CN108831939A - Quaternary co-evaporation AIGS film and preparation method and application thereof - Google Patents
Quaternary co-evaporation AIGS film and preparation method and application thereof Download PDFInfo
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- CN108831939A CN108831939A CN201810615945.2A CN201810615945A CN108831939A CN 108831939 A CN108831939 A CN 108831939A CN 201810615945 A CN201810615945 A CN 201810615945A CN 108831939 A CN108831939 A CN 108831939A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 238000010549 co-Evaporation Methods 0.000 title abstract 4
- 238000001704 evaporation Methods 0.000 claims abstract description 123
- 230000008020 evaporation Effects 0.000 claims abstract description 122
- 239000010408 film Substances 0.000 claims abstract description 101
- 239000000758 substrate Substances 0.000 claims abstract description 89
- 239000011521 glass Substances 0.000 claims abstract description 49
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 45
- 229910052738 indium Inorganic materials 0.000 claims abstract description 45
- 229910052709 silver Inorganic materials 0.000 claims abstract description 45
- 238000000034 method Methods 0.000 claims abstract description 40
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 34
- 229910052751 metal Inorganic materials 0.000 claims abstract description 29
- 239000002184 metal Substances 0.000 claims abstract description 29
- 239000000463 material Substances 0.000 claims abstract description 22
- 239000010409 thin film Substances 0.000 claims abstract description 17
- 238000010521 absorption reaction Methods 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims description 40
- 238000001816 cooling Methods 0.000 claims description 31
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 21
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 claims description 16
- 238000000151 deposition Methods 0.000 claims description 12
- 230000008021 deposition Effects 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- 230000015572 biosynthetic process Effects 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- 238000001451 molecular beam epitaxy Methods 0.000 claims description 10
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- 238000005240 physical vapour deposition Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000005361 soda-lime glass Substances 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 6
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052725 zinc Inorganic materials 0.000 claims description 4
- 239000011701 zinc Substances 0.000 claims description 4
- 239000011787 zinc oxide Substances 0.000 claims description 4
- 230000005611 electricity Effects 0.000 claims description 3
- 238000010025 steaming Methods 0.000 claims description 2
- 238000007740 vapor deposition Methods 0.000 claims 1
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 15
- 238000001755 magnetron sputter deposition Methods 0.000 description 9
- KTSFMFGEAAANTF-UHFFFAOYSA-N [Cu].[Se].[Se].[In] Chemical compound [Cu].[Se].[Se].[In] KTSFMFGEAAANTF-UHFFFAOYSA-N 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000005229 chemical vapour deposition Methods 0.000 description 5
- 235000019082 Osmanthus Nutrition 0.000 description 4
- 241000333181 Osmanthus Species 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 230000000994 depressogenic effect Effects 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 235000011941 Tilia x europaea Nutrition 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000004571 lime Substances 0.000 description 2
- 230000005622 photoelectricity Effects 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 229910004613 CdTe Inorganic materials 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 239000003788 bath preparation Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003519 biomedical and dental material Substances 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
Classifications
-
- 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
- H01L31/036—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 their crystalline structure or particular orientation of the crystalline planes
- H01L31/0392—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 their crystalline structure or particular orientation of the crystalline planes including thin films deposited on metallic or insulating substrates ; characterised by specific substrate materials or substrate features or by the presence of intermediate layers, e.g. barrier layers, on the substrate
- H01L31/03923—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 their crystalline structure or particular orientation of the crystalline planes including thin films deposited on metallic or insulating substrates ; characterised by specific substrate materials or substrate features or by the presence of intermediate layers, e.g. barrier layers, on the substrate including AIBIIICVI compound materials, e.g. CIS, CIGS
-
- 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
- H01L31/04—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
-
- 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
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
-
- 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
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/541—CuInSe2 material PV cells
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses a quaternary co-evaporation AIGS thin film, which comprises a glass substrate, a metal Mo back electrode deposited on the glass substrate and an absorption layer co-evaporated on the Mo back electrode; the absorption layer is an AIGS thin film layer formed by one-step quaternary co-evaporation of Ag, In, Ga and Se. The invention also discloses a preparation method of the quaternary co-evaporation AIGS thin film and an AIGS thin film solar cell. The growth process of the film is accurately controlled by controlling the vapor pressure of the evaporation source material by adopting a one-step method, so that the efficiency and the uniformity of the film are improved.
Description
Technical field
The invention belongs to compound film and photovoltaic cell technical fields, and in particular to a kind of quaternary steam altogether AIGS film and
Preparation method and application.
