CN103400899A - Film flattening method for preparing porous preceding layer and absorption layer - Google Patents
Film flattening method for preparing porous preceding layer and absorption layer Download PDFInfo
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- CN103400899A CN103400899A CN2013103408677A CN201310340867A CN103400899A CN 103400899 A CN103400899 A CN 103400899A CN 2013103408677 A CN2013103408677 A CN 2013103408677A CN 201310340867 A CN201310340867 A CN 201310340867A CN 103400899 A CN103400899 A CN 103400899A
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- 238000000034 method Methods 0.000 title claims abstract description 56
- 238000010521 absorption reaction Methods 0.000 title abstract description 4
- 238000007747 plating Methods 0.000 claims abstract description 52
- 230000008018 melting Effects 0.000 claims description 81
- 238000002844 melting Methods 0.000 claims description 81
- 239000010408 film Substances 0.000 claims description 72
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 52
- 239000002243 precursor Substances 0.000 claims description 41
- 239000007789 gas Substances 0.000 claims description 39
- 239000011521 glass Substances 0.000 claims description 36
- 239000010409 thin film Substances 0.000 claims description 31
- 239000000463 material Substances 0.000 claims description 30
- 230000006698 induction Effects 0.000 claims description 27
- 229910001209 Low-carbon steel Inorganic materials 0.000 claims description 26
- 229910052786 argon Inorganic materials 0.000 claims description 26
- 239000000758 substrate Substances 0.000 claims description 19
- 239000000470 constituent Substances 0.000 claims description 16
- 238000012360 testing method Methods 0.000 claims description 14
- 238000005086 pumping Methods 0.000 claims description 13
- 229910052733 gallium Inorganic materials 0.000 claims description 10
- 229910052738 indium Inorganic materials 0.000 claims description 9
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 230000003746 surface roughness Effects 0.000 abstract description 14
- 238000004519 manufacturing process Methods 0.000 abstract description 13
- 238000004544 sputter deposition Methods 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 238000005336 cracking Methods 0.000 abstract 1
- KTSFMFGEAAANTF-UHFFFAOYSA-N [Cu].[Se].[Se].[In] Chemical compound [Cu].[Se].[Se].[In] KTSFMFGEAAANTF-UHFFFAOYSA-N 0.000 description 31
- 239000010949 copper Substances 0.000 description 26
- 238000012545 processing Methods 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 14
- 239000011248 coating agent Substances 0.000 description 10
- 238000000576 coating method Methods 0.000 description 10
- 238000005259 measurement Methods 0.000 description 10
- 239000000203 mixture Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 238000007654 immersion Methods 0.000 description 4
- 238000010248 power generation Methods 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000003643 water by type Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical group [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 210000001142 back Anatomy 0.000 description 2
- DVRDHUBQLOKMHZ-UHFFFAOYSA-N chalcopyrite Chemical compound [S-2].[S-2].[Fe+2].[Cu+2] DVRDHUBQLOKMHZ-UHFFFAOYSA-N 0.000 description 2
- 229910052951 chalcopyrite Inorganic materials 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 239000011669 selenium Substances 0.000 description 2
- WGPCGCOKHWGKJJ-UHFFFAOYSA-N sulfanylidenezinc Chemical compound [Zn]=S WGPCGCOKHWGKJJ-UHFFFAOYSA-N 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 1
- 229910004613 CdTe Inorganic materials 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 229910000928 Yellow copper Inorganic materials 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- HVMJUDPAXRRVQO-UHFFFAOYSA-N copper indium Chemical compound [Cu].[In] HVMJUDPAXRRVQO-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- JAONJTDQXUSBGG-UHFFFAOYSA-N dialuminum;dizinc;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Al+3].[Zn+2].[Zn+2] JAONJTDQXUSBGG-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 229910000743 fusible alloy Inorganic materials 0.000 description 1
- QNWMNMIVDYETIG-UHFFFAOYSA-N gallium(ii) selenide Chemical compound [Se]=[Ga] QNWMNMIVDYETIG-UHFFFAOYSA-N 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 229910001635 magnesium fluoride Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000005987 sulfurization reaction Methods 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
Classifications
-
- 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
-
- 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 film flattening method for preparing a porous preceding layer and an absorption layer. Sputtering is performed at low powers, wherein the pressure of working atmosphere is greater than 10 mtorr, and the plating rate is smaller than 10 nm/min, so that a porous film is formed by a predecessor, and the surface roughness of the film is greatly reduced (smaller than 100 nm) so as to achieve the optimal flatness, and peeling and cracking are prevented being formed on the film and a base plate; and the surface roughness of the selenized or vulcanized absorption layer (CIGS) can be reduced, and the method is beneficial to manufacturing subsequent buffer layer and light window layer, and the efficiency of CIGS film solar cell is obviously improved.
Description
Technical field
The present invention relates to a kind of method for preparing porousness precursor layer and absorbed layer thin film planarization, belong to the solar cell photovoltaic field.
