CN105776889B - A method of enhancing electro-conductive glass permeability and electric conductivity - Google Patents
A method of enhancing electro-conductive glass permeability and electric conductivity Download PDFInfo
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- CN105776889B CN105776889B CN201610179599.9A CN201610179599A CN105776889B CN 105776889 B CN105776889 B CN 105776889B CN 201610179599 A CN201610179599 A CN 201610179599A CN 105776889 B CN105776889 B CN 105776889B
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- 239000011521 glass Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 32
- 230000002708 enhancing effect Effects 0.000 title claims abstract description 16
- 230000035699 permeability Effects 0.000 title claims abstract description 16
- 238000000576 coating method Methods 0.000 claims abstract description 16
- 239000011248 coating agent Substances 0.000 claims abstract description 15
- 239000002243 precursor Substances 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 5
- 230000007547 defect Effects 0.000 claims abstract description 4
- 150000003839 salts Chemical class 0.000 claims description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 16
- 229910052718 tin Inorganic materials 0.000 claims description 15
- 238000004321 preservation Methods 0.000 claims description 14
- 238000004528 spin coating Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 10
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 10
- 229910052738 indium Inorganic materials 0.000 claims description 9
- 229910052725 zinc Inorganic materials 0.000 claims description 9
- 239000011701 zinc Substances 0.000 claims description 9
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 8
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 8
- 229910052787 antimony Inorganic materials 0.000 claims description 7
- 229910052731 fluorine Inorganic materials 0.000 claims description 7
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims description 6
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 claims description 6
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 5
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 5
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical class [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 4
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- 159000000013 aluminium salts Chemical class 0.000 claims description 4
- 229910000329 aluminium sulfate Inorganic materials 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 4
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 4
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 3
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims description 3
- DAMJCWMGELCIMI-UHFFFAOYSA-N benzyl n-(2-oxopyrrolidin-3-yl)carbamate Chemical group C=1C=CC=CC=1COC(=O)NC1CCNC1=O DAMJCWMGELCIMI-UHFFFAOYSA-N 0.000 claims description 3
- 235000003270 potassium fluoride Nutrition 0.000 claims description 3
- 239000011698 potassium fluoride Substances 0.000 claims description 3
- 235000011150 stannous chloride Nutrition 0.000 claims description 3
- 239000001119 stannous chloride Substances 0.000 claims description 3
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 3
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 3
- 229960001763 zinc sulfate Drugs 0.000 claims description 3
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 3
- OQBLGYCUQGDOOR-UHFFFAOYSA-L 1,3,2$l^{2}-dioxastannolane-4,5-dione Chemical compound O=C1O[Sn]OC1=O OQBLGYCUQGDOOR-UHFFFAOYSA-L 0.000 claims description 2
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 2
- XURCIPRUUASYLR-UHFFFAOYSA-N Omeprazole sulfide Chemical compound N=1C2=CC(OC)=CC=C2NC=1SCC1=NC=C(C)C(OC)=C1C XURCIPRUUASYLR-UHFFFAOYSA-N 0.000 claims description 2
- 239000000443 aerosol Substances 0.000 claims description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 2
- VMPVEPPRYRXYNP-UHFFFAOYSA-I antimony(5+);pentachloride Chemical compound Cl[Sb](Cl)(Cl)(Cl)Cl VMPVEPPRYRXYNP-UHFFFAOYSA-I 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims description 2
- 229910000337 indium(III) sulfate Inorganic materials 0.000 claims description 2
- XGCKLPDYTQRDTR-UHFFFAOYSA-H indium(iii) sulfate Chemical compound [In+3].[In+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O XGCKLPDYTQRDTR-UHFFFAOYSA-H 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 235000013024 sodium fluoride Nutrition 0.000 claims description 2
- 239000011775 sodium fluoride Substances 0.000 claims description 2
- 235000005074 zinc chloride Nutrition 0.000 claims description 2
- 239000011592 zinc chloride Substances 0.000 claims description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 2
- 229910017053 inorganic salt Inorganic materials 0.000 claims 1
- 239000004973 liquid crystal related substance Substances 0.000 abstract description 2
- 239000010409 thin film Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 11
- 239000010408 film Substances 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 5
- 238000003980 solgel method Methods 0.000 description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000005693 optoelectronics Effects 0.000 description 2
- 238000010129 solution processing Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- NGCDGPPKVSZGRR-UHFFFAOYSA-J 1,4,6,9-tetraoxa-5-stannaspiro[4.4]nonane-2,3,7,8-tetrone Chemical compound [Sn+4].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O NGCDGPPKVSZGRR-UHFFFAOYSA-J 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
- C03C17/3417—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials all coatings being oxide coatings
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
- C03C17/3429—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating
- C03C17/3447—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating comprising a halide
- C03C17/3458—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating comprising a halide comprising a chloride
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Surface Treatment Of Glass (AREA)
- Non-Insulated Conductors (AREA)
Abstract
The invention discloses a kind of enhancing electro-conductive glass permeability and the methods of electric conductivity.Conductive glass surface bumps defect is filled by coating transparent conductive nano crystalline substance colloidal sol and its precursor solution, electro-conductive glass translucency and electric conductivity are effectively improved, can be applied to touch screen liquid crystal display, electroluminescent display, solar battery, thin film transistor (TFT), heat-insulating and energy-saving glass art.
