CN103515484B - Matte transparent conductive film of a kind of periodic structure and preparation method thereof - Google Patents
Matte transparent conductive film of a kind of periodic structure and preparation method thereof Download PDFInfo
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- CN103515484B CN103515484B CN201310416643.XA CN201310416643A CN103515484B CN 103515484 B CN103515484 B CN 103515484B CN 201310416643 A CN201310416643 A CN 201310416643A CN 103515484 B CN103515484 B CN 103515484B
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- 230000000737 periodic effect Effects 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000010408 film Substances 0.000 claims abstract description 149
- 239000000758 substrate Substances 0.000 claims abstract description 82
- 239000011521 glass Substances 0.000 claims abstract description 65
- 238000000034 method Methods 0.000 claims abstract description 58
- 239000010409 thin film Substances 0.000 claims abstract description 36
- 230000008569 process Effects 0.000 claims abstract description 29
- 238000001020 plasma etching Methods 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 230000000694 effects Effects 0.000 claims abstract description 12
- 230000009471 action Effects 0.000 claims abstract description 10
- 238000010276 construction Methods 0.000 claims abstract description 9
- 238000012986 modification Methods 0.000 claims abstract description 9
- 230000004048 modification Effects 0.000 claims abstract description 9
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 278
- 239000011787 zinc oxide Substances 0.000 claims description 139
- 239000004793 Polystyrene Substances 0.000 claims description 59
- 239000004005 microsphere Substances 0.000 claims description 33
- 229920002223 polystyrene Polymers 0.000 claims description 33
- 239000000243 solution Substances 0.000 claims description 17
- 239000007787 solid Substances 0.000 claims description 16
- 229960001296 zinc oxide Drugs 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 14
- 239000004816 latex Substances 0.000 claims description 8
- 229920000126 latex Polymers 0.000 claims description 8
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 238000012545 processing Methods 0.000 claims description 8
- 238000001338 self-assembly Methods 0.000 claims description 8
- 239000004065 semiconductor Substances 0.000 claims description 8
- 230000003595 spectral effect Effects 0.000 claims description 8
- 238000005530 etching Methods 0.000 claims description 6
- 230000001795 light effect Effects 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 2
- 238000004544 sputter deposition Methods 0.000 description 39
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 30
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 15
- 229910052786 argon Inorganic materials 0.000 description 15
- 239000011324 bead Substances 0.000 description 11
- 230000015572 biosynthetic process Effects 0.000 description 7
- 238000000151 deposition Methods 0.000 description 7
- 229910052739 hydrogen Inorganic materials 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 6
- 230000008021 deposition Effects 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 229910006404 SnO 2 Inorganic materials 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 229910021424 microcrystalline silicon Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000001505 atmospheric-pressure chemical vapour deposition Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000005543 nano-size silicon particle Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 238000001039 wet etching 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
- H01L31/02—Details
- H01L31/0236—Special surface textures
- H01L31/02366—Special surface textures of the substrate or of a layer on the substrate, e.g. textured ITO/glass substrate or superstrate, textured polymer layer on glass substrate
-
- 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
- H01L31/02—Details
- H01L31/0224—Electrodes
- H01L31/022466—Electrodes made of transparent conductive layers, e.g. TCO, ITO layers
- H01L31/022483—Electrodes made of transparent conductive layers, e.g. TCO, ITO layers composed of zinc oxide [ZnO]
-
- 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
- H01L31/074—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 a heterojunction with an element of Group IV of the Periodic System, e.g. ITO/Si, GaAs/Si or CdTe/Si 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
- H01L31/1884—Manufacture of transparent electrodes, e.g. TCO, ITO
-
- 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
A kind of matte transparent conductive film of periodic structure, comprise glass substrate layer, the ground floor ZnO film of lifting plate effect and the second layer ZnO film of a modification and form laminated construction successively, ground floor ZnO film thickness is 300-1500nm, the thickness of second layer ZnO film is 400-1000nm, forms the periodic structure matte transparent conductive film with scattering process; Its preparation method: utilize water bath Method to assemble PS microballoon, use O
2plasma etching PS microballoon, utilizes the template action of PS microballoon, obtains the sunken light ZnO transparent conductive thin film with periodic structure.Advantage of the present invention is: the ZnO film of preparation has good sunken light effect, thin film solar cell is used for as front electrode, had to good scattering process in the wave-length coverage that 400-1100nm battery can be utilized, the light path of incident light in silicon-base thin-film battery can be increased, improve light utilization efficiency.
