CN107994098A - A kind of matte transparent conductive film and preparation method thereof - Google Patents
A kind of matte transparent conductive film and preparation method thereof Download PDFInfo
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- CN107994098A CN107994098A CN201711162186.0A CN201711162186A CN107994098A CN 107994098 A CN107994098 A CN 107994098A CN 201711162186 A CN201711162186 A CN 201711162186A CN 107994098 A CN107994098 A CN 107994098A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- 239000010408 film Substances 0.000 claims abstract description 135
- 238000005507 spraying Methods 0.000 claims abstract description 80
- 238000000034 method Methods 0.000 claims abstract description 49
- 239000000758 substrate Substances 0.000 claims abstract description 46
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 39
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000005118 spray pyrolysis Methods 0.000 claims abstract description 22
- 239000010409 thin film Substances 0.000 claims abstract description 19
- 239000003595 mist Substances 0.000 claims abstract description 11
- 238000000137 annealing Methods 0.000 claims abstract description 5
- 238000000151 deposition Methods 0.000 claims abstract description 4
- 239000007921 spray Substances 0.000 claims description 64
- 239000011521 glass Substances 0.000 claims description 59
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 56
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 46
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 35
- 229910052757 nitrogen Inorganic materials 0.000 claims description 28
- 239000007789 gas Substances 0.000 claims description 19
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims description 16
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- DAMJCWMGELCIMI-UHFFFAOYSA-N benzyl n-(2-oxopyrrolidin-3-yl)carbamate Chemical compound C=1C=CC=CC=1COC(=O)NC1CCNC1=O DAMJCWMGELCIMI-UHFFFAOYSA-N 0.000 claims description 11
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 8
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 7
- 239000006199 nebulizer Substances 0.000 claims description 6
- 238000000197 pyrolysis Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 238000004544 sputter deposition Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 4
- 230000000873 masking effect Effects 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 241000254173 Coleoptera Species 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 230000003287 optical effect Effects 0.000 abstract description 8
- 238000002834 transmittance Methods 0.000 abstract description 8
- 238000010438 heat treatment Methods 0.000 description 20
- 238000003756 stirring Methods 0.000 description 12
- 230000005540 biological transmission Effects 0.000 description 10
- 230000005418 spin wave Effects 0.000 description 10
- 238000001816 cooling Methods 0.000 description 9
- 210000002268 wool Anatomy 0.000 description 9
- FAPDDOBMIUGHIN-UHFFFAOYSA-K antimony trichloride Chemical class Cl[Sb](Cl)Cl FAPDDOBMIUGHIN-UHFFFAOYSA-K 0.000 description 5
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 5
- 239000012159 carrier gas Substances 0.000 description 5
- 125000005909 ethyl alcohol group Chemical group 0.000 description 5
- 235000008216 herbs Nutrition 0.000 description 5
- 239000010453 quartz Substances 0.000 description 5
- 230000003746 surface roughness Effects 0.000 description 5
- 238000001039 wet etching Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000003912 environmental pollution Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- -1 Acyl acetone Chemical compound 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Substances CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/1884—Manufacture of transparent electrodes, e.g. TCO, ITO
-
- 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
- H01L31/022408—Electrodes for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/022425—Electrodes for devices characterised by at least one potential jump barrier or surface barrier for 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
- H01L31/02—Details
- H01L31/0224—Electrodes
- H01L31/022466—Electrodes made of transparent conductive layers, e.g. TCO, ITO layers
-
- 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
-
- 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
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- Engineering & Computer Science (AREA)
- Computer Hardware Design (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Electromagnetism (AREA)
- General Physics & Mathematics (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- Sustainable Development (AREA)
- Sustainable Energy (AREA)
- Surface Treatment Of Glass (AREA)
Abstract
The invention discloses a kind of matte transparent conductive film, and using quartz glass as substrate, Pt layers, TiO have been sequentially depositing in substrate2Film layer and FTO film layers, the FTO/TiO of formation2The preceding electrode of/Pt laminated films as thin film solar cell；Its preparation method is that magnetron sputtering technique is used under conditions of not higher than 100 DEG C, and Pt layers are deposited on quartz glass substrate；Prepare spray coating liquor A；Spray coating liquor A is sprayed on Pt layers by spray pyrolysis process and obtains TiO2Film layer, to the TiO of preparation2Film layer is made annealing treatment, and obtains cushion；Prepare spray coating liquor B；Spray coating liquor B sprayings are obtained by FTO film layers by spray pyrolysis process on the buffer layer, are finally made annealing treatment.Film prepared by the present invention is compared with single TCO thin film, its mist degree significantly improves, and electric conductivity is good, and optical transmittance is high, suitable for the requirement of electrode transparent conductive film before solar cell.
Description
Technical field
The invention belongs to technical field of function materials, and in particular to a kind of matte transparent conductive film；The invention further relates to
The preparation method of the matte transparent conductive film.
