CN104795455A - CZTS film solar cell with transparent graphene conductive film - Google Patents

CZTS film solar cell with transparent graphene conductive film Download PDF

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Publication number
CN104795455A
CN104795455A CN201410025934.0A CN201410025934A CN104795455A CN 104795455 A CN104795455 A CN 104795455A CN 201410025934 A CN201410025934 A CN 201410025934A CN 104795455 A CN104795455 A CN 104795455A
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film
selenium
zinc
copper
thin
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马给民
保罗比蒂
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Dongguan Zhen Film Photovoltaic Technology Co Ltd
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Dongguan Zhen Film Photovoltaic Technology Co Ltd
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    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L31/00Semiconductor devices sensitive to infra-red 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
    • H01L31/0248Semiconductor devices sensitive to infra-red 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
    • H01L31/0256Semiconductor devices sensitive to infra-red 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
    • H01L31/0264Inorganic materials
    • H01L31/032Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
    • H01L31/0326Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312 comprising AIBIICIVDVI kesterite compounds, e.g. Cu2ZnSnSe4, Cu2ZnSnS4
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L31/00Semiconductor devices sensitive to infra-red 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
    • H01L31/0248Semiconductor devices sensitive to infra-red 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
    • H01L31/036Semiconductor devices sensitive to infra-red 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 their crystalline structure or particular orientation of the crystalline planes
    • H01L31/0392Semiconductor devices sensitive to infra-red 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 their crystalline structure or particular orientation of the crystalline planes including thin films deposited on metallic or insulating substrates ; characterised by specific substrate materials or substrate features or by the presence of intermediate layers, e.g. barrier layers, on the substrate
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L31/00Semiconductor devices sensitive to infra-red 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
    • H01L31/18Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00Energy generation through renewable energy sources
    • Y02E10/50Photovoltaic [PV] energy

Abstract

The invention discloses a novel custerite type film solar cell in which honeycomb-shaped two-dimensional crystal graphene serves as a transparent conductive film and CZTS serves as an absorber layer, and the cell has more strict requirements for stoichiometry of copper, zinc, tin and selenium. A soda-lime glass substrate is plated with a molybdenum film of the thickness of 0.35 to 1.0 micrometer, the molybdenum film is coated with a CZTS film of the thickness of 0.7 to 1.5 micrometer, and crystal is formed after annealing. Cadmium sulfide is deposited on the crystal to establish a p-n node film area; low-temperature sputtering is utilized to overcome the disadvantage of selenium loss; and thus, the solar cell has great advantages in large-area, uniform-stoichiometry and repetitive production, and prompts batch production. The thinnest, extremely conductive and transparent graphene in the thickness of an atom serves as a front electrode to replace an expensive indium tin oxide front electrode, and the cost of batch production is further reduced.

Description

Graphene transparent conductive film copper-zinc-tin-selefilm film solar cell
Technical field
The present invention relates to regarding film " photovoltaic solar " battery chip, be specifically related to the solar cell of low-temperature sputter manufacture technics.
Background technology
Existing common thin-film solar cells, adopt " cadmium telluride ", the thin-film material such as " amorphous silicon " or " Copper Indium Gallium Selenide (CIGS) ", conversion solar photovoltaic electric, adopt soda-lime glass, metal or other flexible base, board, use high temperature evaporation, or first use sputtering technology, after plating metal material, adopt " selenizing " or " telluride " technique again, set up " P-N junction ", then spread front and back electrode in the upper and lower of absorbed layer (absorber layer); Except " amorphous silicon ", these thin-film materials are all a little very expensive rare materials, and the conversion efficiency of " amorphous silicon " is too low, " cadmium telluride " has pollution problem, " Copper Indium Gallium Selenide " manufacturing process is very complicated, is difficult to commercialization, especially to " Copper Indium Gallium Selenide (CIGS) " thin film technique, the electrodeposition technique of common use, or use " metal " or " metal oxide " through nanoimprinting process manufacture; These techniques are neither beneficial to batch production, single " selenizing (Selenization) " technique, just be 8 hours, and a large amount of toxic gas need be used, such as use " hydrogen selenide " progressively to make " copper indium gallium (CIS) " thin layer " selenium (Se) " change into " " Copper Indium Gallium Selenide (CIGS) " thin layer.
  
