CN103668361B - A kind of preparation method of the copper and indium zinc selenium thin film of the photovoltaic cell for photovoltaic generating system - Google Patents
A kind of preparation method of the copper and indium zinc selenium thin film of the photovoltaic cell for photovoltaic generating system Download PDFInfo
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- 239000010409 thin film Substances 0.000 title claims abstract description 60
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 239000010949 copper Substances 0.000 title claims abstract description 27
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 26
- ZYQNKFKPTUYGMQ-UHFFFAOYSA-N [In]=[Se].[Zn] Chemical compound [In]=[Se].[Zn] ZYQNKFKPTUYGMQ-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000004070 electrodeposition Methods 0.000 claims abstract description 30
- 238000000151 deposition Methods 0.000 claims abstract description 14
- 239000011669 selenium Substances 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 12
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000470 constituent Substances 0.000 claims abstract description 8
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 7
- 239000011733 molybdenum Substances 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 238000004062 sedimentation Methods 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 claims description 10
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims description 5
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 5
- 239000011889 copper foil Substances 0.000 claims description 5
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims description 5
- 229910052756 noble gas Inorganic materials 0.000 claims description 5
- 229910052709 silver Inorganic materials 0.000 claims description 5
- 239000004332 silver Substances 0.000 claims description 5
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 5
- 239000011592 zinc chloride Substances 0.000 claims description 5
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 5
- 239000010408 film Substances 0.000 abstract description 6
- 229910052738 indium Inorganic materials 0.000 abstract description 6
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 239000011701 zinc Substances 0.000 abstract description 2
- 229910052725 zinc Inorganic materials 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000005229 chemical vapour deposition Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052733 gallium Inorganic materials 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- MARUHZGHZWCEQU-UHFFFAOYSA-N 5-phenyl-2h-tetrazole Chemical compound C1=CC=CC=C1C1=NNN=N1 MARUHZGHZWCEQU-UHFFFAOYSA-N 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- 229910000928 Yellow copper Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- ZQRRBZZVXPVWRB-UHFFFAOYSA-N [S].[Se] Chemical compound [S].[Se] ZQRRBZZVXPVWRB-UHFFFAOYSA-N 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 210000001142 back Anatomy 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- SPVXKVOXSXTJOY-UHFFFAOYSA-N selane Chemical compound [SeH2] SPVXKVOXSXTJOY-UHFFFAOYSA-N 0.000 description 1
- 229910000058 selane Inorganic materials 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
Classifications
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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
- 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 preparation method that the present invention provides the copper and indium zinc selenium thin film of a kind of photovoltaic cell for photovoltaic generating system, does is each constituent content of copper, indium and selenium film Cu? 20.55-20.59%, In? 25.54-25.60%, Zn? 15.62-15.68%, Se? 38.10-38.19%, above-mentioned each component sum is 100%; Its preparation method is as follows: the 1) preparation of electric depositing solution: electric depositing solution is prepared with deionized water at normal temperatures, and adjustment pH value is 2.5-3.0; 2) electro-deposition of thin film: electro-deposition adopts constant potential-1.0V, solution temperature 25 DEG C, sedimentation time 30min, and during electro-deposition, solution is without stirring, ambient operation; 3) selenization of thin film: selenizing stove put into by the molybdenum box by thin film with equipped with 3g solid selenium, with the ramp of 10-15 DEG C/min to 450 DEG C, the selenizing time is 1h, afterwards furnace cooling; 4) heat treatment of thin film: first heat treatment 10min under 350 DEG C of constant temperature, afterwards with the ramp of 15-20 DEG C/min to 550 DEG C, is incubated 50min, final prepared copper and indium zinc selenium thin film. Above-mentioned preparation method not only can low cost, and operate simple and easy, be conducive to large area to produce and the exploitation of environmental requirement and photovoltaic energy.
Description
Technical field
The present invention relates to Photovoltaic new energy technical field in the preparation of semiconductive thin film, particularly to the preparation method of the copper and indium zinc selenium thin film of a kind of photovoltaic cell for photovoltaic generating system.