Background technology
In the 21st century, energy shortage and problem of environmental pollution are more prominent, and development clean energy resource is imperative.Solar energy
As unlimited reproducible non-polluting energy sources on the earth, it is effectively using the extensive concern for causing people.Wherein, photovoltaic produces
Industry is grown rapidly, and a series of thin-film solar cells such as non-crystalline silicon are used widely with its low cost, steady performance.
Thin-film solar cells is that solar radiant energy is converted to the device of electric energy using photovoltaic principle.Transparent conductive film
As the preceding electrode of thin film solar cell, play the role of to the photoelectric conversion efficiency of battery vital.In order at utmost
Raising thin-film solar cells photoelectric conversion efficiency, it is desirable to electrode has that optical transmittance is high, electrical conductivity before electrically conducting transparent
Outside the characteristics of high, also require that there is stronger scattering power to incident light.So, it is desirable to transparent conductive film matte, makes
Light in battery produces diffusing reflection, improves battery and sunlight is absorbed.
Electrode mainly has the SnO of ZnO (abbreviation AZO) and the F doping of Al doping before common thin film solar cell2(FTO)
Film, the surface wool manufacturing of AZO films usually first prepare AZO films, then using wet etching technique making herbs into wool, but wet etching pair
Environmental pollution is serious, and the uniformity of making herbs into wool is difficult to ensure that.This materials of FTO have stronger acid-alkali-corrosive-resisting, its light
Electrical property is more stable than AZO, and matte FTO films are more suitable for the preceding electrode of thin film solar cell, improves the use of battery
Service life.But the chemical property of FTO films is stablized, it is difficult to using wet etching making herbs into wool.If can direct growth on the glass substrate
FTO films with pyramid pattern, not only realize the surface wool manufacturing of FTO films, but also avoid what wet etching was brought
Problem of environmental pollution.Pyramid pattern is presented in FTO films with C axis oriented growth, surface, but in amorphous glass substrate
The upper extremely difficult film for growing orientation and preferably being grown along C axis.So the surface wool manufacturing of FTO films restricts it thin always
Film solar cell field widely uses, and has the trend substituted by matte AZO films.
Therefore, exploitation is a kind of, and there is high optical transmittance, haze, low resistance, physico-chemical property stabilization, the transparent of matte to lead
Conductive film and preparation method thereof has become the problem of urgent need to resolve.
The content of the invention
The object of the present invention is to provide a kind of matte transparent conductive film, solves FTO films in the prior art and is difficult to reality
The problem of existing effect making herbs into wool.
It is a further object of the present invention to provide the preparation method of the matte transparent conductive film, its preparation process is easy, easily
Realize.
The technical solution adopted in the present invention is a kind of matte transparent conductive film, using quartz glass as substrate, in substrate
On be sequentially depositing Pt layers, TiO2Film layer and FTO film layers, the FTO/TiO of formation2/ Pt laminated films are as film sun electricity
The preceding electrode in pond.
It is of the invention to be further characterized in that,
Pt layers of thickness is 5nm~9nm, TiO2The thickness of film layer is 50nm~110nm, and the thickness of FTO film layers is
400nm~650nm.
Another technical solution of the present invention is a kind of preparation method of matte transparent conductive film, specific steps
It is as follows：
Step 1, magnetron sputtering technique is used under conditions of not higher than 100 DEG C, Pt layers are deposited on quartz glass substrate；
Step 2, spray coating liquor A is prepared；
Step 3, spray coating liquor A is sprayed on Pt layers by spray pyrolysis process and obtains TiO2Film layer, to the TiO of preparation2
Film layer is made annealing treatment, and obtains cushion；
Step 4, spray coating liquor B is prepared；
Step 5, spray coating liquor B sprayings are obtained by FTO film layers by spray pyrolysis process on the buffer layer, it is then annealed
Processing finally obtains the matte transparent conductive film as electrode before thin film solar cell.
It is of the invention to be further characterized in that,
Magnetron sputtering Pt layers of process conditions are in step 1：The time of magnetron sputtering is 1h~2h；The work(of magnetron sputtering
Rate is 100w~150w；The pattern of magnetron sputtering sputters for RF；Vacuum is 8.0 × 10-2Pa；Partial pressure of ar gas is 1Pa.
The preparation method of spray coating liquor A is in step 2：First, under a dry nitrogen atmosphere, by butyl titanate and second respectively
Acyl acetone is dissolved in absolute ethyl alcohol, and 2h is stirred under room temperature, obtains mixed solution, and then closed stand handled into gelatinization, finally
Obtain spray coating liquor A.
In step 2, the molar ratio for preparing the butyl titanate in the raw material of spray coating liquor A, acetylacetone,2,4-pentanedione and absolute ethyl alcohol is：
1:1~1.5:10~50.