Description
Technical field
The invention belongs to the technology of preparing of the transparent conductive film of thin film solar cell, matte transparent conductive film of especially a kind of periodic structure and preparation method thereof.
Background technology
Enter 21 century, energy security and environmental protection have become the problem of globalization.World many countries using the important measures of Renewable Energy Development as alleviation energy supply contradiction, reply climate change, and has formulated development strategy, proposes clear and definite developing goal and corresponding incentive policy.Photovoltaic generation is that the internationally recognized solution energy lacks and one of effective way of problem of environmental pollution.The carrier of photovoltaic generation is solar cell, and the key that solar cell can be made to become future source of energy important component part be photovoltaic generation cost to be dropped to conventional energy resource suitable.
Transparent conductive film is as the important component part of solar cell, and the performance impact of its suede degree characteristic to battery is most important.Transparent conductive oxide (TCO) film be most widely used in current hull cell is F doping SnO
2film (SnO
2: F) and Sn doping In
2o
3film (In
2o
3: Sn).F adulterates SnO
2film normally utilizes atmospheric pressure cvd (APCVD) technology to prepare, growth temperature higher (~ 500 DEG C), there is certain suede structure, but this type TCO is unfavorable for limiting the hull cell material that grows in low temperature depositing and strong H plasma environment it and apply further.And Sn doping In
2o
3film, the In element in its film composition is rare and cost is higher, and is not easy to obtain coarse surface topography, and in strong H plasma environment, performance easily worsens, and also limit its extensive use in thin film solar cell.Compared to In
2o
3and SnO
2thin-film material, ZnO film has source material to be enriched, nontoxic and relative growth temperature is low and the feature such as stable performance obtains extensive investigation and application in strong H plasma environment.Research shows: for Si base thin film solar battery (amorphous silicon battery, micro-crystalline silicon cell and silica-base film many knots laminated cell), the light trapping effect of TCO thin film is particularly important on the impact of device performance.The structure falling into light can improve light scattering ability, increases the light path of incident light.Therefore, the application of light trapping structure effectively can strengthen the optical absorption of intrinsic layer, improves short-circuit current density, thus raising battery efficiency, and what is more important: fall into the introducing of light, can the thickness of thinning battery active layer, this is very important to reducing costs.
Current preparation is with the transparent conductive film of the method mainly random matte of the transparent conductive film of light trapping structure, random matte mainly carries out by doping ZnO (ZnO:Al, ZnO:Ga, ZnO:B, ZnO:H, ZnO:Mo or ZnO:W) film produced sputtering the light trapping structure that wet etching process obtains " cratering ", thus the scattering improved incident light, increase active layer to the absorption of light.But carry out wet method post-etching for sputtering technology making ZnO film and will expect well sunken light, the characteristic size of its " cratering " and roughness need very large, and such ZnO film can only high temperature sputtering (being greater than 250oC).Such one side limits the substrate of battery applications, also improves the cost preparing battery on the other hand.
Summary of the invention
The present invention seeks to the above-mentioned deficiency for overcoming prior art, matte transparent conductive film that a kind of periodic structure is provided and preparation method thereof, the zinc oxide transparent conductive film of the periodic structure in the method has good sunken light effect, increase the light path of incident light in silicon-base thin-film battery, to reach raising light utilization efficiency, and then improve the object of battery efficiency.
Technical scheme of the present invention:
A kind of matte transparent conductive film of periodic structure, comprise substrate layer, the ground floor ZnO film of lifting plate effect and the second layer ZnO film of a modification also form laminated construction successively, substrate layer is hard substrates glass, ZnO film is doping zinc-oxide n-type semiconductor, comprise ZnO:H, ZnO:Al, ZnO:Ga, ZnO:B, ZnO:H, at least one in ZnO:Mo and ZnO:W, wherein ground floor ZnO film thickness is 300-1500nm, the thickness of second layer ZnO film is 400-1000nm, form the matte transparent conductive film with the periodic structure of wide spectral scattering process, the r.m.s. roughness of the ZnO matte transparent conductive film of periodic structure is 30-250 nm.
