CN112201709A - Antimony selenide thin film solar cell and preparation method and application thereof - Google Patents
Antimony selenide thin film solar cell and preparation method and application thereof Download PDFInfo
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- CN112201709A CN112201709A CN202011021159.3A CN202011021159A CN112201709A CN 112201709 A CN112201709 A CN 112201709A CN 202011021159 A CN202011021159 A CN 202011021159A CN 112201709 A CN112201709 A CN 112201709A
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- OQRNKLRIQBVZHK-UHFFFAOYSA-N selanylideneantimony Chemical compound [Sb]=[Se] OQRNKLRIQBVZHK-UHFFFAOYSA-N 0.000 title claims abstract description 56
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- 238000002360 preparation method Methods 0.000 title claims abstract description 16
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- 239000007789 gas Substances 0.000 claims description 10
- 238000002207 thermal evaporation Methods 0.000 claims description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000005137 deposition process Methods 0.000 claims description 5
- YKYOUMDCQGMQQO-UHFFFAOYSA-L Cadmium chloride Inorganic materials Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 4
- 229910052737 gold Inorganic materials 0.000 claims description 4
- 239000010931 gold Substances 0.000 claims description 4
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 4
- 238000009825 accumulation Methods 0.000 claims description 3
- 229910052787 antimony Inorganic materials 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
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- 230000000694 effects Effects 0.000 abstract description 14
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- 230000007547 defect Effects 0.000 abstract description 7
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 29
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 14
- 229940091258 selenium supplement Drugs 0.000 description 14
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- 229910052757 nitrogen Inorganic materials 0.000 description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 238000004544 sputter deposition Methods 0.000 description 6
- 230000001276 controlling effect Effects 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
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- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 description 2
- 239000005695 Ammonium acetate Substances 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 239000005083 Zinc sulfide Substances 0.000 description 2
- KTSFMFGEAAANTF-UHFFFAOYSA-N [Cu].[Se].[Se].[In] Chemical compound [Cu].[Se].[Se].[In] KTSFMFGEAAANTF-UHFFFAOYSA-N 0.000 description 2
- VVTSZOCINPYFDP-UHFFFAOYSA-N [O].[Ar] Chemical compound [O].[Ar] VVTSZOCINPYFDP-UHFFFAOYSA-N 0.000 description 2
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- 238000000137 annealing Methods 0.000 description 2
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 description 2
- FHKUNGMXAOFZLF-UHFFFAOYSA-L cadmium(2+) methanol dichloride Chemical compound CO.[Cl-].[Cd+2].[Cl-] FHKUNGMXAOFZLF-UHFFFAOYSA-L 0.000 description 2
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- 239000004408 titanium dioxide Substances 0.000 description 2
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- 230000009286 beneficial effect Effects 0.000 description 1
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- 229910052738 indium Inorganic materials 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
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- 238000005092 sublimation method Methods 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/0272—Selenium or tellurium
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/032—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
- H01L31/0322—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312 comprising only AIBIIICVI chalcopyrite compounds, e.g. Cu In Se2, Cu Ga Se2, Cu In Ga Se2
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- H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
- H01L31/042—PV modules or arrays of single PV cells
- H01L31/0445—PV modules or arrays of single PV cells including thin film solar cells, e.g. single thin film a-Si, CIS or CdTe solar cells
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- H01L31/1876—Particular processes or apparatus for batch treatment of the devices
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E10/541—CuInSe2 material PV cells
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Abstract
The invention discloses an antimony selenide thin film solar cell and a preparation method and application thereof. The antimony selenide thin film solar cell provided by the invention has the following structure from bottom to top in sequence: the device comprises a transparent conductive glass substrate, a high-resistance layer, an n-type electron transmission layer, a p-type absorption layer and a back electrode; wherein the p-type absorption layer is an antimony selenide film, and the antimony selenide film is formed by Sb2Se3The source is obtained by deposition in the Se vapor atmosphere of 200-300 ℃. According to the invention, by introducing high-temperature high-activity Se steam, the regulation and control of chemical environment in the growth process are realized, the selenium vacancy and defect density in the film are reduced, the electrical property of the film is improved, and further the performance of the antimony selenide film solar cell device is improved.