The preparation method of spray coating liquor B is in step 4：First, under the conditions of drying nitrogen, successively by stannic chloride pentahydrate,
Antimony trichloride is dissolved in absolute methanol, then stirs 2h under the conditions of 60 DEG C, obtains spray coating liquor B.
In step 4, the molar ratio of stannic chloride pentahydrate in the raw material of spray coating liquor B, antimony trichloride and absolute methanol is prepared
For：1:0.5~1:10~100.
The process conditions of spray pyrolysis process are in step 3：Nebulizer gas pressure is 0.1MPa~0.15MPa, and supersonic frequency is
2.4MHz, power are 100W~300W, and ullrasonic spraying Spray gun nozzle is 3cm~10cm, spray time 30s with glass substrate distance
~60s, pyrolysis temperature are 500 DEG C~580 DEG C.
The process conditions of spray pyrolysis process are in step 5：Nebulizer gas pressure is 0.1MPa~0.3MPa, and supersonic frequency is
2.4MHz, power are 100W~300W, and ullrasonic spraying Spray gun nozzle is 3cm~10cm with glass substrate distance, and spray time is
1min~3min, pyrolysis temperature are 520 DEG C~600 DEG C.
The invention has the advantages that by Pt, TiO2, FTO (fluorine doped tin oxide) deposit to respectively on quartz glass, pass through
Pt、TiO2Preferred orientation inductive formation there is the FTO films of (200) orientation, grain morphology is also changed into pyramid by bar-shaped
Shape, completes the making herbs into wool of film surface, and compared with single TCO thin film, its mist degree significantly improves, and electric conductivity is good, optics
Transmitance is high, suitable for the requirement of electrode transparent conductive film before solar cell.
Brief description of the drawings
Fig. 1 is a kind of structure diagram of matte transparent conductive film of the present invention；
Fig. 2 is the suede structure figure of FTO thin-film surfaces in a kind of matte transparent conductive film of the present invention；
Fig. 3 be the present invention a kind of matte transparent conductive film be thin film solar cell before electrode when, thin film solar cell
Quantum efficiency curve map；
Fig. 4 is a kind of matte transparent conductive film of the present invention for during electrode, the film of test is too before thin film solar cell
The current density in positive electricity pond with voltage change curve.
Embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
The present invention provides a kind of matte transparent conductive film, using quartz glass as substrate, it has been sequentially depositing in substrate
Pt layers, TiO2Film layer and FTO film layers, the FTO/TiO of formation2The preceding electrode of/Pt laminated films as thin film solar cell.
Pt layers of thickness is 5nm~9nm, TiO2The thickness of film layer is 50nm~110nm, and the thickness of FTO film layers is
400nm~650nm, and there is stronger (200) face preferred orientation.
Present invention also offers a kind of preparation method of matte transparent conductive film, comprise the following steps：
Step 1, magnetron sputtering technique is used under conditions of not higher than 100 DEG C, Pt layers are deposited on quartz glass substrate；
Magnetron sputtering Pt layers of process conditions are in step 1：The time of magnetron sputtering is 1h~2h；The work(of magnetron sputtering
Rate is 100w~150w；The pattern of magnetron sputtering sputters for RF；Vacuum is 8.0 × 10-2Pa；Partial pressure of ar gas is 1Pa；
Step 2, spray coating liquor A is prepared；
The preparation method of spray coating liquor A is in step 2：First, under a dry nitrogen atmosphere, by butyl titanate and second respectively
Acyl acetone is dissolved in absolute ethyl alcohol, and 2h is stirred under room temperature, obtains mixed solution, and then closed stand handled into gelatinization, finally
Obtain spray coating liquor A；
In step 2, the molar ratio for preparing the butyl titanate in the raw material of spray coating liquor A, acetylacetone,2,4-pentanedione and absolute ethyl alcohol is：
1:1~1.5:10~50；
Step 3, spray coating liquor A is sprayed on Pt layers by spray pyrolysis process and obtains TiO2Film layer, to the TiO of preparation2
Film layer is made annealing treatment, and obtains cushion；
The process conditions of spray pyrolysis process are in step 3：Nebulizer gas pressure is 0.1MPa~0.15MPa, and supersonic frequency is
2.4MHz, power are 100W~300W, and ullrasonic spraying Spray gun nozzle is 3cm~10cm, spray time 30s with glass substrate distance
~60s, pyrolysis temperature are 500 DEG C~580 DEG C；
Step 4, spray coating liquor B is prepared；
The preparation method of spray coating liquor B is in step 4：First, under the conditions of drying nitrogen, successively by stannic chloride pentahydrate,
Antimony trichloride is dissolved in absolute methanol, then stirs 2h under the conditions of 60 DEG C, obtains spray coating liquor B；
In step 4, the molar ratio of stannic chloride pentahydrate in the raw material of spray coating liquor B, antimony trichloride and absolute methanol is prepared
For：1:0.5~1:10~100；
Step 5, spray coating liquor B sprayings are obtained by FTO film layers by spray pyrolysis process on the buffer layer, it is then annealed
Processing finally obtains the matte transparent conductive film as electrode before thin film solar cell；
The process conditions of spray pyrolysis process are in step 5：Nebulizer gas pressure is 0.1MPa~0.3MPa, and supersonic frequency is
2.4MHz, power are 100W~300W, and ullrasonic spraying Spray gun nozzle is 3cm~10cm with glass substrate distance, and spray time is
1min~3min, pyrolysis temperature are 520 DEG C~600 DEG C.
