CN114645257A - Stannous selenide p-type semiconductor film and preparation method and application thereof - Google Patents

Stannous selenide p-type semiconductor film and preparation method and application thereof Download PDF

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CN114645257A
CN114645257A CN202210254539.4A CN202210254539A CN114645257A CN 114645257 A CN114645257 A CN 114645257A CN 202210254539 A CN202210254539 A CN 202210254539A CN 114645257 A CN114645257 A CN 114645257A
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chloride
stannous selenide
stannous
film layer
type semiconductor
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潘锋
梁军
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Peking University Shenzhen Graduate School
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Peking University Shenzhen Graduate School
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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
    • 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
    • C23C14/0623—Sulfides, selenides or tellurides

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
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  • Organic Chemistry (AREA)
  • Physical Deposition Of Substances That Are Components Of Semiconductor Devices (AREA)
  • Photovoltaic Devices (AREA)

Abstract

The application discloses a stannous selenide p-type semiconductor film and a preparation method and application thereof. The preparation method of the stannous selenide p-type semiconductor film comprises the steps of depositing a stannous selenide film layer on a substrate by adopting magnetron sputtering; carrying out chloride solution treatment on the substrate on which the stannous selenide film layer is deposited to obtain the stannous selenide film layer with the surface covered with chloride; and then heating the film for 10 to 60 minutes at the temperature of 600 ℃ in vacuum or inert atmosphere or weak reducing atmosphere, and cooling the film to room temperature to obtain the stannous selenide p-type semiconductor film. According to the preparation method, the amorphous stannous selenide film layer is prepared by magnetron sputtering, and then chloride solution treatment and 100-DEG C and 600-DEG C annealing treatment are carried out to obtain the crystallized stannous selenide p-type semiconductor film. The preparation method is simple, easy to operate and low in cost, is suitable for large-area production, and solves the problem that the SnSe material is difficult to form a film.

