CN106024977A - Method for preparing copper gallium sulfide photoelectric thin film from copper sulfate - Google Patents
Method for preparing copper gallium sulfide photoelectric thin film from copper sulfate Download PDFInfo
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- CN106024977A CN106024977A CN201610418998.6A CN201610418998A CN106024977A CN 106024977 A CN106024977 A CN 106024977A CN 201610418998 A CN201610418998 A CN 201610418998A CN 106024977 A CN106024977 A CN 106024977A
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- 239000010409 thin film Substances 0.000 title claims abstract description 34
- CDZGJSREWGPJMG-UHFFFAOYSA-N copper gallium Chemical compound [Cu].[Ga] CDZGJSREWGPJMG-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 18
- 229910000365 copper sulfate Inorganic materials 0.000 title claims abstract description 9
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 title claims abstract description 9
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 title abstract 6
- 239000000758 substrate Substances 0.000 claims abstract description 23
- 239000011521 glass Substances 0.000 claims abstract description 20
- 239000002243 precursor Substances 0.000 claims abstract description 20
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 11
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 229910009112 xH2O Inorganic materials 0.000 claims abstract description 6
- 238000004140 cleaning Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 19
- 229910052717 sulfur Inorganic materials 0.000 claims description 19
- 239000011593 sulfur Substances 0.000 claims description 19
- 230000005693 optoelectronics Effects 0.000 claims description 14
- 239000010408 film Substances 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 229910000336 copper(I) sulfate Inorganic materials 0.000 claims description 5
- WIVXEZIMDUGYRW-UHFFFAOYSA-L copper(i) sulfate Chemical compound [Cu+].[Cu+].[O-]S([O-])(=O)=O WIVXEZIMDUGYRW-UHFFFAOYSA-L 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 4
- 230000014759 maintenance of location Effects 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 2
- 230000000873 masking effect Effects 0.000 claims description 2
- 230000010355 oscillation Effects 0.000 claims description 2
- 235000011149 sulphuric acid Nutrition 0.000 claims description 2
- 239000001117 sulphuric acid Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000004528 spin coating Methods 0.000 abstract description 4
- CHPZKNULDCNCBW-UHFFFAOYSA-N gallium nitrate Inorganic materials [Ga+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O CHPZKNULDCNCBW-UHFFFAOYSA-N 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 238000004321 preservation Methods 0.000 abstract 1
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 abstract 1
- 239000010949 copper Substances 0.000 description 4
- 239000002803 fossil fuel Substances 0.000 description 3
- 229910052733 gallium Inorganic materials 0.000 description 3
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000004917 polyol method Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 208000033962 Fontaine progeroid syndrome Diseases 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000005361 soda-lime glass Substances 0.000 description 1
- 239000003643 water by type Substances 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
- H01L31/0256—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
-
- 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 provides a method for preparing a copper gallium sulfide photoelectric thin film from copper sulfate, and belongs to the technical field of preparation of photoelectric thin films for solar cells. The copper gallium sulfide photoelectric thin film is obtained through the following steps of: firstly, cleaning a glass substrate and then putting Cu2SO4.5H2O, Ga(NO3)3.xH2O and CH3CSNH2 into a solvent for mixing evenly; obtaining a precursor thin film on a glass sheet through a spin-coating method, drying the precursor thin film and putting the precursor thin film into a closed container with hydrazine hydrate; preventing a precursor thin film sample from being in contact with the hydrazine hydrate and arranging the closed container with the sample into an oven for heating and heat preservation treatment; and finally taking out the sample to soak for 24 hours and then drying the sample to obtain the copper gallium sulfide photoelectric thin film. A high-temperature and high-vacuum condition is not needed; the method is low in demands on instruments and equipment, low in production cost, high in production efficiency and easy to operate; the obtained copper gallium sulfide photoelectric thin film has relatively good continuity and uniformity; the main phase is a CuGaS2 phase; by the novel technology, the component and the structure of a target product are easy to control; and a low-cost production method capable of achieving industrialization is provided for preparation of the high-performance copper gallium sulfide photoelectric thin film.