Background technology
Photovoltaic generating system is a kind of energy conversion system directly converting the solar into electric energy, the theoretical basis of its opto-electronic conversion is the photovoltaic effect near semiconductor PN or semiconductor-metal interface, therefore solaode is otherwise known as photovoltaic cells, is called for short photovoltaic cell or light cell. Photovoltaic cell is developed so far, and can be largely classified into three major types, and one is the crystal silicon solar energy battery based on monocrystal silicon and polysilicon silicon chip; Two is silica-base film (amorphous, polycrystalline, crystallite etc.), CIS and cadmium telluride diaphragm solar battery, dye sensitization and other organic solar batteries; Three is still in novel solar batteries such as the SQW of conceptual phase, multipotency band, hot carriers. Current crystal silicon solar energy battery is occupied an leading position, and market share is about 90%, and thin-film solar cells market share only has about 10%.The core of thin-film solar cells is light absorbing zone and the heterojunction semiconductor of another semiconductor layer composition, the thin film such as light-absorption layer, Window layer and dorsum electrode layer organically combine, and substrate is glass or the flexible material of low cost. Owing to light absorbing zone is direct band-gap semicondictor, so the absorption coefficient of light is high, several microns of thickness just can absorb overwhelming majority sunlight, and therefore device gross thickness is smaller than 10 microns. It is also advantageous in that solar energy in large area battery module can entirety be made, and does not need to assemble. Material owing to needing is few, and compared with silion cell, production cost has substantial degradation space.
The thin-film solar cells of China starts from the eighties, wherein copper and indium (gallium) selenium CI (G) S solaode due to transformation efficiency be in thin-film solar cells the highest, and have that band gap is adjustable, radiation resistance good, production process environmental protection, to constituent content nonstoichiometry than tolerance advantages of higher, thus in recent years under the superperformance of copper and indium (gallium) Se solar cell and broad prospect of application, many scientific research institutions and company proceed by research and the production of CIGS solaode. Such as Guangxi Di Kai limited company and Tsing-Hua University's R & D Cooperation CIGS solaode. Blue star company of Weihai in Shandong province has introduced two conversion ratios manufacture of solar cells line more than 8% from TETTASOLAR company of the U.S.. Safe and sound company also contracts in German company, the technology of CIS solaode is prepared in joint development electro-deposition, Shandong Fu limited company has introduced the CIGSSe thin film solar cell technologies of the JOHANNASOLAR of Germany, has built up extensive battery production base.
Copper and indium (gallium) selenium material is the direct band-gap semicondictor of a kind of yellow copper structure, and under room temperature, energy gap is 1.04eV, owing to it has high photoelectric transformation efficiency (18%) and the absorption coefficient of light (α > 10-5cm-1), capability of resistance to radiation is strong, is one of best photovoltaic semiconductors material of absorbent properties known today. Along with the development of solaode industry, CIS (CuInSe2) research be also affected by increasingly focusing on, it is believed that be the important component part of thin-film solar cells, used the aspect such as solaode and some light-sensitive elements both at home and abroad at present.
Summary of the invention
The preparation method of photovoltaic cell thin film is varied, such as methods such as chemical vapour deposition (CVD), SILAR method (SILAR), electrochemical depositions. In these methods, magnetron sputtering technique comparative maturity, but due to appointed condition reason, make the method at preparation large area CuInSe2Thin film aspect is restricted, and relatively costly. Chemical vapour deposition (CVD), SILAR method prepare CuInSe2Thin film has bibliographical information, but all haves much room for improvement in large area preparation and film quality control etc. Electrochemical deposition rule adopts the method for electro-deposition and selenium (sulfur) annealing to prepare high-quality CIGS polycrystal film on the substrate of plating molybdenum electrode. But it is complicated all to there is equipment in various degree in said method, complex operation, and production cost is high, is unfavorable for large-scale production, is unsatisfactory for environmental requirement simultaneously.
The preparation method that it is an object of the invention to provide a kind of copper and indium zinc selenium thin film for photovoltaic cell, not only low cost can prepare copper and indium zinc selenium thin film, and operate simple and easy, is conducive to large area to produce the exploitation with environmental requirement and photovoltaic energy. For achieving the above object, the technical solution used in the present invention is the preparation method of a kind of copper and indium zinc selenium thin film for photovoltaic cell, each constituent content of copper, indium and selenium film is Cu20.55-20.59%, In25.54-25.60%, Zn15.62-15.68%, Se38.10-38.19%, above-mentioned each component sum is 100%;
Its preparation method is as follows:
1) preparation of electric depositing solution: electric depositing solution is prepared with deionized water at normal temperatures, and adjustment pH value is 2.5-3.0;
2) electro-deposition of thin film: electro-deposition adopts constant potential-1.0V, solution temperature 25 DEG C, sedimentation time 30min, and during electro-deposition, solution is without stirring, ambient operation;
3) selenization of thin film: selenizing stove put into by the molybdenum box by thin film with equipped with 3g solid selenium, with the ramp of 10-15 DEG C/min to 450 DEG C, the selenizing time is 1h, afterwards furnace cooling;
4) heat treatment of thin film: first heat treatment 10min under 350 DEG C of constant temperature, afterwards with the ramp of 15-20 DEG C/min to 550 DEG C, is incubated 50min, final prepared copper and indium zinc selenium thin film.