A preparation method for the matte transparent conductive film of described periodic structure, utilizes water bath Method to assemble PS microballoon, uses O
2plasma etching PS microballoon, utilizes the template action of PS microballoon, and obtain the sunken light ZnO transparent conductive thin film with periodic structure, step is as follows:
1) glass substrate is immersed in H
2sO
4with H
2o
2volume ratio be 2:1 mixed solution in carry out hydrophilic treated, the processing time is 2-10 hour;
2) above-mentioned glass substrate is placed on horizontal stand, be 1-5 μm by particle diameter, concentration is that the polystyrene microsphere latex solution of 5wt% vertically drips on a glass substrate, solution slowly spreads apart and makes that ethene microballoon is uneven to be interspersed among in glass substrate, then glass substrate is placed on steam and carries out self assembly, through the water-bath of 30min, the polystyrene microsphere of the formation individual layer six side solid matter in glass substrate;
3) by the polystyrene microsphere of above-mentioned individual layer six side solid matter, O is carried out
2plasma etching (RIE), after etching, the size of polystyrene microsphere is 0.5-4 μm;
4) polystyrene microsphere after etching adopting magnetically controlled sputter method deposit ground floor thickness is the ZnO film of 300-1500nm, then glass substrate is placed in water and carries out ultrasonic process until ethene bead processes totally completely;
5) adopt the method for magnetron sputtering to deposit the ZnO film that second layer thickness is 400-1000nm again, the matte transparent conductive film with periodic structure can be obtained.
A kind of application of matte transparent conductive film of described periodic structure, for make thin film solar cell electrically conducting transparent before electrode, described thin film solar cell is that amorphous is silica-based, microcrystalline silicon, nano silicon-based thin film solar cell or tie laminated silicon-base film solar cell more.
Advantage of the present invention and good effect:
The present invention utilizes the template action of PS microballoon and the ZnO film of deposition, achieves the preparation of the ZnO film of high suede degree periodic structure, and has good sunken light effect; Zinc oxide conductive thin film is used for thin film solar cell as front electrode, in the wave-length coverage that 400-1100nm battery can be utilized, is there is to good scattering process, the light path of incident light in silicon-base thin-film battery can be increased, improve light utilization efficiency.
Accompanying drawing explanation
Fig. 1 is the structural representation of the ZnO film of periodic structure.
Fig. 2 adopts PS bead to be the shape appearance figure of the Textured ZnO Transparent Conductive Thin Film of the periodic structure of Template preparation.
Fig. 3 adopts PS bead to be integrated reflection and the suede degree of the Textured ZnO Transparent Conductive Thin Film of the periodic structure of Template preparation.
Embodiment
embodiment 1:
A kind of matte transparent conductive film of periodic structure, as shown in Figure 1, comprise substrate layer, the ground floor ZnO film of lifting plate effect and the second layer ZnO film of a modification also form laminated construction successively, substrate layer is hard substrates glass, ZnO film is doping zinc-oxide n-type semiconductor ZnO:H, wherein ground floor ZnO film thickness is 800nm, the thickness of second layer ZnO film is 400nm, form the matte transparent conductive film with the periodic structure of wide spectral scattering process, the r.m.s. roughness of the ZnO matte transparent conductive film of periodic structure is 80 nm.
A preparation method for the matte transparent conductive film of described periodic structure, utilizes water bath Method to assemble PS microballoon, uses O
2plasma etching PS microballoon, utilizes the template action of PS microballoon, and obtain the sunken light ZnO transparent conductive thin film with periodic structure, step is as follows:
1) glass substrate is immersed in H
2sO
4with H
2o
2volume ratio be 2:1 mixed solution in carry out hydrophilic treated, the processing time is 6 hours;
2) above-mentioned glass substrate is placed on horizontal stand, be 2 μm by particle diameter, concentration is that the polystyrene microsphere latex solution of 5wt% vertically drips on a glass substrate, solution slowly spreads apart and makes that ethene microballoon is uneven to be interspersed among in glass substrate, then glass substrate is placed on steam and carries out self assembly, through the water-bath of 30min, the polystyrene microsphere of the formation individual layer six side solid matter in glass substrate;
3) by the polystyrene microsphere of above-mentioned individual layer six side solid matter, O is carried out
2plasma etching (RIE), oxygen flow 10 Sccm, air pressure 11pa, radio-frequency power 150W, etch period 6min, the particle diameter of microballoon is 1.8 μm;
4) ethene microballoon after etching adopts magnetically controlled sputter method deposit ZnO:H (HZO) film that ground floor thickness is 800nm: target is ZnO ceramic target, prepare the zinc-oxide film of low-resistivity and high transmission: underlayer temperature is room temperature, base vacuum is 5 × 10
-5pa, hydrogen flowing quantity is 3sccm, argon flow amount is 52sccm, sputtering pressure is 4.5mTorr, electrode spacing is 30 mm, and sputtering power is 380 W, and sputtering time is 40 min, obtain the ZnO:H transparent conductive film that thickness is about 800 nm, then glass substrate is placed in water and carries out ultrasonic process until ethene bead processes totally completely;
5) method of magnetron sputtering is adopted to deposit the ZnO:H film that second layer thickness is 400nm again: underlayer temperature is room temperature, and base vacuum is 5 × 10
-5pa, hydrogen flowing quantity is 3sccm, argon flow amount is 52sccm, and sputtering pressure is 4.5mTorr, and electrode spacing is 30 mm, sputtering power is 380 W, sputtering time is 20min, and thickness is 400 nm, can obtain the matte transparent conductive film with periodic structure, its r.m.s. roughness is 80nm, and square resistance is 16.5
.
