CN103996609A - Preparation method of magnetron sputtering CdTe polycrystalline film solar cell - Google Patents
Preparation method of magnetron sputtering CdTe polycrystalline film solar cell Download PDFInfo
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- CN103996609A CN103996609A CN201310053822.1A CN201310053822A CN103996609A CN 103996609 A CN103996609 A CN 103996609A CN 201310053822 A CN201310053822 A CN 201310053822A CN 103996609 A CN103996609 A CN 103996609A
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- 238000001755 magnetron sputter deposition Methods 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 39
- 229910004613 CdTe Inorganic materials 0.000 title claims abstract description 14
- 239000000758 substrate Substances 0.000 claims abstract description 147
- 238000010438 heat treatment Methods 0.000 claims abstract description 30
- 238000000137 annealing Methods 0.000 claims abstract description 12
- 238000001704 evaporation Methods 0.000 claims abstract description 10
- 230000008020 evaporation Effects 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims description 44
- 239000000523 sample Substances 0.000 claims description 12
- 238000004873 anchoring Methods 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 5
- 238000012546 transfer Methods 0.000 claims description 2
- 238000004544 sputter deposition Methods 0.000 abstract description 20
- 238000012545 processing Methods 0.000 abstract description 6
- 238000010792 warming Methods 0.000 abstract description 3
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 abstract 2
- 239000010408 film Substances 0.000 description 184
- MARUHZGHZWCEQU-UHFFFAOYSA-N 5-phenyl-2h-tetrazole Chemical compound C1=CC=CC=C1C1=NNN=N1 MARUHZGHZWCEQU-UHFFFAOYSA-N 0.000 description 132
- 239000007789 gas Substances 0.000 description 30
- 210000004027 cell Anatomy 0.000 description 23
- 230000009466 transformation Effects 0.000 description 11
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 10
- 229910021389 graphene Inorganic materials 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 238000005259 measurement Methods 0.000 description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical class OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 238000005229 chemical vapour deposition Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000011521 glass Substances 0.000 description 5
- 238000002207 thermal evaporation Methods 0.000 description 5
- 239000004020 conductor Substances 0.000 description 4
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 4
- 239000010445 mica Substances 0.000 description 4
- 229910052618 mica group Inorganic materials 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000005566 electron beam evaporation Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000005240 physical vapour deposition Methods 0.000 description 3
- 238000007747 plating Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 238000004070 electrodeposition Methods 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 210000002381 plasma Anatomy 0.000 description 2
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 2
- 239000004926 polymethyl methacrylate Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002061 vacuum sublimation 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
- H01L31/0248—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
- H01L31/0296—Inorganic materials including, apart from doping material or other impurities, only AIIBVI compounds, e.g. CdS, ZnS, HgCdTe
-
- 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
- H01L31/04—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 adapted as photovoltaic [PV] conversion devices
- H01L31/06—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 adapted as photovoltaic [PV] conversion devices characterised by at least one potential-jump barrier or surface barrier
- H01L31/072—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 adapted as photovoltaic [PV] conversion devices characterised by at least one potential-jump barrier or surface barrier the potential barriers being only of the PN heterojunction type
- H01L31/073—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 adapted as photovoltaic [PV] conversion devices characterised by at least one potential-jump barrier or surface barrier the potential barriers being only of the PN heterojunction type comprising only AIIBVI compound semiconductors, e.g. CdS/CdTe solar cells
-
- 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
- H01L31/1836—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 comprising a growth substrate not being an AIIBVI compound
-
- 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 relates to a preparation method of a magnetron sputtering CdTe polycrystalline film solar cell. The preparation method is characterized in that: a CdS polycrystalline film grows on a transparent conductive polycrystalline film of a substrate and heating is stopped, temperature reduction and re-warning processing, or heating keeping processing, or re-warming and re-temperature reducing processing is carried out on the CdS polycrystalline film that has finished growing on the vacuum condition, and then CdTe polycrystalline film sputtering is carried out on the prepared CdS polycrystalline film; annealing treatment is carried out on the prepared CdS polycrystalline film and the CdTe polycrystalline film in a CdCl2 atmosphere; and conductive back electrode evaporation is carried out on the CdTe polycrystalline film that has been processed by annealing.
Description
Technical field
The present invention relates to a kind of CdTe polycrystalline polycrystal film battery and preparation method thereof.
