CN105977317B - A kind of preparation method of CIGS solar cell absorbed layer - Google Patents

A kind of preparation method of CIGS solar cell absorbed layer Download PDF

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CN105977317B
CN105977317B CN201610550956.8A CN201610550956A CN105977317B CN 105977317 B CN105977317 B CN 105977317B CN 201610550956 A CN201610550956 A CN 201610550956A CN 105977317 B CN105977317 B CN 105977317B
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solar cell
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cigs solar
absorbed layer
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CN105977317A (en
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黄勇亮
孟凡英
沈文忠
吴敏
刘正新
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Shanghai Jiaotong University
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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
    • H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
    • 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
    • H01L31/032—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
    • 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
    • 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
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Abstract

The invention discloses a kind of preparation method of CIGS solar cell absorbed layer, including：Step 1, one layer of In Se compound layer is prepared in substrate；Step 2, Cu In Ga layers are prepared on the In Se compound layers, obtain the double-deck preformed layer that preformed layer is In Se/Cu In Ga；Step 3, the double-deck preformed layer is subjected to selenizing heat treatment, obtains CuInGaSe absorbed layer.CIGS solar cell absorbed layer prepared by the present invention can promote the grain growth at CuInGaSe absorbed layer back surface, while adjust the bandgap structure of absorbed layer, so as to improve the open-circuit voltage of CIGS solar cell, fill factor, curve factor and transformation efficiency.

