CN103972329A - Preparation method of cadmium-free buffer layer of copper indium gallium selenium thin-film solar cell - Google Patents
Preparation method of cadmium-free buffer layer of copper indium gallium selenium thin-film solar cell Download PDFInfo
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- CN103972329A CN103972329A CN201410192004.4A CN201410192004A CN103972329A CN 103972329 A CN103972329 A CN 103972329A CN 201410192004 A CN201410192004 A CN 201410192004A CN 103972329 A CN103972329 A CN 103972329A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000010409 thin film Substances 0.000 title claims abstract description 16
- HVMJUDPAXRRVQO-UHFFFAOYSA-N copper indium Chemical compound [Cu].[In] HVMJUDPAXRRVQO-UHFFFAOYSA-N 0.000 title abstract 3
- QNWMNMIVDYETIG-UHFFFAOYSA-N gallium(ii) selenide Chemical compound [Se]=[Ga] QNWMNMIVDYETIG-UHFFFAOYSA-N 0.000 title abstract 3
- 229910052984 zinc sulfide Inorganic materials 0.000 claims abstract description 57
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 45
- 238000000137 annealing Methods 0.000 claims abstract description 23
- 238000005566 electron beam evaporation Methods 0.000 claims abstract description 20
- 238000001704 evaporation Methods 0.000 claims abstract description 18
- 239000000758 substrate Substances 0.000 claims abstract description 18
- 239000011248 coating agent Substances 0.000 claims abstract description 17
- 238000000576 coating method Methods 0.000 claims abstract description 17
- 230000008020 evaporation Effects 0.000 claims abstract description 17
- 239000010949 copper Substances 0.000 claims abstract description 14
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052802 copper Inorganic materials 0.000 claims abstract description 12
- 239000005083 Zinc sulfide Substances 0.000 claims abstract description 7
- 239000011521 glass Substances 0.000 claims abstract description 7
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 6
- 230000003287 optical effect Effects 0.000 claims abstract description 5
- 229910001873 dinitrogen Inorganic materials 0.000 claims abstract description 3
- 239000010408 film Substances 0.000 claims description 46
- 238000000034 method Methods 0.000 claims description 24
- 229910052757 nitrogen Inorganic materials 0.000 claims description 21
- 238000005245 sintering Methods 0.000 claims description 16
- 229910052793 cadmium Inorganic materials 0.000 claims description 14
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 14
- 238000000151 deposition Methods 0.000 claims description 11
- 230000008021 deposition Effects 0.000 claims description 11
- 229910052711 selenium Inorganic materials 0.000 claims description 7
- 239000011669 selenium Substances 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 3
- 238000005516 engineering process Methods 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- 239000010453 quartz Substances 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims 1
- 238000002834 transmittance Methods 0.000 claims 1
- 238000010894 electron beam technology Methods 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- 238000001228 spectrum Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 229910000928 Yellow copper Inorganic materials 0.000 description 1
- 238000000231 atomic layer deposition Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000224 chemical solution deposition Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 239000010808 liquid waste Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000000411 transmission spectrum Methods 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
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/1828—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof the active layers comprising only AIIBVI compounds, e.g. CdS, ZnS, CdTe
-
- 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
- Y02E10/543—Solar cells from Group II-VI materials
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses a preparation method of a cadmium-free buffer layer of a copper indium gallium selenium thin-film solar cell. The preparation method includes the steps that zinc sulfide powder is kept for 10 s under the pressure of 15 MPa to be compacted into thin cylindrical pieces, wherein the diameter of the thin cylindrical pieces is 1.3 cm, and the thickness of the thin cylindrical pieces is 2 mm; then under the protection of nitrogen gas, the thin cylindrical pieces are sintered at the temperature of 800 DEG C or 1000 DEG C, the thin cylindrical pieces are taken out after the temperature is reduced to the room temperature, the thin cylindrical pieces are placed into a copper crucible of an electron beam evaporation coating system until the two thirds of the copper crucible is filled with the thin cylindrical pieces, electron beam evaporation coating is conducted on a common glass substrate, a ZnS thin film is prepared, and a polycrystalline ZnS buffer layer thin film of a wurtzite structure is prepared by appropriately changing the conditions such as electron beam currents, the beam current scanning range, evaporation high voltage, evaporation pressure, evaporation time, substrate temperature and post-annealing treatment temperature. The thin film has the advantages of being wide in optical band gap, high in visible region transmissivity, high in surface evenness and small in particle diameter and is suitable for being used as a cadmium-free buffer layer thin film of the copper indium gallium selenium thin-film solar cell.
Description
Technical field
The invention belongs to thin-film solar cells critical material technical field, be specifically related to the preparation method of a kind of copper-indium-galliun-selenium film solar cell without cadmium resilient coating.