Material added by described electric depositing solution and concentration thereof is: the CuCl of 0.02-0.025mol/L2, 0.05-0.055mol/L InCl3, 0.025-0.03mol/L ZnCl2, the citric acid of 0.8-0.85mol/L, 0.05-0.06mol/L LiCl.
Described electro-deposition is to be placed in container of electrodeposition by the solution of described preparation, is platinized and titanized anode to electrode, and reference electrode is silver/silver chloride electrode, and working electrode is Copper Foil, and area is 3cm × 3cm.
Described selenization also includes the step that noble gas passes into the air displaced in selenizing stove in stove.
The present invention compared with prior art, 1) accurately control each constituent content of thin film, and with the addition of the zinc element Substitute For Partial phosphide element that reserves are abundant and cost is low, not only ensure film performance but also production cost can be reduced;
2) conventional selenization adopts H2Se gas, the present invention adopts solid-state selenium to instead of the H of severe toxicity2Se gas, more environmentally-friendly;
3) after electro-deposition, thin film is carried out heat treatment, further ensure quality and the crystal form of thin film;
4) equipment is simple, and reaction condition is gentle;
5) preparation parameter can be readily changed by change the correlated performance of thin film, such as energy gap, be actually needed to meet.
Accompanying drawing explanation
Fig. 1 is the preparation flow figure of the copper and indium zinc selenium thin film of photovoltaic cell.
Fig. 2 CuInZnSe photovoltaic cell structure schematic diagram.
Detailed description of the invention
Embodiment 1:
Each constituent content of copper and indium zinc selenium thin film is Cu20.58%, In25.57%, Zn15.66%, Se38.19%. Its step is as follows:
1) preparation of electric depositing solution: electric depositing solution is prepared with deionized water at normal temperatures, and added material and concentration thereof is: the CuCl of 0.02mol/L2, 0.05mol/L InCl3, 0.025mol/L ZnCl2, the citric acid of 0.8mol/L, 0.05mol/L LiCl, adjust pH value be 2.5;
2) electro-deposition of thin film: the solution of above-mentioned preparation is placed in container of electrodeposition, it is platinized and titanized anode to electrode, reference electrode is silver/silver chloride electrode, working electrode is Copper Foil, and area is 3cm*3cm, and electro-deposition adopts constant potential-1.0V, solution temperature 25 DEG C, sedimentation time 30min, during electro-deposition, solution is without stirring, ambient operation;
3) selenization of thin film: noble gas is passed into the air displacing in stove in selenizing stove, selenizing stove put into by the molybdenum box by thin film with equipped with 3g solid selenium afterwards, and with the ramp of 12 DEG C/min to 450 DEG C, the selenizing time is 1h, afterwards furnace cooling;
4) heat treatment of thin film: first heat treatment 10min under 350 DEG C of constant temperature, afterwards with the ramp of 20 DEG C/min to 550 DEG C, is incubated 50min, final prepared copper and indium zinc selenium thin film.
Embodiment 2:
Each constituent content of copper and indium zinc selenium thin film is Cu20.59%, In25.60%, Zn15.62%, Se38.19%, and its step is as follows:
1) preparation of electric depositing solution: electric depositing solution is prepared with deionized water at normal temperatures, and added material and concentration thereof is: the CuCl of 0.023mol/L2, 0.053mol/L InCl3, 0.028mol/L ZnCl2, the citric acid of 0.84mol/L, 0.056mol/L LiCl, adjust pH value be 2.8;2) electro-deposition of thin film: the solution of above-mentioned preparation is placed in container of electrodeposition, it is platinized and titanized anode to electrode, reference electrode is silver/silver chloride electrode, working electrode is Copper Foil, and area is 3cm*3cm, and electro-deposition adopts constant potential-1.0V, solution temperature 25 DEG C, sedimentation time 30min, during electro-deposition, solution is without stirring, ambient operation; 3) selenization of thin film: noble gas is passed into the air displacing in stove in selenizing stove, selenizing stove put into by the molybdenum box by thin film with equipped with 3g solid selenium afterwards, and with the ramp of 15 DEG C/min to 450 DEG C, the selenizing time is 1h, afterwards furnace cooling; 4) heat treatment of thin film: first heat treatment 10min under 350 DEG C of constant temperature, afterwards with the ramp of 15 DEG C/min to 550 DEG C, is incubated 50min, final prepared copper and indium zinc selenium thin film.