Background technique
Chemical vapor deposition is using one or more of gas phase compounds or simple substance containing film element, in substrate surface
On carry out chemical reaction generate film method.It can use the reaction between gas phase, in the ingredient that does not change basis material and
Under the strength condition for not weakening basis material, some special performances of material surface are assigned.At present, by chemical vapour deposition technique
The material of preparation is not only applicable to cutter material, wear-resisting heat-resisting corrosion-resisting material, the special composite material in aerospace industry, original
The fields such as sub- pile materials and bio-medical material, and be widely used in preparation and synthesize various powder body materials, block
Material, new crystalline material, ceramic fibre and diamond thin etc..As large scale integrated circuit technology ferroelectric material, absolutely
The film preparing technology aspect of edge material, magnetic material, photoelectron material, it is even more indispensable.
Solar battery is also photovoltaic cell, is a kind of device that luminous energy can be directly translated into electric energy.According to the sun
Solar battery can be divided into first generation solar battery, i.e. shoes base semiconductor electricity by the development course and making material of energy battery
Pond, including monocrystalline osmanthus battery, polycrystalline osmanthus battery and amorphous osmanthus battery, such osmanthus based solar battery development time is long, technology compared with
It is mature；Second generation solar battery, i.e., how towering compound film solar battery, including cadmium sulfide (CdTe), copper indium selenide
(CIS), GaAs (GaAs), copper indium gallium selenide (CIGS)；Third generation solar cell is the introduction of organic matter and nanotechnology
Novel thin film solar battery, including dye-sensitized solar cells, organic polymer solar cell etc..
Since third generation solar cell is also in conceptual phase, and its cost is accordingly higher, is being also difficult to reach at present
Therefore the demand of application leads to be applied or second generation solar battery, due to CIGS material itself at present in photovoltaic cell
With the very high absorption coefficient of light, battery device photoelectric conversion efficiency is high, the performance stable service life is long, dim light is good and anti-spoke
It penetrates that performance is strong, therefore gets a good chance of becoming the solar cell material of large-scale use of new generation.Currently, the small area film sun
The peak efficiency of energy battery device has reached.But preparation process is complicated, equipment cost is high and raw material utilization rate is low, resistance
Its industrialized development is hindered.Therefore, how to prepare efficient solar battery and reduce its overall cost, becoming research should
Two Main ways in field.Currently, the laboratory transfer efficiency of CIGS has reached 21.3%, slightly below polysilicon and monocrystalline
Silicon photrouics.The preparation of CIGS at present mostly use it is polynary steam method altogether, mainly by thermal evaporation by required elements vaporization, and
So that it is deposited in the form of atom or molecule.The solar battery efficiency of the method preparation is very high, but existing method
Cumbersome, equipment cost is high.
Summary of the invention
For overcome the deficiencies in the prior art, the purpose of the present invention is to provide a kind of quaternarys to steam AIGS film altogether, improves
The uniformity and photoelectricity performance of film.
Further technical problems to be solved of the invention are to provide the preparation method that a kind of quaternary steams AIGS film altogether, adopt
With one-step method, the growth course of film is accurately controlled by controlling evaporation source material vapour pressure, improve efficiency with it is thin
The uniformity of film.
The present invention further also solves quaternary and steams the application of AIGS film in solar cells altogether.
To solve the above problems, the technical solution adopted in the present invention is as follows：
A kind of quaternary steams AIGS film altogether, including substrate of glass, deposition metal Mo back electrode on the glass substrate and
The absorbed layer on Mo back electrode is steamed altogether；The absorbed layer is the AIGS film that one-step method quaternary steams Ag, In, Ga, Se formation altogether
Layer.
As further embodiment, each element accounts for atomic percent and is in absorbed layer of the present invention：1:0.25:
0.75:2, absorption layer component basic structural formula is Ag (In0.25Ga0.75)Se2。
As further embodiment, the overall thickness of absorbed layer of the present invention is 1.5-2 μm；The substrate of glass is sodium
Lime glass, substrate of glass with a thickness of 1.5-2.5mm；The Mo back electrode with a thickness of 0.8-1.2 μm.