From figure 1 it appears that prepared film shows sandwich construction, preparation is simple.
From figure 2 it can be seen that prepared film surface shows obvious pyramidal structure, can effectively scatter
Into the light of thin-film solar cells.
From figure 3, it can be seen that wavelength or energy of the quantum efficiency of solar battery with being radiated at solar cell light
Related, wherein the sheet resistance of FTO is 5 Ω, and the visible ray mean transmissivity of laminated film is 81%, mist degree 20%.
Figure 4, it is seen that solar cell photogenerated current is 16.3mA/cm2, the wherein sheet resistance of FTO is 5 Ω, multiple
The visible ray mean transmissivity for closing film is 81%, mist degree 20%.
Embodiment 1
A kind of preparation method of matte transparent conductive film, comprises the following steps that：
Step 1, magnetron sputtering technique is used under conditions of not higher than 100 DEG C, Pt layers are deposited on quartz glass substrate；
Wherein magnetron sputtering Pt layers of process conditions are：The time of magnetron sputtering is 1h；The power of magnetron sputtering is 100w；Magnetic control splashes
The pattern penetrated sputters for RF；The vacuum used during magnetron sputtering is 8.0 × 10-2Pa；Partial pressure of ar gas is 1Pa, Pt layers prepared
Thickness is 5nm；
Step 2, spray coating liquor A is prepared：Under a dry nitrogen atmosphere, first by 100.00g butyl titanates, 29.42g acetyl
Acetone is added in 94.15g absolute ethyl alcohols respectively, stirring at normal temperature 2h, and then closed stand handled into gelatinization, must finally spray
Liquid A；Spray coating liquor A is matched：Butyl titanate, acetylacetone,2,4-pentanedione, the molar ratio of absolute ethyl alcohol are：1:1:10；
Step 3, TiO is prepared by spray pyrolysis process2Film.First, the quartz glass glass for having deposited Pt layers is put
Enter in heating furnace and heat, when temperature rises to 500 DEG C, driven by transmission device and moved to spray booth, nitrogen buffer gas,
Nitrogen valve is opened, sets atmospheric pressure value as 0.1MPa, while opens ultrasonic magnon switch, sets supersonic frequency as 2.4MHz,
Power is 100W, ullrasonic spraying spray gun is put into heating furnace, adjustment Spray gun nozzle, to 10cm, sets 30s's with glass substrate distance
Spray time, starts to spray.After to be sprayed, TiO will be coated with2The glass substrate of film moves to cooling zone, is air-cooled to room
Temperature, unloads coated glass, obtains cushion --- TiO2Film.Prepared TiO2Film thickness is 50nm；
Step 4, spray coating liquor B is prepared：First, under the conditions of drying nitrogen, successively by 100.00g stannic chloride pentahydrates,
32.53g antimony trichlorides are dissolved in 131.40g absolute methanols, then stir 2h under the conditions of 60 DEG C, obtain spray coating liquor B；Wherein,
Spray coating liquor B is matched：Stannic chloride pentahydrate, antimony trichloride, the molar ratio of absolute methanol are：1:0.5:10.
Step 5, FTO films are prepared by spray pyrolysis process.First, Pt layers/TiO will have been deposited2The quartz of film layer
Glass glass is put into heating furnace and heats, and when temperature rises to 520 DEG C, is driven by transmission device and is moved to spray booth, with
Nitrogen is carrier gas, opens nitrogen valve, sets atmospheric pressure value as 0.1MPa, while opens ultrasonic magnon switch, sets supersonic frequency
Rate is 2.4MHz, power 100W, ullrasonic spraying spray gun is put into heating furnace, adjustment Spray gun nozzle is with glass substrate apart from extremely
10cm, sets the spray time of 1min, starts to spray.After to be sprayed, the glass substrate for being coated with FTO films is moved to cold
But area, is air-cooled to room temperature, unloads coated glass.Prepared FTO film thicknesses are 400nm；
FTO/TiO2The optical transmittance of/Pt/ glass structures is more than 85% at 550nm wavelength, and surface square resistance is 5
Ω, mist degree can reach 40% in 700nm wavelength, and surface roughness reaches 40nm and surface uniformity within 2.7%.