Description
Technical Field
The invention belongs to the field of photovoltaic new energy materials and devices, relates to an antimony selenide thin film solar cell and a preparation method and application thereof, and particularly relates to a method for preparing an antimony selenide thin film under a high-activity selenium atmosphere, regulating and controlling chemical components and defects of the antimony selenide thin film, and further improving the performance of an antimony selenide thin film solar cell device.
Background
Energy is the basis and the power of modern society development, and fossil energy still is the main energy source in the present world, and along with the overuse of fossil energy, the environmental problem that human faces is also showing day by day. Therefore, the exploration and development of new and efficient clean energy is the key to solving the energy and environmental problems. Among the many clean energy sources, solar energy attracts the attention of many researchers because it has a huge total amount of storage and a simple collection method, in which a solar cell is a device that converts light into electric energy. Among the numerous solar cells, the thin film solar cell has the advantages of high conversion efficiency, flexibility, light weight, small material consumption, strong environmental adaptability and the like, and thus, the thin film solar cell gradually becomes a very important member of a solar cell family, for example, a Copper Indium Gallium Selenide (CIGS) and cadmium telluride (CdTe) thin film solar cell is widely researched. However, the toxicity of Cd and the high price of In and Ga cannot meet the increasingly strict environmental protection requirement and the high-speed growing energy demand In the future.
For this purpose, antimony selenide (Sb) which is a simple binary compound consisting of non-toxic, earth-abundant elements2Se3) Is widely used for the research of thin film solar cells. Sb2Se3Has the characteristics of proper band gap, large light absorption coefficient, simple phase, non-toxic raw materials, low crystal growth temperature, theoretical conversion efficiency of 30 percent and the like. However, during the conventional high temperature deposition of antimony selenide films, the higher substrate temperature tends to cause Sb to be deposited2Se3The film is decomposed into Sb, Se and SbSe for the second time, and the Se has higher vapor pressure, so that Sb is caused2Se3Se deficiency of the film from stoichiometry, leading to Se vacancy related defects; direct influence of both Se-rich and Se-poor environments on Sb2Se3Electrical properties of the film, Sb2Se3P-type Sb required for solar cell2Se3Thin films need to be realized in a Se-rich environment.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention mainly aims to provide an antimony selenide thin-film solar cell.
The invention also aims to provide a preparation method of the antimony selenide thin-film solar cell.
The invention provides a method for realizing Sb by introducing a high-activity Se atmosphere2Se3The effective selenium supplement process in the film deposition process regulates and controls Sb2Se3The chemical components of the film reduce the selenium vacancy and the defect density in the film, improve the electrical property of the film and further improve the performance of the antimony selenide film solar cell device.
The invention further aims to provide application of the antimony selenide thin film solar cell.
The purpose of the invention is realized by the following technical scheme:
the utility model provides an antimony selenide thin film solar cell, its structure is from bottom to top in proper order: the device comprises a transparent conductive glass substrate, a high-resistance layer, an n-type electron transmission layer, a p-type absorption layer and a back electrode;
wherein the p-type absorption layer is an antimony selenide film, and the antimony selenide film is formed by Sb2Se3The source is obtained by deposition in the Se vapor atmosphere of 200-300 ℃.
Preferably, in the deposition process, the Se vapor gas flow is 1-20 sccm.
Preferably, the thickness of the antimony selenide film is 300-1000 nm; the temperature of the substrate in the deposition process is 200-370 ℃.
Preferably, the preparation method of the antimony selenide film is at least one of a thermal evaporation method, a magnetron sputtering method, a chemical vapor deposition method, a near space sublimation method, rapid thermal evaporation and a carrier gas transportation method.