A kind of quaternary steams the preparation method of AIGS film altogether, including
The step of preparing Mo back electrode：Method deposited metal Mo on the glass substrate is penetrated with direct magnetic control Destroy, is obtained with Mo
The substrate of back electrode；
The setting steps of evaporation cavity：By the rotation sample of the above-mentioned basal molecular beam epitaxy equipment evaporation cavity with Mo back electrode
In sample platform, with Mo back electrode one downwards, heating source is equipped with above substrate, raw material evaporation source is located at the bottom of evaporation cavity
Portion, raw material evaporation source exit are equipped with the switch for controlling raw material, vacuumize with the cooling evaporation cavity of liquid nitrogen and to evaporation cavity,
Adjust the vapour pressure of raw material setting in evaporation source；
Quaternary steams the step of standby absorbed layer altogether：Substrate with Mo back electrode is heated to 520 DEG C, open Ag, In,
Ga, Se evaporation source co-evaporate Ag, In, Ga, Se on Mo back electrode, form AIGS film layer；
Cooling step：Ag, In, Ga evaporation source are closed, the cooling substrate under Se atmosphere protection, when base reservoir temperature is down to 400
DEG C when close evaporation source Se, simultaneously close off heating source, when base reservoir temperature is down to 200 DEG C, sample stage taken to sample switch room,
It obtains quaternary and steams AIGS film altogether.
As further embodiment, in the setting steps of evaporation cavity of the present invention, Ag, In, Ga, Se evaporation source Central Plains
The vapour pressure of material is respectively Ag：8.5×10-5Torr, In：4.0×10-5Torr, Ga：8×10-5Torr, Se：2.0×10- 3Torr。
As further embodiment, in the step of quaternary of the present invention steams standby absorbed layer altogether, the coevaporation time is
35-42min。
As further embodiment, in cooling step of the present invention, under Se atmosphere protection, cooling velocity 15
DEG C/minute.
A kind of AIGS thin-film solar cells, including substrate of glass, deposition metal Mo back electrode on the glass substrate, altogether
Steam on Mo back electrode absorbed layer, be arranged in and receive CdS buffer layer on layer and the on the buffer layer intrinsic zinc oxide that is arranged
Layer and boron-doping zinc oxide transparent conductive film Window layer, production has metal in the boron-doping zinc oxide transparent conductive film Window layer
Aluminum gate electrode, the absorbed layer are the AIGS film layer that one-step method quaternary steams Ag, In, Ga, Se formation altogether.
A kind of preparation method of AIGS thin-film solar cells, including
The step of preparing Mo back electrode：Method deposited metal Mo on the glass substrate is penetrated with direct magnetic control Destroy, is obtained with Mo
The substrate of back electrode；
The setting steps of evaporation cavity：By the rotation sample of the above-mentioned basal molecular beam epitaxy equipment evaporation cavity with Mo back electrode
In sample platform, with Mo back electrode one downwards, heating source is equipped with above substrate, raw material evaporation source is located at the bottom of evaporation cavity
Portion, raw material evaporation source exit are equipped with the switch for controlling raw material, vacuumize with the cooling evaporation cavity of liquid nitrogen and to evaporation cavity,
Adjust the vapour pressure of raw material setting in evaporation source；
Quaternary steams the step of standby absorbed layer altogether：Substrate with Mo back electrode is heated to 520 DEG C, open Ag, In,
Ga, Se evaporation source co-evaporate Ag, In, Ga, Se on Mo back electrode, form AIGS film layer；
Cooling step：Ag, In, Ga evaporation source are closed, the cooling substrate under Se atmosphere protection, when base reservoir temperature is down to 400
DEG C when close evaporation source Se, simultaneously close off heating source, when base reservoir temperature is down to 200 DEG C, sample stage taken to sample switch room,
It obtains quaternary and steams AIGS film altogether；
The step of making thin-film solar cells：CdS buffer layer is prepared using chemical water bath, is adopted on CdS buffer layer
Native oxide zinc layers and boron-doping zinc oxide transparent conductive film Window layer are prepared with Metalorganic chemical vapor deposition method, later
Metal aluminum gate electrode is prepared in boron-doping zinc oxide transparent conductive film Window layer using physical vapour deposition (PVD), obtains AIGS film
Solar battery.
Compared with the existing technology, beneficial effects of the present invention are as follows：
1. quaternary of the present invention steams AIGS film uniformity with higher and good photoelectricity performance altogether；
2. the preparation method whole process that quaternary of the present invention steams AIGS film altogether uses one-step method one in a vacuum
Secondary completion is accurately controlled the growth course of film by control evaporation source material vapour pressure high with one after another, accurate
The advantages that property is high.
Present invention will be further explained below with reference to the attached drawings and examples.
Detailed description of the invention
Fig. 1 is substrate of glass temperature profile of the present invention；
Fig. 2 is the cross-section diagram that quaternary of the present invention steams AIGS film altogether.