Background technology
The global energy demand is climbed to a higher point year by year, and under energy-conservation and environmental consciousness came back, the development renewable energy resources were the common target in the whole world; With the renewable energy resources, no matter waterpower, wind-force, geothermal power generation, all need to obtain conversion efficiency with the kinetic energy conversion regime, solar power generation is to utilize sunlight to convert the electricity generation system of electric energy to,, without moving part,, unlike using rotary machine in the electricity generation systems such as wind-force, waterpower, underground heat, therefore do not have the puzzlements such as HTHP and noise in solar power system, not causing environmental pressure in power generation process, is a green energy resource cleanly.In addition, the characteristic that solar source is inexhaustible, make solar power system can have the large advantage of one of continuous utilization; Although the photoelectric conversion efficiency of solar power generation is still not high now, it is its advantage that solar power system need not expend extra energy cost, and in other words, these energy that originally by people, do not utilized have the part ratio now as power source.The sun shines the energy on earth's surface every day, surpasses 30 years needed energy of the whole mankind, and solar cell has become the main flow of following alternative energy source.
The kind of solar cell is numerous, and CIGS (Copper Indium Gallium Selenide) thin-film solar cells has high conversion efficiency and development potentiality and is attracted attention, at present the high conversion efficiency of CIGS (Copper Indium Gallium Selenide) thin-film solar cells is created by U.S.'s renewable energy resources laboratory (NREL), and its efficiency has reached 20%.CIGS develops so far conversion efficiency from nineteen ninety-five and has improved and have fully 7% more than, compared to CdTe in the same time 4%, monocrystalline silicon and polysilicon be respectively 3% and amorphous silicon 1%, be enough to find out the development potentiality of CIGS on conversion efficiency.CIGS belongs to polycrystalline yellow copper structure (Chalcopyrite) compound of I-III-VI family, a kind ofly by II-VI compounds of group zincblende lattce structure (Zinc-Blend Structure), derived and the semi-conducting material that comes, unit cell storehouse by two zincblende forms, the lattice position that belongs to II family element originally is replaced and is formed by I family and III family, and the inner In of chalcopyrite lattice position of living in can be the Ga element that is added and replaces.CIGS (Copper Indium Gallium Selenide) has the P-type characteristic of semiconductor of direct gap (Direct band-gap) character, and quite high absorption coefficient of light α (α=10 are arranged
4~ 10
5cm
-1), be 100 times of monocrystalline silicon, can contain most solar spectrum, compare with other solar cell,, therefore only need the thickness of 1 ~ 3 μ m, can absorb the incident sunlight more than 99%.At present the high conversion efficiency of CIGS thin-film solar cells is created by U.S.'s renewable energy resources laboratory (NREL), and its efficiency has reached 20%.And NREL shows in assessment report in 2011, and CIGS (Copper Indium Gallium Selenide) can up grow up with annual 0.3% on conversion efficiency.
CIGS (Copper Indium Gallium Selenide) thin-film solar cells development so far its modular construction roughly part formed with substrate (SS/GLASS/PET) by top electrode (AL/Ni), anti-reflecting layer (MgF2), optical window layer (AZO/ITO), resilient coating (CdS), absorbed layer (CIGS), back electrode (Mo), in single rete, the parameter allotment that each material composition compares, the film crystal structure, the processing procedure mode is the challenge in its preparation with various factorss such as optimizing processing procedure, in addition, also need consider that each rete is stacked into the matching of assembly, the many factors such as influence each other between each Film preparation mode and processing procedure, especially show that from pertinent literature CIGS (Copper Indium Gallium Selenide) is for extremely responsive for component influences under various process parameter, more increase the difficulty of CIGS (Copper Indium Gallium Selenide) thin-film solar cells in preparation, simultaneously also make the technology door relatively improve, think at international photovoltaic circle a kind of solar cell that technical difficulty is larger.
Target is to have solid shape to be used for the mother metal of sputter coating.If target can be divided into metal and pottery two large classes simply according to materials classification, if according to the processing procedure classification, usually can generally divide into melting processing procedure and the large class of powder metallurgy processing procedure two.The factors such as the most metals target is adopted the melting processing procedure, and minority target grain size when using is controlled, alloy composition fusing point gap is too large just adopt the powder metallurgy processing procedure.Generally adopt vacuum induction melting to allocate composition for metal or alloy target material, and the machining mode such as the forging of process back segment and heat treatment obtain required target., as touch screen, integrated circuit, liquid crystal display screen, building glass, blooming and thin-film solar cells etc., be to obtain large-area uniformity and production in present photoelectricity and semiconductor industry, relevant film all uses the vacuum magnetic control sputter process in a large number.
The multi-element compounds solar cell is for being belonged to most at present one of purpose material, be that can its composition regulation and control to carry out with solar battery obsorbing layer that I family-III family-IV family was formed can be change and reach best photoelectric conversion efficiency, wherein, I family is copper (Cu), silver (Ag), gold (Au), III family is aluminium (Al), gallium (Ga), indium (In), IV family is sulphur (S), selenium (Se), antimony (Te), and is the highest with the copper indium gallium selenium solar cell photoelectric conversion efficiency at present.