For solving low cost batch production, make solar chip can compete free of contamination energy supply with traditional kerosene power plant, impel the commercialization of solar energy, we must use the raw material of high-conversion rate performance and low cost, the graphene transparent conductive film (TCO) of this invention use atom thick is front electrode, copper-zinc-tin-selenium (CZTS) " film is absorbed layer (absorber layer)." copper-zinc-tin-selenium (CZTS) " film will be carried out at low temperatures, and can ensure that it holds optimized chemical composition ratio, become the mass production processes of standard, we use " copper-zinc-tin-selenium " the four element solid target material having matched chemical composition, by radio frequency or anion direct current pulsed magnetron sputtering technique, disposable plated film; Meanwhile, be the loss of " selenium (Se) " under avoiding high temperature, the technique that general industry adopts utilizes " hydrogen selenide " gas, supplements the loss of " selenium (Se) "; But this gas is poisonous, inadaptable batch production; In order to avoid this defect, after we use low-temperature sputter, re-use high-temperature vacuum annealing furnace, anneal respectively, use solid-state " selenium (Se) " to control the loss of " selenium (Se) ", both avoided poisonous " hydrogen selenide " gas, simultaneously, we by the annealing furnace of low cost separately out alleviate the equipment cost of high vacuum sputtering stove.
  
Summary of the invention
The main purpose of the present invention is to set up the manufacturing process that is applicable to film " copper-zinc-tin-selenium (the CZTS) " solar chip of batch production; First we use one piece to match the four element composite solid state targets such as " copper; indium; gallium, the selenium (CIGS) " of " chemical composition (stoichiometry) ", under lower substrate temperature (250-300 degree Celsius), with " radio frequency or the sputtering of anion pulse dc power " plated film, by elements such as " copper, zinc, tin; selenium ", disposable plating on the glass substrate; And then adopt the annealing furnace closing envelope atmosphere with " selenium (Se) ", anneal under 500-550 ° of C high temperature.
  
This this invention adopts " copper, zinc, tin, selenium " material of very low cost, and its manufacturing process ensure that the optimization of thin layer " chemical composition (stoichiometry) "; Eliminate in traditional handicraft reach eight few time traditional " selenizing " means of " selenization process (selenization) " –; use " hydrogen selenide " gas that band is poisonous; through the chemical reaction of a few hours, from type metal film layer, carry out " selenizing ".
  
We adopt not higher than the substrate temperature of 300 degrees Celsius, when can avoid four element sputterings, and the loss of selenium (Se); And then, we will possess " copper-zinc-tin-selenium (the CZTS) " film substrate of good " chemical composition (stoichiometry) ", leave vacuum sputtering production line under order (for avoiding taking " copper-zinc-tin-selenium (CZTS) " vacuum line, it is bottleneck process procedure the most complicated on production line), and adopt independent cheap annealing furnace to carry out high annealing; Solid-state selenium element placed by this annealing furnace crucible, carries out high annealing under vacuum conditions, grows " copper-zinc-tin-selenium (CZTS) " crystal of large volume; Owing to adopting four element solid target materials above, ensure that the chemical composition of " copper-zinc-tin-selenium (CZTS) ", without the need to adding selenium element; Solid-state " selenium (Se) " that place in annealing furnace, it is not to add " selenium (Se) " in " copper-zinc-tin-selenium (CZTS) " film, but have rich " selenium (Se) " gas atmosphere in annealing furnace to ensure, control the loss of " selenium (Se) " in " copper-zinc-tin-selenium (CZTS) " film.This technique ensure that " copper-zinc-tin-selenium (CZTS) " crystal of large volume, ensure that optimization and the repeatability of " copper-zinc-tin-selenium (CZTS) " chemical composition, ensure that During Annealing " copper-zinc-tin-selenium (CZTS) " film does not have the loss of " selenium (Se) ", ensure that the uniformity of selenium between whole " copper-zinc-tin-selenium (CZTS) " thin layer, ensure that " copper-zinc-tin-selenium (CZTS) " mass production processes of high-conversion rate.
  
Accompanying drawing illustrates:
Fig. 1 is " copper-zinc-tin-selenium (CZTS) " matrix cross section (" copper-zinc-tin-selenium (CZTS) " thin layer cross section)
1. usual, 1.0 to 4.0 millimeters thick, or the soda-lime glass substrate of 3.2 millimeters of standard thicknesses;
2. about 0.35 micron thickness molybdenum (Mo) film;
3. about 0.5 to 1.5 micron thickness, or " copper-zinc-tin-selenium (the CZTS) " film of 1.0 micron nominal thickness and the crystal of similar size;
4. the cadmium sulfide (CdS) of 0.05 micron thickness;
5. insulating barrier " the zinc oxide (i-ZnO) of about 0.1 micron thickness;
6. " graphene transparent conductive film (TCO) " of about 0.35 micron thickness is front electrode;
7. the nickel of about 0.05 micron thickness, for strengthening the conductive grid of superficial layer conductance;
8. about 3.0 micron thickness aluminium films are the conductive grid of most last layer;
9. one deck nickel of about 0.05 micron thickness, to protect aluminium;
10. about 1.0 to 4.0 millimeters thick, or the sodium calcium cover glass of 3.2 millimeters of standard thicknesses;
11. Copper Indium Gallium Selenide (CIGS) film and its upper surface, band " p-n knot " thin membrane regions.
  