Specific embodiment
Quaternary of the present invention steams AIGS film altogether, the metal Mo back including substrate of glass, deposition on the glass substrate
Electrode and altogether absorbed layer of the steaming on Mo back electrode；The absorbed layer is that one-step method quaternary steams Ag, In, Ga, Se formation altogether
AIGS film layer.
It is 1 that as further embodiment, in absorbed layer of the present invention, each element, which accounts for atomic percent,:0.25:0.75:
2, absorption layer component basic structural formula is Ag (In0.25Ga0.75)Se2
As further embodiment, the overall thickness of absorbed layer of the present invention is 1.5-2 μm；The substrate of glass is sodium
Lime glass, substrate of glass with a thickness of 1.5-2.5mm；The Mo back electrode with a thickness of 0.8-1.2 μm.
A kind of quaternary steams the preparation method of AIGS film altogether, including
The step of preparing Mo back electrode：With direct current magnetron sputtering process deposited metal Mo on the glass substrate, obtain with Mo
The substrate of back electrode；In this step, direct current magnetron sputtering process can be effectively ensured Mo film electric conductivity and adhesive force and its
Microscopic appearance；
The setting steps of evaporation cavity：By the rotation sample of the above-mentioned basal molecular beam epitaxy equipment evaporation cavity with Mo back electrode
In sample platform, with Mo back electrode one downwards, heating source is equipped with above substrate, raw material evaporation source is located at the bottom of evaporation cavity
Portion, raw material evaporation source exit are equipped with the switch for controlling raw material, vacuumize with the cooling evaporation cavity of liquid nitrogen and to evaporation cavity,
Adjust the vapour pressure of raw material setting in evaporation source；
Quaternary steams the step of standby absorbed layer altogether：Substrate with Mo back electrode is heated to 520 DEG C, open Ag, In,
Ga, Se evaporation source co-evaporate Ag, In, Ga, Se on Mo back electrode, form AIGS film layer；
Cooling step：Ag, In, Ga evaporation source are closed, the cooling substrate under Se atmosphere protection, when base reservoir temperature is down to 400
DEG C when close evaporation source Se, simultaneously close off heating source, when base reservoir temperature is down to 200 DEG C, sample stage taken to sample switch room,
It obtains quaternary and steams AIGS film altogether.
In order to avoid pollution high-vacuum equipment will necessarily also introduce it is objectionable, cause battery device efficiency reduction.As
Further embodiment further includes carrying out to substrate of glass before the step of preparation prepares Mo back electrode in above-mentioned preparation method
The step of cleaning, present invention preferably employs calcium soda-lime glass, specific as follows to the cleaning step of calcium soda-lime glass：Calcium soda-lime glass is immersed
In the aqueous solution of NaOH, it is cleaned by ultrasonic 10 minutes；It then takes out, is rinsed with a large amount of deionized waters, while being wiped with dust-free paper, so
It is dried up afterwards with elevated pressure nitrogen air gun；It is put into high vacuum baking chamber, 300 DEG C are toasted 10 minutes.
In above-mentioned preparation method, prepare Mo back electrode the step of in, direct current magnetron sputtering process is to be with operating air pressure
0.3Pa, sputtering power are the first layer Mo film that 350W deposition thickness is 0.3-0.5 μm, then to operating air pressure 0.05Pa,
Sputtering power 500W deposited the second layer with a thickness of 0.5-0.7 μm of Mo film, and the overall thickness of the Mo back electrode is 0.8-1.2
μm。
As further embodiment, in the setting steps of evaporation cavity of the present invention, Ag, In, Ga, Se evaporation source Central Plains
The vapour pressure of material is respectively Ag：8.5×10-5Torr, In：4.0×10-5Torr, Ga：8×10-5Torr, Se：2.0×10- 3Torr。
As further embodiment, in the step of quaternary of the present invention steams standby absorbed layer altogether, the coevaporation time is
35-42min。
As further embodiment, in cooling step of the present invention, under Se atmosphere protection, cooling velocity 15
DEG C/minute.
A kind of AIGS thin-film solar cells, including substrate of glass, deposition metal Mo back electrode on the glass substrate, altogether
Steam on Mo back electrode absorbed layer, be arranged in and receive CdS buffer layer on layer and the on the buffer layer intrinsic zinc oxide that is arranged
Layer and boron-doping zinc oxide transparent conductive film Window layer, production has metal in the boron-doping zinc oxide transparent conductive film Window layer
Aluminum gate electrode, the absorbed layer are the AIGS film layer that one-step method quaternary steams Ag, In, Ga, Se formation altogether.