Preferably, the Se vapor (selenium supplement process) required by the preparation process of the antimony selenide film is realized by an independent accessory device connected with the deposition device, the independent accessory device comprises a source container pipeline system, a heating control system and a flow control system, wherein Se particles are contained in a source container, a pipeline is connected with the source container to a substrate surrounding the deposition device, and a pipeline surrounding the substrate part is provided with holes densely along the inner side so as to ensure that a uniform Se-rich atmosphere environment is formed around the substrate; the heating control system comprises a source container heating system and a pipeline heating system, wherein the source container heating system is used for heating the Se source to form Se vapor, and the pipeline heating system is used for maintaining and adjusting the temperature of the Se vapor, controlling the activity of Se and avoiding the accumulation of Se on the wall of the low-temperature pipe; the flow control system controls the gas flow through an angle valve manual control or a gas flow meter.
More preferably, the source container pipeline is made of quartz or stainless steel; the source container heating system and the pipeline heating system heat through resistance wires surrounding the source container and the pipeline, and realize temperature control through controlling the current.
Preferably, the transparent conductive glass substrate is a transparent conductive oxide layer, more preferably FTO (SnO)2F) and ITO (SnO)2In); the thickness of the transparent conductive glass substrate is 200-400 nm.
Preferably, the high-resistance layer is a high-resistance transparent oxide layer, and is more preferably SnO2(tin dioxide); the thickness of the high-resistance layer is 10-50 nm.
Preferably, the n-type electron transport layer is an n-type semiconductor thin film, and more preferably CdS (cadmium sulfide), CdS: O (oxygen-doped cadmium sulfide), TiO (titanium dioxide)2(titanium dioxide) SnO2At least one of (tin dioxide), ZnO (zinc oxide) and ZnS (zinc sulfide), most preferably CdS; the thickness of the n-type electron transmission layer is 40-100 nm.
Preferably, the back electrode is a metal electrode with high work function, and more preferably at least one of gold and nickel; the thickness of the back electrode is 50-500 nm.
The preparation method of the antimony selenide thin film solar cell comprises the following steps:
(1) preparing a high-resistance layer on a transparent conductive glass substrate to obtain the transparent conductive glass substrate/the high-resistance layer;
(2) preparing an n-type electron transmission layer on the high-resistance layer to obtain a transparent conductive glass substrate/the high-resistance layer/the n-type electron transmission layer;
(3) in a Se vapor atmosphere of 200-300 ℃, Sb is added2Se3Preparation of p-type Sb by depositing source on n-type electron transport layer2Se3Absorbing layer to obtain transparent conductive glass substrate/high-resistance layer/n-type electron transport layer/p-type Sb2Se3An absorbing layer;
(4) finally in p-type Sb2Se3And preparing a back electrode on the absorption layer to obtain the antimony selenide thin film solar cell.
Preferably, the temperature of the transparent conductive glass substrate in the step (1) is 100-300 ℃.
Preferably, the electron transport layer in the step (2) adopts a chemical water bath method and CdCl2Performing heat treatment for preparation, wherein the temperature of the heat treatment is 370-430 ℃, and the time is 10 min; the temperature of the chemical water bath method is 70-90 ℃.
Preferably, the p-type Sb in the step (3)2Se3The deposition temperature of the absorption layer is 200-370 ℃.
The application of the antimony selenide thin film solar cell is provided.
Compared with the prior art, the invention has the following advantages and beneficial effects:
the traditional process is difficult to realize the effective Se supplement in the growth process and realize the Sb in the Se-rich environment2Se3And (5) growing the film. According to the invention, by introducing high-temperature high-activity Se steam, effective regulation and control of chemical environment in the growth process are realized, selenium vacancy and defect density in the film are reduced, electrical properties of the film are improved, and further, performance of the antimony selenide film solar cell device is improved.