Background technology
Cadmium telluride (CdTe) is group Ⅱ-Ⅵ compound semiconductor, is a kind of very desirable solar battery obsorbing layer material.CdTe is direct gap semiconductor, and its room temperature band gap width is 1.45eV, and its spectral response is mated with solar spectrum very much.CdTe absorption coefficient is greater than 5 × 10
5/ cm, in sunlight, approximately 99% energy can absorb higher than the photon of its energy gap in the thick absorbed layer of approximately 2 μ m, has greatly saved the demand to material.The thickness of CdTe polycrystal film solar cell is only 1/100 of silicon solar cell thickness, has reduced material cost and the cost of manufacture of solar cell.At present, the manufacturing cost of the commercial rollout CdTe polycrystal film solar module of batch production has dropped to 0.75 dollar/peak watt, be that in present various solar module, cost of manufacture is minimum, become one of main study subject in photovoltaic industry.CdTe polycrystal film solar cell is heterojunction solar battery, and heterojunction is made up of n-CdS/p-CdTe conventionally.Conventionally CdS is prepared by chemical bath method (CBD), and CdTe preparation method is varied, there are near space sublimed method (CSS), electro-deposition (ED) method, physical vapour deposition (PVD) (PVD) method, chemical vapour deposition (CVD) (CVD) method, CBD, silk screen printing sintering process, vacuum magnetic-control sputtering method, Vacuum sublimation etc.It is a kind of preparation method of low temperature that magnetron sputtering method is compared conventional CSS method.Magnetron sputtering apparatus is easy to popularize, the technical parameter that can regulate in growth polycrystal film process is many, the flow of such as gas, grow air pressure, base reservoir temperature, plasma density, target-substrate distance, Distribution of Magnetic Field etc., thus these all can be used for the transformation efficiency of the quality raising CdTe solar cell that improves CdTe polycrystal film.CdTe polycrystal film solar cell thoroughly on glass at height, to have prepared transformation efficiency under the low temperature of 250 DEG C be 14%.Magnetron sputtering apparatus is general, stable, preparation temperature is low, film thickness controllability is good, is well suited for preparing ultra-thin CdTe polycrystal film solar cell.At present, utilizing CdTe absorber thickness prepared by magnetron sputtering is the CdTe polycrystal film solar cell of 0.25 μ m, and transformation efficiency has reached 8%.And, utilize magnetron sputtering method can in same chamber, complete the preparation of CdS and CdTe simultaneously.In magnetron sputtering, prepare after CdS polycrystal film, then, under the condition of not fail temperature and vacuum, can on CdS polycrystal film surface, prepare CdTe polycrystal film at once.At present, in magnetron sputtering C dTe polycrystal film solar cell, conventionally in preparation CdS process, pass into certain oxygen ([1] A.Gupta, K.Allada, S.H.Lee, and A.D.Compaan, " Oxygenated CdS Window Layer for Sputtered CdS/CdTe Solar Cells, " in Materials Research Societ Symposium Proceedings, 2003, vol.763, pp.341-346.[2] X.Wu, Y.Van, R.G.Dhere, Y.Zhang, J.Zhou, C.Perkins, and B.To, " Nanostructured CdS:0 flm:preparation, properties, and application, " physica status solidi (c), vol.1, no.4, pp.1062-1066, 2004.), or after the CdS that grown, CdS polycrystal film is carried out to CdCl
2process (Lee, Jae-Hyeong, Lee, Dong-Jin, Effects of CdCl
2treatment on the properties of CdS films prepared by r.f.magnetron sputtering, THIN SOLID FILMS, volume: 515 phases: 15 pages: 6055-6059 DOI:10.1016/j.tsf.2006.12.069 imp d: MAY 31 2007), increase the band gap of CdS, reduce the absorption of CdS to light, reach the object that increases short-circuit current density.But, CdS is carried out to CdCl
2process surface C dCl
2particle is not easy to remove, and has increased complexity and the uncontrollability of technique.Pass into oxygen in growth in CdS, although can increase short-circuit current density, open circuit voltage and transformation efficiency be not significantly improved (Kephart, J.M.; Geisthardt, R.; Sampath, W.S.Photovoltaic Specialists Conference (PVSC), 2012 38th IEEE Topic (s): Components, Circuits, Devices & Systems; Engineered Materials, Dielectrics & Plasmas; Photonics & Electro-Optics; Power, Energy, & Industry Applications Digital Object Identifier:10.1109/PVSC.2012.6317737 Publication Year:2012, Page (s): 000854-000858).
Magnetron sputtering is prepared in CdTe polycrystal film process, can be by changing preparation condition, such as applying substrate bias, Chinese patent 201210265539.0 has proposed a kind of method of the CdTe of preparation polycrystal film, it is by preparing at magnetron sputtering in CdTe polycrystal film process, substrate is applied to bias voltage, improved the transformation efficiency of CdTe polycrystal film solar cell.But, in magnetron sputtering C dTe polycrystal film solar cell process, prepared CdS in same chamber after, in the situation that not destroying vacuum and temperature, at CdS superficial growth CdTe polycrystal film, do not anneal through the cooling of CdS polycrystal film at once, or insulating process.