A kind of preparation method of AIGS thin-film solar cells, including
The step of preparing Mo back electrode：Method deposited metal Mo on the glass substrate is penetrated with direct magnetic control Destroy, is obtained with Mo
The substrate of back electrode；
The setting steps of evaporation cavity：By the rotation sample of the above-mentioned basal molecular beam epitaxy equipment evaporation cavity with Mo back electrode
In sample platform, with Mo back electrode one downwards, heating source is equipped with above substrate, raw material evaporation source is located at the bottom of evaporation cavity
Portion, raw material evaporation source exit are equipped with the switch for controlling raw material, vacuumize with the cooling evaporation cavity of liquid nitrogen and to evaporation cavity,
Adjust the vapour pressure of raw material setting in evaporation source；
Quaternary steams the step of standby absorbed layer altogether：Substrate with Mo back electrode is heated to 520 DEG C, open Ag, In,
Ga, Se evaporation source co-evaporate Ag, In, Ga, Se on Mo back electrode, form AIGS film layer；
Cooling step：Ag, In, Ga evaporation source are closed, the cooling substrate under Se atmosphere protection, when base reservoir temperature is down to 400
DEG C when close evaporation source Se, simultaneously close off heating source, when base reservoir temperature is down to 200 DEG C, sample stage taken to sample switch room,
It obtains quaternary and steams AIGS film altogether；
The step of making thin-film solar cells：CdS buffer layer is prepared using chemical water bath, is adopted on CdS buffer layer
Native oxide zinc layers and boron-doping zinc oxide transparent conductive film Window layer are prepared with Metalorganic chemical vapor deposition method, later
Metal aluminum gate electrode is prepared in boron-doping zinc oxide transparent conductive film Window layer using physical vapour deposition (PVD), obtains AIGS film
Solar battery.
In above-mentioned preparation method, using chemical water bath preparation CdS buffer layer, specific step is as follows：
1) by 7.5 × l0-2The thin urea of moI is dissolved in the deionized water of 150mL, is stirred evenly；
2) by 7.5 × l0-2The CdSO of mol4It is dissolved in the deionized water of 60mL；
3) aqueous solution of above-mentioned thiocarbamide and CdS are mixed and is poured into built-in reactor, and the ammonium hydroxide and 425mL of 45mL is added
Deionized water；
4) at the same time, external water-bath bath temperature rises to 67 DEG C and keeps the temperature；
5) quaternary is total to and is steamed on the specimen holder that AIGS film is put into down in built-in reactor, built-in reactor is put into
In external cleansing bath tub, start reaction and timing；
6) reaction takes out sample, completes the deposition of CdS to after ten minutes.
In order to reduce the series resistance of battery device, the loss of photogenerated current is reduced, the thickness of CdS buffer layer should be as far as possible
It is thin, in the present invention CdS buffer layer with a thickness of 60nm.
Fig. 1 is substrate of glass temperature profile of the present invention, which is divided into three sections, calefactive interzone, constant temperature
Section, cool down section.Substrate is heated using heating source in calefactive interzone, is heated to 550 DEG C by room temperature in 15min；Into
After entering constant temperature section, evaporation source baffle is opened, starts to prepare film；After evaporating 30min, film preparation is completed, closes Ag, In,
Ga evaporation source baffle, while entering cooling section, Se evaporation source baffle, film are closed after dropping to 250 by 550 DEG C in 15 minutes
Preparation is completed.
Fig. 2 is
Quaternary of the present invention steams the cross-section diagram of AIGS film altogether.It will be apparent from this figure that the surface of film is flat,
Without fluctuating, film thickness is uniform.Embodiment 1
A kind of quaternary steams AIGS film altogether, including substrate of glass, deposition metal Mo back electrode on the glass substrate and
The absorbed layer on Mo back electrode is steamed altogether；The absorbed layer is the AIGS film that one-step method quaternary steams Ag, In, Ga, Se formation altogether
Layer；The overall thickness of the absorbed layer is 1.5 μm；The substrate of glass be soda-lime glass, substrate of glass with a thickness of 2.5mm；
The Mo back electrode with a thickness of 0.8 μm；
The preparation method that the quaternary steams AIGS film altogether includes
The step of preparing Mo back electrode：With direct current magnetron sputtering process deposited metal Mo on the glass substrate, obtain with Mo
The substrate of back electrode；In this step, direct current magnetron sputtering process can be effectively ensured Mo film electric conductivity and adhesive force and its
Microscopic appearance；
The setting steps of evaporation cavity：By the rotation sample of the above-mentioned basal molecular beam epitaxy equipment evaporation cavity with Mo back electrode
In sample platform, with Mo back electrode one downwards, heating source is equipped with above substrate, raw material evaporation source is located at the bottom of evaporation cavity
Portion, raw material evaporation source exit are equipped with the switch for controlling raw material, cool down evaporation cavity diffusion pump for evaporation cavity with liquid nitrogen
Interior is evacuated to 10-5Pa, the steam for adjusting raw material in each evaporation source are depressed into Ag：8.5×10-5Torr, In：4.0×10- 5Torr, Ga：8×10-5Torr, Se：2.0×10-3Torr。
Quaternary steams the step of standby absorbed layer altogether：Substrate with Mo back electrode is heated to 520 DEG C, open Ag, In,
Ga, Se evaporation source co-evaporate Ag, In, Ga, Se on Mo back electrode, form AIGS film layer；
Cooling step：Ag, In, Ga evaporation source are closed, substrate is cooled down with 15 DEG C/minute of speed under Se atmosphere protection, when
Base reservoir temperature closes evaporation source Se when being down to 400 DEG C, heating source is simultaneously closed off, when base reservoir temperature is down to 200 DEG C, by sample stage
It takes to sample switch room, obtains quaternary and steam AIGS film altogether.