Drawings
Fig. 1 is a schematic device structure diagram of an antimony selenide solar cell in which an antimony selenide thin film is prepared as a p-type absorption layer in a high-activity selenium atmosphere according to an embodiment of the invention.
Fig. 2 is a J-V curve of antimony selenide solar cells in example 1 of the invention and comparative example 1.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto.
Those who do not specify specific conditions in the examples of the present invention follow conventional conditions or conditions recommended by the manufacturer. The raw materials, reagents and the like which are not indicated for manufacturers are all conventional products which can be obtained by commercial purchase.
The selenium supplementing process of the antimony selenide absorption layer provided by the embodiment of the invention is realized by an independent accessory device connected with a deposition device, and the accessory device has the following characteristics: (1) the equipment accessories comprise a source container pipeline system, a heating control system and a flow control system; (2) the source container pipeline is made of quartz or stainless steel, Se particles are contained in the source container, the pipeline is connected with the source container to a substrate surrounding the deposition equipment, and holes are densely formed along the inner side of the pipeline surrounding the substrate part, so that a uniform Se-rich environment is ensured to be formed around the substrate; (3) the heating control system comprises a source container heating system and a pipeline heating system respectively, heating is carried out through resistance wires surrounding the source container and the pipeline, and temperature control is realized by controlling the current, wherein the source container heating system is used for heating the Se source to form Se vapor, and the pipeline heating system is used for maintaining and adjusting the temperature of the Se vapor, controlling the activity of Se and avoiding accumulation on the wall of the low-temperature pipe; (4) the flow control system controls the gas flow manually through an angle valve or through a gas flowmeter; (5) a highly reactive Se atmosphere is achieved by increasing the Se vapor temperature.
Example 1
The embodiment provides a method for preparing an antimony selenide thin film solar cell in a high-activity selenium atmosphere, which comprises the following steps:
1) cleaning the FTO conductive glass;
placing FTO conductive glass (the thickness of the FTO conductive layer is about 300nm) in a beaker, ultrasonically cleaning the FTO conductive glass by using a cleaning solvent, deionized water, acetone and alcohol which are prepared according to the proportion of 3mL of detergent to 3L of deionized water, and then drying the FTO conductive glass by using nitrogen.
2) Deposition of SnO2BufferLayer (b):
SnO preparation on FTO conductive glass substrate by radio frequency magnetron sputtering method2Film, the target material is SnO with purity of 99.99 percent2A target. Firstly, putting a clean FTO conductive glass substrate into a cavity, vacuumizing the cavity until the vacuum degree is lower than 5 multiplied by 10-4When Pa is needed, closing a part of gate valve, adjusting the argon-oxygen ratio to 1:20 to ensure that the mixed gas pressure reaches 0.4Pa, the power of the radio frequency power supply is 90W, and the temperature of the substrate is 200 ℃. The pre-sputtering time is 10min, and impurities on the surface of the target material are removed. The sputtering time was 6min and the sputtering thickness was 35 nm.
3) Depositing an n-type CdS electron transport layer:
and preparing the CdS electron transport layer by adopting a chemical water bath method. In the first step, containers required in the reaction process are cleaned, alcohol and deionized water are sequentially subjected to ultrasonic cleaning for 10min, and then the containers are placed into a baking oven to be dried. And preparing a reaction solution, namely adding 940mL of distilled water, 20mL of cadmium acetate, 20mL of ammonium acetate and 20mL of thiourea into a beaker in sequence, and then dripping complexing agent ammonia water. The SnO obtained in the step 2) is contained2The substrate is put into the prepared solution, then the reaction beaker is put into a water bath kettle which is constant at 85 ℃ for heating and stirring, the color of the solution needs to be observed in the reaction process, the solution reaction is stopped when the solution turns yellow and becomes turbid gradually, finally the substrate is taken out and washed by a large amount of deionized water, and finally the substrate is dried by nitrogen. With a target control thickness of 65 nm.