Description
Technical field
The present invention relates to a kind of conductive film and preparation method thereof, more particularly to a kind of enhancing electro-conductive glass permeability and
The method of electric conductivity.
Background technique
Transparent conductive film is to combine with electric conductivity the transparency, becomes in functional material that have distinctive one kind thin
Film has broad application prospects in opto-electronics.Transparent conductive oxide film has higher light transmittance in visible region,
And there is excellent electric conductivity, resistivity is minimum, which to be can achieve excellent photoelectric properties and make it in the opto-electronic device, has extensively
Application, such as flat liquid crystal display, solar battery, gas sensitization device, energy saving form, automotive anti-mist glass.
The conductive film for being usually applied to glass has FTO (SnO2:F)、ATO(SnO2:Sb)、ITO(In2O3: Sn) and AZO
(ZnO:Al).They have the advantages that translucency is good, resistivity is low etc..They general square resistance is both less than 10 Ω/, can
Light-exposed transmitance is both greater than 80%, if to improve electric conductivity, translucency just be will be greatly reduced.But excessive square resistance
It is unable to satisfy the demand of the following solar battery glass substrate, although square resistance can be reduced by increasing film thickness, will lead to pair
The light of certain wave band generates absorption.
The conductivity that glass how is improved under conditions of not reducing translucency becomes critical issue.Herein by conduction
Vitreous coating transparent conductive nano crystalline substance colloidal sol and its precursor solution fill concave-convex surface defect, can effectively improve transmission
Square resistance is reduced while property.
Summary of the invention
In order to solve prior art problem, it is an object of the present invention to overcome the deficiencies of the prior art, and to provide one kind
The method for enhancing electro-conductive glass permeability and electric conductivity, can effectively improve electro-conductive glass translucency and electric conductivity.
Purpose is created to reach foregoing invention, the present invention adopts the following technical solutions:
(1) a kind of method of enhancing electro-conductive glass permeability and electric conductivity, which is characterized in that received by coating electrically conducting transparent
The brilliant colloidal sol of rice and its precursor solution fill conductive glass surface bumps defect, effectively improve electro-conductive glass translucency and conduction
Property, include the following steps:
A. electrically conducting transparent colloidal sol is coated in conductive glass surface first, then calcined；
B. precursor solution is coated again, is calcined again；
C. calcining step are as follows: the sample after coating is first placed in 40-80 DEG C of heat preservation 20-50min and is dried, then is placed in
It is calcined in Muffle furnace, 5-15 DEG C of heating rate/min, then in 350-500 DEG C of heat preservation 10-50min, Temperature fall obtains sample；
(2) electro-conductive glass is FTO, ATO, ITO or AZO；
(3) the electrically conducting transparent colloidal sol is SnO2、In2O3, ZnO and F, Sb element doping SnO2Colloidal sol, Sn element are mixed
Miscellaneous In2O3Colloidal sol, the ZnO colloidal sol of Al element doping；
(4) the electrically conducting transparent colloidal sol solvent is one kind of ethyl alcohol, isopropanol or water, and aerosol particle size is 2~20nm, square
100 Ω of resistance </ (powder tabletting), mass fraction be 0.1~10.0%, wherein the mass ratio of the material of F and Sn be 0.01~
The mass ratio of the material of 4: 1, Sb and Sn are that the mass ratio of the material of 0.01~4: 1, Sn and In is the substance of 0.01~4:1, Al and Zn
Amount ratio be 0.01~8: 1；
(5) precursor solution is that villiaumite adulterates stanniferous inorganic salts or organic salt, antimonic salt adulterate stanniferous inorganic salts or have
Machine salt, pink salt doping inorganic salts containing indium or organic salt, aluminium salt doping inorganic salts containing zinc or organic salt are one of, wherein F and Sn