In the CIGS rete, absorbed layer is the important rete that affects battery efficiency and the mode of production, and absorbed layer generally uses vacuum evaporation and vacuum magnetic control sputter to add the heat treated two kinds of main processing procedures of rear selenizing, has the large tracts of land film forming and obtains better inhomogeneity characteristic.Typical case's CIGS solar cell is Mo (molybdenum dorsum electrode layer)/CIGS (CuInGaSe absorbed layer)/CdS (cadmium sulfide resilient coating)/ZnO+AZO (zinc oxide with mix aluminum zinc oxide optical window layer)/Al (aluminium upper electrode layer) from lower to upper according to base material, general dorsum electrode layer, optical window layer are adopted the vacuum splashing and plating mode, resilient coating is adopted chemical waters mode, in each rete of modular construction, the absorbed layer preparation method is divided into two large classes: 1. vacuum process comprises common evaporation and sputter precursors and selenizing processing procedure; 2. antivacuum processing procedure, comprise plating and coating etc.; Use wherein that to prepare the resilient coating main cause in the chemical bath mode very thick as current stage made absorbed layer surface, needing to reach complete batch of resilient coating by immersion method is overlying on absorbed layer, yet, in whole production CIGS solar cell process, use immersion method processing procedure mode that several restrictions are arranged: 1. do not add for continuous production; 2. large-area uniformity is wayward; 3. need the large water gaging of consumption in immersion method manufacturing process; 4. immersion method uses the chemical solvent subsequent treatment cost high.If can just can not adopt the waters method to do resilient coating the flattening surface of absorbed layer, avoid the discontinuity of producing to enhance productivity and yield, and reduce production costs.
prepare the absorbed layer film for a large amount of and large tracts of land, the processing procedure mode is to adopt sputter precursors and rear selenizing processing procedure at present, wherein, early stage precursors metallic film is designed to single-element or the double base alloying metal adopts the multiple gun sputter, the processing procedure passage is many, time is long and the factor such as low-melting alloy processing procedure unsteadiness arranged, no matter the present invention was that binary (CuGa) predecessor or ternary (CuInGa) predecessor process parameter are mainly to make thin film densification in the past, the filming parameter that uses is being mainly less than 5mtorr aspect work atmosphere pressure, and use the high power plated film, make the plating rate obtain high fine and close rete greater than 10nm/min.But the phosphide element that contains low melting point due to the precursor layer, use the predecessor roughness of film that traditional filming parameter will make to become large (〉 300nm), CIGS surface after the high temperature selenizing can't reach desirable planarization in the future, be unfavorable for the preparation of follow-up resilient coating and optical window layer, and required formation absorbed layer phase change temperature reduces, causing follow-up selenizing can't continue to diffuse in the precursors film reacts, making selenizing not exclusively reach conversion efficiency can't effectively promote, because of above-mentioned former thereby improve manufacturing cost and reduced process rate and productive rate.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing porousness precursor layer and absorbed layer thin film planarization, use work atmosphere pressure greater than 10mtorr, and the plating rate is less than 10nm/mins low-power sputter, make predecessor form porous film, and make roughness of film greatly reduce (＜100nm), reached optimum flatness, avoided film and substrate to produce and peeled off and slight crack; And absorbed layer (CIGS) surface roughness after selenizing or sulfuration is reduced, be conducive to the making of follow-up resilient coating and optical window layer, obviously promote the efficiency of CIGS thin-film solar cells.
A kind of method for preparing porousness precursor layer and absorbed layer thin film planarization, predecessor weight ratio of constituents example is controlled to be: Cu/ (In+Ga)=0.6-0.95, Ga/ (In+Ga)=0.2-0.42; At first the Cu of part by weight, Ga material are put into vacuum induction melting furnace and carry out melting, vacuum degree 5 * 10
-2Torr, melting temperature is at 650 ℃/15mins, then casts in the mould of mild steel of three cun, wait to lower the temperature 12 as a child demoulding to take out the target idiosomes standby with the CuGa targets through being machined to three cun sputters; In addition the In material is put into vacuum induction melting furnace and carry out melting, vacuum degree 5 * 10
-2Torr, melting temperature is at 200 ℃/15mins, then casts in the mould of mild steel of three cun, wait to lower the temperature 12 as a child demoulding to take out the target idiosomes standby with the In targets through being machined to three cun sputters; Then take alkali-free glass as substrate, then the required glass baseplate, CuGa target, In target of plating put into the sputter cavity, with vacuum-pumping system, sputter cavity background pressure is evacuated to 0.7 * 10
-5-0.9 * 10
-5After torr, utilize argon gas to be used as working gas, the operating pressure that will pass into argon gas control sputter cavity through choke valve is 2 * 10
-3Torr, plating rate 40nm/min, first with the thick Mo film of DC power supply sputter ground floor 500nm, then uses operating pressure 20 * 10
-3-30 * 10
-3Torr, plating rate 2-6nm/min carrys out the thick CIG absorbed layer precursors film of sputter second layer 1000nm, then coated film is placed in the selenizing stove and carries out rear selenizing, selenizing temperature 500-650 ℃, time 10-30mins, selenizing rear film thickness is that 1950-2050nm is thick, then takes out test piece and carries out the measurement of surface roughness.