Fig. 2 be adopt PS bead be the periodic structure of Template preparation the shape appearance figure of Textured ZnO Transparent Conductive Thin Film.Show from shape appearance figure: the ZnO film of this periodic structure can obtain larger matte roughness, and periodic structure is obvious.
Fig. 3 be adopt PS bead be the periodic structure of Template preparation the integrated reflection of shape appearance figure of Textured ZnO Transparent Conductive Thin Film and suede degree.Show in figure: this periodic structure transparent conductive film at 800nm and 1100nm place the suede degree factor reaches 58% and 28% respectively, there is good light trapping effect.
Before the matte transparent conductive film of prepared periodic structure can be used as electrically conducting transparent, electrode is for microcrystalline silicon film solar cell, in the wave-length coverage that 400-1100nm battery can be utilized, be there is to good scattering process, the light path of incident light in silicon-base thin-film battery can be increased, improve light utilization efficiency.
embodiment 2:
A kind of matte transparent conductive film of periodic structure, as shown in Figure 1, comprise substrate layer, the ground floor ZnO film of lifting plate effect and the second layer ZnO film of a modification also form laminated construction successively, substrate layer is hard substrates glass, ZnO film is doping zinc-oxide n-type semiconductor ZnO:Al (AZO) film, wherein ground floor ZnO film thickness is 700nm, the thickness of second layer ZnO film is 400nm, form the matte transparent conductive film with the periodic structure of wide spectral scattering process, the r.m.s. roughness of the ZnO matte transparent conductive film of periodic structure is 85 nm.
A preparation method for the matte transparent conductive film of described periodic structure, utilizes water bath Method to assemble PS microballoon, uses O
2plasma etching PS microballoon, utilizes the template action of PS microballoon, and obtain the sunken light ZnO transparent conductive thin film with periodic structure, step is as follows:
1) glass substrate is immersed in H
2sO
4with H
2o
2volume ratio be 2:1 mixed solution in carry out hydrophilic treated, the processing time is 5 hours;
2) above-mentioned glass substrate is placed on horizontal stand, be 2 μm by particle diameter, concentration is that the polystyrene microsphere latex solution of 5wt% vertically drips on a glass substrate, solution slowly spreads apart and makes that ethene microballoon is uneven to be interspersed among in glass substrate, then glass substrate is placed on steam and carries out self assembly, through the water-bath of 30min, the polystyrene microsphere of the formation individual layer six side solid matter in glass substrate;
3) by the polystyrene microsphere of above-mentioned individual layer six side solid matter, O is carried out
2plasma etching (RIE), oxygen flow 10 Sccm, air pressure 11pa, radio-frequency power 150W, etch period 8min, the particle diameter of microballoon is 1.6 μm;
4) employing magnetically controlled sputter method deposition ground floor thickness is ZnO:Al (AZO) film of 700nm, adopts ZnO:Al
2o
3ceramic target, wherein Al
2o
3mass fraction is 2 wt.%; Employing pure argon sputters, and prepare the polycrystalline zinc oxide film of low-resistivity: underlayer temperature is room temperature, base vacuum is 5 × 10
-5pa, argon flow amount is 55 sccm, and sputtering pressure is 3.3 mTorr, electrode spacing is 50 mm, and sputtering power is 460W, sputtering 30min, obtain the ZnO:Al transparent conductive film that thickness is 700nm, then glass substrate is placed in water and carries out ultrasonic process until ethene bead processes totally completely;
5) method of magnetron sputtering is adopted to deposit the ZnO:Al transparent conductive film that second layer thickness is 400nm again: underlayer temperature is room temperature, and base vacuum is 5 × 10
-5pa, argon flow amount is 55 sccm, and sputtering pressure is 3.3 mTorr, and electrode spacing is 50 mm, and sputtering power is 460W, and sputtering 17min, obtain the ZnO:Al transparent conductive film of thickness 400nm, its r.m.s. roughness is 85nm, and square resistance is 15
.
