CN105870255A - Method for preparing CIGS thin-film solar cell absorption layer employing co-sputtering method - Google Patents
Method for preparing CIGS thin-film solar cell absorption layer employing co-sputtering method Download PDFInfo
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- CN105870255A CN105870255A CN201610270066.1A CN201610270066A CN105870255A CN 105870255 A CN105870255 A CN 105870255A CN 201610270066 A CN201610270066 A CN 201610270066A CN 105870255 A CN105870255 A CN 105870255A
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- 238000000034 method Methods 0.000 title claims abstract description 42
- 238000004544 sputter deposition Methods 0.000 title claims abstract description 31
- 239000010409 thin film Substances 0.000 title claims abstract description 27
- 238000010521 absorption reaction Methods 0.000 title abstract description 6
- 229910052738 indium Inorganic materials 0.000 claims abstract description 20
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000758 substrate Substances 0.000 claims abstract description 13
- 239000011669 selenium Substances 0.000 claims description 11
- 238000010792 warming Methods 0.000 claims description 10
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 8
- 229910052711 selenium Inorganic materials 0.000 claims description 6
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 5
- 229910052750 molybdenum Inorganic materials 0.000 claims description 5
- 239000011733 molybdenum Substances 0.000 claims description 5
- 238000007747 plating Methods 0.000 claims description 5
- 239000005361 soda-lime glass Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 5
- 238000000137 annealing Methods 0.000 abstract description 3
- 238000013459 approach Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- KTSFMFGEAAANTF-UHFFFAOYSA-N [Cu].[Se].[Se].[In] Chemical compound [Cu].[Se].[Se].[In] KTSFMFGEAAANTF-UHFFFAOYSA-N 0.000 abstract 3
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 10
- 239000010949 copper Substances 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 238000012876 topography Methods 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910052774 Proactinium Inorganic materials 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000009466 transformation Effects 0.000 description 3
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 229910052733 gallium Inorganic materials 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 206010054949 Metaplasia Diseases 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000000224 chemical solution deposition Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/032—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
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- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Electromagnetism (AREA)
- General Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Photovoltaic Devices (AREA)
Abstract
The invention belongs to a method for preparing a CIGS thin-film solar cell absorption layer employing a co-sputtering method. The method comprises the steps as follows: (1) a substrate is provided, radio-frequency sputtering is carried out by a copper indium gallium selenide target, meanwhile, DC sputtering is carried out by an indium target and a copper indium gallium selenide preformed layer is prepared in a co-sputtering manner; and (2) the copper indium gallium selenide preformed layer is put into a quick annealing furnace, is selenized under nitrogen protection for twice and is naturally cooled to a room temperature to obtain the CIGS thin-film solar cell absorption layer. By a technological approach of carrying out sputtering by a standard CIGS quaternary target, large-scale industrial production is facilitated; the loss of an indium element caused by the standard CIGS quaternary target in the sputtering process can be effectively avoided through the method; and a CIGS absorption layer material in accordance with the stoichiometric ratio can be obtained. Annealing treatment is carried out on the prepared CIGS absorption layer through a two-step heating method; the selenylation completeness and crystallinity can be further strengthened; and the high-quality CIGS with a uniform surface and a consistent thickness can be obtained.
Description
Technical field
The invention belongs to photoelectric functional material and film photovoltaic device field, be specifically related to a kind of method that cosputtering method prepares CIGS thin film solar battery obsorbing layer.
Background technology
First of 21 century 10 years, along with people recognize the raising day by day constantly deepened and to environmental consciousness to traditional fossil energy day by day exhaustion, the development of new forms of energy enters fast traffic lane.Various new forms of energy science and technology move towards industry application from laboratory research, gradually change the mode of production and life of people.Prelude has slowly been pulled open in one Industrial Revolution with new forms of energy as foundation stone.The research development in recent years of thin-film solar cells is rapid, become most active direction in area of solar cell, and wherein CIGS is the most noticeable, it is that solar cell material system can be taken into account high efficiency and low cost, best and the most real system simultaneously.The light absorbing zone of copper-indium-galliun-selenium film solar cell is made up of the copper-based conductors material of low cost, and its absorbing ability is much stronger than crystalline silicon, and it is up to micron dimension in solar spectrum district optical absorption depth.