Summary of the invention
The object of the invention is to overcome existing magnetron sputtering prepares the CdS that CdTe polycrystalline solar cell method exists and carries out CdCl
2after processing, be difficult for removing surperficial CdCl
2, or pass into oxygen when magnetron sputtering C dS, and can not obviously increase the deficiency of the open circuit voltage of battery, a kind of new preparation method is proposed.The present invention is lowered the temperature, is heated up by the CdS polycrystal film to after having grown or keeps heating or the cooling that heats up again, carry out the growth of CdTe polycrystal film on CdS polycrystal film surface more afterwards, can greatly improve the junction characteristic of PN junction, obviously improve transformation efficiency and the open circuit voltage of CdTe polycrystal film solar cell.
The inventive method sequence of process steps is as follows:
1, place and on the position of substrate, place the substrate with transparent conductive film at magnetron sputtering stove, the probe of the anchoring base by conduction, makes the transparent conductive film of substrate be connected with applied voltage equipment.Then close the vacuum chamber of magnetron sputtering stove, to vacuumizing in vacuum chamber, and substrate is heated;
2, when back end vacuum arrives 10
-3below Pa, base reservoir temperature reaches 25 DEG C-1100 DEG C, starts sputter CdS polycrystal film in the substrate with transparent conductive film; In the time that the thickness of CdS polycrystal film arrives the thickness of setting, CdS film stops growing.Then the CdS polycrystal film of having grown is kept to 1min-72h under 25 DEG C of-1100 DEG C of temperature ranges, or stop, to substrate heating, making CdS polycrystal film cool to room temperature, then at room temperature keep 0-72h.Afterwards, the position transfer of substrate is arrived to the just position to CdTe target, start radio-frequency power supply and start sputter CdTe polycrystal film, substrate is applied to bias voltage+8.8V--100V.When the thickness of CdTe polycrystal film reaches default thickness, close additional power source and stop the bias voltage to substrate, close radio-frequency power supply simultaneously, stop the growth of CdTe polycrystal film, stop substrate heating.The substrate of CdS polycrystal film and CdTe polycrystal film of having made to grow is cooling with stove.Then take out the substrate of grown CdS polycrystal film and CdTe polycrystal film;
3, the CdS being prepared by step 2 and CdTe polycrystal film carry out CdCl
2annealing in process;
4, through CdCl
2evaporation conduction back electrode on CdTe polycrystal film after annealing in process; Electric conducting material is this professional domain material known by the technical staff, as Au, Ni, Mo, Al, Mg, Graphene etc.The method of evaporation electric conducting material is this professional domain method known by the technical staff, such as: thermal evaporation, electron beam, CVD etc.
In described step 1, place on the position of substrate and put the substrate with transparent conductive film at magnetron sputtering stove, the probe of the anchoring base by conduction, makes substrate transparent conductive film be connected with applied voltage equipment.By the conductivity between universal instrument measurement additional equipment and substrate conductive film, to guarantee that the two can conducting.Close magnetron sputtering vacuum chamber, to vacuumizing in chamber, substrate is heated simultaneously.The temperature of substrate heating is 25 DEG C to 1100 DEG C.
The method of operation of described step 2 is: when the back end vacuum of magnetron sputtering chamber chamber arrives 10
-3below Pa, start sputter CdS polycrystal film.The sputtering condition of CdS polycrystal film is: 25 DEG C-1100 DEG C of base reservoir temperatures, pass into high-purity Ar gas, gas flow rate 5sccm-100sccm, pressure in vacuum tank 0.1Pa-10Pa; In the time that the CdS thickness of institute's sputter in substrate is 20nm-500nm, stop the preparation of CdS polycrystal film.Then the CdS having grown is kept to 1min-72h at 25 DEG C-1100 DEG C, or stop, to substrate heating, making CdS polycrystal film be down to room temperature, then at room temperature keep 0-72h.Substrate is turned to the just position to CdTe target, start sputter CdTe polycrystal film.The sputtering condition of CdTe polycrystal film is: 25 DEG C-1100 DEG C of base reservoir temperatures, pass into high-purity Ar gas, gas flow rate 5sccm-100sccm, pressure in vacuum tank 0.1Pa-10Pa; Substrate bias is :+8.8V～-100V.When the CdTe thickness of institute's sputter in substrate reaches the thickness of setting: when 0.5 μ m-10 μ m, close additional power source and stop the bias voltage to substrate, stop the preparation of CdTe polycrystal film, stop substrate heating simultaneously, in the time that base reservoir temperature is reduced to room temperature, take out the substrate that has deposited CdS polycrystal film and CdTe polycrystal film.
In described step 3, CdS polycrystal film and the CdTe polycrystal film of preparation are carried out to CdCl
2annealing in process.Its operating procedure is as follows: at CdCl
2in atmosphere, at 350 DEG C of-450 DEG C of temperature, CdTe polycrystal film is processed to 5min-120min.
In described step 4 through CdCl
2evaporation conduction back electrode on CdTe polycrystal film after treatment.Electric conducting material is that this professional domain is known by the technical staff, as Au, Ni, Mo, Al, Mg, Graphene etc.The method of evaporation electric conducting material is this professional domain method known by the technical staff, such as: thermal evaporation, electron beam, CVD etc.