Description

Stannous selenide p-type semiconductor film and preparation method and application thereof
Technical Field
The application relates to the technical field of p-type semiconductor films, in particular to a stannous selenide p-type semiconductor film and a preparation method and application thereof.
Background
p-type semiconductors are a hot spot in the field of semiconductors, and doping properties, heat sensitivity, and photosensitivity thereof are advantageous for application to thin film solar cells, detectors, thin film transistors, displays, and the like. The thin film semiconductor material has the thickness in the micron or even nanometer level, greatly reduces the consumption of the material, has simple growth process, is convenient for manufacturing portable and bendable devices, has dominant cost performance and better industrialization prospect.
The p-type semiconductor material which is relatively conventional at present comprises Cu2O, CdTe and NiO. Wherein, Cu2O is unstable, CdTe contains heavy metals, and NiO is easy to reduce; thus, existing p-type semiconductors suffer from various drawbacks and deficiencies.
Research shows that a stannous selenide (SnSe) film can be used for preparing a thin film lithium ion battery or a photoelectric detector. However, the SnSe material is a layered structure, and the conventional method is not easy to form a film. Therefore, how to more effectively prepare the stannous selenide semiconductor thin film is a problem to be solved urgently.
Disclosure of Invention
The application aims to provide a novel preparation method of a stannous selenide p-type semiconductor film, the stannous selenide p-type semiconductor film prepared by the preparation method and application of the stannous selenide p-type semiconductor film.
The following technical scheme is adopted in the application:
one aspect of the application discloses a preparation method of a stannous selenide p-type semiconductor film, which comprises the steps of depositing a stannous selenide film layer on a substrate by adopting magnetron sputtering; carrying out chloride solution treatment on the substrate on which the stannous selenide film layer is deposited to obtain the stannous selenide film layer with the surface covered with chloride; then, heating the film for 10 to 60 minutes at the temperature of 600 ℃ in vacuum or inert atmosphere or weak reducing atmosphere, and cooling the film to room temperature to obtain the stannous selenide p-type semiconductor film; the chloride is at least one of stannous chloride, cadmium chloride, magnesium chloride, ruthenium chloride, niobium chloride, tantalum chloride, calcium chloride, zinc chloride, palladium chloride, rhodium chloride, stannic chloride, indium chloride, copper chloride and barium chloride; the chloride solution treatment comprises the steps of soaking the substrate deposited with the stannous selenide film layer into a chloride solution; or, coating the chloride solution on the surface of the stannous selenide film layer.
The method comprises the steps of preparing an amorphous stannous selenide film layer on a substrate through magnetron sputtering, and then carrying out chloride solution treatment and annealing treatment at the temperature of 600 ℃ on the stannous selenide film layer to obtain the high-crystallization stannous selenide p-type semiconductor film. The preparation method is simple in whole preparation process, easy to operate, low in cost and suitable for large-area production, and solves the problem that the SnSe material is difficult to form a film.
In one implementation of the present application, the chloride solution treatment further comprises UV irradiation treatment of the substrate on which the stannous selenide film layer is deposited before the substrate on which the stannous selenide film layer is deposited is immersed in the chloride solution.
Preferably, the soaking condition is that the soaking is carried out for 10 to 20 minutes at a temperature of between 50 and 60 ℃.
In one implementation of the present application, the chloride solution treatment, after coating the chloride solution on the surface of the stannous selenide film layer, further comprises heating to remove the solvent.
Preferably, the coating mode is smearing or spraying.
In one implementation mode of the application, magnetron sputtering conditions include that the pressure of a sputtering cavity is 0.1-10 Pa, the atmosphere of the sputtering cavity is argon, nitrogen or argon-hydrogen mixed gas, the temperature of a substrate is 10-500 ℃, and the sputtering power is 0.01-10W/cm2The deposition rate is 0.1-500 nm/min, and the sputtering time is 0.01-5 hours.
In one implementation of the present application, the solvent of the chloride solution is at least one of methanol, ethanol, isopropanol, N-butanol, ethylene glycol, N-dimethylformamide, dimethyl sulfoxide, ethyl acetate, propyl acetate, acetone, glacial acetic acid, and tetrahydrofuran.
In an implementation manner of the present application, the preparation method further includes, before magnetron sputtering the stannous selenide film layer, preparing a silicon dioxide layer on the substrate in advance; and then, carrying out magnetron sputtering on the stannous selenide film layer on the surface of the silicon dioxide layer.
It should be noted that, the preparation of the silicon dioxide layer in advance is mainly considered, and under the condition that the substrate undulates greatly, the substrate is flatter by preparing the silicon dioxide layer of tens of nanometers in advance, so that the stannous selenide film layer with more uniform thickness is prepared. The thickness of the silicon dioxide layer depends on the degree of undulation of the substrate, and may be, for example, 10nm, 20nm, 30nm, 40nm, or 50nm, as long as the purpose of flattening the substrate can be achieved. As for the preparation method of the silicon dioxide layer, magnetron sputtering is specifically used in the present application, but of course, it is not excluded that other methods may also be used.
In one implementation of the present application, the substrate is at least one of glass, conductive glass, a flexible substrate, a quartz plate, and sapphire.
In one implementation of the present application, the weakly reducing atmosphere is H2And Ar in a mixed gas of H and Ar2Accounting for 1 to 20 percent of the volume of the mixed gas.