A kind of method for preparing porousness precursor layer and absorbed layer thin film planarization, predecessor weight ratio of constituents example is controlled to be: Cu/ (In+Ga)=0.6-0.95, Ga/ (In+Ga)=0.2-0.42; At first the Cu of part by weight, In, Ga material are put into vacuum induction melting furnace and carry out melting, vacuum degree 5 * 10
-2Torr, melting temperature is at 650 ℃/15mins, then casts in the mould of mild steel of three cun, wait to lower the temperature 12 as a child demoulding to take out the target idiosomes standby with the CuInGa targets through being machined to three cun sputters; Then take alkali-free glass as substrate, then required, plating glass baseplate and the CuInGa target is put into the sputter cavity, with vacuum-pumping system, sputter cavity background pressure is evacuated to 0.7 * 10
-5-0.9 * 10
-5After torr, utilize argon gas to be used as working gas, the operating pressure that will pass into argon gas control sputter cavity through choke valve is 2 * 10
-3Torr, plating rate 40nm/min, first with the thick Mo film of DC power supply sputter ground floor 500nm, then uses operating pressure 20 * 10
-3-30 * 10
-3Torr, plating rate 2-6nm/min carrys out the thick CIG absorbed layer precursors film of sputter second layer 1000nm, then coated film is placed in the selenizing stove and carries out rear selenizing, selenizing temperature 500-650 ℃, time 10-30mins, selenizing rear film thickness is that 1950-2050nm is thick, then takes out test piece and carries out the measurement of surface roughness.
characteristics of the present invention are in a kind of method for preparing porousness precursor layer and absorbed layer thin film planarization of preparation, make alloy composition fully mix to improve density and the uniformity of target with vacuum melting, and by the adjustment of the operating pressure of magnetic control sputtering plating and plating rate, make the surface roughness of the absorbed layer film after selenizing reduce, obtain large-area uniformity, make the procedure for producing of CIGS battery to carry out fully in a vacuum, and all over the CdS that exempts to use the waters method, the problem of having avoided Cd to pollute, make the volume production of CIGS thin-film solar cells more feasible, and obtain better PN characteristic, can obtain the CIGS battery of high conversion efficiency, reduce production costs and the requirement that has met volume production.
Embodiment:
Embodiment 1:
A kind of method for preparing porousness precursor layer and absorbed layer thin film planarization, predecessor weight ratio of constituents example is controlled to be: Cu/ (In+Ga)=0.6, Ga/ (In+Ga)=0.2; At first the Cu of part by weight, Ga material are put into vacuum induction melting furnace and carry out melting, vacuum degree 5 * 10
-2Torr, melting temperature is at 650 ℃/15mins, then casts in the mould of mild steel of three cun, wait to lower the temperature 12 as a child demoulding to take out the target idiosomes standby with the CuGa targets through being machined to three cun sputters; In addition the In material is put into vacuum induction melting furnace and carry out melting, vacuum degree 5 * 10
-2Torr, melting temperature is at 200 ℃/15mins, then casts in the mould of mild steel of three cun, wait to lower the temperature 12 as a child demoulding to take out the target idiosomes standby with the In targets through being machined to three cun sputters; Then take alkali-free glass as substrate, then the required glass baseplate, CuGa target, In target of plating put into the sputter cavity, with vacuum-pumping system, sputter cavity background pressure is evacuated to 0.7 * 10
-5After torr, utilize argon gas to be used as working gas, the operating pressure that will pass into argon gas control sputter cavity through choke valve is 2 * 10
-3Torr, plating rate 40nm/min, first with the thick Mo film of DC power supply sputter ground floor 500nm, then uses operating pressure 20 * 10
-3Torr, plating rate 2nm/min carry out the thick CIG absorbed layer precursors film of sputter second layer 1000nm, then coated film are placed in the selenizing stove and carry out rear selenizing, 500 ℃ of selenizing temperature, time 10mins, selenizing rear film thickness is that 1950nm is thick, then takes out test piece and carries out the measurement of surface roughness.
