for standby. Preparation of ammonium polysulfide solution: weighing 0.1g of sulfur powder, adding the sulfur powder into 10mL of ammonium sulfide aqueous solution (40-48 wt%), and stirring until the sulfur powder is completely dissolved to obtain a clear and transparent ammonium polysulfide aqueous solution for later use.
2. The reaction steps are as follows: and (3) putting the substrate material sputtered with the 100nm simple substance silver film into the prepared ammonium polysulfide aqueous solution, and reacting for 20s at normal temperature and normal pressure to completely convert the silvery white simple substance silver film into a gray black silver sulfide film. No film formed during the reaction was seen to fall off the substrate surface. Carefully cleaning the prepared silver sulfide film in deionized water, removing the ammonium polysulfide aqueous solution on the surface, and drying at 80 ℃. The scanning electron micrograph is shown in figure 1, the film is composed of nano-scale particles, and the particle size distribution of the particles is relatively uniform. The X-ray powder diffraction pattern is shown in figure 2, and the prepared film is pure phase silver sulfide compared with a standard powder diffraction PDF card.
Example 2
1. Preparation work: a100 nm-thick simple substance silver film is sputtered on the surface of the polyimide film by a magnetron sputtering method (in the embodiment, the film thickness is controlled by film thickness monitoring) for standby. Preparation of ammonium polysulfide solution: 0.2mg of sulfur powder is weighed and added into 10mL of ammonium sulfide aqueous solution (40-48 wt%), and the mixture is stirred until the sulfur powder is completely dissolved, so that clear and transparent ammonium polysulfide aqueous solution is obtained for standby.
2. The reaction steps are as follows: and (3) putting the substrate material sputtered with the 100nm simple substance silver film into the prepared ammonium polysulfide aqueous solution, and reacting for 20s at normal temperature and normal pressure to completely convert the silvery white simple substance silver film into a gray black silver sulfide film. No film formed during the reaction was seen to fall off the substrate surface. Carefully cleaning the prepared silver sulfide film in deionized water, removing the ammonium polysulfide aqueous solution on the surface, and drying at 80 ℃. The scanning electron micrograph is shown in figure 3, the film is composed of nano-scale particles, the particle size distribution of the particles is uniform, and the particles on the surface of the film have a tendency to become larger compared with the particles on the surface of the film in example 2. The X-ray powder diffraction pattern is shown in figure 4, and the prepared film is pure phase silver sulfide compared with the standard powder diffraction PDF card.
Example 3
1. Preparation work: a300 nm-thick simple substance silver film is sputtered on the surface of the polyimide film by a magnetron sputtering method (in the embodiment, the film thickness is controlled by film thickness monitoring) for standby. Preparation of ammonium polysulfide solution: 0.3g of sulfur powder is weighed and added into 10mL of ammonium sulfide aqueous solution (40-48 wt%), and the mixture is stirred until the sulfur powder is completely dissolved, so that clear and transparent ammonium polysulfide aqueous solution is obtained for standby.
2. The reaction steps are as follows: and (3) putting the substrate material sputtered with the 300nm simple substance silver film into the prepared ammonium polysulfide aqueous solution, and reacting for 50s at normal temperature and normal pressure to completely convert the silvery white simple substance silver film into a gray black silver sulfide film. The film formed during the reaction was seen to continuously fall off the substrate surface. Carefully cleaning the prepared silver sulfide film in deionized water, removing the ammonium polysulfide aqueous solution on the surface, and drying at 80 ℃. The scanning electron micrograph is shown in figure 5, the film is composed of nano-scale particles, the particle size distribution of the particles is relatively uniform, and the surface compactness of the film is increased compared with that of the films in examples 2 and 3.
Example 4
1. Preparation work: a100 nm-thick simple substance silver film is sputtered on the glass surface by a magnetron sputtering method (the film thickness is controlled by film thickness monitoring in the embodiment) for standby. Preparation of ammonium polysulfide solution: 0.1g of sulfur powder is weighed and added into 10mL of ammonium sulfide aqueous solution (40-48 wt%), and the mixture is stirred until the sulfur powder is completely dissolved, so that clear and transparent ammonium polysulfide aqueous solution is obtained for standby.