In many technology preparing CIGS absorbed layer, magnetron sputtering method is prepared CIGS thin film solar cell and is easily realized large-scale production, the easiest preparation method is directly to sputter CIGS quaternary target, but be not quite similar due to the sputter rate of four kinds of elements in sputter procedure, the especially sputtering yield of phosphide element is relatively low, and the original scale of prepared CIGS absorbed layer stoichiometric proportion and target can be caused to there is bigger deviation.
Summary of the invention
It is an object of the invention to provide a kind of simple, convenient, can the cosputtering method of the large-scale industrial production method of preparing CIGS thin film solar battery obsorbing layer.
For achieving the above object, the technical solution used in the present invention is, a kind of method that cosputtering method prepares CIGS thin film solar battery obsorbing layer, comprise the following steps: 1. substrate is provided, CIGS target is used to carry out radio-frequency sputtering, using indium target to carry out d.c. sputtering, cosputtering prepares CIGS preformed layer simultaneously；The process conditions of cosputtering are: body vacuum reaches 7 ~ 8 × 10-4Below Pa, operating pressure is 0.5 ~ 0.6 Pa, and the cosputtering time is 110-120 min, and the radio-frequency sputtering power of CIGS target is 110 W, and the power of indium target d.c. sputtering is 70 W；2. CIGS preformed layer is put in quick anneal oven; it is warming up to 245 ~ 255 DEG C in the lower 80 ~ 90s of nitrogen protection; then solid selenium source selenizing 20 ~ 30 min at 245 ~ 255 DEG C is used; then in 20 ~ 30s, it is warming up to 545 ~ 500 DEG C; secondary selenizing 15 ~ 20 min at 545 ~ 500 DEG C; naturally cool to room temperature, i.e. can get CIGS(CIGS) absorbing layer of thin film solar cell.
Preferably, step 1. in CIGS target used use CIGS standard quaternary target, atomic number ratio is for Cu:In:Ga:Se=1:0.7:0.3:2, and the purity of indium target is 99.99%.
Preferably, step 1. in substrate used be the soda-lime glass substrate of plating molybdenum.
The beneficial effect comprise that: the present invention utilizes the method for cosputtering (while radio-frequency power supply sputtering CIGS standard quaternary target, synchronize to utilize DC source sputtering indium target to carry out supplementing of phosphide element), the loss of the phosphide element that standard CIGS quaternary target causes in sputter procedure can be efficiently solved by the present invention, can obtain meeting the CIGS absorbed layer material of stoichiometric proportion.Being made annealing treatment prepared CIGS absorbed layer by two step temperature-raising methods, can further enhance degree completely and the crystallinity of its selenizing, available surface is uniform, consistency of thickness, chemical constituent meet the high-quality CIGS measuring ratio.After prepared high-quality CIGS absorbed layer material composition complete membrane photovoltaic device, its efficiency is more than 10%, and the technological approaches that the present invention uses CIGS standard quaternary target to carry out sputtering simultaneously is conducive to technical scale metaplasia to produce.
Accompanying drawing explanation
Fig. 1 is the surface topography map of the CIGS preformed layer of embodiment 1 preparation, and surfacing is fine and close；
Fig. 2 is the cross section structure figure of the CIGS preformed layer of embodiment 1 preparation, and thickness is homogeneous；
Fig. 3 is the surface topography map of the CIGS thin film solar battery obsorbing layer of embodiment 1 preparation, surface compact；
Fig. 4 is the cross section structure figure of the CIGS thin film solar battery obsorbing layer of embodiment 1 preparation, has preferable degree of crystallinity；
Fig. 5 is the photoelectric transformation efficiency test result figure of the complete photovoltaic device that embodiment 1 is made.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described, but protection scope of the present invention is not limited to this.