Embodiment 2:
A kind of method for preparing porousness precursor layer and absorbed layer thin film planarization, predecessor weight ratio of constituents example is controlled to be: Cu/ (In+Ga)=0.85, Ga/ (In+Ga)=0.31; At first the Cu of part by weight, Ga material are put into vacuum induction melting furnace and carry out melting, vacuum degree 5 * 10
-2Torr, melting temperature is at 650 ℃/15mins, then casts in the mould of mild steel of three cun, wait to lower the temperature 12 as a child demoulding to take out the target idiosomes standby with the CuGa targets through being machined to three cun sputters; In addition the In material is put into vacuum induction melting furnace and carry out melting, vacuum degree 5 * 10
-2Torr, melting temperature is at 200 ℃/15mins, then casts in the mould of mild steel of three cun, wait to lower the temperature 12 as a child demoulding to take out the target idiosomes standby with the In targets through being machined to three cun sputters; Then take alkali-free glass as substrate, then the required glass baseplate, CuGa target, In target of plating put into the sputter cavity, with vacuum-pumping system, sputter cavity background pressure is evacuated to 0.8 * 10
-5After torr, utilize argon gas to be used as working gas, the operating pressure that will pass into argon gas control sputter cavity through choke valve is 2 * 10
-3Torr, plating rate 40nm/min, first with the thick Mo film of DC power supply sputter ground floor 500nm, then uses operating pressure 25 * 10
-3Torr, plating rate 4nm/min carry out the thick CIG absorbed layer precursors film of sputter second layer 1000nm, then coated film are placed in the selenizing stove and carry out rear selenizing, 620 ℃ of selenizing temperature, time 20mins, selenizing rear film thickness is that 2000nm is thick, then takes out test piece and carries out the measurement of surface roughness.
Embodiment 3:
A kind of method for preparing porousness precursor layer and absorbed layer thin film planarization, predecessor weight ratio of constituents example is controlled to be: Cu/ (In+Ga)=0.95, Ga/ (In+Ga)=0.42; At first the Cu of part by weight, Ga material are put into vacuum induction melting furnace and carry out melting, vacuum degree 5 * 10
-2Torr, melting temperature is at 650 ℃/15mins, then casts in the mould of mild steel of three cun, wait to lower the temperature 12 as a child demoulding to take out the target idiosomes standby with the CuGa targets through being machined to three cun sputters; In addition the In material is put into vacuum induction melting furnace and carry out melting, vacuum degree 5 * 10
-2Torr, melting temperature is at 200 ℃/15mins, then casts in the mould of mild steel of three cun, wait to lower the temperature 12 as a child demoulding to take out the target idiosomes standby with the In targets through being machined to three cun sputters; Then take alkali-free glass as substrate, then the required glass baseplate, CuGa target, In target of plating put into the sputter cavity, with vacuum-pumping system, sputter cavity background pressure is evacuated to 0.9 * 10
-5After torr, utilize argon gas to be used as working gas, the operating pressure that will pass into argon gas control sputter cavity through choke valve is 2 * 10
-3Torr, plating rate 40nm/min, first with the thick Mo film of DC power supply sputter ground floor 500nm, then uses operating pressure 30 * 10
-3Torr, plating rate 6nm/min carry out the thick CIG absorbed layer precursors film of sputter second layer 1000nm, then coated film are placed in the selenizing stove and carry out rear selenizing, 650 ℃ of selenizing temperature, time 30mins, selenizing rear film thickness is that 2050nm is thick, then takes out test piece and carries out the measurement of surface roughness.
Embodiment 4:
A kind of method for preparing porousness precursor layer and absorbed layer thin film planarization, predecessor weight ratio of constituents example is controlled to be: Cu/ (In+Ga)=0.6, Ga/ (In+Ga)=0.2; At first the Cu of part by weight, In, Ga material are put into vacuum induction melting furnace and carry out melting, vacuum degree 5 * 10
-2Torr, melting temperature is at 650 ℃/15mins, then casts in the mould of mild steel of three cun, wait to lower the temperature 12 as a child demoulding to take out the target idiosomes standby with the CuInGa targets through being machined to three cun sputters; Then take alkali-free glass as substrate, then required, plating glass baseplate and the CuInGa target is put into the sputter cavity, all the other are with embodiment 1.
Embodiment 5:
A kind of method for preparing porousness precursor layer and absorbed layer thin film planarization, predecessor weight ratio of constituents example is controlled to be: Cu/ (In+Ga)=0.85, Ga/ (In+Ga)=0.31; At first the Cu of part by weight, In, Ga material are put into vacuum induction melting furnace and carry out melting, vacuum degree 5 * 10
-2Torr, melting temperature is at 650 ℃/15mins, then casts in the mould of mild steel of three cun, wait to lower the temperature 12 as a child demoulding to take out the target idiosomes standby with the CuInGa targets through being machined to three cun sputters; Then take alkali-free glass as substrate, then required, plating glass baseplate and the CuInGa target is put into the sputter cavity, all the other are with embodiment 2.
Embodiment 6:
A kind of method for preparing porousness precursor layer and absorbed layer thin film planarization, predecessor weight ratio of constituents example is controlled to be: Cu/ (In+Ga)=0.95, Ga/ (In+Ga)=0.42; At first the Cu of part by weight, In, Ga material are put into vacuum induction melting furnace and carry out melting, vacuum degree 5 * 10
-2Torr, melting temperature is at 650 ℃/15mins, then casts in the mould of mild steel of three cun, wait to lower the temperature 12 as a child demoulding to take out the target idiosomes standby with the CuInGa targets through being machined to three cun sputters; Then take alkali-free glass as substrate, then required, plating glass baseplate and the CuInGa target is put into the sputter cavity, all the other are with embodiment 3.