Adopt the shape appearance figure of sunken light ZnO transparent conductive thin film of periodic structure and integrated reflection and suede degree and embodiment 1 roughly the same.
embodiment 3:
A kind of matte transparent conductive film of periodic structure, as shown in Figure 1, comprise substrate layer, the ground floor ZnO film of lifting plate effect and the second layer ZnO film of a modification also form laminated construction successively, substrate layer is hard substrates glass, ZnO film is doping zinc-oxide n-type semiconductor ZnO:H (HZO) film, wherein ground floor ZnO film thickness is 900nm, the thickness of second layer ZnO film is 400nm, form the matte transparent conductive film with the periodic structure of wide spectral scattering process, the r.m.s. roughness of the ZnO matte transparent conductive film of periodic structure is 120 nm.
A preparation method for the matte transparent conductive film of described periodic structure, utilizes water bath Method to assemble PS microballoon, uses O
2plasma etching PS microballoon, utilizes the template action of PS microballoon, and obtain the sunken light ZnO transparent conductive thin film with periodic structure, step is as follows:
1) glass substrate is immersed in H
2sO
4with H
2o
2volume ratio be 2:1 mixed solution in carry out hydrophilic treated, the processing time is 5 hours;
2) above-mentioned glass substrate is placed on horizontal stand, be 3 μm by particle diameter, concentration is that the polystyrene microsphere latex solution of 5wt% vertically drips on a glass substrate, solution slowly spreads apart and makes that ethene microballoon is uneven to be interspersed among in glass substrate, then glass substrate is placed on steam and carries out self assembly, through the water-bath of 30min, the polystyrene microsphere of the formation individual layer six side solid matter in glass substrate;
3) by the polystyrene microsphere of above-mentioned individual layer six side solid matter, O is carried out
2plasma etching (RIE), oxygen flow 10 Sccm, air pressure 11pa, radio-frequency power 150W, etch period 10min, the particle diameter of microballoon is 2.4 μm;
4) employing magnetically controlled sputter method deposition ground floor thickness is ZnO:H (HZO) film of 900nm, and target is ZnO ceramic target, prepares the zinc-oxide film of low-resistivity and high transmission: underlayer temperature is room temperature, and base vacuum is 5 × 10
-5pa, hydrogen flowing quantity is 3sccm, and argon flow amount is 52sccm, and sputtering pressure is 4.5mTorr, and electrode spacing is 30 mm, and sputtering power is 380 W, and sputtering time is 45 min, obtains the ZnO:H transparent conductive film that thickness is 900 nm; , then glass substrate is placed in water and carries out ultrasonic process until ethene bead processes totally completely;
5) method of magnetron sputtering is adopted to deposit the ZnO:H transparent conductive film that second layer thickness is 400nm again: underlayer temperature is room temperature, and base vacuum is 5 × 10
-5pa, hydrogen flowing quantity is 3sccm, argon flow amount is 52sccm, and sputtering pressure is 4.5mTorr, and electrode spacing is 30 mm, sputtering power is 380 W, sputtering time is 20 min, and thickness is 400nm, so just obtains the transparent conductive film with periodic structure, its r.m.s. roughness is 120nm, and square resistance is 10
.
Adopt the shape appearance figure of sunken light ZnO transparent conductive thin film of periodic structure and integrated reflection and suede degree and embodiment 1 roughly the same.
embodiment 4:
A kind of matte transparent conductive film of periodic structure, as shown in Figure 1, comprise substrate layer, the ground floor ZnO film of lifting plate effect and the second layer ZnO film of a modification also form laminated construction successively, substrate layer is hard substrates glass, ZnO film is doping zinc-oxide n-type semiconductor ZnO:Ga (GZO) film, wherein ground floor ZnO film thickness is 1200nm, the thickness of second layer ZnO film is 500nm, form the matte transparent conductive film with the periodic structure of wide spectral scattering process, the r.m.s. roughness of the ZnO matte transparent conductive film of periodic structure is 160 nm.