The present invention is in magnetron sputtering process, after growth CdS polycrystal film, the CdTe polycrystal film of not growing immediately, but to after the process that the CdS polycrystal film after having grown is lowered the temperature, heated up or heating keeps or intensification is lowered the temperature again, again at CdS polycrystal film superficial growth CdTe polycrystal film, can improve the junction characteristic of PN junction, improve transformation efficiency and the open circuit voltage of CdTe polycrystal film solar cell.
Brief description of the drawings
Fig. 1 is the J-V curve of the prepared CdTe polycrystalline solar cell of the embodiment of the present invention 3, and wherein the parameter of the prepared CdTe polycrystalline solar cell of embodiment 3 respectively as shown in Figure 1.
Fig. 2 is ESEM (SEM) photo of the CdTe polycrystal film prepared of the embodiment of the present invention 4.
Fig. 3 is the CdTe polycrystal film process CdCl of the embodiment of the present invention 4 example preparations
2eSEM after treatment (SEM) photo.
Embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described.
Embodiment 1
On the position of magnetron sputtering stove placement substrate, put the mica substrate with tin dioxide transparent conductive film, the conductive film of substrate is connected by the probe of the anchoring base of conduction with applied voltage equipment.The bell that covers magnetron sputtering stove, vacuumizes vacuum chamber, and to substrate heating, makes base reservoir temperature remain on 25 DEG C of room temperatures.When back end vacuum arrives 1 × 10
-4when Pa, start sputter CdS polycrystal film in the substrate with conductive film.CdS polycrystal film sputtering condition is: 25 DEG C of base reservoir temperatures, and the high-purity Ar gas flow rate 100sccm passing into, pressure in vacuum tank 10Pa, the bias voltage of substrate is the bias voltage that floats, size is+8.8V.In the time that CdS polycrystal film thickness is 20nm, close additional power source and stop the bias voltage to substrate, stop the preparation of CdS polycrystal film.Then substrate is kept at 25 DEG C, after 72h, closing magnetron sputtering apparatus.Then to vacuumizing in vacuum chamber, make base reservoir temperature remain on 25 DEG C of room temperatures.When back end vacuum arrives 1 × 10
-4pa, turns to the just position to CdTe target substrate, starts sputter CdTe polycrystal film, and the bias voltage of substrate is the bias voltage that floats, and size is+8.8V.CdTe sputtering condition is: 25 DEG C of base reservoir temperatures, pass into high-purity Ar gas, gas flow rate 100sccm, pressure in vacuum tank 10Pa.In the time that CdTe polycrystal film thickness is 0.5 μ m, stop the preparation of CdTe polycrystal film, take out the substrate that has deposited CdS polycrystal film and CdTe polycrystal film.
CdCl
2saturated methanol solution evenly drops on CdTe polycrystal film, at 350 DEG C, CdS and CdTe polycrystal film is carried out to annealing in process 120min.Then use thermal evaporation at CdCl
2the Au conduction back electrode that on CdTe polycrystal film after treatment, evaporation 5nm is thick.
Embodiment 2
On the position of magnetron sputtering stove placement substrate, put the mica substrate with transparent conductive film, the conductive film of substrate is connected by the probe of the anchoring base of conduction with applied voltage equipment, by the conductivity between universal instrument measurement additional equipment and substrate, to guarantee that the two can conducting.The bell that covers magnetron sputtering stove, vacuumizes vacuum chamber, substrate is heated simultaneously, and heating setpoint temperature is 250 DEG C.When back end vacuum arrives 5 × 10
-4when Pa, start sputter CdS polycrystal film in the substrate with conductive film.CdS polycrystal film sputtering condition is: 250 DEG C of base reservoir temperatures, pass into high-purity Ar gas, and gas flow rate 5sccm, pressure in vacuum tank 0.1Pa, the bias voltage of substrate is the bias voltage that floats, size is+8.8V.In the time that CdS polycrystal film thickness is 500nm, close additional power source and stop the bias voltage to substrate, stop the preparation of CdS polycrystal film, stop substrate heating simultaneously.After treating that substrate temperature is reduced to room temperature, then to substrate heating, heating setpoint temperature is 250 DEG C.When back end vacuum arrives 5 × 10
-4when Pa, substrate is turned to the position of CdTe target, start sputter CdTe polycrystal film in the substrate with CdS polycrystal film and conductive film.Open the external voltage apparatus that applies simultaneously, to apply+10V of substrate voltage, start sputter CdTe polycrystal film, CdTe polycrystal film sputtering condition is: 250 DEG C of base reservoir temperatures, the high-purity Ar gas flow rate 5sccm passing into, pressure in vacuum tank 0.1Pa.In the time that CdTe thickness is 10 μ m, stop the preparation of CdTe polycrystal film.Stop substrate heating simultaneously.In the time that base reservoir temperature drops to room temperature, take out the substrate that has deposited CdS polycrystal film and CdTe polycrystal film.