4) CdCl for CdS thin film2And (3) heat treatment:
the prepared FTO/SnO2Putting the CdS substrate into a pulling machine filled with a cadmium chloride methanol saturated solution for pulling, and ensuring the pulling to be carried out in nitrogen. In the process of pulling, the pulling speed is 1mm/s, the methanol solvent is volatilized, and CdCl2Separating out to cover a layer of CdCl on the surface of CdS2And then putting the CdS core tube into a tube furnace to perform annealing treatment at 400 ℃ in the air for 10min, finally taking out the CdS core tube, cleaning the CdS core tube with deionized water, and drying the CdS core tube with nitrogen.
5) Deposition of Sb2Se3An absorption layer:
adopt aSb deposition by near-space sublimation integrated equipment with additional independent accessories2Se3And the pipeline in the source container pipeline system of the thin film extends to the CdS substrate surrounding the close space sublimation equipment. CdS substrate is fixed on the upper graphite substrate, and Sb is fixed on the lower graphite substrate2Se3A source, introduced into the chamber, evacuated to a vacuum of 1X 10-1Pa or less, provided with Sb2Se3The source temperature was 510 deg.C, the CdS substrate temperature was 270 deg.C, the source vessel heating current was 50A, and the tube heating temperature was set at 200 deg.C (Se vapor temperature). The absorption layer deposition rate was about 200 nm/min. In the deposition of Sb2Se3Se vapor is generated through a source container in the film process, the Se vapor flow is 4sccm, high activity is kept through a high-temperature pipeline, finally the Se vapor is led to a CdS substrate to continuously supplement selenium, the experiment is finished after deposition is carried out for 2.5min, and the thickness of the film is 500 nm.
6) Evaporating an electrode:
in Sb by adopting vacuum thermal evaporation equipment2Se3And depositing a gold electrode on the absorption layer, wherein the thickness of the electrode is 100 nm.
Example 2
The embodiment provides a method for preparing an antimony selenide thin film solar cell in a high-activity selenium atmosphere, which comprises the following steps:
1) cleaning the FTO conductive glass;
placing FTO conductive glass (the thickness of the FTO conductive layer is about 300nm) in a beaker, ultrasonically cleaning the FTO conductive glass by using a cleaning solvent, deionized water, acetone and alcohol which are prepared according to the proportion of 3mL of detergent to 3L of deionized water, and then drying the FTO conductive glass by using nitrogen.
2) Deposition of SnO2Buffer layer:
SnO preparation on FTO conductive glass substrate by radio frequency magnetron sputtering method2Film, the target material is SnO with purity of 99.99 percent2A target. Firstly, putting a clean FTO conductive glass substrate into a cavity, vacuumizing the cavity until the vacuum degree is lower than 5 multiplied by 10-4When Pa is needed, closing a part of gate valve, adjusting the argon-oxygen ratio to 1:20 to ensure that the mixed gas pressure reaches 0.4Pa, the power of the radio frequency power supply is 90W, and the temperature of the substrate is 200 ℃. The pre-sputtering time is 10min, and the target material table is removedImpurities of the face. The sputtering time was 6min and the sputtering thickness was 35 nm.
3) Depositing an n-type CdS electron transport layer:
and preparing the CdS electron transport layer by adopting a chemical water bath method. In the first step, containers required in the reaction process are cleaned, alcohol and deionized water are sequentially subjected to ultrasonic cleaning for 10min, and then the containers are placed into a baking oven to be dried. And preparing a reaction solution, namely adding 940mL of distilled water, 20mL of cadmium acetate, 20mL of ammonium acetate and 20mL of thiourea into a beaker in sequence, and then dripping complexing agent ammonia water. The SnO obtained in the step 2) is contained2The substrate is put into the prepared solution, then the reaction beaker is put into a water bath kettle which is constant at 85 ℃ for heating and stirring, the color of the solution needs to be observed in the reaction process, the solution reaction is stopped when the solution turns yellow and becomes turbid gradually, finally the substrate is taken out and washed by a large amount of deionized water, and finally the substrate is dried by nitrogen. With a target control thickness of 65 nm.