A preparation method for the matte transparent conductive film of described periodic structure, utilizes water bath Method to assemble PS microballoon, uses O
2plasma etching PS microballoon, utilizes the template action of PS microballoon, and obtain the sunken light ZnO transparent conductive thin film with periodic structure, step is as follows:
1) glass substrate is immersed in H
2sO
4with H
2o
2volume ratio be 2:1 mixed solution in carry out hydrophilic treated, the processing time is 7 hours;
2) above-mentioned glass substrate is placed on horizontal stand, be 4 μm by particle diameter, concentration is that the polystyrene microsphere latex solution of 5wt% vertically drips on a glass substrate, solution slowly spreads apart and makes that ethene microballoon is uneven to be interspersed among in glass substrate, then glass substrate is placed on steam and carries out self assembly, through the water-bath of 30min, the polystyrene microsphere of the formation individual layer six side solid matter in glass substrate;
3) by the polystyrene microsphere of above-mentioned individual layer six side solid matter, O is carried out
2plasma etching (RIE), oxygen flow 10 Sccm, air pressure 9pa, radio-frequency power 150W, etch period 8min, the particle diameter of microballoon is 3.4 μm;
4) employing magnetically controlled sputter method deposition ground floor thickness is ZnO:Ga (GZO) film of 1200nm, adopts ZnO:Ga
2o
3ceramic target, wherein Ga
2o
3mass fraction is 2 wt.%; Employing pure argon sputters, and prepare the polycrystalline zinc oxide film of low-resistivity: underlayer temperature is room temperature, base vacuum is 5 × 10
-5pa, argon flow amount is 55 sccm, and sputtering pressure is 3.3 mTorr, electrode spacing is 50 mm, and sputtering power is 460W, sputtering 50min, obtain the GZO transparent conductive film that thickness is about 1200nm, then glass substrate is placed in water and carries out ultrasonic process until ethene bead processes totally completely;
5) method of magnetron sputtering is adopted to deposit the GZO transparent conductive film that second layer thickness is 500nm again: underlayer temperature is room temperature, and base vacuum is 5 × 10
-5pa, argon flow amount is 55 sccm, and sputtering pressure is 3.3 mTorr, and electrode spacing is 50 mm, sputtering power is 460W, and sputtering time is 21 min, and thickness is 500nm, so just obtain the transparent conductive film with periodic structure, its r.m.s. roughness is 160nm, and square resistance is 8
.
Adopt the shape appearance figure of sunken light ZnO transparent conductive thin film of periodic structure and integrated reflection and suede degree and embodiment 1 roughly the same.
embodiment 5:
A kind of matte transparent conductive film of periodic structure, as shown in Figure 1, comprise substrate layer, the ground floor ZnO film of lifting plate effect and the second layer ZnO film of a modification also form laminated construction successively, substrate layer is hard substrates glass, ZnO film is doping zinc-oxide n-type semiconductor ZnO:H (HZO) film, wherein ground floor ZnO film thickness is 1000nm, the thickness of second layer ZnO film is 500nm, form the matte transparent conductive film with the periodic structure of wide spectral scattering process, the r.m.s. roughness of the ZnO matte transparent conductive film of periodic structure is 140 nm.
A preparation method for the matte transparent conductive film of described periodic structure, utilizes water bath Method to assemble PS microballoon, uses O
2plasma etching PS microballoon, utilizes the template action of PS microballoon, and obtain the sunken light ZnO transparent conductive thin film with periodic structure, step is as follows:
1) glass substrate is immersed in H
2sO
4with H
2o
2volume ratio be 2:1 mixed solution in carry out hydrophilic treated, the processing time is 4 hours;
2) above-mentioned glass substrate is placed on horizontal stand, be 3 μm by particle diameter, concentration is that the polystyrene microsphere latex solution of 5wt% vertically drips on a glass substrate, solution slowly spreads apart and makes that ethene microballoon is uneven to be interspersed among in glass substrate, then glass substrate is placed on steam and carries out self assembly, through the water-bath of 30min, the polystyrene microsphere of the formation individual layer six side solid matter in glass substrate;
3) by the polystyrene microsphere of above-mentioned individual layer six side solid matter, O is carried out
2plasma etching (RIE), oxygen flow 10 Sccm, air pressure 9pa, radio-frequency power 150W, etch period 12min, the particle diameter of microballoon is 2.2 μm;
4) employing magnetically controlled sputter method deposition ground floor thickness is ZnO:H (HZO) film of 1000nm, and target is ZnO ceramic target, prepares the zinc-oxide film of low-resistivity and high transmission: underlayer temperature is room temperature, and base vacuum is 5 × 10
-5pa, hydrogen flowing quantity is 3sccm, argon flow amount is 52sccm, sputtering pressure is 4.5mTorr, electrode spacing is 30 mm, and sputtering power is 380 W, and sputtering time is 50min, obtain the ZnO:H transparent conductive film that ground floor thickness is about 1000 nm, then glass substrate is placed in water and carries out ultrasonic process until ethene bead processes totally completely;
5) method of magnetron sputtering is adopted to deposit the ZnO:H transparent conductive film that second layer thickness is 500nm again: underlayer temperature is room temperature, and base vacuum is 5 × 10
-5pa, hydrogen flowing quantity is 3sccm, argon flow amount is 52sccm, and sputtering pressure is 4.5mTorr, and electrode spacing is 30 mm, sputtering power is 380 W, sputtering time is 25 min, obtains the ZnO:H transparent conductive film that second layer thickness is 500 nm, so just obtains the transparent conductive film with periodic structure, its r.m.s. roughness is 140nm, and square resistance is 9
.