CdCl
2saturated methanol solution evenly drops on CdTe polycrystal film, at 450 DEG C, CdS and CdTe is processed to 5min.Then at CdCl
2the Ni conduction back electrode that on CdTe polycrystal film after treatment, evaporation 200nm is thick.
Embodiment 3
On the position of magnetron sputtering stove placement substrate, put the TEC15 glass with tin dioxide transparent conductive film, the conductive film of substrate is connected by the probe of the anchoring base of conduction with applied voltage equipment, by the conductivity between universal instrument measurement additional equipment and substrate, to guarantee that the two can conducting.Cover the bell of magnetron sputtering stove, to vacuumizing in vacuum chamber, and to substrate heating, make base reservoir temperature be elevated to 300 DEG C.When back end vacuum arrives 3 × 10
-4pa, starts sputter CdS polycrystal film in the substrate with conductive film.The sputtering condition of CdS polycrystal film is: 300 DEG C of base reservoir temperatures, pass into high-purity Ar gas, and gas flow rate 40sccm, pressure in vacuum tank 4Pa, the bias voltage of substrate is the bias voltage that floats, size is+8.8V.In the time that CdS thickness is 100nm, stop the preparation of CdS polycrystal film, stop substrate heating simultaneously, after substrate temperature arrives room temperature, close magnetron sputtering apparatus.After 12h, magnetron sputtering apparatus is opened, to vacuumizing in vacuum chamber, substrate is heated to 300 DEG C, when back end vacuum arrives 3 × 10
-4pa, turns to the just position to CdTe target substrate, and the bias voltage of substrate, for the bias voltage that floats, size is+8.8V, starts sputter CdTe polycrystal film, and CdTe sputtering condition is: 300 DEG C of base reservoir temperatures, pass into high-purity Ar gas, gas flow rate 40sccm, pressure in vacuum tank 4Pa.In the time that CdTe polycrystal film thickness is 2.3 μ m, close additional power source and stop the bias voltage to substrate, stop the preparation of CdTe polycrystal film.Stop, to substrate heating, in the time that base reservoir temperature is reduced to room temperature, taking out the substrate that has deposited CdS and CdTe polycrystal film.
CdCl
2saturated methanol solution evenly drops on CdTe polycrystal film, at 400 DEG C, CdS and CdTe polycrystal film is processed to 30min.Then through CdCl
2on CdTe polycrystal film after treatment, pass through the Au conduction back electrode that electron beam evaporation plating 25nm is thick.
Utilize Newport Oriel 91159A solar simulator, at the AM1.5 of standard, under 1000W/m2 simulated solar irradiation, 25 DEG C carry out J-V curve, use Keithley2400 to gather J-V data, the J-V curve that Figure 1 shows that the CdTe polycrystal film solar cell that the present embodiment obtains, its parameter is: transformation efficiency (Eff)=13.31%, open circuit voltage (Voc)=828mV, short-circuit current density (Jsc)=25.32mA/cm2, fill factor, curve factor (FF)=63.49%., through CdS cooling annealing in process, the conversion efficiency of the CdTe polycrystal film solar cell of grow continuously CdS and CdTe film is not 12.00%, and open circuit voltage is 789mV.(document Liu Li Hui is to prosperous, rf magnetron sputtering is prepared transformation efficiency up to 12.78% CdTe thin-film solar cells, the 12nd Chinese photovoltaic conference and international photovoltaic exhibition paper (thin-film solar cells)) can see, through CdS annealing in process, transformation efficiency brings up to 13.31%, open circuit voltage rises to 828mV, the annealing in process of visible CdS, greatly improve transformation efficiency and the open circuit voltage of magnetron sputtering C dTe film, improved the PN junction performance of CdTe polycrystal film solar cell.
Embodiment 4
On the position of magnetron sputtering stove placement substrate, put the TEC15 glass with tin dioxide transparent conductive film, substrate transparent conductive film is connected by the probe of the anchoring base of conduction with applied voltage equipment, by the conductivity between universal instrument measurement additional equipment and substrate, to guarantee that the two can conducting.Cover the bell of magnetron sputtering stove, to vacuumizing in vacuum chamber, substrate is heated to 300 DEG C simultaneously.When back end vacuum arrives 9 × 10
-4pa, starts sputter CdS polycrystal film in the substrate with conductive film.CdS polycrystal film sputtering condition is: 300 DEG C of base reservoir temperatures, and the high-purity Ar gas gas flow rate 40sccm passing into, pressure in vacuum tank 3Pa, the bias voltage of substrate is the bias voltage that floats, size is+8.8V.In the time that CdS polycrystal film thickness is 100nm, stop the preparation of CdS polycrystal film, the temperature of substrate is elevated to 350 DEG C simultaneously, at 350 DEG C, keep 10min, then substrate temperature is dropped to 300 DEG C.Substrate is turned to the just position to CdTe target, open the external voltage apparatus that applies simultaneously, the bias voltage of substrate is the bias voltage that floats, size is+8.8V, starts sputter CdTe polycrystal film, and CdTe sputtering condition is: 300 DEG C of base reservoir temperatures, pass into high-purity Ar gas, gas flow rate 40sccm, chamber pressure 2Pa.In the time that CdTe polycrystal film thickness is 2.3 μ m, close additional power source and stop the bias voltage to substrate, stop the preparation of CdTe polycrystal film.Stop, to substrate heating, in the time that base reservoir temperature is reduced to room temperature, taking out the substrate that has deposited CdS and CdTe polycrystal film.