Embodiment 2
A kind of preparation method of matte transparent conductive film, comprises the following steps that：
Step 1, magnetron sputtering technique is used under conditions of not higher than 100 DEG C, Pt layers are deposited on quartz glass substrate；
Wherein magnetron sputtering Pt layers of process conditions are：The time of magnetron sputtering is 1.2h；The power of magnetron sputtering is 120w；Magnetic control
The pattern of sputtering sputters for RF；The vacuum used during magnetron sputtering is 8.0 × 10-2Pa；Partial pressure of ar gas is 1Pa, prepared Pt
Layer thickness is 6nm；
Step 2, spray coating liquor A is prepared：Under a dry nitrogen atmosphere, first by 100.00g butyl titanates, 32.36g acetyl
Acetone is added in 188.29g absolute ethyl alcohols respectively, stirring at normal temperature 2h, and then closed stand handled into gelatinization, must finally spray
Masking liquid A；Spray coating liquor A is matched：Butyl titanate, acetylacetone,2,4-pentanedione, the molar ratio of absolute ethyl alcohol are：1:1.1:20；
Step 3, TiO is prepared by spray pyrolysis process2Film.First, the quartz glass glass for having deposited Pt layers is put
Enter in heating furnace and heat, when temperature rises to 520 DEG C, driven by transmission device and moved to spray booth, nitrogen buffer gas,
Nitrogen valve is opened, sets atmospheric pressure value as 0.11MPa, while opens ultrasonic magnon switch, sets supersonic frequency as 2.4MHz,
Power is 100W, ullrasonic spraying spray gun is put into heating furnace, adjustment Spray gun nozzle, to 4cm, sets the spray of 42s with glass substrate distance
The time is applied, starts to spray.After to be sprayed, TiO will be coated with2The glass substrate of film moves to cooling zone, is air-cooled to room temperature,
Coated glass is unloaded, obtains cushion --- TiO2Film.Prepared TiO2Film thickness is 70nm；
Step 4, spray coating liquor B is prepared：First, under the conditions of drying nitrogen, successively by 100.00g stannic chloride pentahydrates,
39.04g antimony trichlorides are dissolved in 394.21g absolute methanols, then stir 2h under the conditions of 60 DEG C, obtain spray coating liquor B；Wherein,
Spray coating liquor B is matched：Stannic chloride pentahydrate, antimony trichloride, the molar ratio of absolute methanol are：1:0.6:30.
Step 5, FTO films are prepared by spray pyrolysis process.First, Pt layers/TiO will have been deposited2The quartz of film layer
Glass glass is put into heating furnace and heats, and when temperature rises to 530 DEG C, is driven by transmission device and is moved to spray booth, with
Nitrogen is carrier gas, opens nitrogen valve, sets atmospheric pressure value as 0.15MPa, while opens ultrasonic magnon switch, sets supersonic frequency
Rate is 2.4MHz, power 150W, and ullrasonic spraying spray gun is put into heating furnace, adjustment Spray gun nozzle and glass substrate distance to 8cm,
The spray time of 1.5min is set, starts to spray.After to be sprayed, the glass substrate for being coated with FTO films is moved into cooling
Area, is air-cooled to room temperature, unloads coated glass.Prepared FTO film thicknesses are 440nm；
FTO/TiO2The optical transmittance of/Pt/ glass structures is more than 84% at 550nm wavelength, and surface square resistance exists
4.8 Ω, mist degree can reach 42% in 700nm wavelength, and surface roughness reaches 42nm and surface uniformity within 2.5%.
Embodiment 3
A kind of preparation method of matte transparent conductive film, comprises the following steps that：
Step 1, magnetron sputtering technique is used under conditions of not higher than 100 DEG C, Pt layers are deposited on quartz glass substrate；
Wherein magnetron sputtering Pt layers of process conditions are：The time of magnetron sputtering is 1.4h；The power of magnetron sputtering is 130w；Magnetic control
The pattern of sputtering sputters for RF；The vacuum used during magnetron sputtering is 8.0 × 10-2Pa；Partial pressure of ar gas is 1Pa, prepared Pt
Layer thickness is 7nm；
Step 2, spray coating liquor A is prepared：Under a dry nitrogen atmosphere, first by 100.00g butyl titanates, 35.30g acetyl
Acetone is added dropwise into 282.44g absolute ethyl alcohols respectively, stirring at normal temperature 2h, and then closed stand handled into gelatinization, finally
Spray coating liquor A；Spray coating liquor A is matched：Butyl titanate, acetylacetone,2,4-pentanedione, the molar ratio of absolute ethyl alcohol are：1:1.2:30；
Step 3, TiO is prepared by spray pyrolysis process2Film.First, the quartz glass glass for having deposited Pt layers is put
Enter in heating furnace and heat, when temperature rises to 540 DEG C, driven by transmission device and moved to spray booth, nitrogen buffer gas,
Nitrogen valve is opened, sets atmospheric pressure value as 0.13MPa, while opens ultrasonic magnon switch, sets supersonic frequency as 2.4MHz,
Power is 200W, ullrasonic spraying spray gun is put into heating furnace, adjustment Spray gun nozzle, to 6cm, sets the spray of 50s with glass substrate distance
The time is applied, starts to spray.After to be sprayed, TiO will be coated with2The glass substrate of film moves to cooling zone, is air-cooled to room temperature,
Coated glass is unloaded, obtains cushion --- TiO2Film.Prepared TiO2Film thickness is 80nm；
Step 4, spray coating liquor B is prepared：First, under the conditions of drying nitrogen, successively by 100.00g stannic chloride pentahydrates,
52.05g antimony trichlorides are dissolved in 657.02g absolute methanols, then stir 2h under the conditions of 60 DEG C, obtain spray coating liquor B；Wherein,
Spray coating liquor B is matched：Stannic chloride pentahydrate, antimony trichloride, the molar ratio of absolute methanol are：1:0.8:50.