Description

A kind of preparation method of CIGS solar cell absorbed layer
Technical field
The present invention relates to thin film solar cell manufacturing technology field, more particularly to a kind of CIGS (CIGS) solar cell The preparation method of absorbed layer.
Background technology
Regenerative resource of the solar cell as clean environment firendly, is just increasingly valued by people.CIGS thin-film Solar cell is a kind of new solar cell technology, compared to the common solar cell based on silicon materials, has and uses material Less, the advantages that cost is low, radiation resistance is good, and it is also possible to prepare on a flexible substrate flexibility solar cell, can subtract Light battery quality, that further expands solar cell installs and uses scope.In addition, CIGS solar cell has higher turn Efficiency is changed, laboratory peak efficiency can reach 22.6%, already close to even more than crystal silicon cell efficiency.
In the production of CIGS solar cells, the quality of CIGS absorbed layers is to determine the key of battery efficiency.CIGS absorbs Layer film mainly has two kinds of preparation technologies, it is a kind of be with the copper of simple substance (Cu), indium (In), gallium (Ga) and selenium (Se) for raw material, Deposited in vacuum chamber in a manner of coevaporation in substrate；Another kind is first to use magnetic control as raw material using simple substance or alloy target material Sputtering mode deposits copper and indium gallium preformed layer in substrate, then preformed layer selenizing is absorbed into layer film for CIGS.The work of vacuum evaporation Skill is readily available higher conversion efficiency, but good uniformity is extremely difficult in the preparation of large area, and sputtering and selenization technique Technique, be more beneficial for mass producing.At present Japan Solar Frontier companies, using sputtering and selenization technique technique Through the volume production for realizing CIGS solar cells.
Sputtering and selenization technique technique prepare CIGS absorbed layers in have one it is very crucial the problem of be exactly, in selenizing by More faster than the reaction of selenium and gallium in the reaction of selenium and indium, In can quickly move to absorption layer surface, when this results in selenizing The low CIGS phases of gallium content can be quickly formed absorbing layer surface, and substantial amounts of gallium element gathers substrate and CIGS absorbed layers Interface.This can cause the surface band gap of absorbed layer low, and back side band gap is high, and because gallium element is overleaf assembled, causes to carry on the back The crystalline quality in face is poor, so as to reduce the conversion efficiency of battery.In order to optimize the distribution of gallium element in CIGS absorbed layers, and The crystalline quality of absorbed layer, high annealing and sulfuration process are all widely used.But CIGS absorbed layers prepared by selenization process All the time the problem of gallium content is high, and crystallite dimension is small near back surface be present.
The content of the invention
In view of the deficiencies in the prior art, the technical problems to be solved by the invention are to improve the crystallinity and gallium of absorbed layer The distribution of element, so as to improve the conversion efficiency of CIGS solar cells.
To achieve the above object, the invention provides a kind of new method for preparing CIGS absorbed layers, specifically, the present invention The technical scheme of offer is as follows：
A kind of preparation method of CIGS solar cell absorbed layer, comprises the following steps：
Step 1, one layer of In-Se compound layer is prepared in substrate；
Step 2, Cu-In-Ga layers are prepared on In-Se compound layers, it is the double of In-Se/Cu-In-Ga to obtain preformed layer Layer preformed layer；
Step 3, double-deck preformed layer is subjected to selenizing heat treatment, obtains CuInGaSe absorbed layer.
Preferably, In-Se compound layers can use sputtering, evaporation, electro-deposition or selenizing heat treatment indium thin in step 1 It is prepared by the methods of film.
Preferably, In-Se compound layer thickness is 50-200nm in step 1, and meets atomic ratio In/Se=1.1- 2.0。
Preferably, Cu-In-Ga layers are prepared using magnetically controlled sputter method in step 2, can use Cu-Ga, Cu-In, Cu- In-Ga alloys targets and In targets are target, and sputtering atmosphere is argon gas, air pressure 0.3-1.0Pa.
Preferably, double-deck preformed layer gross thickness is 300-1000nm, and overall atomic composition ratios meet Cu/ (In+Ga) =0.70-0.99.
Preferably, the selenizing heat treatment that double-deck preformed layer is carried out in step 3 is included in the selenium having under atmosphere existing for selenium source Change reaction, and the annealing under inert gas shielding.
Further, selenium source includes selenium powder, selenium steam, hydrogen selenide or organic selenides.
Preferably, sputtering has one layer of molybdenum film as back electrode in substrate.
Preferably, substrate includes soda-lime glass, low Fe glass, solar energy float glass, stainless steel foil, Al paper tinsels, Mo paper tinsels, Cu Paper tinsel, polyimides (PI) or pet resin (PET).
The preparation method of CIGS solar cell absorbed layer provided by the invention proposes In-Se/Cu-In-Ga bilayers The technical scheme of preformed layer, after In-Se is formed on molybdenum surface, In is not easy to move to surface in follow-up selenizing heat treatment, Therefore the In contents in CIGS absorbed layers at back surface can be increased, the raising of In contents can be effectively improved the crystalline substance at absorbed layer back Particle size.Meanwhile liquid phase occurs more than 550 DEG C in In-Se phases, it can further promote grain growth and the expansion of gallium element Dissipate, so as to improve the distribution of the crystallinity of CIGS absorbed layers and gallium element.Therefore, using this double-deck preformed layer, Ke Yiti Open-circuit voltage, fill factor, curve factor and the transformation efficiency of high CIGS solar cells.
The method of the present invention and caused technique effect are described further below with reference to accompanying drawing, to be fully understood from The purpose of the present invention, feature and effect.
Brief description of the drawings
Fig. 1 is the structural representation of CIGS solar cell
Fig. 2 is the process chart for preparing CuInGaSe absorbed layer of the embodiment of the present invention 1
Embodiment
Fig. 1 show the general structure of CIGS solar cells, including be arranged in order substrate 1, molybdenum film 2, CIGS absorb Layer 3, transition zone 4, Window layer 5, antireflective coating 6 and gate-shaped electrode 7.
Substrate can be soda-lime glass, low Fe glass, solar energy float glass, stainless steel foil, Al paper tinsels, Mo paper tinsels, Cu paper tinsels, gather Acid imide (PI), pet resin (PET) and other suitable substrates.For follow-up CIGS battery works Skill, being sputtered on base material has one layer of molybdenum film as back electrode material.
The preparation method of CIGS solar cells absorbed layer proposed by the present invention is explained below by specific embodiment.
Embodiment 1
Technological process is as shown in Figure 2：
Step 1, pass through one layer of indium selenium (In-Se) chemical combination of magnetron sputtering in the soda-lime glass substrate 1 that molybdenum film 2 covers Nitride layer 9, In/Se atomic ratios are 1.3 in target, and sputtering atmosphere is argon gas, and the thickness of air pressure 0.3-1.0Pa, In-Se layer is about 100nm。
Step 2, on In-Se layers, using Cu-Ga alloys targets (Ga content at.25%) and In targets as target, using magnetic control The mode of sputtering sputters copper and indium gallium (Cu-In-Ga) layer 10, and sputtering atmosphere is argon gas, and air pressure 0.3-1.0Pa, thickness is 0.6 μ M, obtain double-deck prefabricated layer film, overall atomic composition ratios Cu/ (In+Ga)=0.91.
Step 3, the film of the double-deck preformed layer of preparation is transferred in selenizing stove, using H2Se is as selenium source, 400 DEG C of selenium Change 40min, anneal 30min in 580 DEG C of nitrogen atmospheres, and then natural cooling, obtains CIGS absorbed layers 3, and thickness is about 1.5 μm.
Embodiment 2
Step 1, it is by one layer of In layer of magnetron sputtering, sputtering atmosphere in the soda-lime glass substrate 1 that molybdenum film 2 covers Argon gas, the thickness of air pressure 0.3-1.0Pa, In layer is about 60nm.
Step 2, the substrate that sputtering there are In layers is transferred in selenizing stove, using H2Se is as selenium source, 190 DEG C of selenizings 15min, room temperature is then naturally cooled to, obtain In-Se compound layers 9.In-Se thickness degree about 100nm, In/Se are former after selenizing Son is than being 1.36.
Step 3, the substrate that preparation there are In-Se layers is transferred in sputtering equipment, on In-Se layers, with Cu-Ga alloys Target (Ga content at.25%) and In targets are target, copper and indium gallium layer 10 are sputtered by the way of magnetron sputtering, sputtering atmosphere is argon Gas, air pressure 0.3-1.0Pa, thickness are about 0.6 μm, obtain double-deck prefabricated layer film.The overall atomic composition of double-deck preformed layer Ratio is Cu/ (In+Ga)=0.85.
Step 4, the film of the double-deck preformed layer of preparation is transferred in selenizing stove, using H2Se is as selenium source, 400 DEG C of selenium Change 30min, anneal 30min in 580 DEG C of nitrogen atmospheres, and then natural cooling, obtains CIGS absorbed layers 3, and thickness is about 1.4 μm.
In other embodiments, In-Se compounds can use sputtering, evaporation, electro-deposition and indium selenide film etc. various It is prepared by method, it is only necessary to ensure atomic ratio In/Se=1.1-2.0 in In-Se layers, the thickness of In-Se layers is 50-200nm, and Other objectionable impurities are not introduced.
Preformed layer needs to ensure that gross thickness be 300-1000nm, overall atomic composition ratios for Cu/ (In+Ga)= 0.70-0.99。
Selenizing heat treatment can use selenium powder, selenium steam, hydrogen selenide, organic selenides (such as diethyl selenide (C4H10Se), two Methyl selenium (C2H6Se), dimethyl selenide (C2H6)) etc. Se it is used as selenium source.Selenization process process (such as selenizing temperature, time, rises Temperature, temperature fall time etc.) need to make adjustment with the change of selenium source, preformed layer thickness and component.
Preferred embodiment of the invention described in detail above.It should be appreciated that the ordinary skill of this area is without wound The property made work can makes many modifications and variations according to the design of the present invention.Therefore, all technician in the art Pass through the available technology of logical analysis, reasoning, or a limited experiment on the basis of existing technology under this invention's idea Scheme, all should be in the protection domain being defined in the patent claims.