At CdCl
2in vapor atmosphere, at 400 DEG C, CdS and CdTe are processed to 30min.Then at CdCl
2on CdTe polycrystal film after treatment, pass through the Au conduction back electrode that electron beam evaporation plating 25nm is thick.
Fig. 2 is ESEM (SEM) photo of the CdTe polycrystal film prepared of the present embodiment, and from Fig. 2 has grown, the ESEM picture of CdTe can be found out, the CdTe polycrystal film crystal grain of preparation is in conjunction with densification, and maximum crystallite dimension has reached 500nm.Fig. 3 is CdTe polycrystal film process CdCl prepared by the present embodiment
2stereoscan photograph after treatment can be seen from ESEM picture, through CdCl
2crystal grain particle after treatment is obviously grown up, and more than maximum crystallite dimension has reached 1 μ m, and crystal grain is in conjunction with very fine and close, does not see vacuum and empty in stereoscan photograph.
Embodiment 5
On the position of magnetron sputtering stove placement substrate, put the mica substrate of the tin dioxide transparent conductive film with fluorine doping, the conductive film of substrate is connected by the probe of the anchoring base of conduction with applied voltage equipment, by the conductivity between universal instrument measurement additional equipment and substrate, to guarantee that the two can conducting.The bell that covers magnetron sputtering stove, vacuumizes vacuum chamber, and substrate is heated to 1100 DEG C, when back end vacuum arrives 3 × 10
-4pa, starts sputter CdS polycrystal film in the substrate with conductive film.CdS sputtering condition is: 1100 DEG C of base reservoir temperatures, the high-purity Ar gas flow rate 60sccm passing into, pressure in vacuum tank 5Pa.In the time that CdS thickness is 200nm, stop the preparation of CdS polycrystal film.Meanwhile, keep 5min at 1100 DEG C.Substrate is turned to the just position to CdTe target, start sputter CdTe polycrystal film, substrate is applied to bias voltage for-20V, start sputter CdTe polycrystal film, CdTe polycrystal film sputtering condition is: 1100 DEG C of base reservoir temperatures, the high-purity Ar gas passing into, gas flow rate 60sccm, pressure in vacuum tank 5Pa.In the time that CdTe thickness is 6 μ m, close additional power source and stop the bias voltage to substrate, stop the preparation of CdTe polycrystal film.Stop, to substrate heating, in the time that base reservoir temperature is reduced to room temperature, taking out the substrate that has deposited CdS and CdTe polycrystal film.
CdCl
2saturated methanol solution evenly drops on CdTe polycrystal film, at 350 DEG C, CdS and CdTe is processed to 5min.Then at CdCl
2on CdTe polycrystal film after treatment by the thick Mg of thermal evaporation evaporation 50nm conduction back electrode.
Embodiment 6
On the position of magnetron sputtering stove placement substrate, put the TEC7 glass with tin dioxide transparent conductive film, the transparent conductive film of substrate is connected by the probe of the anchoring base of conduction with applied voltage equipment, by the conductivity between universal instrument measurement additional equipment and substrate, to guarantee that the two can conducting.Cover the lid of magnetron sputtering stove, to vacuumizing in vacuum chamber, substrate is heated to 300 DEG C simultaneously, when back end vacuum arrives 8 × 10
-4pa, starts sputter CdS polycrystalline polycrystal film in the substrate with conductive film.The sputtering condition of CdS polycrystal film is: 300 DEG C of base reservoir temperatures, and the high-purity Ar gas flow rate 40sccm passing into, pressure in vacuum tank 0.5Pa, the bias voltage of substrate is the bias voltage that floats, size is+8.8V.In the time that CdS thickness is 100nm, stop the preparation of CdS polycrystal film.Then keep 1h at 300 DEG C.Substrate is turned to the just position to CdTe target, start sputter CdTe polycrystal film, CdTe polycrystal film sputtering condition is: 250 DEG C of base reservoir temperatures, and gas flow rate 40sccm, chamber pressure 0.5Pa, substrate bias is the bias voltage that floats, size is+8.8V.In the time that CdTe polycrystal film thickness is 2 μ m, close additional power source and stop the bias voltage to substrate, stop the preparation of CdTe polycrystal film.Stop, to substrate heating, in the time that base reservoir temperature is reduced to room temperature, taking out the substrate that has deposited CdS polycrystal film and CdTe polycrystal film.Then under dry air, utilize the method for near space distillation at 400 DEG C, CdS and CdTe to be processed to 20min, wherein sample and CdCl
2the distance in source is 2mm.Then at CdCl
2on CdTe polycrystal film after treatment by the thick Al of thermal evaporation evaporation 25nm conduction back electrode.