Background technology
The thin-film solar cells of yellow copper structure is high with its conversion efficiency, band gap is adjustable, steady performance is considered to comparatively desirable electrooptical device, it is Cu (In that this based thin film solar cell typically refers to absorbed layer, Ga) Se2 (CIGS), CuInS2 (CIS) and Cu (In, Ga) (S, Se) solar cell of 2 (CIGSSe), as mainly this class battery of solar spectrum response generally being had to of this sort laminated construction: glass/Mo/CIGS (CZTS)/CdS/i-ZnO/ZnO:Al, need to be at transparency electrode Window layer (transparent conductive oxide, and between absorbed layer, deposit one deck buffer layer thin film TCO), the buffer layer thin film that CdS film the most often adopts, but resilient coating CdS causes it unfavorable to environment because of the existence of heavy metal element Cd, therefore seek environment-friendly type CIGS battery resilient coating and become the focus of this type of battery research in recent years.On the other hand, the optical band gap (2.4 ~ 2.5eV) of CdS is limited in short wavelength range, thereby be difficult to make the performance of battery to reach optimum, this is also one of principal element hindering in recent years the technical development of CIGS thin film solar cell, therefore, seek well behaved most important to the further extensive industrialization of CIGS hull cell without cadmium resilient coating! ZnS film has not only been eliminated the environmental pollution hidden danger existing containing cadmium resilient coating, and band gap length, can there is better coupling with absorbed layer, can widen the response range of battery to solar spectrum, be considered to a kind of material of comparatively desirable alternative CdS buffer layer thin film.Prepare at present copper-indium-galliun-selenium film solar cell a lot of without the method for cadmium resilient coating, mainly there is chemical bath deposition method as main taking chemical bath, other are as less in sputtering method, chemical vapour deposition technique, atomic layer deposition method, evaporation etc., and adopt chemical method to prepare buffer layer thin film, not only introduce the process of liquid waste processing, also increased last handling process.
Summary of the invention
The object of the invention is to propose the preparation method of a kind of copper-indium-galliun-selenium film solar cell without cadmium resilient coating.
The copper-indium-galliun-selenium film solar cell that the present invention proposes, without the preparation method of cadmium resilient coating, is specially:
Taking commercially available chemical pure ZnS powder as raw material, under 15 MPa, keep 10 s to be compacted into thin cylindrical, diameter 1.3 cm, thickness 2 mm, by slice of cylinder under nitrogen protection 800
oc or 1000
oc degree sintering 12 h, treat temperature reduce to room temperature take out, put into electron beam evaporation deposition system with copper crucible, be advisable to be full of 2/3rds of copper crucible, in glass substrate and quartz substrate, carry out respectively electron beam evaporation deposition, preparation ZnS film, background pressure is 5.0 × 10
-3pa~5.0 × 10
-4pa; be room temperature or be heated under the condition of uniform temperature at substrate temperature; controlling electron beam evaporation high pressure is 6 kV or 8 kV gears; sweep current is that X is 0.6 mA; Y is 0 mA; scanning fluctuation range is positive and negative 0.05 mA; when evaporation, pressure is 0.05 Pa ~ 0.1 Pa; electronic beam current is 25 mA ~ 250 mA, and evaporation time is 5 ~ 45 min, obtains zinc sulfide film; film is moved into and in annealing furnace, carries out annealing in process; and carry out, the annealing in process time is 1 ~ 3 h, form the ZnS film with wurtzite structure under nitrogen protection.
Furtherly, after ZnS compacting slice of cylinder sintering, be wurtzite structure, the ZnS film of preparing through electron beam evaporation room temperature is non crystalline structure, after nitrogen protection annealing, is wurtzite structure.
Furtherly, evaporation time substrate temperature is 25
oc.
Furtherly, do not pass into any gas when evaporation, when substrate room temperature, operating pressure is 0.05 Pa.
Furtherly, the ZnS slice of cylinder quantity of sintering is 20 and just can reaches the more than 2/3rds of evaporator crucible.
Furtherly, in the process of ZnS slice of cylinder sintering and the annealing process of ZnS film, the protection of flow of nitrogen gas state, passes into nitrogen while starting to heat up until temperature-fall period drops to 80
obefore the following taking-up of C, close nitrogen.
Furtherly, the protection nitrogen of sintering and annealing process is high pure nitrogen, and purity is 99.999%.
Furtherly, the grain diameter of prepared ZnS film is 13.2 nanometers.
The invention has the beneficial effects as follows: the method prepare without cadmium resilient coating ZnS film, have the advantages that crystal property is good, crystal grain is tiny, surface smoothness is high, and the band gap length of film, the visible region transparency are good, be beneficial to the efficiency that improves solar cell.