Fig. 2 is annealing furnace and " selenium (Se) " crucible (vacuum annealing furnace)
12. quartz ampoules;
13. " selenium (Se) " crucible;
14. glass substrates
Fig. 3 is the plane graph of stove in Fig. 2
embodiment describes in detail:
Fig. 1 shows the cross section of typical case " copper-zinc-tin-selenium (CZTS) " photovoltaic cell diaphragm; The superiors of attention " copper-zinc-tin-selenium (CZTS) " " absorbed layer " are very narrow " p-n junction " districts; Act on " negatron " that discharge and " hole " of soaring through sunlight " photovoltaic ", form " p-n junction " region in " negatron-hole ", the superiors of it must be arranged on " copper-zinc-tin-selenium (CZTS) " layer.The bottom of " copper-zinc-tin-selenium (CZTS) ", rich " p-type " conduction must be had, and the topside position of " copper-zinc-tin-selenium (CZTS) ", need to reduce " p-type conduction " composition, make the last layer of " copper-zinc-tin-selenium (CZTS) " thin layer, " cadmium (Cd) " or " zinc (Zn) " then in " cadmium sulfide (CdS) " or " zinc sulphide (ZnS) " thin layer, can down spread, penetrate into the upper epidermis of " copper-zinc-tin-selenium (CZTS) " film, make it convert to " n-type conduction ".
  
Meanwhile, " sodium " that we also will control well in " soda-lime glass " upwards permeates, and ensures not allow " selenium (Se) " to run off, because " scarce copper " and have the film of " natrium doping agent ", all can promote " copper-zinc-tin-selenium (the CZTS) " film of " p-type "; And lack the film of " selenium (Se) ", but can promote " copper-zinc-tin-selenium (the CZTS) " film of " n-type ".
  
With following table one, we adopt " X " light fluorescence analyser to check the atomic percent of " copper-zinc-tin-selenium (CZTS) " four elements, and we see after about 250 ° of C sputter coatings here, and four elemental compositions in target and film almost do not have anything to change; Meanwhile, four element atomic components listed by Fig. 2, are just accord with the composition of symbol needed for optimized " alpha phase "; Use low-temperature sputter, " selenium (Se) " can not be made to run off, and can promote that glass substrate is exitted, promote the degree of adhesion between film, and start the growth of " copper-zinc-tin-selenium (CZTS) " crystal.
  
Table 1: Target & Film Compositions
Item Cu Zn Sn Se
As- deposited film 24.60 18.45 6.90 50.00
Ceramic target 24.36 18.40 6.98 50.25
Stoichiometric CZTS 25.00 18.75 6.25 50.00
Before plating other thin layers, that we place fritter in annealing furnace or powdery " selenium (Se) ", then will plate the substrate of " copper-zinc-tin-selenium (CZTS) ", in this annealing furnace with " selenium (Se) " atmosphere, carry out 500-550 degree C; The annealing (see figure 2) of 3 hours.
  
Fig. 2 display is wherein a kind of can in the method for laboratory operation: first in the quartz ampoule of four cun of diameters, a placement plates the substrate of " copper-zinc-tin-selenium (CZTS) " film; Other end, places solid-state " selenium (Se) " of number grammes per square metre; And then vacuumize to quartz ampoule, sealing, and press the temperature curve heating of table 2; Like this, " selenium (Se) " that be evaporated, can make to place in quartz ampoule in the scope of " Copper Indium Gallium Selenide " film substrate position, keep the atmosphere of " selenium (Se) ", control the loss of " selenium (Se) ", and after annealing, allow " selenium (Se) " atmosphere in another warm area condensation.
  
Table 2: " selenium (Se) " evaporating pressure and temperature
Fig. 3, another kind of equipment de-sign scheme is the large vacuum chamber body of employing one, interior device heating source and as the crucible deposited selenium (Se) and evaporate; This vacuum chamber body band cooling system, can hold large-area glass substrate, such as the substrate of the area of 1000 x 1600 mm, point two warm areas, respectively placing glass substrate zone and " selenium (Se) " crucible district.
  