Embodiment 7
On the position of magnetron sputtering stove placement substrate, put the mica substrate with AZO transparent conductive film, the conductive film of substrate is connected by the probe of the anchoring base of conduction with applied voltage equipment, by the conductivity between universal instrument measurement additional equipment and substrate, to guarantee that the two can conducting.Cover the bell of magnetron sputtering stove, to vacuumizing in vacuum chamber, and to substrate heating, make base reservoir temperature be warming up to 300 DEG C.When back end vacuum arrives 3 × 10
-4pa, starts sputter CdS polycrystal film in the substrate with conductive film.CdS sputtering condition is: 300 DEG C of base reservoir temperatures, and the high-purity Ar gas flow rate 40sccm passing into, pressure in vacuum tank 4Pa, the bias voltage of substrate is the bias voltage that floats, size is+8.8V.In the time that CdS thickness is 130nm, stop the preparation of CdS polycrystal film, stop substrate heating simultaneously, after substrate temperature arrives room temperature, close magnetron sputtering apparatus.After 12h, magnetron sputtering apparatus is opened, to vacuumizing in vacuum chamber, substrate is heated to 300 DEG C, when back end vacuum arrives 3 × 10
-4pa, turns to the just position to CdTe target substrate, and the bias voltage of substrate is-100V, starts sputter CdTe polycrystal film, and CdTe sputtering condition is: 300 DEG C of base reservoir temperatures, pass into high-purity Ar gas, gas flow rate 40sccm, chamber pressure 2Pa.In the time that CdTe polycrystal film thickness is 2.0 μ m, close additional power source and stop the bias voltage to substrate, stop the preparation of CdTe polycrystal film.Stop, to substrate heating, in the time that base reservoir temperature is reduced to room temperature, taking out the substrate that has deposited CdS and CdTe polycrystal film.
CdCl
2saturated methanol solution evenly drops on CdTe polycrystalline polycrystal film, at 400 DEG C, CdS and CdTe is processed to 30min.Then through CdCl
2on CdTe polycrystal film after treatment, pass through the Mo conduction back electrode that electron beam evaporation plating 25nm is thick.
Embodiment 8
On the position of magnetron sputtering stove placement substrate, put 7059 glass substrate with AZO transparent conductive film, the conductive film of substrate is connected by the probe of the anchoring base of conduction with applied voltage equipment, by the conductivity between universal instrument measurement additional equipment and substrate, to guarantee that the two can conducting.Cover the bell of magnetron sputtering stove, to vacuumizing in vacuum chamber, and to substrate heating, make base reservoir temperature be warming up to 200 DEG C.When back end vacuum arrives 6 × 10
-4pa, starts sputter CdS polycrystal film in the substrate with conductive film.CdS sputtering condition is: 200 DEG C of base reservoir temperatures, and the high-purity Ar gas flow rate 20sccm passing into, pressure in vacuum tank 3Pa, the bias voltage of substrate is the bias voltage that floats, size is+8.8V.In the time that CdS thickness is 100nm, stop the preparation of CdS polycrystal film, stop substrate heating simultaneously, after substrate temperature arrives room temperature, close magnetron sputtering apparatus.After 36h, magnetron sputtering apparatus is opened, to vacuumizing in vacuum chamber, substrate is heated to 200 DEG C, when back end vacuum arrives 7 × 10
-4pa, turns to the just position to CdTe target substrate, and the bias voltage of substrate, for the bias voltage that floats, size is+8.8V, starts sputter CdTe polycrystal film, and CdTe sputtering condition is: 200 DEG C of base reservoir temperatures, pass into high-purity Ar gas, gas flow rate 20sccm, chamber pressure 3Pa.In the time that CdTe polycrystal film thickness is 2.0 μ m, close radio-frequency power supply, stop the preparation of CdTe polycrystal film.Stop, to substrate heating, in the time that base reservoir temperature is reduced to room temperature, taking out the substrate that has deposited CdS and CdTe polycrystal film.