Adopt the shape appearance figure of sunken light ZnO transparent conductive thin film of periodic structure and integrated reflection and suede degree and embodiment 1 roughly the same.
embodiment 6:
A kind of matte transparent conductive film of periodic structure, as shown in Figure 1, comprise substrate layer, the ground floor ZnO film of lifting plate effect and the second layer ZnO film of a modification also form laminated construction successively, substrate layer is hard substrates glass, ZnO film is doping zinc-oxide n-type semiconductor ZnO:W (WZO) film, wherein ground floor ZnO film thickness is 700nm, the thickness of second layer ZnO film is 350nm, form the matte transparent conductive film with the periodic structure of wide spectral scattering process, the r.m.s. roughness of the ZnO matte transparent conductive film of periodic structure is 70 nm.
A preparation method for the matte transparent conductive film of described periodic structure, utilizes water bath Method to assemble PS microballoon, uses O
2plasma etching PS microballoon, utilizes the template action of PS microballoon, and obtain the sunken light ZnO transparent conductive thin film with periodic structure, step is as follows:
1) glass substrate is immersed in H
2sO
4with H
2o
2volume ratio be 2:1 mixed solution in carry out hydrophilic treated, the processing time is 5 hours;
2) above-mentioned glass substrate is placed on horizontal stand, be 2 μm by particle diameter, concentration is that the polystyrene microsphere latex solution of 5wt% vertically drips on a glass substrate, solution slowly spreads apart and makes that ethene microballoon is uneven to be interspersed among in glass substrate, then glass substrate is placed on steam and carries out self assembly, through the water-bath of 30min, the polystyrene microsphere of the formation individual layer six side solid matter in glass substrate;
3) by the polystyrene microsphere of above-mentioned individual layer six side solid matter, O is carried out
2plasma etching (RIE), oxygen flow 10 Sccm, air pressure 9pa, radio-frequency power 100W, etch period 15min, the particle diameter of microballoon is 1.4 μm;
4) employing magnetically controlled sputter method deposition ground floor thickness is ZnO:W (WZO) film of 700nm, target is ZnO ceramic target, employing pure argon sputters, and prepare the zinc-oxide film of low-resistivity and high transmission: underlayer temperature is room temperature, base vacuum is 5 × 10
-5pa, argon flow amount is 55sccm, sputtering pressure is 4.5mTorr, electrode spacing is 30 mm, sputtering power is 430 W, sputtering time is 20 min, obtains the ground floor WZO transparent conductive film that thickness is about 700 nm, then glass substrate is placed in water and carries out ultrasonic process until ethene bead processes totally completely;
5) method of magnetron sputtering is adopted to deposit the WZO transparent conductive film that second layer thickness is 350nm again: underlayer temperature is room temperature, and base vacuum is 5 × 10
-5pa, argon flow amount is 55sccm, and sputtering pressure is 4.5mTorr, and electrode spacing is 30 mm, sputtering power is 430 W, and sputtering time is 10min, and thickness is 350 nm, so just obtain the transparent conductive film with periodic structure, its r.m.s. roughness is 70nm, and square resistance is 14
.
Adopt the shape appearance figure of sunken light ZnO transparent conductive thin film of periodic structure and integrated reflection and suede degree and embodiment 1 roughly the same.