4) CdCl for CdS thin film2And (3) heat treatment:
the prepared FTO/SnO2Putting the CdS substrate into a pulling machine filled with a cadmium chloride methanol saturated solution for pulling, and ensuring the pulling to be carried out in nitrogen. In the process of pulling, the pulling speed is 1mm/s, the methanol solvent is volatilized, and CdCl2Separating out to cover a layer of CdCl on the surface of CdS2And then putting the CdS core tube into a tube furnace to perform annealing treatment at 400 ℃ in the air for 10min, finally taking out the CdS core tube, cleaning the CdS core tube with deionized water, and drying the CdS core tube with nitrogen.
5) Deposition of Sb2Se3An absorption layer:
sb deposition by thermal evaporation integrated equipment with additional independent accessory2Se3And the thin film extends to the CdS substrate of the surrounding thermal evaporation device through a pipeline in the source container pipeline system. Fixing CdS substrate on sample table, Sb2Se3Placing the source in an evaporation boat, and vacuumizing to 5 × 10-3Pa or less, adjusting Sb2Se3The current of the evaporation boat is 60A, the temperature of the CdS substrate is 200 ℃, and the deposition rate is 50 nm/min. The Se source container heating current is set to 50A, and the pipe heating temperature is set to 200 ℃ (Se vapor)Temperature). In the deposition of Sb2Se3Se vapor is generated through a source container in the film process, the Se vapor flow is 2sccm, high activity is kept through a high-temperature pipeline, finally the Se vapor is led to a CdS substrate to continuously supplement selenium, the experiment is finished after deposition is carried out for 10min, and the thickness of the film is 500 nm.
6) Evaporating an electrode:
using thermal evaporation equipment in Sb2Se3And depositing a gold electrode on the absorption layer, wherein the thickness of the electrode is 100 nm.
Example 3
The conditions of ' the Se vapor temperature is 200 ℃ in the step (5) of the example 1 are changed into ' the Se vapor temperature is 250 ℃ in the step (5) ' and other conditions are the same as those of the example 1, so that the antimony selenide thin film solar cell is finally prepared.
Comparative example 1
The conditions "Se vapor flow rate of 4 sccm" in step (5) of example 1 were changed to "Se vapor flow rate of 0 sccm", that is, no Se vapor was introduced, and the other conditions were the same as in example 1, to finally obtain an antimony selenide thin film solar cell.
Two kinds of antimony selenide thin film solar cells of example 1 (containing Se atmosphere) and comparative example 1 (not containing Se atmosphere) at AM (air mass)1.5, 100mW/cm2The J-V performance curve of the cell was tested with a solar simulator under illumination, as shown in fig. 2. The short-circuit current density of the antimony selenide thin-film solar cell prepared in the high-activity selenium atmosphere is 26.5cm-2The open circuit voltage was 400mV, the fill factor was 58.9%, and the photoelectric conversion efficiency was 6.24%. The short-circuit current density of the antimony selenide thin film solar cell obtained without introducing high-activity Se atmosphere is 25.3mA cm-2The open circuit voltage was 372mV, the fill factor was 55.1%, and the photoelectric conversion efficiency was 5.19%.
The result shows that the antimony selenide film is prepared in the high-activity selenium atmosphere, the chemical components of the film are regulated, the selenium vacancy and defect density in the film are reduced, the electrical property of the film is improved, and the performance of the antimony selenide solar cell device is improved.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. The utility model provides an antimony selenide thin film solar cell which characterized in that, its structure from bottom to top does in proper order: the device comprises a transparent conductive glass substrate, a high-resistance layer, an n-type electron transmission layer, a p-type absorption layer and a back electrode;
wherein the p-type absorption layer is an antimony selenide film, and the antimony selenide film is formed by Sb2Se3The source is obtained by deposition in the Se vapor atmosphere of 200-300 ℃.