The application also discloses a stannous selenide p-type semiconductor film prepared by the preparation method.
Preferably, the thickness of the stannous selenide film layer is 10-1000 nm.
The application also discloses application of the stannous selenide p-type semiconductor film in a thin film solar cell, a detector, a thin film transistor or a display.
The beneficial effect of this application lies in:
according to the preparation method of the stannous selenide p-type semiconductor film, the amorphous stannous selenide film layer is prepared by magnetron sputtering, and then chloride solution treatment and 100-plus-600-DEG annealing treatment are carried out to obtain the crystalline stannous selenide p-type semiconductor film. The preparation method is simple, easy to operate and low in cost, is suitable for large-area production, and solves the problem that the SnSe material is difficult to form a film.
Drawings
FIG. 1 is an SEM image of the surface topography of a stannous selenide film in an embodiment of the application;
FIG. 2 is a crystalline XRD spectrum of a stannous selenide thin film in an example of the application.
Detailed Description
The present application will be described in further detail with reference to specific examples. The following examples are intended to be illustrative of the present application only and should not be construed as limiting the present application.
Examples
In the method, a stannous selenide film layer is prepared on a glass substrate by adopting a magnetron sputtering method, and then chloride solution treatment and heating at the temperature of 100-. The preparation method comprises the following steps:
(1) cleaning a glass substrate: the glass adopted in the embodiment is ultra-white glass, the glass is soaked in a glass cleaning solution for 10 minutes, a high-pressure water gun is used for washing for 5 minutes, an air gun is used for drying, and the glass is placed in a drying furnace at 105 ℃ for 30 minutes to prepare for subsequent coating.
(2) Preparation of the silicon dioxide layer: by adopting a radio frequency sputtering method, the target material is silicon dioxide, and the background vacuum of a sputtering cavity is 2 multiplied by 10-4And Pa, introducing nitrogen, vacuumizing the cavity to 1Pa, turning on a radio frequency power supply, setting the power to be 15W, and sputtering the 20nm silicon dioxide film.
(3) Preparing a stannous selenide prefabricated film: adopting a direct current sputtering method, the target material is stannous selenide, and the background vacuum of a sputtering cavity is 2 multiplied by 10-4And Pa, introducing nitrogen, vacuumizing the cavity to 1Pa, turning on a direct-current power supply, setting the power to be 30W, and sputtering the 200nm stannous selenide film layer.
(4) Soaking the stannous selenide film in saturated glycol solution of stannous chloride with the concentration of 75 percent for 10 minutes at the temperature of 60 ℃, and taking out.
(5) The stannous selenide film is placed in a weak reducing atmosphere, wherein the weak reducing atmosphere is H2And Ar in a mixed gas of H and Ar25 percent of the volume of the mixed gas, annealing at 350 ℃ for 30 minutes, and naturally cooling to room temperature to obtain the crystallized stannous selenide p-type semiconductor film.
The scanning electron microscope SEM observation of the stannous selenide p-type semiconductor film prepared in the example shows that the result is shown in figure 1. The results in fig. 1 show that a highly crystalline SnSe film can be directly observed, and that SnSe having good crystallinity has good preferential performance and large columnar crystal grains.
In this example, X-ray diffraction measurements were performed on stannous selenide p-type semiconductor films prepared by annealing at 280 c and 380 c, respectively, and no annealing was used as a control, and the results are shown in fig. 2. The results show that after annealing at 280 ℃ and 380 ℃, a crystalline stannous selenide p-type semiconductor film can be obtained, which is in line with the expectation.
Further, the stannous selenide p-type semiconductor film prepared in the embodiment is tested by a Hall test resistance instrument, and the result shows that the Hall mobility of the SnSe film in the embodiment reaches 0.3cm2V (vs), the conductivity reached 103S/m, carrier concentration of 1018cm3。
The above results show that the stannous selenide p-type semiconductor film prepared in the embodiment has high mobility, can passivate the surface of a p-type semiconductor device, and can provide high-performance products for related solar cells, detectors and the like.
Based on the above tests, the results of further testing different annealing temperatures in this example show that after chloride treatment, annealing treatment by heating at 100-. The annealing temperature is lower than 100 ℃, and the crystalline stannous selenide cannot be effectively formed; while annealing temperatures are too high, e.g. above 600 ℃, on the one hand, they have a high energy consumption, and on the other hand, temperatures that are too high may have a negative effect on the substrate and also may not be beneficial for obtaining higher stannous selenide crystals.
In addition to stannous chloride used in this example, other chlorides such as cadmium chloride, magnesium chloride, ruthenium chloride, niobium chloride, tantalum chloride, calcium chloride, zinc chloride, palladium chloride, rhodium chloride, tin chloride, indium chloride, copper chloride, and barium chloride can achieve the same effect. As the solvent for the chloride, a conventional organic solvent such as methanol, ethanol, isopropanol, N-butanol, N-dimethylformamide, dimethyl sulfoxide, ethyl acetate, propyl acetate, acetone, glacial acetic acid, tetrahydrofuran and the like can be used.
The foregoing is a more detailed description of the present application in connection with specific embodiments thereof, and it is not intended that the present application be limited to the specific embodiments thereof. It will be apparent to those skilled in the art from this disclosure that many more simple derivations or substitutions can be made without departing from the spirit of the disclosure.