Claims (10)

1. a kind of preparation method of CIGS solar cell absorbed layer, it is characterised in that comprise the following steps：
Step 1, one layer of In-Se compound layer is prepared in substrate, and cause the In-Se compound layers to meet atomic ratio In/ Se=1.1-2.0；
Step 2, Cu-In-Ga layers are prepared on the In-Se compound layers, it is the double of In-Se/Cu-In-Ga to obtain preformed layer Layer preformed layer；
Step 3, the double-deck preformed layer is subjected to selenizing heat treatment, the selenizing heat treatment includes selenizing and annealing process, moved back The temperature of fiery process is higher than 550 DEG C, obtains CuInGaSe absorbed layer.
2. the preparation method of CIGS solar cell absorbed layer as claimed in claim 1, In-Se wherein described in step 1 Compound layer is prepared using sputtering, evaporation, electro-deposition or selenizing heat treatment indium film process.
3. the preparation method of CIGS solar cell absorbed layer as claimed in claim 1, In-Se wherein described in step 1 Compound layer thickness is 50-200nm.
4. the preparation method of CIGS solar cell absorbed layer as claimed in claim 1, Cu- wherein described in step 2 In-Ga layers are prepared using magnetically controlled sputter method, use Cu-Ga, Cu-In, Cu-In-Ga alloys target and In targets as target, sputter gas Atmosphere is argon gas, air pressure 0.3-1.0Pa.
5. the preparation method of CIGS solar cell absorbed layer as claimed in claim 1, wherein the double-deck preformed layer is total Thickness is 300-1000nm, and overall atomic composition ratios meet Cu/ (In+Ga)=0.70-0.99.
6. the preparation method of CIGS solar cell absorbed layer as claimed in claim 1, double-deck wherein described in step 3 Preformed layer carries out selenizing heat treatment and is included in the selenylation reaction having under atmosphere existing for selenium source, and the annealing under inert gas shielding Processing.
7. the preparation method of CIGS solar cell absorbed layer as claimed in claim 6, wherein the selenium source include selenium powder, Selenium steam, hydrogen selenide or organic selenides.
8. the preparation method of CIGS solar cell absorbed layer as claimed in claim 6, wherein the annealing be Anneal 30min in 580 DEG C of nitrogen atmospheres, then natural cooling.
9. the preparation method of CIGS solar cell absorbed layer as claimed in claim 1, wherein there is sputtering in the substrate One layer of molybdenum film is as back electrode.
10. the preparation method of CIGS solar cell absorbed layer as claimed in claim 1, wherein the substrate includes sodium calcium Glass, low Fe glass, solar energy float glass, stainless steel foil, Al paper tinsels, Mo paper tinsels, Cu paper tinsels, polyimides or poly terephthalic acid second Terephthalate resin.
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