Embodiment 2
A kind of quaternary steams AIGS film altogether, including substrate of glass, deposition metal Mo back electrode on the glass substrate and
The absorbed layer on Mo back electrode is steamed altogether；The absorbed layer is the AIGS film that one-step method quaternary steams Ag, In, Ga, Se formation altogether
Layer；The overall thickness of the absorbed layer is 1.8 μm；The substrate of glass be soda-lime glass, substrate of glass with a thickness of 2.0；Institute
State Mo back electrode with a thickness of 1.0 μm；
The preparation method that the quaternary steams AIGS film altogether includes
The step of preparing Mo back electrode：With direct current magnetron sputtering process deposited metal Mo on the glass substrate, obtain with Mo
The substrate of back electrode；In this step, direct current magnetron sputtering process can be effectively ensured Mo film electric conductivity and adhesive force and its
Microscopic appearance；
The setting steps of evaporation cavity：By the rotation sample of the above-mentioned basal molecular beam epitaxy equipment evaporation cavity with Mo back electrode
In sample platform, with Mo back electrode one downwards, heating source is equipped with above substrate, raw material evaporation source is located at the bottom of evaporation cavity
Portion, raw material evaporation source exit are equipped with the switch for controlling raw material, cool down evaporation cavity diffusion pump for evaporation cavity with liquid nitrogen
Interior is evacuated to 10-5Pa, the steam for adjusting raw material in each evaporation source are depressed into Ag：8.5×10-5Torr, In：4.0×10- 5Torr, Ga：8×10-5Torr, Se：2.0×10-3Torr。
Quaternary steams the step of standby absorbed layer altogether：Substrate with Mo back electrode is heated to 520 DEG C, open Ag, In,
Ga, Se evaporation source co-evaporate Ag, In, Ga, Se on Mo back electrode, form AIGS film layer；
Cooling step：Ag, In, Ga evaporation source are closed, substrate is cooled down with 15 DEG C/minute of speed under Se atmosphere protection, when
Base reservoir temperature closes evaporation source Se when being down to 400 DEG C, heating source is simultaneously closed off, when base reservoir temperature is down to 200 DEG C, by sample stage
It takes to sample switch room, obtains quaternary and steam AIGS film altogether.
Embodiment 3
A kind of quaternary steams AIGS film altogether, including substrate of glass, deposition metal Mo back electrode on the glass substrate and
The absorbed layer on Mo back electrode is steamed altogether；The absorbed layer is the AIGS film that one-step method quaternary steams Ag, In, Ga, Se formation altogether
Layer；The overall thickness of the absorbed layer is 2 μm；The substrate of glass be soda-lime glass, substrate of glass with a thickness of 1.5mm；Institute
State Mo back electrode with a thickness of 1.2 μm；
The preparation method that the quaternary steams AIGS film altogether includes
The step of preparing Mo back electrode：With direct current magnetron sputtering process deposited metal Mo on the glass substrate, obtain with Mo
The substrate of back electrode；In this step, direct current magnetron sputtering process can be effectively ensured Mo film electric conductivity and adhesive force and its
Microscopic appearance；
The setting steps of evaporation cavity：By the rotation sample of the above-mentioned basal molecular beam epitaxy equipment evaporation cavity with Mo back electrode
In sample platform, with Mo back electrode one downwards, heating source is equipped with above substrate, raw material evaporation source is located at the bottom of evaporation cavity
Portion, raw material evaporation source exit are equipped with the switch for controlling raw material, cool down evaporation cavity diffusion pump for evaporation cavity with liquid nitrogen
Interior is evacuated to 10-5Pa, the steam for adjusting raw material in each evaporation source are depressed into Ag：8.5×10-5Torr, In：4.0×10- 5Torr, Ga：8×10-5Torr, Se：2.0×10-3Torr。
Quaternary steams the step of standby absorbed layer altogether：Substrate with Mo back electrode is heated to 520 DEG C, open Ag, In,
Ga, Se evaporation source co-evaporate Ag, In, Ga, Se on Mo back electrode, form AIGS film layer；
Cooling step：Ag, In, Ga evaporation source are closed, substrate is cooled down with 15 DEG C/minute of speed under Se atmosphere protection, when
Base reservoir temperature closes evaporation source Se when being down to 400 DEG C, heating source is simultaneously closed off, when base reservoir temperature is down to 200 DEG C, by sample stage
It takes to sample switch room, obtains quaternary and steam AIGS film altogether.