Description
Technical field
The invention belongs to solar cell optoelectronic film preparing technical field, particularly relate to a kind of method being prepared copper gallium sulfur optoelectronic film by copper sulfate.
Background technology
Along with society and expanding economy; the Fossil fuels such as coal, oil, natural gas are applied to produce and the various aspects of life; the continuous utilization of Fossil fuel; tellurian resource is constantly reduced; so seeking a kind of new energy to become the task of top priority of every country; on the other hand; the continuous utilization of Fossil fuel also brings the impact in terms of environment; particularly in terms of greenhouse effect, therefore develop clean reproducible energy and to protection environment, sustainable economic development and construct harmonious society and have important meaning.Photovoltaic generation have safe and reliable, noiseless, pollution-free, restriction less, the advantage such as failure rate is low, easy maintenance, this cleaning of solar energy, safety and the regenerative resource of environmental protection, the research and development of solar cell the most in recent decades can be utilized to be increasingly subject to pay attention to.
Copper and indium sulfenyl thin film solar cell may be considered one of the most promising hull cell at present, and replace phosphide element to make copper gallium sulfur with gallium and also have very many advantages as absorbed layer: (1) CuGaS2It is direct band-gap semicondictor, at room temperature CuGaS2Energy gap be 2.53eV.(2) price of sulfur is relatively low, and time prepared by large area, price is relatively low.(3) at CuGaS2On the basis of adulterate other element, as made In or Al part replace Ga atom, replace S by Se part, be i.e. prepared as Cu (In1-xGax)Se2, Cu (In1-xGax)(Se2-ySy), Cu (In1-xAlx)(Se2-xSx), its crystal structure remains Chalkopyrite.Change the atomic ratio of wherein Ga/ (Ga+In) etc., its energy gap can be made to change between 1.04～1.72 eV, comprise high efficiency and absorb the bandgap range 1.4～1.6eV of sunlight；(4) the least in wider composition range internal resistance rate；(5) capability of resistance to radiation is strong, does not has photo attenuation effect, thus service life is long；(6) lattice structure of p-type CIGS material can be mated with common N-type window material (such as CdS, ZnO) with electron affinity.
The preparation method of copper gallium sulfur thin film mainly has metal organic chemical vapor deposition, solvent-thermal method, polyol process etc. at present.Copper gallium sulfur is the most rising a kind of optoelectronic thin film material, but existing process route is complicated, preparation cost high, it is difficult to make the thin-film material of preferred orientation, thus needs also exist for exploring the preparation technology of low cost, and can to make thin film be preferred orientation growth.
Method is the same as previously described, and other method also has different defects.Related to the present invention also has such as Publication about Document:
[1]Sin Kyu Kim, Jong
Pil Park, Min Kyung Kim, Kang Min OK, Il-Wun Shim, Preparation of CuGaS2 thin films by
two-stage MOCVD method, Solar Energy Materials & Solar Cells 92 (2008)
1311-1314.
Essentially describe and prepare CuGaS with Metalorganic Chemical Vapor Deposition2Thin film, and have studied the performance being reached demand by the element proportioning of process conditions regulation copper and gallium.
[2] Yang Yu, CuInS2And Cu (InGa) S2Film preparation and processing performance research, Tsing-Hua University's master thesis (2009).
Essentially describe employing Mid frequency alternative magnetron sputtering method deposition CuIn and CuInGa prefabricated membrane, and use solid-state vulcanization process to prepare CuInS2With Cu (InGa) S2Thin film, have studied the technological parameter impacts on film performance such as cure time, temperature, atom ratio and sulfur content.
[3]Ningru Xiao, Li Zhu, Kai Wang, Quanqin
Dai, Yingnan Wang. et, Synthesis and high-pressure
transformation of metastable wurtzite-structured
CuGaS2 nanocrystals, Nanoscale 4 (2012) 7443–7447.
Article describes the CuGaS of the wurtzite structure metastable by an a kind of simple and effective step solvent structure2Nanocrystalline.