2. The reaction steps are as follows: and (3) placing the substrate material sputtered with the 100nm simple substance silver film into the prepared ammonium polysulfide aqueous solution, reacting for 20s at normal temperature and normal pressure, completely converting the silvery white simple substance silver film into a gray black silver sulfide film, and enabling the film which is not generated to fall off from the surface of the substrate in the reaction process. Carefully cleaning the prepared silver sulfide film in deionized water, removing the ammonium polysulfide aqueous solution on the surface, and drying at 80 ℃. The X-ray powder diffraction pattern is shown in figure 6, and the prepared film is pure phase silver sulfide compared with the standard powder diffraction PDF card.
Comparative example 1
1. Preparation work: a100 nm-thick simple substance silver film is sputtered on the surface of the polyimide film by a magnetron sputtering method (in the embodiment, the film thickness is controlled by film thickness monitoring) for standby.
2. The reaction steps are as follows: and (3) placing the substrate material sputtered with the 100nm simple substance silver film into a saturated sodium sulfide water solution, and keeping the substrate material at normal temperature and normal pressure for 20min, wherein no gray black silver sulfide film is generated.
Comparative example 2
1. Preparation work: a100 nm-thick simple substance silver film is sputtered on the surface of the polyimide film by a magnetron sputtering method (in the embodiment, the film thickness is controlled by film thickness monitoring) for standby.
2. Preparation of sodium polysulfide aqueous solution: firstly, preparing saturated sodium sulfide aqueous solution, then adding excessive sulfur powder, stirring at room temperature to obtain clear bright yellow aqueous solution, and floating the excessive sulfur powder on the water surface.
3. The reaction steps are as follows: the substrate material sputtered with the 100nm simple substance silver film is put into the sodium polysulfide aqueous solution and is kept for 30min at normal temperature and normal pressure, and no gray black silver sulfide film is generated.
Claims (9)
1. A chemical method for rapidly synthesizing silver sulfide film at normal temperature is characterized in that: and reacting the substrate deposited with the simple substance silver film with an ammonium polysulfide aqueous solution at normal temperature and normal pressure to prepare the silver sulfide semiconductor film material on the surface of the substrate material in situ.
2. The chemical process according to claim 1, characterized in that: the substrate material is ITO, FTO and polyimide.
3. The chemical process according to claim 1, characterized in that: the deposition method comprises magnetron sputtering, evaporation and electroplating.
4. The chemical process according to claim 1, characterized in that: the thickness of the silver simple substance film is 100 nm-300 nm.
5. The chemical process according to claim 1, characterized in that: the ammonium polysulfide aqueous solution is obtained by adding sulfur powder into an ammonium sulfide aqueous solution and stirring until the sulfur powder is completely dissolved.
6. The chemical process according to claim 5, characterized in that: in the preparation of the ammonium polysulfide aqueous solution, the dosage of the sulfur powder is 0.01 g/mL-0.03 g/mL of ammonium sulfide aqueous solution.
7. The chemical process according to claim 5, characterized in that: the concentration of the ammonium sulfide solution used in the preparation of the aqueous ammonium polysulfide solution is 40 to 48%.
8. The chemical process according to claim 1, characterized in that: the reaction time is less than or equal to 1 min.
9. The chemical process according to claim 1, characterized in that: the prepared silver sulfide film has uniform surface, 100-500nm silver sulfide crystal grains and high crystallinity.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115285946A (en) * | 2021-09-14 | 2022-11-04 | 许昌学院 | Ultrahigh-performance flexible silver selenide film with (201) dominant crystal face orientation and power generation device |
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| CN103247718A (en) * | 2013-04-09 | 2013-08-14 | 许昌学院 | Chemical method for in-situ control and synthesis of AgCuS/Ag3CuS2 ternary semiconductor photoelectric thin-film material at normal temperature |
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2020
- 2020-04-06 CN CN202010262158.1A patent/CN111533462A/en active Pending
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| CN101786650A (en) * | 2010-02-08 | 2010-07-28 | 许昌学院 | Chemical method for in situ synthesis of platy silver sulphide nano crystal photoelectric film at low temperature |
| CN102509769A (en) * | 2011-10-28 | 2012-06-20 | 许昌学院 | Ag2S flaky nanocrystal array and P3HT hybridized film photoelectric converting apparatus prepared based on low temperature |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115285946A (en) * | 2021-09-14 | 2022-11-04 | 许昌学院 | Ultrahigh-performance flexible silver selenide film with (201) dominant crystal face orientation and power generation device |
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Application publication date: 20200814 |