Comparative Examples 1:
A kind of method for preparing porousness precursor layer and absorbed layer thin film planarization, predecessor weight ratio of constituents example is controlled to be: Cu/ (In+Ga)=0.7, Ga/ (In+Ga)=0.25; At first the Cu of part by weight, Ga material are put into vacuum induction melting furnace and carry out melting, vacuum degree 5 * 10
-2Torr, melting temperature is at 650 ℃/15mins, then casts in the mould of mild steel of three cun, wait to lower the temperature 12 as a child demoulding to take out the target idiosomes standby with the CuGa targets through being machined to three cun sputters; In addition the In material is put into vacuum induction melting furnace and carry out melting, vacuum degree 5 * 10
-2Torr, melting temperature is at 200 ℃/15mins, then casts in the mould of mild steel of three cun, wait to lower the temperature 12 as a child demoulding to take out the target idiosomes standby with the In targets through being machined to three cun sputters; Then take alkali-free glass as substrate, then the required glass baseplate, CuGa target, In target of plating put into the sputter cavity, with vacuum-pumping system, sputter cavity background pressure is evacuated to 0.75 * 10
-5After torr, utilize argon gas to be used as working gas, the operating pressure that will pass into argon gas control sputter cavity through choke valve is 2 * 10
-3Torr, plating rate 40nm/min, first with the thick Mo film of DC power supply sputter ground floor 500nm, then uses operating pressure 2.5 * 10
-3Torr, plating rate 12nm/min carrys out the thick CIG absorbed layer precursors film of sputter second layer 1000nm, then coated film is placed in the selenizing stove and carries out rear selenizing, 550 ℃ of selenizing temperature, time 15mins, selenizing rear film thickness is that 1980nm is thick, then takes out test piece and carries out the measurement of surface roughness.
Comparative Examples 2:
A kind of method for preparing porousness precursor layer and absorbed layer thin film planarization, predecessor weight ratio of constituents example is controlled to be: Cu/ (In+Ga)=0.9, Ga/ (In+Ga)=0.39; At first the Cu of part by weight, In, Ga material are put into vacuum induction melting furnace and carry out melting, vacuum degree 5 * 10
-2Torr, melting temperature is at 650 ℃/15mins, then casts in the mould of mild steel of three cun, wait to lower the temperature 12 as a child demoulding to take out the target idiosomes standby with the CuInGa targets through being machined to three cun sputters; Then take alkali-free glass as substrate, then required, plating glass baseplate and the CuInGa target is put into the sputter cavity, with vacuum-pumping system, sputter cavity background pressure is evacuated to 0.85 * 10
-5After torr, utilize argon gas to be used as working gas, the operating pressure that will pass into argon gas control sputter cavity through choke valve is 2 * 10
-3Torr, plating rate 40nm/min, first with the thick Mo film of DC power supply sputter ground floor 500nm, then uses operating pressure 2.5 * 10
-3Torr, plating rate 12nm/min carrys out the thick CIG absorbed layer precursors film of sputter second layer 1000nm, then coated film is placed in the selenizing stove and carries out rear selenizing, 620 ℃ of selenizing temperature, time 25mins, selenizing rear film thickness is that 2020nm is thick, then takes out test piece and carries out the measurement of surface roughness.
Comparative Examples 3:
A kind of method for preparing porousness precursor layer and absorbed layer thin film planarization, predecessor weight ratio of constituents example is controlled to be: Cu/ (In+Ga)=0.5, Ga/ (In+Ga)=0.15; At first the Cu of part by weight, Ga material are put into vacuum induction melting furnace and carry out melting, vacuum degree 5 * 10
-2Torr, melting temperature is at 650 ℃/15mins, then casts in the mould of mild steel of three cun, wait to lower the temperature 12 as a child demoulding to take out the target idiosomes standby with the CuGa targets through being machined to three cun sputters; In addition the In material is put into vacuum induction melting furnace and carry out melting, vacuum degree 5 * 10
-2Torr, melting temperature is at 200 ℃/15mins, then casts in the mould of mild steel of three cun, wait to lower the temperature 12 as a child demoulding to take out the target idiosomes standby with the In targets through being machined to three cun sputters; Then take alkali-free glass as substrate, then the required glass baseplate, CuGa target, In target of plating put into the sputter cavity, with vacuum-pumping system, sputter cavity background pressure is evacuated to 0.6 * 10
-5After torr, utilize argon gas to be used as working gas, the operating pressure that will pass into argon gas control sputter cavity through choke valve is 2 * 10
-3Torr, plating rate 40nm/min, first with the thick Mo film of DC power supply sputter ground floor 500nm, then uses operating pressure 22 * 10
-3Torr, plating rate 3nm/min carry out the thick CIG absorbed layer precursors film of sputter second layer 1000nm, then coated film are placed in the selenizing stove and carry out rear selenizing, 480 ℃ of selenizing temperature, time 8mins, selenizing rear film thickness is that 1900nm is thick, then takes out test piece and carries out the measurement of surface roughness.