Brief description of the drawings
X-ray diffractogram after the prepared ZnS slice of cylinder sintering of Fig. 1.
The X-ray diffractogram without cadmium resilient coating ZnS film that Fig. 2 is prepared.
The SEM photo without cadmium resilient coating ZnS film that Fig. 3 is prepared.
Fig. 4 prepared without cadmium resilient coating ZnS film transmission spectrum curve.
The optical band gap figure without cadmium resilient coating ZnS film that Fig. 5 is prepared.
Embodiment
Further describe the present invention below by specific embodiment:
Embodiment 1 taking commercially available chemical pure ZnS powder as raw material, keeps 10 s to be compacted into thin cylindrical under 15 MPa, diameter 1.3 cm, thickness 2 mm, by slice of cylinder under nitrogen protection 800
oc and 1000
oc degree sintering 12 h take out after temperature is reduced to room temperature, put into electron beam evaporation deposition system with copper crucible, be advisable to be full of 2/3rds of copper crucible, on simple glass substrate, carry out electron beam evaporation deposition, preparation ZnS film, background pressure is 5.0 × 10
-4pa, under the condition that is room temperature at substrate temperature, controlling electron beam evaporation high pressure is 6 kV gears, and sweep current is that X is 0.6 mA, and Y is 0 mA, scanning fluctuation range is positive and negative 0.05 mA, when evaporation, pressure is 0.05 Pa, and electronic beam current is 25 mA, and evaporation time is 5 min, obtain zinc sulfide film, film is moved in annealing furnace and carries out 400
oc annealing in process, and carry out under nitrogen protection, the annealing in process time is 3 h, forms the ZnS film with wurtzite structure.Fig. 1 is the X-ray diffractogram of the ZnS slice of cylinder after sintering.
Embodiment 2 taking commercially available chemical pure ZnS powder as raw material, keeps 10 s to be compacted into thin cylindrical under 15 MPa, diameter 1.3 cm, thickness 2 mm, by slice of cylinder under nitrogen protection 1000
oc degree sintering 12 h take out after temperature is reduced to room temperature, put into electron beam evaporation deposition system with copper crucible, be advisable to be full of 2/3rds of copper crucible, on simple glass substrate, carry out electron beam evaporation deposition, preparation ZnS film, background pressure is 5.0 × 10
-4pa, under the condition that is room temperature at substrate temperature, controlling electron beam evaporation high pressure is 6 kV gears, and sweep current is that X is 0.6 mA, and Y is 0 mA, scanning fluctuation range is positive and negative 0.05 mA, when evaporation, pressure is 0.1 Pa, and electronic beam current is 25 mA, and evaporation time is 15 min, obtain zinc sulfide film, film is moved in annealing furnace and carries out 400
oc annealing in process, and carry out under nitrogen protection, the annealing in process time is 3 h, forms the ZnS film with wurtzite structure.Fig. 2 is that prepared ZnS film is in unannealed and 400
oxRD figure after C annealing relatively.
Embodiment 3 taking commercially available chemical pure ZnS powder as raw material, keeps 10 s to be compacted into thin cylindrical under 15 MPa, diameter 1.3 cm, thickness 2 mm, by slice of cylinder under nitrogen protection 1000
oc degree sintering 12 h take out after temperature is reduced to room temperature, put into electron beam evaporation deposition system with copper crucible, be advisable to be full of 2/3rds of copper crucible, on simple glass substrate, carry out electron beam evaporation deposition, preparation ZnS film, background pressure is 5.0 × 10
-4pa, under the condition that is room temperature at substrate temperature, controlling electron beam evaporation high pressure is 6 kV gears, and sweep current is that X is 0.6 mA, and Y is 0 mA, scanning fluctuation range is positive and negative 0.05 mA, when evaporation, pressure is 0.1 Pa, and electronic beam current is 50 mA, and evaporation time is 5 min, obtain zinc sulfide film, film is moved in annealing furnace and carries out 600
oc annealing in process, and carry out under nitrogen protection, the annealing in process time is 3 h, forms the ZnS film with wurtzite structure.Fig. 3 is the SEM figure of prepared ZnS film, and Fig. 4 and Fig. 5 are respectively transmissivity spectrum and the optical band gap figure of prepared film.