Embodiment 4
A kind of AIGS thin-film solar cells, including substrate of glass, deposition metal Mo back electrode on the glass substrate, altogether
Steam on Mo back electrode absorbed layer, be arranged in and receive CdS buffer layer on layer and the on the buffer layer intrinsic zinc oxide that is arranged
Layer and boron-doping zinc oxide transparent conductive film Window layer, production has metal in the boron-doping zinc oxide transparent conductive film Window layer
Aluminum gate electrode, the absorbed layer are the AIGS film layer that one-step method quaternary steams Ag, In, Ga, Se formation altogether；
The preparation method of the AIGS thin-film solar cells includes
The step of preparing Mo back electrode：Method deposited metal Mo on the glass substrate is penetrated with direct magnetic control Destroy, is obtained with Mo
The substrate of back electrode；
The setting steps of evaporation cavity：By the rotation sample of the above-mentioned basal molecular beam epitaxy equipment evaporation cavity with Mo back electrode
In sample platform, with Mo back electrode one downwards, heating source is equipped with above substrate, raw material evaporation source is located at the bottom of evaporation cavity
Portion, raw material evaporation source exit are equipped with the switch for controlling raw material, vacuumize with the cooling evaporation cavity of liquid nitrogen and to evaporation cavity,
Adjust the vapour pressure of raw material setting in evaporation source；
Quaternary steams the step of standby absorbed layer altogether：Substrate with Mo back electrode is heated to 520 DEG C, open Ag, In,
Ga, Se evaporation source co-evaporate Ag, In, Ga, Se on Mo back electrode, form AIGS film layer；
Cooling step：Ag, In, Ga evaporation source are closed, the cooling substrate under Se atmosphere protection, when base reservoir temperature is down to 400
DEG C when close evaporation source Se, simultaneously close off heating source, when base reservoir temperature is down to 200 DEG C, sample stage taken to sample switch room,
It obtains quaternary and steams AIGS film altogether；
The step of making thin-film solar cells：CdS buffer layer is prepared using chemical water bath, is adopted on CdS buffer layer
Native oxide zinc layers and boron-doping zinc oxide transparent conductive film Window layer are prepared with Metalorganic chemical vapor deposition method, later
Metal aluminum gate electrode is prepared in boron-doping zinc oxide transparent conductive film Window layer using physical vapour deposition (PVD), obtains AIGS film
Solar battery.
The above embodiment is only the preferred embodiment of the present invention, and the scope of protection of the present invention is not limited thereto,
The variation and replacement for any unsubstantiality that those skilled in the art is done on the basis of the present invention belong to institute of the present invention
Claimed range.
Claims (9)
1. a kind of quaternary steams AIGS film altogether, which is characterized in that including the metal Mo back of substrate of glass, deposition on the glass substrate
Electrode and altogether absorbed layer of the steaming on Mo back electrode；The absorbed layer is that one-step method quaternary steams Ag, In, Ga, Se formation altogether
AIGS film layer.
2. quaternary according to claim 1 steams AIGS film altogether, which is characterized in that each element accounts for atom in the absorbed layer
Percentage is 1:0.25:0.75:2, absorption layer component basic structural formula is Ag (In0.25Ga0.75) Se2.