Comparative Examples 4:
A kind of method for preparing porousness precursor layer and absorbed layer thin film planarization, predecessor weight ratio of constituents example is controlled to be: Cu/ (In+Ga)=0.98, Ga/ (In+Ga)=0.5; At first the Cu of part by weight, In, Ga material are put into vacuum induction melting furnace and carry out melting, vacuum degree 5 * 10
-2Torr, melting temperature is at 650 ℃/15mins, then casts in the mould of mild steel of three cun, wait to lower the temperature 12 as a child demoulding to take out the target idiosomes standby with the CuInGa targets through being machined to three cun sputters; Then take alkali-free glass as substrate, then required, plating glass baseplate and the CuInGa target is put into the sputter cavity, with vacuum-pumping system, sputter cavity background pressure is evacuated to 0.95 * 10
-5After torr, utilize argon gas to be used as working gas, the operating pressure that will pass into argon gas control sputter cavity through choke valve is 2 * 10
-3Torr, plating rate 40nm/min, first with the thick Mo film of DC power supply sputter ground floor 500nm, then uses operating pressure 28 * 10
-3Torr, plating rate 7nm/min carry out the thick CIG absorbed layer precursors film of sputter second layer 1000nm, then coated film are placed in the selenizing stove and carry out rear selenizing, 700 ℃ of selenizing temperature, time 35mins, selenizing rear film thickness is that 2080nm is thick, then takes out test piece and carries out the measurement of surface roughness.
After the predecessor film that each embodiment and Comparative Examples make and selenizing, the measurement of absorbed layer film surface rugosity is as shown in the table:
Can find out from upper table result, the work atmosphere pressure that the present invention adopts is greater than 10mtorr, and the plating rate is less than 10nm/mins low-power sputter, made CIG precursor layer and CIGS absorbed layer film can effectively significantly reduce surface roughness, are starkly lower than Comparative Examples 1, the 2 work atmosphere pressure 2.5 * 10 that adopt
-3Torr, the sputter of plating rate 12nm/min; The sputtering process that the present invention simultaneously adopts has also promoted the efficiency of CIGS thin-film solar cells, especially best with the resultant effect of embodiment 2 and embodiment 5, therefore the present invention has simplified the plated film of follow-up resilient coating and optical window layer, can reduce production costs and improve conversion efficiency and volume production efficiency, meet the needs of production.
Claims (5)
1. method for preparing porousness precursor layer and absorbed layer thin film planarization, it is characterized by: at first Cu, Ga material are put into vacuum induction melting furnace and carry out melting, then cast in the mould of mild steel of three cun, wait to lower the temperature 12 as a child demoulding to take out the target idiosomes standby with the CuGa targets through being machined to three cun sputters; In addition the In material is put into vacuum induction melting furnace and carries out melting, then cast in the mould of mild steel of three cun, wait to lower the temperature 12 as a child demoulding to take out the target idiosomes standby with the In targets through being machined to three cun sputters; Then take alkali-free glass as substrate, then the required glass baseplate, CuGa target, In target of plating put into the sputter cavity, first with the thick Mo film of DC power supply sputter ground floor 500nm, then the CIG absorbed layer precursors film that sputter second layer 1000nm is thick, then coated film is placed in the selenizing stove and carries out rear selenizing, then take out test piece, obtain.
2. method for preparing porousness precursor layer and absorbed layer thin film planarization, it is characterized by: predecessor weight ratio of constituents example is controlled to be: Cu/ (In+Ga)=0.6-0.95, Ga/ (In+Ga)=0.2-0.42; At first the Cu of part by weight, Ga material are put into vacuum induction melting furnace and carry out melting, vacuum degree 5 * 10
-2Torr, melting temperature is at 650 ℃/15mins, then casts in the mould of mild steel of three cun, wait to lower the temperature 12 as a child demoulding to take out the target idiosomes standby with the CuGa targets through being machined to three cun sputters; In addition the In material is put into vacuum induction melting furnace and carry out melting, vacuum degree 5 * 10
-2Torr, melting temperature is at 200 ℃/15mins, then casts in the mould of mild steel of three cun, wait to lower the temperature 12 as a child demoulding to take out the target idiosomes standby with the In targets through being machined to three cun sputters; Then take alkali-free glass as substrate, then the required glass baseplate, CuGa target, In target of plating put into the sputter cavity, with vacuum-pumping system, sputter cavity background pressure is evacuated to 0.7 * 10
-5-0.9 * 10
-5After torr, utilize argon gas to be used as working gas, the operating pressure that will pass into argon gas control sputter cavity through choke valve is 2 * 10
-3Torr, plating rate 40nm/min, first with the thick Mo film of DC power supply sputter ground floor 500nm, then uses operating pressure 20 * 10
-3-30 * 10
-3Torr, plating rate 2-6nm/min carrys out the thick CIG absorbed layer precursors film of sputter second layer 1000nm, then coated film is placed in the selenizing stove and carries out rear selenizing, selenizing temperature 500-650 ℃, time 10-30mins, selenizing rear film thickness is that 1950-2050nm is thick, then takes out test piece, obtains.