Claims (8)
1. a copper-indium-galliun-selenium film solar cell is without the preparation method of cadmium resilient coating, this is zinc sulfide film without cadmium buffer layer thin film material, prepared by nitrogen protective sintering and the combination of electron beam evaporation deposition technology, wherein film thickness is that 30 ~ 500 nm are adjustable, there is wurtzite structure, the optical band gap width of film is 3.75 eV, the average transmittance of visible region is higher than 60%, concrete preparation process is as follows: taking commercially available chemical pure ZnS powder as raw material, under 15 MPa, keep 10 s to be compacted into thin cylindrical, diameter 1.3 cm, thickness 2 mm, by slice of cylinder under nitrogen protection 800
oc or 1000
oc degree sintering 12 h, treat temperature reduce to room temperature take out, put into electron beam evaporation deposition system with copper crucible, be advisable to be full of 2/3rds of copper crucible, in glass substrate and quartz substrate, carry out respectively electron beam evaporation deposition, preparation ZnS film, background pressure is 5.0 × 10
-3pa~5.0 × 10
-4pa, be room temperature or be heated under the condition of uniform temperature at substrate temperature, controlling electron beam evaporation high pressure is 6 kV or 8 kV gears, sweep current is that X is 0.6 mA, Y is 0 mA, scanning fluctuation range is positive and negative 0.05 mA, when evaporation, pressure is 0.05 Pa ~ 0.1 Pa, electronic beam current is 25 mA ~ 250 mA, and evaporation time is 5 ~ 45 min, obtains zinc sulfide film, film is moved into and in annealing furnace, carries out annealing in process, and carry out, the annealing in process time is 1 ~ 3 h, form the ZnS film with wurtzite structure under nitrogen protection.
2. preparation method according to claim 1, is characterized in that being wurtzite structure after ZnS compacting slice of cylinder sintering, and the ZnS film of preparing through electron beam evaporation room temperature is non crystalline structure, after nitrogen protection annealing, is wurtzite structure.
3. preparation method according to claim 1, it is characterized in that evaporating time substrate temperature is 25
oc.
4. preparation method according to claim 1, does not pass into any gas while it is characterized in that evaporation, when substrate room temperature, operating pressure is 0.05 Pa.
5. preparation method according to claim 1, the ZnS slice of cylinder quantity that it is characterized in that sintering is 20 just can reach the more than 2/3rds of evaporator crucible.
6. preparation method according to claim 1, is characterized in that in the process of ZnS slice of cylinder sintering and the annealing process of ZnS film, and the protection of flow of nitrogen gas state, passes into nitrogen while starting to heat up until temperature-fall period drops to 80
obefore the following taking-up of C, close nitrogen.
7. preparation method according to claim 1, the protection nitrogen that it is characterized in that sintering and annealing process is high pure nitrogen, purity is 99.999%.
8. preparation method according to claim 1, the grain diameter that it is characterized in that prepared ZnS film is 13.2 nanometers.
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CN201410192004.4A CN103972329B (en) | 2014-05-07 | 2014-05-07 | A kind of copper-indium-galliun-selenium film solar cell is without the preparation method of cadmium resilient coating |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110047948A (en) * | 2019-03-04 | 2019-07-23 | 杭州电子科技大学 | A kind of copper-indium-galliun-selenium film solar cell is without cadmium buffer layer thin film and preparation method |
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CN101330112A (en) * | 2007-06-20 | 2008-12-24 | 济南荣达电子有限公司 | Flexible substrate film solar battery and dedicated device |
CN102254998A (en) * | 2011-07-18 | 2011-11-23 | 中国科学院深圳先进技术研究院 | Cadmium-free CuInGaSe thin film solar cell assembly and preparing method of zinc sulfide buffer layer thin film thereof |
CN102270699A (en) * | 2011-07-18 | 2011-12-07 | 中国科学院深圳先进技术研究院 | Preparation methods of CIGS (Cu (In, Ga) Se2)-free thin film solar cell and zinc sulfide buffer layer |
CN102337516A (en) * | 2011-09-29 | 2012-02-01 | 中国建材国际工程集团有限公司 | Deposition method for buffer layer of cadmium-free copper-indium-gallium-selenium thin film solar cell |
CN103560169A (en) * | 2013-10-25 | 2014-02-05 | 济南晶力新能源科技有限公司 | Large solar thin film battery piece assembly production process and equipment |
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2014
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Patent Citations (5)
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CN101330112A (en) * | 2007-06-20 | 2008-12-24 | 济南荣达电子有限公司 | Flexible substrate film solar battery and dedicated device |
CN102254998A (en) * | 2011-07-18 | 2011-11-23 | 中国科学院深圳先进技术研究院 | Cadmium-free CuInGaSe thin film solar cell assembly and preparing method of zinc sulfide buffer layer thin film thereof |
CN102270699A (en) * | 2011-07-18 | 2011-12-07 | 中国科学院深圳先进技术研究院 | Preparation methods of CIGS (Cu (In, Ga) Se2)-free thin film solar cell and zinc sulfide buffer layer |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110047948A (en) * | 2019-03-04 | 2019-07-23 | 杭州电子科技大学 | A kind of copper-indium-galliun-selenium film solar cell is without cadmium buffer layer thin film and preparation method |
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