Step 5, FTO films are prepared by spray pyrolysis process.First, Pt layers/TiO will have been deposited2The quartz of film layer
Glass glass is put into heating furnace and heats, and when temperature rises to 550 DEG C, is driven by transmission device and is moved to spray booth, with
Nitrogen is carrier gas, opens nitrogen valve, sets atmospheric pressure value as 0.2MPa, while opens ultrasonic magnon switch, sets supersonic frequency
Rate is 2.4MHz, power 220W, and ullrasonic spraying spray gun is put into heating furnace, adjustment Spray gun nozzle and glass substrate distance to 6cm,
The spray time of 2min is set, starts to spray.After to be sprayed, the glass substrate for being coated with FTO films is moved into cooling zone,
Room temperature is air-cooled to, unloads coated glass.Prepared FTO film thicknesses are 540nm；
FTO/TiO2The optical transmittance of/Pt/ glass structures is more than 83% at 550nm wavelength, and surface square resistance exists
4.7 Ω, mist degree can reach 43% in 700nm wavelength, and surface roughness reaches 43nm and surface uniformity within 2.4%.
Embodiment 4
A kind of preparation method of matte transparent conductive film, comprises the following steps that：
Step 1, magnetron sputtering technique is used under conditions of not higher than 100 DEG C, Pt layers are deposited on quartz glass substrate；
Wherein magnetron sputtering Pt layers of process conditions are：The time of magnetron sputtering is 1.4h；The power of magnetron sputtering is 140w；Magnetic control
The pattern of sputtering sputters for RF；The vacuum used during magnetron sputtering is 8.0 × 10-2Pa；Partial pressure of ar gas is 1Pa, prepared Pt
Layer thickness is 8nm；
Step 2, spray coating liquor A is prepared：Under a dry nitrogen atmosphere, first by 100.00g butyl titanates, 41.18g acetyl
Acetone is added dropwise into 376.57g absolute ethyl alcohols respectively, stirring at normal temperature 2h, and then closed stand handled into gelatinization, finally
Spray coating liquor A；Spray coating liquor A is matched：Butyl titanate, acetylacetone,2,4-pentanedione, the molar ratio of absolute ethyl alcohol are：1:1.4:40；
Step 3, TiO is prepared by spray pyrolysis process2Film.First, the quartz glass glass for having deposited Pt layers is put
Enter in heating furnace and heat, when temperature rises to 550 DEG C, driven by transmission device and moved to spray booth, nitrogen buffer gas,
Nitrogen valve is opened, sets atmospheric pressure value as 0.14MPa, while opens ultrasonic magnon switch, sets supersonic frequency as 2.4MHz,
Power is 250W, ullrasonic spraying spray gun is put into heating furnace, adjustment Spray gun nozzle, to 3cm, sets the spray of 60s with glass substrate distance
The time is applied, starts to spray.After to be sprayed, TiO will be coated with2The glass substrate of film moves to cooling zone, is air-cooled to room temperature,
Coated glass is unloaded, obtains cushion --- TiO2Film.Prepared TiO2Film thickness is 100nm；
Step 4, spray coating liquor B is prepared：First, under the conditions of drying nitrogen, successively by 100.00g stannic chloride pentahydrates,
58.55g antimony trichlorides are dissolved in 1051.23g absolute methanols, then stir 2h under the conditions of 60 DEG C, obtain spray coating liquor B；Wherein,
Spray coating liquor B is matched：Stannic chloride pentahydrate, antimony trichloride, the molar ratio of absolute methanol are：1:0.9:80.