3. quaternary according to claim 1 steams AIGS film altogether, which is characterized in that the overall thickness of the absorbed layer is 1.5-
2μm；The substrate of glass be soda-lime glass, substrate of glass with a thickness of 1.5-2.5mm；The Mo back electrode with a thickness of 0.8-
1.2μm。
4. the preparation method that a kind of quaternary as described in claim 1 steams AIGS film altogether, which is characterized in that including
The step of preparing Mo back electrode：Method deposited metal Mo on the glass substrate is penetrated with direct magnetic control Destroy, is obtained with Mo back electricity
The substrate of pole；
The setting steps of evaporation cavity：By the specimen rotating holder of the above-mentioned basal molecular beam epitaxy equipment evaporation cavity with Mo back electrode
On, with Mo back electrode one downwards, heating source is equipped with above substrate, raw material evaporation source is located at the bottom of evaporation cavity, former
Material evaporation source exit is equipped with the switch for controlling raw material, vacuumizes with the cooling evaporation cavity of liquid nitrogen and to evaporation cavity, adjusts
The vapour pressure that raw material is set in evaporation source；
Quaternary steams the step of standby absorbed layer altogether：Substrate with Mo back electrode is heated to 520 DEG C, opens Ag, In, Ga, Se
Evaporation source co-evaporates Ag, In, Ga, Se on Mo back electrode, forms AIGS film layer；
Cooling step：Ag, In, Ga evaporation source are closed, the cooling substrate under Se atmosphere protection, when base reservoir temperature is down to 400 DEG C
Evaporation source Se is closed, heating source is simultaneously closed off, when base reservoir temperature is down to 200 DEG C, sample stage is taken to sample switch room, is obtained
Quaternary steams AIGS film altogether.
5. the preparation method that quaternary according to claim 4 steams AIGS film altogether, which is characterized in that the setting of evaporation cavity walks
In rapid, the vapour pressure of raw material is respectively Ag in Ag, In, Ga, Se evaporation source：8.5 × 10-5Torr, In：4.0 × 10-5Torr,
Ga：8 × 10-5Torr, Se：2.0×10-3Torr.
6. the preparation method that quaternary according to claim 4 steams AIGS film altogether, which is characterized in that quaternary steams standby suction altogether
In the step of receiving layer, the coevaporation time is 35-42min.
7. the preparation method that quaternary according to claim 4 steams AIGS film altogether, which is characterized in that in cooling step,
Under Se atmosphere protection, cooling velocity is 15 DEG C/minute.
8. a kind of AIGS thin-film solar cells, which is characterized in that including substrate of glass, the metal Mo of deposition on the glass substrate
Back electrode, steam altogether on Mo back electrode absorbed layer, be arranged in and receive CdS buffer layer on layer and the on the buffer layer sheet that is arranged
Zinc oxide film and boron-doping zinc oxide transparent conductive film Window layer are levied, is made in the boron-doping zinc oxide transparent conductive film Window layer
Work has metal aluminum gate electrode, and the absorbed layer is the AIGS film layer that one-step method quaternary steams Ag, In, Ga, Se formation altogether.
9. a kind of preparation method of AIGS thin-film solar cells as claimed in claim, which is characterized in that including
The step of preparing Mo back electrode：Method deposited metal Mo on the glass substrate is penetrated with direct magnetic control Destroy, is obtained with Mo back electricity
The substrate of pole；
The setting steps of evaporation cavity：By the specimen rotating holder of the above-mentioned basal molecular beam epitaxy equipment evaporation cavity with Mo back electrode
On, with Mo back electrode one downwards, heating source is equipped with above substrate, raw material evaporation source is located at the bottom of evaporation cavity, former
Material evaporation source exit is equipped with the switch for controlling raw material, vacuumizes with the cooling evaporation cavity of liquid nitrogen and to evaporation cavity, adjusts
The vapour pressure that raw material is set in evaporation source；
Quaternary steams the step of standby absorbed layer altogether：Substrate with Mo back electrode is heated to 520 DEG C, opens Ag, In, Ga, Se
Evaporation source co-evaporates Ag, In, Ga, Se on Mo back electrode, forms AIGS film layer；
Cooling step：Ag, In, Ga evaporation source are closed, the cooling substrate under Se atmosphere protection, when base reservoir temperature is down to 400 DEG C
Evaporation source Se is closed, heating source is simultaneously closed off, when base reservoir temperature is down to 200 DEG C, sample stage is taken to sample switch room, is obtained
Quaternary steams AIGS film altogether；
The step of making thin-film solar cells：CdS buffer layer is prepared using chemical water bath, using on CdS buffer layer has
Machine metallochemistry vapor deposition method prepares native oxide zinc layers and boron-doping zinc oxide transparent conductive film Window layer, uses later
Physical vapour deposition (PVD) prepares metal aluminum gate electrode in boron-doping zinc oxide transparent conductive film Window layer, obtains the AIGS film sun
It can battery.
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