The third design adds the gas containing " selenium (Se) ", such as nitrogen at similar device; This way is the same with the handling principle of InP4, ensures that " phosphorus " of InPh mixture can not run off by the phosphorus atmosphere of band heating.
  
4th kind of design is the heater arranging Timing at similar cabin body, and uses " element sulphur " gas, at " copper-zinc-tin-selenium (CZTS) " film surface layer " sulfuration ", can increase the conversion efficiency (seeing reference 6) of battery.

Claims (7)

1. the thin-film solar cells (see Figure of description 1) of a low-temperature sputter manufacture technics, it is characterized in that: on soda-lime glass substrate (1), be coated with about 0.35 to 1.0 micron thickness molybdenum film, about 0.7 to 1.5 micron thickness is coated with at described molybdenum film, or 1.0 " copper-zinc-tin-selenium " films of micron nominal thickness, the crystal (3) after " copper-zinc-tin-selenium " film and annealing has " p-n junction " thin membrane regions (11) with its upper surface.
2. the thin-film solar cells of a kind of low-temperature sputter manufacture technics according to claim 1, is characterized in that: on described " copper-zinc-tin-selenium " film and crystal (3), be coated with " cadmium sulfide " or " zinc sulphide (4) " of 0.05 micron thickness.
3. the thin-film solar cells of low-temperature sputter manufacture technics according to claim 2, is characterized in that: on described " cadmium sulfide " or " zinc sulphide (4) ", the insulating barrier zinc oxide (5) of plating about 0.1 micron thickness.
4. the thin-film solar cells of low-temperature sputter manufacture technics according to claim 3, is characterized in that: on described " zinc oxide (5) ", and " graphene transparent conductive film (TCO) " of plating about 0.35 to 1.9 micron thickness is front electrode (6) ".
5. the thin-film solar cells of a kind of low-temperature sputter manufacture technics according to claim 4, it is characterized in that: described " graphene transparent conductive film (TCO) " is front electrode (6) " on; optionally plate the nickel (7) of about 0.05 micron thickness, this nickel (7) is coated with about 3.0 micron thickness aluminium films (8).
6. the thin-film solar cells of a kind of low-temperature sputter manufacture technics according to claim 5, is characterized in that: on described aluminium film (8), optionally plates one deck protection nickel (9) of about 0.05 micron thickness.
7. the thin-film solar cells of a kind of low-temperature sputter manufacture technics according to claim 6, is characterized in that: on described protection nickel (9), places the sodium calcium cover glass (10) of about 1.0 to 4.0 millimeters thick.
CN201410025934.0A 2014-01-21 2014-01-21 CZTS film solar cell with transparent graphene conductive film Pending CN104795455A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105161556A (en) * 2015-09-29 2015-12-16 赵玉兰 Rare earth (Er+3) doped infrared light up-conversion effect wide spectrum solar energy battery
CN106449849A (en) * 2016-10-28 2017-02-22 浙江大学 Graphene/copper zinc tin sulfur (CZTS) thin-film solar battery and production method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090314649A1 (en) * 2005-03-15 2009-12-24 Solopower, Inc. Precursor containing copper indium and gallium for selenide (sulfide) compound formation
CN102437237A (en) * 2011-11-29 2012-05-02 福建钧石能源有限公司 Chalcopyrite type thin film solar cell and manufacturing method thereof
CN202721169U (en) * 2012-07-04 2013-02-06 广东凯盛光伏技术研究院有限公司 Copper indium gallium selenium solar battery
CN103354252A (en) * 2013-07-17 2013-10-16 深圳先进技术研究院 Manufacturing methods of PN junction of CZTS solar cell and CZTS solar cell device

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090314649A1 (en) * 2005-03-15 2009-12-24 Solopower, Inc. Precursor containing copper indium and gallium for selenide (sulfide) compound formation
CN102437237A (en) * 2011-11-29 2012-05-02 福建钧石能源有限公司 Chalcopyrite type thin film solar cell and manufacturing method thereof
CN202721169U (en) * 2012-07-04 2013-02-06 广东凯盛光伏技术研究院有限公司 Copper indium gallium selenium solar battery
CN103354252A (en) * 2013-07-17 2013-10-16 深圳先进技术研究院 Manufacturing methods of PN junction of CZTS solar cell and CZTS solar cell device

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105161556A (en) * 2015-09-29 2015-12-16 赵玉兰 Rare earth (Er+3) doped infrared light up-conversion effect wide spectrum solar energy battery
CN106449849A (en) * 2016-10-28 2017-02-22 浙江大学 Graphene/copper zinc tin sulfur (CZTS) thin-film solar battery and production method thereof

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