Step 5, FTO films are prepared by spray pyrolysis process.First, Pt layers/TiO will have been deposited2The quartz of film layer
Glass glass is put into heating furnace and heats, and when temperature rises to 580 DEG C, is driven by transmission device and is moved to spray booth, with
Nitrogen is carrier gas, opens nitrogen valve, sets atmospheric pressure value as 0.25MPa, while opens ultrasonic magnon switch, sets supersonic frequency
Rate is 2.4MHz, power 260W, and ullrasonic spraying spray gun is put into heating furnace, adjustment Spray gun nozzle and glass substrate distance to 5cm,
The spray time of 2,4min is set, starts to spray.After to be sprayed, TiO will be coated with2The glass substrate of film moves to cooling
Area, is air-cooled to room temperature, unloads coated glass, obtains cushion --- TiO2Film.Prepared TiO2Film thickness is 580nm；
FTO/TiO2The optical transmittance of/Pt/ glass structures is more than 81% at 550nm wavelength, and surface square resistance exists
4.5 Ω, mist degree can reach 44% in 700nm wavelength, and surface roughness reaches 44nm and surface uniformity within 2.3%.
Embodiment 5
A kind of preparation method of matte transparent conductive film, comprises the following steps that：
Step 1, magnetron sputtering technique is used under conditions of not higher than 100 DEG C, Pt layers are deposited on quartz glass substrate；
Wherein magnetron sputtering Pt layers of process conditions are：The time of magnetron sputtering is 1.5h；The power of magnetron sputtering is 150w；Magnetic control
The pattern of sputtering sputters for RF；The vacuum used during magnetron sputtering is 8.0 × 10-2Pa；Partial pressure of ar gas is 1Pa, prepared Pt
Layer thickness is 9nm；
Step 2, spray coating liquor A is prepared：Under a dry nitrogen atmosphere, first by 100.00g butyl titanates, 44.12g acetyl
Acetone is added dropwise into 470.73g absolute ethyl alcohols respectively, stirring at normal temperature 2h, and then closed stand handled into gelatinization, finally
Spray coating liquor A；Spray coating liquor A is matched：Butyl titanate, acetylacetone,2,4-pentanedione, the molar ratio of absolute ethyl alcohol are：1:1.5:50；
Step 3, TiO is prepared by spray pyrolysis process2Film.First, the quartz glass glass for having deposited Pt layers is put
Enter in heating furnace and heat, when temperature rises to 580 DEG C, driven by transmission device and moved to spray booth, nitrogen buffer gas,
Nitrogen valve is opened, sets atmospheric pressure value as 0.15MPa, while opens ultrasonic magnon switch, sets supersonic frequency as 2.4MHz,
Power is 300W, ullrasonic spraying spray gun is put into heating furnace, adjustment Spray gun nozzle, to 3cm, sets the spray of 60s with glass substrate distance
The time is applied, starts to spray.After to be sprayed, TiO will be coated with2The glass substrate of film moves to cooling zone, is air-cooled to room temperature,
Coated glass is unloaded, obtains cushion --- TiO2Film.Prepared TiO2Film thickness is 110nm；
Step 4, spray coating liquor B is prepared：First, under the conditions of drying nitrogen, successively by 100.00g stannic chloride pentahydrates,
65.06g antimony trichlorides are dissolved in 1314.03g absolute methanols, then stir 2h under the conditions of 60 DEG C, obtain spray coating liquor B；Wherein,
Spray coating liquor B is matched：Stannic chloride pentahydrate, antimony trichloride, the molar ratio of absolute methanol are：1:1:100.
Step 5, FTO films are prepared by spray pyrolysis process.First, Pt layers/TiO will have been deposited2The quartz of film layer
Glass glass is put into heating furnace and heats, and when temperature rises to 600 DEG C, is driven by transmission device and is moved to spray booth, with
Nitrogen is carrier gas, opens nitrogen valve, sets atmospheric pressure value as 0.3MPa, while opens ultrasonic magnon switch, sets supersonic frequency
Rate is 2.4MHz, power 300W, and ullrasonic spraying spray gun is put into heating furnace, adjustment Spray gun nozzle and glass substrate distance to 3cm,
The spray time of 3min is set, starts to spray.After to be sprayed, TiO will be coated with2The glass substrate of film moves to cooling
Area, is air-cooled to room temperature, unloads coated glass, obtains cushion --- TiO2Film.Prepared TiO2Film thickness is 650nm；
FTO/TiO2The optical transmittance of/Pt/ glass structures is more than 80% at 550nm wavelength, and surface square resistance exists
4.4 Ω, mist degree can reach 45% in 700nm wavelength, and surface roughness reaches 45nm and surface uniformity within 2.1%.
Advantages of the present invention is that the chemical property of FTO films is stablized, and is grown on the glass substrate with gold according to the method
The FTO films of word turriform looks, not only realize the surface wool manufacturing of FTO films, but also it is dirty to avoid the environment that wet etching is brought
Dye problem.Simplify preparation process, obtain the transparent conductive film for being applicable to electrode before solar cell of excellent performance.