Embodiment 1
A kind of method that cosputtering method prepares CIGS thin film solar battery obsorbing layer, comprise the following steps: 1. the soda-lime glass substrate of plating molybdenum is provided, using CIGS target to carry out radio-frequency sputtering, use indium target to carry out d.c. sputtering simultaneously, cosputtering prepares CIGS preformed layer；The process conditions of cosputtering are: body vacuum reaches 8 × 10-4Below Pa, in sputter procedure, target spacing is for remaining 8 cm, argon flow amount is 20 sccm, and substrate rotating speed is 20 r/min, and operating pressure is 0.5Pa, the cosputtering time is 120 min, and the radio-frequency sputtering power of CIGS target is 110 W, and the power of indium target d.c. sputtering is 70 W；2. CIGS preformed layer is put in quick anneal oven; it is warming up to 250 DEG C in the lower 90s of nitrogen protection; then solid selenium source (selenium powder) selenizing 20 min at 250 DEG C is used; then in 30s, it is warming up to 500 DEG C; secondary selenizing 15 min at 500 DEG C; naturally cool to room temperature, i.e. can get CIGS thin film solar battery obsorbing layer.
Step 1. in the atomic number ratio of CIGS target used for Cu:In:Ga:Se=1:0.7:0.3:2, the purity of indium target is 99.99%.
Chemical bath deposition method is used to prepare the thick CdS cushion of 60 nm on CIGS thin film solar battery obsorbing layer embodiment 1 prepared, recycling magnetron sputtering method sputters intrinsic ZnO and ITO successively, vacuum vapour deposition is finally used to construct Ag electrode, assemble out complete CIGS thin film solar cell device (these methods are all prior aries, do not repeat them here).
Embodiment 1 preparation copper and indium gallium preformed layer surface topography map as it is shown in figure 1, embodiment 1 preparation copper and indium gallium preformed layer cross section structure figure as in figure 2 it is shown, by Fig. 1-2 it can be seen that preparation CuInGa alloy preformed layer surface texture uniform sequential；The surface topography map of the CIGS thin film solar battery obsorbing layer of embodiment 1 preparation is as shown in Figure 3, the cross section structure figure of the CIGS thin film solar battery obsorbing layer of embodiment 1 preparation is as shown in Figure 4, be can be seen that by Fig. 3-4, the plane densification of the CIGS thin film solar battery obsorbing layer after selenization is smooth, and the big crystal grain good from micron-size crystalline seen from Cross Section Morphology exists；Photoelectric transformation efficiency test result Fig. 5 of the complete photovoltaic device that embodiment 1 is made, from fig. 5, it can be seen thatJ-VTest result shows that prepared CIGS absorbed layer has higher photoelectric transformation efficiency, and its efficiency is higher than 10%.
Embodiment 2
A kind of method that cosputtering method prepares CIGS thin film solar battery obsorbing layer, comprise the following steps: 1. the soda-lime glass substrate of plating molybdenum is provided, using CIGS target to carry out radio-frequency sputtering, use indium target to carry out d.c. sputtering simultaneously, cosputtering prepares CIGS preformed layer；The process conditions of cosputtering are: body vacuum reaches 7 × 10-4Below Pa, in sputter procedure, target spacing is for remaining 8 cm, argon flow amount is 20 sccm, and substrate rotating speed is 20 r/min, and operating pressure is 0.5Pa, the cosputtering time is 120 min, and the radio-frequency sputtering power of CIGS target is 110 W, and the power of indium target d.c. sputtering is 70 W；2. CIGS preformed layer is put in quick anneal oven; it is warming up to 245 DEG C in the lower 90s of nitrogen protection; then solid selenium source (selenium powder) selenizing 30 min at 245 DEG C is used; then in 20s, it is warming up to 545 DEG C; secondary selenizing 20 min at 545 DEG C; naturally cool to room temperature, i.e. can get CIGS thin film solar battery obsorbing layer.
Step 1. in the atomic number ratio of CIGS target used for Cu:In:Ga:Se=1:0.7:0.3:2, the purity of indium target is 99.99%.