Claims (10)

1. A preparation method of a stannous selenide p-type semiconductor film is characterized by comprising the following steps: comprises adopting magnetron sputtering to deposit a stannous selenide film layer on a substrate; carrying out chloride solution treatment on the substrate on which the stannous selenide film layer is deposited to obtain the stannous selenide film layer with the surface covered with chloride; then, heating the film for 10 to 60 minutes at the temperature of 600 ℃ in vacuum or inert atmosphere or weak reducing atmosphere, and cooling the film to room temperature to obtain the stannous selenide p-type semiconductor film;
the chloride is at least one of stannous chloride, cadmium chloride, magnesium chloride, ruthenium chloride, niobium chloride, tantalum chloride, calcium chloride, zinc chloride, palladium chloride, rhodium chloride, stannic chloride, indium chloride, copper chloride and barium chloride;
the chloride solution treatment comprises the steps of soaking the substrate deposited with the stannous selenide film layer into a chloride solution; or, coating the chloride solution on the surface of the stannous selenide film layer.
2. The method of claim 1, wherein: in the chloride solution treatment, before the substrate deposited with the stannous selenide film layer is soaked into the chloride solution, the UV irradiation treatment is carried out on the substrate deposited with the stannous selenide film layer; preferably, the soaking condition is soaking for 10-20 minutes at 50-60 ℃.
3. The method of claim 1, wherein: in the chloride solution treatment, after the chloride solution is coated on the surface of the stannous selenide film layer, the method also comprises the steps of heating to remove the solvent;
preferably, the coating mode is smearing or spraying.
4. The method of claim 1, wherein: the magnetron sputtering conditions are that the pressure of the sputtering cavity is 0.1-10 Pa, the atmosphere of the sputtering cavity is argon, nitrogen or argon-hydrogen mixed gas, and the substrate temperature is10-500 ℃ and the sputtering power is 0.01-10W/cm2The deposition rate is 0.1-500 nm/min, and the sputtering time is 0.01-5 hours.
5. The method of claim 1, wherein: the solvent of the chloride solution is at least one of methanol, ethanol, isopropanol, N-butanol, ethylene glycol, N-dimethylformamide, dimethyl sulfoxide, ethyl acetate, propyl acetate, acetone, glacial acetic acid and tetrahydrofuran.
6. The production method according to any one of claims 1 to 5, characterized in that: the method also comprises the steps of preparing a silicon dioxide layer on the substrate in advance before magnetron sputtering the stannous selenide film layer; and then, carrying out magnetron sputtering on the stannous selenide film layer on the surface of the silicon dioxide layer.
7. The production method according to any one of claims 1 to 5, characterized in that: the substrate is at least one of glass, conductive glass, a flexible substrate, a quartz plate and sapphire;
preferably, the weak reducing atmosphere is H2And Ar in a mixed gas of H and Ar2Accounting for 1 to 20 percent of the volume of the mixed gas.
8. The stannous selenide p-type semiconductor film prepared by the preparation method according to any one of claims 1-7.
9. The stannous selenide p-type semiconductor thin film of claim 8, wherein: the thickness of the stannous selenide film layer is 10-1000 nm.
10. Use of a stannous selenide p-type semiconductor thin film according to claim 8 or 9 in a thin film solar cell, a detector, a thin film transistor or a display.
CN202210254539.4A 2022-03-15 2022-03-15 Stannous selenide p-type semiconductor film and preparation method and application thereof Pending CN114645257A (en)

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Publication number Priority date Publication date Assignee Title
US5393675A (en) * 1993-05-10 1995-02-28 The University Of Toledo Process for RF sputtering of cadmium telluride photovoltaic cell
US20040248340A1 (en) * 2001-10-05 2004-12-09 Nicola Romeo Process for large-scale production of cdte/cds thin film solar cells
CN1794488A (en) * 2005-09-15 2006-06-28 复旦大学 Film lithium ion battery using stannous selenide film as anode material and its preparation method
US20130130433A1 (en) * 2011-11-18 2013-05-23 First Solar, Inc. Method and apparatus providing single step vapor chloride treatment and photovoltaic modules
CN107492584A (en) * 2017-09-07 2017-12-19 北京大学深圳研究生院 A kind of cadmium telluride preparation method of solar battery and cadmium telluride solar cell
CN109534305A (en) * 2019-01-23 2019-03-29 陕西科技大学 A kind of method that solwution method prepares SnSe
CN110257872A (en) * 2019-07-23 2019-09-20 北京化工大学 A kind of Ag doping SnSe semiconductive thin film and its electrochemical preparation method
CN110257873A (en) * 2019-07-23 2019-09-20 北京化工大学 A kind of Cu doping SnSe semiconductive thin film and its electrochemical preparation method

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5393675A (en) * 1993-05-10 1995-02-28 The University Of Toledo Process for RF sputtering of cadmium telluride photovoltaic cell
US20040248340A1 (en) * 2001-10-05 2004-12-09 Nicola Romeo Process for large-scale production of cdte/cds thin film solar cells
CN1794488A (en) * 2005-09-15 2006-06-28 复旦大学 Film lithium ion battery using stannous selenide film as anode material and its preparation method
US20130130433A1 (en) * 2011-11-18 2013-05-23 First Solar, Inc. Method and apparatus providing single step vapor chloride treatment and photovoltaic modules
CN107492584A (en) * 2017-09-07 2017-12-19 北京大学深圳研究生院 A kind of cadmium telluride preparation method of solar battery and cadmium telluride solar cell
CN109534305A (en) * 2019-01-23 2019-03-29 陕西科技大学 A kind of method that solwution method prepares SnSe
CN110257872A (en) * 2019-07-23 2019-09-20 北京化工大学 A kind of Ag doping SnSe semiconductive thin film and its electrochemical preparation method
CN110257873A (en) * 2019-07-23 2019-09-20 北京化工大学 A kind of Cu doping SnSe semiconductive thin film and its electrochemical preparation method

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