3. method for preparing porousness precursor layer and absorbed layer thin film planarization, it is characterized by: predecessor weight ratio of constituents example is controlled to be: Cu/ (In+Ga)=0.6-0.95, Ga/ (In+Ga)=0.2-0.42; At first the Cu of part by weight, In, Ga material are put into vacuum induction melting furnace and carry out melting, vacuum degree 5 * 10
-2Torr, melting temperature is at 650 ℃/15mins, then casts in the mould of mild steel of three cun, wait to lower the temperature 12 as a child demoulding to take out the target idiosomes standby with the CuInGa targets through being machined to three cun sputters; Then take alkali-free glass as substrate, then required, plating glass baseplate and the CuInGa target is put into the sputter cavity, with vacuum-pumping system, sputter cavity background pressure is evacuated to 0.7 * 10
-5-0.9 * 10
-5After torr, utilize argon gas to be used as working gas, the operating pressure that will pass into argon gas control sputter cavity through choke valve is 2 * 10
-3Torr, plating rate 40nm/min, first with the thick Mo film of DC power supply sputter ground floor 500nm, then uses operating pressure 20 * 10
-3-30 * 10
-3Torr, plating rate 2-6nm/min carrys out the thick CIG absorbed layer precursors film of sputter second layer 1000nm, then coated film is placed in the selenizing stove and carries out rear selenizing, selenizing temperature 500-650 ℃, time 10-30mins, selenizing rear film thickness is that 1950-2050nm is thick, then takes out test piece, obtains.
4. a kind of method for preparing porousness precursor layer and absorbed layer thin film planarization as claimed in claim 2, it is characterized by: predecessor weight ratio of constituents example is controlled to be: Cu/ (In+Ga)=0.85, Ga/ (In+Ga)=0.31; At first the Cu of part by weight, Ga material are put into vacuum induction melting furnace and carry out melting, vacuum degree 5 * 10
-2Torr, melting temperature is at 650 ℃/15mins, then casts in the mould of mild steel of three cun, wait to lower the temperature 12 as a child demoulding to take out the target idiosomes standby with the CuGa targets through being machined to three cun sputters; In addition the In material is put into vacuum induction melting furnace and carry out melting, vacuum degree 5 * 10
-2Torr, melting temperature is at 200 ℃/15mins, then casts in the mould of mild steel of three cun, wait to lower the temperature 12 as a child demoulding to take out the target idiosomes standby with the In targets through being machined to three cun sputters; Then take alkali-free glass as substrate, then the required glass baseplate, CuGa target, In target of plating put into the sputter cavity, with vacuum-pumping system, sputter cavity background pressure is evacuated to 0.8 * 10
-5After torr, utilize argon gas to be used as working gas, the operating pressure that will pass into argon gas control sputter cavity through choke valve is 2 * 10
-3Torr, plating rate 40nm/min, first with the thick Mo film of DC power supply sputter ground floor 500nm, then uses operating pressure 25 * 10
-3Torr, plating rate 4nm/min carry out the thick CIG absorbed layer precursors film of sputter second layer 1000nm, then coated film are placed in the selenizing stove and carry out rear selenizing, 620 ℃ of selenizing temperature, time 20mins, selenizing rear film thickness is that 2000nm is thick, then take out test piece, obtain.
5. a kind of method for preparing porousness precursor layer and absorbed layer thin film planarization as claimed in claim 3, it is characterized by: predecessor weight ratio of constituents example is controlled to be: Cu/ (In+Ga)=0.85, Ga/ (In+Ga)=0.31; At first the Cu of part by weight, In, Ga material are put into vacuum induction melting furnace and carry out melting, vacuum degree 5 * 10
-2Torr, melting temperature is at 650 ℃/15mins, then casts in the mould of mild steel of three cun, wait to lower the temperature 12 as a child demoulding to take out the target idiosomes standby with the CuInGa targets through being machined to three cun sputters; Then take alkali-free glass as substrate, then required, plating glass baseplate and the CuInGa target is put into the sputter cavity, with vacuum-pumping system, sputter cavity background pressure is evacuated to 0.8 * 10
-5After torr, utilize argon gas to be used as working gas, the operating pressure that will pass into argon gas control sputter cavity through choke valve is 2 * 10
-3Torr, plating rate 40nm/min, first with the thick Mo film of DC power supply sputter ground floor 500nm, then uses operating pressure 25 * 10
-3Torr, plating rate 4nm/min carry out the thick CIG absorbed layer precursors film of sputter second layer 1000nm, then coated film are placed in the selenizing stove and carry out rear selenizing, 620 ℃ of selenizing temperature, time 20mins, selenizing rear film thickness is that 2000nm is thick, then take out test piece, obtain.
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