[4] Li Zhenrong, Zhong Jiasong, Chen Zhaoping, Cai Qian, Liang Xiaojuan, Xiang Weidong, L-cysteine auxiliary CuGaS2The solvent-thermal process of microsphere and sign, artificial intraocular lenses's journal 40 (2011) 441 444.
Essentially describe by solvent structure CuGaS2Microsphere, and gained sample XRD, EDS, XPS etc. are characterized, pass through experimental result, it is proposed that CuGaS2The growth mechanism that microsphere is possible.
[5]Qiangchun
Liu, Kaibin Tang, Synthesis and Morphological
Evolution of CuGaS2 Nanostructures via a polyol
Method, CHINESE JOURNAL OF CHEMICAL PHYSICS 19 (2006) 335–340.
Essentially describe and synthesize CuGaS by polyol process2, and its Form Development is studied.
Summary of the invention
The present invention is to solve the deficiencies in the prior art, and invented a kind of diverse with the preparation method of prior art, the preparation technology of copper gallium sulfur solar energy thin-film material.
The present invention uses spin coating-chemistry co-reducing process to prepare copper gallium sulfur thin-film material, and employing soda-lime glass is substrate, with Cu2SO4·5H2O, Ga (NO3)3·xH2O, CH3CSNH2For raw material, with deionized water thing as solvent, (element metering ratio is as CuGaS first to prepare certain thickness cupric gallium sulfur with spin-coating method2) precursor thin-film, with hydrazine hydrate as reducing agent, heat at a lower temperature in hermetic container, make precursor thin-film reduce concurrent GCMS computer reaction obtain target product.
The concrete preparation method of the present invention includes following steps in sequence:
A. carry out the cleaning of glass substrate, be to be 20mm × 20mm by glass substrate size, put into volume ratio concentrated sulphuric acid: in the solution of distilled water=1:20, boil 30 minutes；Then the above-mentioned back glass sheet that boils is put into water-bath 1 hour in 90 DEG C of water-baths；Again by glass substrate sonic oscillation 30 minutes in distilled water；Finally glass substrate obtained above is emitted in glass dish in feeding baking oven and dries for masking.
B. by Cu2SO4·5H2O、Ga(NO3)3·xH2O、CH3CSNH2Put in solvent, make the material in solution uniformly mix.Specifically, can be by 1.66 parts of Cu2SO4·5H2O, 1.71 parts of Ga (NO3)3·xH2O and 1.0 parts of CH3CSNH2Putting in the solvent of 13.3 parts, make the material in solution uniformly mix, wherein solvent is deionized water.
C. make the substrate of solution described in outside uniform application step b, and dry, obtain precursor thin-film sample.Above-mentioned solution can be dripped on the glass substrate that is placed on sol evenning machine, start sol evenning machine and rotate certain time with 300～2500 revs/min, after making the solution on dripping be coated with uniformly, substrate is dried, dry again after again repeating to drip upper previous solu and spin coating, so repeat 3～5 times, obtained certain thickness precursor thin-film sample the most on a glass substrate.
D. step c gained precursor thin-film sample is placed on support, be placed with hydrazine hydrate can hermetic container, make precursor thin-film sample not contact with hydrazine hydrate.The hydrazine hydrate amount of putting into is 4.0 parts.The hermetic container that will be equipped with precursor thin film sample is put in baking oven, is heated between 160～220 DEG C, temperature retention time 5～40 hours, is then cooled to room temperature and takes out.
E. step d gains are soaked 24 hours in deionized water, after carrying out room temperature natural drying, i.e. obtain copper gallium sulfur optoelectronic film.
The present invention need not high temperature high vacuum condition, requires low to instrument and equipment, and production cost is low, and production efficiency is high, it is easy to operation.Gained copper gallium sulfur optoelectronic film has preferable seriality and uniformity, and principal phase is CuGaS2Phase, this new technology is easily controlled composition and the structure of target product, provides a kind of low cost for preparing high performance copper gallium sulfur optoelectronic film, can realize large-scale industrial production.
Detailed description of the invention
Embodiment 1
A. the cleaning of glass substrate: be carried out glass substrate as previously mentioned, substrate size is 20mm × 20mm.