Claims (10)
1. a kind of matte transparent conductive film, it is characterised in that using quartz glass as substrate, Pt has been sequentially depositing in substrate
Layer, TiO2Film layer and FTO film layers, the FTO/TiO of formation2The preceding electrode of/Pt laminated films as thin film solar cell.
A kind of 2. matte transparent conductive film according to claim 1, it is characterised in that Pt layers of thickness for 5nm~
9nm, TiO2The thickness of film layer is 50nm~110nm, and the thickness of FTO film layers is 400nm~650nm.
3. a kind of preparation method of matte transparent conductive film, it is characterised in that comprise the following steps that：
Step 1, magnetron sputtering technique is used under conditions of not higher than 100 DEG C, Pt layers are deposited on quartz glass substrate；
Step 2, spray coating liquor A is prepared；
Step 3, spray coating liquor A is sprayed on Pt layers by spray pyrolysis process and obtains TiO2Film layer, to the TiO of preparation2Film
Layer is made annealing treatment, and obtains cushion；
Step 4, spray coating liquor B is prepared；
Step 5, spray coating liquor B sprayings are obtained by FTO film layers by spray pyrolysis process on the buffer layer, then annealed processing
Finally obtain the matte transparent conductive film as electrode before thin film solar cell.
A kind of 4. preparation method of matte transparent conductive film according to claim 3, it is characterised in that magnetic in step 1
Pt layers of process conditions are plated in control sputtering：The time of magnetron sputtering is 1h~2h；The power of magnetron sputtering is 100w~150w；Magnetic
The pattern for controlling sputtering sputters for RF；Vacuum is 8.0 × 10-2Pa；Partial pressure of ar gas is 1Pa.
5. the preparation method of a kind of matte transparent conductive film according to claim 3, it is characterised in that sprayed in step 2
The preparation method of masking liquid A is：First, under a dry nitrogen atmosphere, butyl titanate respectively and acetylacetone,2,4-pentanedione are dissolved in anhydrous second
In alcohol, 2h is stirred under room temperature, obtains mixed solution, then closed stand handled into gelatinization, finally obtains spray coating liquor A.
A kind of 6. preparation method of matte transparent conductive film according to claim 5, it is characterised in that in step 2, system
The molar ratio of butyl titanate, acetylacetone,2,4-pentanedione and absolute ethyl alcohol in the raw material of standby spray coating liquor A is：1:1~1.5:10~50.
7. the preparation method of a kind of matte transparent conductive film according to claim 3, it is characterised in that sprayed in step 4
The preparation method of masking liquid B is：First, under the conditions of drying nitrogen, stannic chloride pentahydrate, antimony trichloride are dissolved in no water beetle successively
In alcohol, 2h then is stirred under the conditions of 60 DEG C, obtains spray coating liquor B.
A kind of 8. preparation method of matte transparent conductive film according to claim 7, it is characterised in that in step 4, system
The molar ratio of stannic chloride pentahydrate, antimony trichloride and absolute methanol in the raw material of standby spray coating liquor B is：1:0.5~1:10~
100。
9. the preparation method of a kind of matte transparent conductive film according to claim 3, it is characterised in that sprayed in step 3
The process conditions of mist pyrolytic process are：Nebulizer gas pressure is 0.1MPa~0.15MPa, supersonic frequency 2.4MHz, power 100W
~300W, ullrasonic spraying Spray gun nozzle are 3cm~10cm with glass substrate distance, and spray time is 30s~60s, and pyrolysis temperature is
500 DEG C~580 DEG C.
10. the preparation method of a kind of matte transparent conductive film according to claim 3, it is characterised in that sprayed in step 5
The process conditions of mist pyrolytic process are：Nebulizer gas pressure is 0.1MPa~0.3MPa, supersonic frequency 2.4MHz, power for 100W~
300W, ullrasonic spraying Spray gun nozzle are 3cm~10cm with glass substrate distance, and spray time is 1min~3min, and pyrolysis temperature is
520 DEG C~600 DEG C.
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| CN102034901A (en) * | 2010-10-27 | 2011-04-27 | 新奥光伏能源有限公司 | Transparent conductive thin film and preparation method thereof |
| CN102779944A (en) * | 2012-08-06 | 2012-11-14 | 上海电力学院 | Transparent conductive thin film and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102034901A (en) * | 2010-10-27 | 2011-04-27 | 新奥光伏能源有限公司 | Transparent conductive thin film and preparation method thereof |
| CN102779944A (en) * | 2012-08-06 | 2012-11-14 | 上海电力学院 | Transparent conductive thin film and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| YANG REN等: ""Fabrication of Textured Rough SnO2:F Films on Glass Using TiO2 Film as a Buffer Layer"", 《JOURNAL OF ELECTRONIC MATERIALS》 * |
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