To sum up, the invention provides a kind of improve silicon-based thin film solar cell before electrode fall into the effective ways of light effect, before the method and traditional silicon-base thin-film battery, technology for preparing electrode is completely compatible, and is generally applicable to that amorphous is silica-based, microcrystalline silicon, nano silicon-based thin-film single junction and multijunction solar cell.
The above; be only the present invention's preferably embodiment, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection range of claim.
Claims (1)
1. the preparation method of the matte transparent conductive film of a periodic structure, described matte transparent conductive film comprises substrate layer, the ground floor ZnO film of lifting plate effect and the second layer ZnO film of a modification also form laminated construction successively, substrate layer is hard substrates glass, ZnO film is doping zinc-oxide n-type semiconductor, comprise ZnO:H, ZnO:Al, ZnO:Ga, ZnO:B, at least one in ZnO:Mo and ZnO:W, wherein ground floor ZnO film thickness is 300-1500nm, the thickness of second layer ZnO film is 400-1000nm, form the matte transparent conductive film with the periodic structure of wide spectral scattering process, the r.m.s. roughness of the ZnO matte transparent conductive film of periodic structure is 30-250nm, it is characterized in that: utilize water bath Method to assemble polystyrene microsphere, use O
2plasma etching polystyrene microsphere, utilizes the template action of polystyrene microsphere, and obtain the sunken light ZnO transparent conductive thin film with periodic structure, step is as follows:
1) glass substrate is immersed in H
2sO
4with H
2o
2volume ratio be 2:1 mixed solution in carry out hydrophilic treated, the processing time is 2-10 hour;
2) above-mentioned glass substrate is placed on horizontal stand, be 1-5 μm by particle diameter, concentration is that the polystyrene microsphere latex solution of 5wt% vertically drips on a glass substrate, solution slowly spreads apart and makes that polystyrene microsphere is uneven to be interspersed among in glass substrate, then glass substrate is placed on steam and carries out self assembly, through the water-bath of 30min, glass substrate is formed the polystyrene microsphere of individual layer six side solid matter;
3) by the polystyrene microsphere of above-mentioned individual layer six side solid matter, O is carried out
2plasma etching, after etching, the size of polystyrene microsphere is 0.5-4 μm;
4) polystyrene microsphere after etching adopting magnetically controlled sputter method deposit ground floor thickness is the ZnO film of 300-1500nm, then glass substrate is placed in water and carries out ultrasonic process until polystyrene microsphere processes totally completely;
5) adopt the method for magnetron sputtering to deposit the ZnO film that second layer thickness is 400-1000nm again, the matte transparent conductive film with periodic structure can be obtained.
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| CN103956395B (en) * | 2014-05-09 | 2017-11-10 | 中国科学院宁波材料技术与工程研究所 | Array structure matte and its preparation method and application |
| CN106675429B (en) * | 2016-12-21 | 2019-12-03 | 蚌埠玻璃工业设计研究院 | Method for manufacturing thin film a kind of transferable and with surface micro-structure |
| CN106835012A (en) * | 2016-12-21 | 2017-06-13 | 蚌埠玻璃工业设计研究院 | A kind of preparation method of matte aluminum-doped zinc oxide films |
| CN107579135A (en) * | 2017-09-06 | 2018-01-12 | 蚌埠玻璃工业设计研究院 | A kind of surface has the zno-based transparent conducting glass preparation method of micro-structural |
| CN107681035B (en) * | 2017-09-18 | 2019-12-17 | 厦门三安光电有限公司 | Transparent conducting layer, manufacturing method thereof and light emitting diode |
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| CN109851832B (en) * | 2018-12-28 | 2021-05-25 | 中国科学院合肥物质科学研究院 | Method for constructing surface roughened PS ball array on flexible substrate |
| CN110931165B (en) * | 2019-11-19 | 2021-09-24 | 深圳市华星光电半导体显示技术有限公司 | Preparation method of transparent silver electrode |
| CN112071503A (en) * | 2020-08-04 | 2020-12-11 | 南开大学 | Method for realizing multifunctional composite transparent conductive film and application |
| CN112909178B (en) * | 2021-01-18 | 2022-07-08 | 香港科技大学深圳研究院 | Light trap substrate, preparation method and application thereof, and semitransparent solar cell |
| CN113044808A (en) * | 2021-03-10 | 2021-06-29 | 东南大学 | Preparation method of high-refractive-index all-dielectric nanosphere particles |
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