B. by 1.66 parts of Cu2SO4·5H2O, 1.71 parts of Ga (NO3)3·xH2O and 1.0 parts of CH3CSNH2Put in 13.3 parts of deionized waters and uniformly mix, utilize ultrasonic activation more than 30 minutes, make the material in solution uniformly mix.
C. above-mentioned solution is dripped on the glass substrate that is placed on sol evenning machine, start sol evenning machine, sol evenning machine is rotated 5 seconds with 300 revs/min, rotate 15 seconds with 2150 revs/min, after making the solution on dripping be coated with uniformly, after substrate is dried, dry again after again repeating to drip upper previous solu and spin coating, so repeat 3～5 times, obtained certain thickness precursor thin-film sample the most on a glass substrate.
D., the precursor thin-film sample of above-mentioned technique gained being put into sealable container, and puts into 4.0 parts of hydrazine hydrates, precursor thin-film sample is placed on support and makes it not contact with hydrazine hydrate.The hermetic container that will be equipped with precursor thin film sample is put in baking oven, is heated between 160～200 DEG C, temperature retention time 20 hours, is then cooled to room temperature and takes out.
E. step d gains are soaked 24 hours in deionized water, carry out room temperature natural drying, obtain copper gallium sulfur optoelectronic film.
Claims (5)
1. the method being prepared copper gallium sulfur optoelectronic film by copper sulfate, including following steps in sequence:
A. the cleaning of glass substrate；
B. by 1.66 parts of Cu2SO4·5H2O, 1.71 parts of Ga (NO3)3·xH2O and 1.0 parts of CH3CSNH2Put in the solvent of 13.3 parts, make the material in solution uniformly mix；
C. make the substrate of solution described in outside uniform application step b, and dry, obtain precursor thin-film sample；
D. step c gained precursor thin-film sample is placed on support, be placed with hydrazine hydrate can hermetic container, make precursor thin-film sample not contact with hydrazine hydrate；The hermetic container that will be equipped with precursor thin film sample is put in baking oven, is heated between 160～220 DEG C, temperature retention time 5～20 hours, is then cooled to room temperature and takes out；
E. step d gains are soaked in deionized water 24 hours, then carry out room temperature natural drying, obtain copper gallium sulfur optoelectronic film.
A kind of method being prepared copper gallium sulfur optoelectronic film by copper sulfate, it is characterised in that clean described in step a, is to be 20mm × 20mm by glass substrate size, puts into volume ratio concentrated sulphuric acid: in the solution of distilled water=1:20, boil 30 minutes；Then the above-mentioned back glass sheet that boils is put into water-bath 1 hour in 90 DEG C of water-baths；Again by glass substrate sonic oscillation 30 minutes in distilled water；Finally glass substrate obtained above is emitted in glass dish in feeding baking oven and dries for masking.
A kind of method being prepared copper gallium sulfur optoelectronic film by copper sulfate, it is characterised in that the solvent described in step b is deionized water.
A kind of method being prepared copper gallium sulfur optoelectronic film by copper sulfate, it is characterized in that, the substrate of uniform application described in step c, it is to be smeared by sol evenning machine, sol evenning machine is with 300～2500 revs/min of rotations, then, after substrate being dried, the most so repeat 3～5 times, obtained certain thickness precursor thin-film sample.
A kind of method being prepared copper gallium sulfur optoelectronic film by copper sulfate, it is characterised in that put into 4.0 parts of hydrazine hydrates in hermetic container described in step d.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610418998.6A CN106024977A (en) | 2016-06-15 | 2016-06-15 | Method for preparing copper gallium sulfide photoelectric thin film from copper sulfate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610418998.6A CN106024977A (en) | 2016-06-15 | 2016-06-15 | Method for preparing copper gallium sulfide photoelectric thin film from copper sulfate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115612863A (en) * | 2022-08-30 | 2023-01-17 | 中南大学 | Method for separating gallium from alkaline solution |
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2016
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| CN115612863B (en) * | 2022-08-30 | 2024-01-16 | 中南大学 | Method for separating gallium from alkaline solution |
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Application publication date: 20161012 |