Embodiment 3
A kind of method that cosputtering method prepares CIGS thin film solar battery obsorbing layer, comprise the following steps: 1. the soda-lime glass substrate of plating molybdenum is provided, using CIGS target to carry out radio-frequency sputtering, use indium target to carry out d.c. sputtering simultaneously, cosputtering prepares CIGS preformed layer；The process conditions of cosputtering are: body vacuum reaches 8 × 10-4Below Pa, in sputter procedure, target spacing is for remaining 8 cm, argon flow amount is 20 sccm, and substrate rotating speed is 20 r/min, and operating pressure is 0.5Pa, the cosputtering time is 120 min, and the radio-frequency sputtering power of CIGS target is 110 W, and the power of indium target d.c. sputtering is 70 W；2. CIGS preformed layer is put in quick anneal oven; it is warming up to 255 DEG C in the lower 90s of nitrogen protection; then solid selenium source (selenium powder) selenizing 30 min at 255 DEG C is used; then in 30s, it is warming up to 500 DEG C; secondary selenizing 15 min at 500 DEG C; naturally cool to room temperature, i.e. can get CIGS thin film solar battery obsorbing layer.
Step 1. in the atomic number ratio of CIGS target used for Cu:In:Ga:Se=1:0.7:0.3:2, the purity of indium target is 99.99%.
Claims (3)
1. the method that a cosputtering method prepares CIGS thin film solar battery obsorbing layer, it is characterized in that, comprise the following steps: 1. substrate is provided, use CIGS target to carry out radio-frequency sputtering, using indium target to carry out d.c. sputtering, cosputtering prepares CIGS preformed layer simultaneously；The process conditions of cosputtering are: body vacuum reaches 7 ~ 8 × 10-4Below Pa, operating pressure is 0.5 ~ 0.6 Pa, and the cosputtering time is 110-120 min, and the radio-frequency sputtering power of CIGS target is 110 W, and the power of indium target d.c. sputtering is 70 W；2. CIGS preformed layer is put in quick anneal oven, 245 ~ 255 DEG C it are warming up in 80 ~ 90s, then solid selenium source selenizing 20 ~ 30 min at 245 ~ 255 DEG C is used, then in 20 ~ 30s, it is warming up to 545 ~ 500 DEG C, secondary selenizing 15 ~ 20 min at 545 ~ 500 DEG C, naturally cool to room temperature, i.e. can get CIGS thin film solar battery obsorbing layer.
2. the method that cosputtering method as claimed in claim 2 prepares CIGS thin film solar battery obsorbing layer, it is characterised in that: step 1. in the atomic number ratio of CIGS target used for Cu:In:Ga:Se=1:0.7:0.3:2, the purity of indium target is 99.99%.
3. the method that cosputtering method as claimed in claim 1 prepares CIGS thin film solar battery obsorbing layer, it is characterised in that: step 1. in substrate used be the soda-lime glass substrate of plating molybdenum.
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| CN201610270066.1A CN105870255B (en) | 2016-04-27 | 2016-04-27 | A kind of method that cosputtering method prepares CIGS thin film solar battery obsorbing layer |
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| CN201610270066.1A CN105870255B (en) | 2016-04-27 | 2016-04-27 | A kind of method that cosputtering method prepares CIGS thin film solar battery obsorbing layer |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050028861A1 (en) * | 2002-02-14 | 2005-02-10 | Honda Giken Kogyo Kabushiki Kaisha | Light absorbing layer producing method |
| CN102154622A (en) * | 2010-12-06 | 2011-08-17 | 电子科技大学 | Method for preparing copper-indium-gallium-selenium thin film serving as light absorbing layer of solar cell |
| CN104810417A (en) * | 2015-04-28 | 2015-07-29 | 清华大学 | Light absorbing layer and preparation method thereof of thin-film solar battery |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050028861A1 (en) * | 2002-02-14 | 2005-02-10 | Honda Giken Kogyo Kabushiki Kaisha | Light absorbing layer producing method |
| CN102154622A (en) * | 2010-12-06 | 2011-08-17 | 电子科技大学 | Method for preparing copper-indium-gallium-selenium thin film serving as light absorbing layer of solar cell |
| CN104810417A (en) * | 2015-04-28 | 2015-07-29 | 清华大学 | Light absorbing layer and preparation method thereof of thin-film solar battery |
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