2. The antimony selenide thin film solar cell according to claim 1, wherein the thickness of the antimony selenide thin film is 300-1000 nm; the temperature of the substrate in the deposition process is 200-370 ℃.
3. The antimony selenide thin film solar cell according to claim 1, wherein the Se vapor gas flow rate is 1-20 sccm during the deposition process.
4. The antimony selenide thin film solar cell according to claim 1, wherein Se vapor required by the antimony selenide thin film in the preparation process is realized by a separate accessory device connected with a deposition device, the separate accessory device comprises a source container pipeline system, a heating control system and a flow control system, wherein Se particles are contained in a source container, a pipeline is connected with the source container to a substrate surrounding the deposition device, and a pipeline surrounding the substrate part is densely perforated along the inner side so as to ensure that a uniform Se-rich atmosphere environment is formed around the substrate; the heating control system comprises a source container heating system and a pipeline heating system, wherein the source container heating system is used for heating the Se source to form Se vapor, and the pipeline heating system is used for maintaining and adjusting the temperature of the Se vapor and avoiding the accumulation of Se on the low-temperature pipe wall; the flow control system controls the gas flow through an angle valve manual control or a gas flow meter.
5. The antimony selenide thin film solar cell according to claim 1, wherein the transparent conductive glass substrate is at least one of FTO and ITO; the thickness of the transparent conductive glass substrate is 200-400 nm;
the high-resistance layer is SnO2(ii) a The thickness of the high-resistance layer is 10-50 nm;
the n-type electron transport layer is CdS and CdS O, TiO2、SnO2At least one of ZnO and ZnS, wherein the thickness of the n-type electron transport layer is 40-100 nm;
the back electrode is at least one of gold and nickel; the thickness of the back electrode is 50-500 nm.
6. The antimony selenide thin film solar cell according to claim 1, wherein the antimony selenide thin film is prepared by at least one of a thermal evaporation method, a magnetron sputtering method, a chemical vapor deposition method, a close-space sublimation method, a rapid thermal evaporation method and a carrier gas transport method.
7. The antimony selenide thin film solar cell according to claim 4, wherein the source container pipeline is made of quartz or stainless steel; the source container heating system and the pipeline heating system heat through resistance wires surrounding the source container and the pipeline, and realize temperature control through controlling the current.
8. The preparation method of the antimony selenide thin film solar cell as claimed in any one of claims 1 to 7, which is characterized by comprising the following steps:
(1) preparing a high-resistance layer on a transparent conductive glass substrate to obtain the transparent conductive glass substrate/the high-resistance layer;
(2) preparing an n-type electron transmission layer on the high-resistance layer to obtain a transparent conductive glass substrate/the high-resistance layer/the n-type electron transmission layer;
(3) in a Se vapor atmosphere of 200-300 ℃, Sb is added2Se3Preparation of p-type Sb by depositing source on n-type electron transport layer2Se3An absorption layer to obtainTransparent conductive glass substrate/high-resistance layer/n-type electron transport layer/p-type Sb2Se3An absorbing layer;
(4) finally in p-type Sb2Se3And preparing a back electrode on the absorption layer to obtain the antimony selenide thin film solar cell.
9. The antimony selenide thin film solar cell according to claim 8, wherein the temperature of the transparent conductive glass substrate in the step (1) is 100-300 ℃; the electron transport layer in the step (2) adopts a chemical water bath method and CdCl2Performing heat treatment for preparation, wherein the temperature of the heat treatment is 370-430 ℃, and the time is 10 min; the temperature of the chemical water bath method is 70-90 ℃; p-type Sb in step (3)2Se3The temperature of the absorption layer is 200-370 ℃.
10. Use of an antimony selenide thin film solar cell according to any one of claims 1 to 7.
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