CdCl
2saturated methanol solution evenly drops on CdTe polycrystal film, at 400 DEG C, CdS and CdTe is processed to 50min.Then graphene conductive back electrode is transferred to through CdCl
2cdTe polycrystal film after treatment surface.Graphene growing method is as follows: in tube furnace, prepare Graphene by chemical vapour deposition technique, Cu paper tinsel thick 0.5mm is put into tube furnace, then diamond heating to 1000 DEG C, pass into methane and hydrogen, keep 15min at 1000 DEG C, obtain needed Graphene.Then by the solution of ferric trichloride and hydrochloric acid, Graphene is transferred on polymethyl methacrylate, Graphene is being put into through CdCl
2after processing, on CdTe polycrystal film, by acetone, polymethyl methacrylate is dissolved, obtain through CdCl
2graphene conductive back electrode after processing on CdTe polycrystal film.
Claims (3)
1. a preparation method for magnetron sputtering C dTe polycrystal film solar cell, is characterized in that, described preparation method's step is as follows:
1) place and on the position of substrate, place the substrate with transparent conductive film at magnetron sputtering stove, the probe of the anchoring base by conduction, makes the transparent conductive film of substrate be connected with applied voltage equipment; Then close the vacuum chamber of magnetron sputtering stove, described vacuum chamber is vacuumized, and substrate is heated;
2) when vacuum chamber back end vacuum arrives 10
-3below Pa, described base reservoir temperature reaches 25 DEG C-1100 DEG C, starts sputter CdS polycrystal film in the substrate with electrically conducting transparent polycrystal film; In the time that the thickness of CdS polycrystal film reaches 20nm-500nm, CdS polycrystal film stops growing; Then the CdS polycrystal film of having grown is kept to 1min-72h under 25 DEG C of-1100 DEG C of temperature ranges, or stop, to substrate heating, making CdS polycrystal film cool to room temperature, then at room temperature keep 0-72h; Afterwards, the position transfer of substrate is arrived to the just position to CdTe target, start radio-frequency power supply and start sputter CdTe polycrystal film, substrate is applied to bias voltage+8.8V--100V; In the time that the thickness of CdTe polycrystal film reaches 0.5 μ m-10 μ m, close additional power source and stop the bias voltage to substrate, close radio-frequency power supply simultaneously, stop the growth of CdTe polycrystal film, stop substrate heating, the substrate of CdS polycrystal film and CdTe polycrystal film of having made to grow is cooling with stove, then takes out the substrate of grown CdS polycrystal film and CdTe polycrystal film;
3) CdS being prepared by step 2 and CdTe polycrystal film carry out CdCl
2annealing in process;
4) through CdCl
2cdTe polycrystal film surface evaporation conduction back electrode after annealing in process.
2. according to preparation method claimed in claim 1, it is characterized in that described step 2) when sputter CdS polycrystal film, in described vacuum chamber, pass into Ar gas, gas flow rate 5sccm-100sccm, pressure in vacuum tank is 0.1Pa-10Pa.
3. according to preparation method claimed in claim 1, it is characterized in that, described step 3) is at CdCl
2in atmosphere, at 350 DEG C-450 DEG C to CdTe annealing in process 5min-120min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106340554A (en) * | 2016-11-25 | 2017-01-18 | 中国科学院电工研究所 | CIGS/CdTe dual-junction laminated thin-film solar cell and preparation method thereof |
| CN108183143A (en) * | 2017-12-27 | 2018-06-19 | 四川大学 | The technology of ultra-thin CdTe solar cells is prepared with more target radio frequency magnetron sputtering methods |
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|---|---|---|---|---|
| JPS57115879A (en) * | 1981-01-12 | 1982-07-19 | Ricoh Co Ltd | Method for forming cds thin film |
| CN101673786A (en) * | 2009-10-12 | 2010-03-17 | 上海联孚新能源科技有限公司 | Preparation method of CdTe solar cells under magnetic field |
| CN102787295A (en) * | 2012-07-27 | 2012-11-21 | 中国科学院电工研究所 | Method for preparing CdTe polycrystalline film |
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2013
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS57115879A (en) * | 1981-01-12 | 1982-07-19 | Ricoh Co Ltd | Method for forming cds thin film |
| CN101673786A (en) * | 2009-10-12 | 2010-03-17 | 上海联孚新能源科技有限公司 | Preparation method of CdTe solar cells under magnetic field |
| CN102787295A (en) * | 2012-07-27 | 2012-11-21 | 中国科学院电工研究所 | Method for preparing CdTe polycrystalline film |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106340554A (en) * | 2016-11-25 | 2017-01-18 | 中国科学院电工研究所 | CIGS/CdTe dual-junction laminated thin-film solar cell and preparation method thereof |
| CN106340554B (en) * | 2016-11-25 | 2017-10-03 | 中国科学院电工研究所 | A kind of CIGS/CdTe binodes overlapping thin film solar battery and preparation method thereof |
| CN108183143A (en) * | 2017-12-27 | 2018-06-19 | 四川大学 | The technology of ultra-thin CdTe solar cells is prepared with more target radio frequency magnetron sputtering methods |
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