Embodiment 3:
Each constituent content of copper and indium zinc selenium thin film is Cu20.57%, In25.57%, Zn15.64%, Se38.22%, and its step is as follows:
1) preparation of electric depositing solution: electric depositing solution is prepared with deionized water at normal temperatures, and added material and concentration thereof is: the CuCl of 0.025mol/L2, 0.055mol/L InCl3, 0.03mol/L ZnCl2, the citric acid of 0.85mol/L, 0.06mol/L LiCl, adjust pH value be 3.0; 2) electro-deposition of thin film: the solution of above-mentioned preparation is placed in container of electrodeposition, it is platinized and titanized anode to electrode, reference electrode is silver/silver chloride electrode, working electrode is Copper Foil, and area is 3cm*3cm, and electro-deposition adopts constant potential-1.0V, solution temperature 25 DEG C, sedimentation time 30min, during electro-deposition, solution is without stirring, ambient operation; 3) selenization of thin film: noble gas is passed into the air displacing in stove in selenizing stove, selenizing stove put into by the molybdenum box by thin film with equipped with 3g solid selenium afterwards, and with the ramp of 12 DEG C/min to 450 DEG C, the selenizing time is 1h, afterwards furnace cooling; 4) heat treatment of thin film: first heat treatment 10min under 350 DEG C of constant temperature, afterwards with the ramp of 18 DEG C/min to 550 DEG C, is incubated 50min, final prepared copper and indium zinc selenium thin film.
Claims (3)
1. the preparation method for the copper and indium zinc selenium thin film of the photovoltaic cell of photovoltaic generating system, it is characterized in that, each constituent content of described copper and indium zinc selenium thin film is Cu20.55-20.59%, In25.54-25.60%, Zn15.62-15.68%, Se38.10-38.19%, above-mentioned each component sum is 100%;
Its preparation method is as follows:
1) preparation of electric depositing solution: electric depositing solution is prepared with deionized water at normal temperatures, and adjustment pH value is 2.5-3.0;
2) electro-deposition of thin film: electro-deposition adopts constant potential-1.0V, solution temperature 25 DEG C, sedimentation time 30min, and during electro-deposition, solution is without stirring, ambient operation;
3) selenization of thin film: selenizing stove put into by the molybdenum box by thin film with equipped with 3g solid selenium, with the ramp of 10-15 DEG C/min to 450 DEG C, the selenizing time is 1h, afterwards furnace cooling;
4) heat treatment of thin film: first heat treatment 10min under 350 DEG C of constant temperature, afterwards with the ramp of 15-20 DEG C/min to 550 DEG C, is incubated 50min, final prepared copper and indium zinc selenium thin film;
Material added by described electric depositing solution and concentration thereof is: the CuCl of 0.02-0.025mol/L2, 0.05-0.055mol/L InCl3, 0.025-0.03mol/L ZnCl2, the citric acid of 0.8-0.85mol/L, 0.05-0.06mol/L LiCl.
2. the preparation method of copper and indium zinc selenium thin film as claimed in claim 1, it is characterized in that described electro-deposition is to be placed in container of electrodeposition by the solution of described preparation, be platinized and titanized anode to electrode, reference electrode is silver/silver chloride electrode, working electrode is Copper Foil, and area is 3cm × 3cm.
3. the preparation method of copper and indium zinc selenium thin film as claimed in claim 1, it is characterised in that described selenization also includes the step that noble gas passes into the air displaced in selenizing stove in stove.
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Band gap engineering of RF-sputtered CuInZnSe2 thin films for indium-reduced thin-film solar cell application;Rachmat Adhi Wibowo et al.;《Solar Energy Materials & Solar Cells》;20090103;第93卷(第6-7期);第941-944页 * |
Investigation of CuInZnSe2 thin films for solar cell applications;V.F. Gremenok et al.;《Thin Solid Films》;20050226;第487卷(第1-2期);第194、197-198页 * |
欧铜钢 等;Cu-In合金硒化法制备CuInSe2薄膜;《材料学报:研究篇》;20091125;第23卷(第11期);第90-91页实验部分、表1 * |
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