The mass ratio of the material be 0.01~4: 1, Sb and Sn the mass ratio of the material be 0.01~4: 1, Sn and In the mass ratio of the material be
The mass ratio of the material of 0.01~4:1, Al and Zn are 0.01~8: 1, and solvent is one kind of ethyl alcohol, isopropanol or water, and concentration is
0.01~6mM；
(6) villiaumite is that sodium fluoride, potassium fluoride or ammonium fluoride are one of；
(7) the stanniferous inorganic salts or organic salt are that stannous chloride, tin tetrachloride or stannous oxalate are one of；
(8) antimonic salt is that antimony trichloride or Antimony pentachloride are one of；
(9) inorganic salts containing indium or organic salt are that indium trichloride, indium sulfate or indium nitrate are one of；
(10) aluminium salt is that alchlor or aluminum sulfate are one of；
(11) the zinc inorganic salts or organic salt are that zinc sulfate, zinc nitrate or zinc chloride are one of；
(12) coating method is spin-coating method or czochralski method；When using spin-coating method film, revolving speed 1000-
3000rpm, time 5-30s, spin coating number are 1-3 times；When using czochralski method film, pull rate 5-15mm/min,
In 30-50 DEG C of heat preservation 30-50min, lifting number is 1-3 times；
(13) the modified transmitance of the electro-conductive glass and electric conductivity improve 5% or more.
The present invention has the following advantages and beneficial effects:
1. the present invention is suitble to heavy industrialization application without expensive mechanical equipment, simple process and low cost.
2. treatment process of the present invention adapts to the various surface roughness situation of material surface, not by the shadow of substrate shape, material
It rings, application surface is extensive.
Detailed description of the invention
(No. 1 is reference FTO glass sample to pictorial diagram to Fig. 1 FTO electro-conductive glass, after No. 2 is the processing of FTO colloidal sol before and after the processing
Sample, No. 3 are sample after FTO colloidal sol and precursor solution processing)
(a is reference FTO glass sample to section electron microscope to Fig. 2 FTO electro-conductive glass, and b is after FTO colloidal sol is handled before and after the processing
Sample, c are sample after FTO colloidal sol and precursor solution processing)
Fig. 3 FTO electro-conductive glass transmitance before and after the processing
Fig. 4 FTO electro-conductive glass electric conductivity before and after the processing
Specific embodiment
Embodiment 1:
1, F:Sn=2:1, partial size 15nm are prepared using sol-gel method, square resistance is 90 Ω/, mass fraction
For 2.0% FTO ethyl alcohol phase colloidal sol.
2, with 3000rpm on FTO electro-conductive glass, time 30s spin coating FTO colloidal sol, spin coating number is 2 times.
3, the sample after coating is first placed in 50 DEG C of heat preservation 50min to be dried, then is placed in Muffle furnace and is calcined,
5 DEG C/min of heating rate, keeps the temperature 30min, then Temperature fall at 500 DEG C.
4, using potassium fluoride as Fluorine source, stannous chloride is tin source, and it is 1mM FTO aqueous solution that F:Sn=1:1, which prepares concentration,.
5, FTO solution is lifted on the sample of preparation using method of pulling up, pull rate 10mm/min is kept the temperature at 30 DEG C
30min, lifting number are 2 times.
6, the sample after coating is first placed in 50 DEG C of heat preservation 50min to be dried, then is placed in Muffle furnace and is calcined,
5 DEG C/min of heating rate, keeps the temperature 30min, then Temperature fall at 450 DEG C.
Embodiment 2:
1, Sb:Sn=0.08:1, partial size 12nm are prepared using sol-gel method, square resistance is 100 Ω/, quality
The ATO ethyl alcohol phase colloidal sol that score is 2.0%.
2, with 3000rpm on ATO electro-conductive glass, time 20s spin coating ATO colloidal sol, spin coating number is 1 time.
3, the sample after coating is first placed in 50 DEG C of heat preservation 30min to be dried, then is placed in Muffle furnace and is calcined,
5 DEG C/min of heating rate, keeps the temperature 20min, then Temperature fall at 450 DEG C.
4, using antimony trichloride as antimony source, tin tetrachloride is tin source, and it is 0.5mM ATO water that Sb:Sn=0.05:1, which prepares concentration,
Solution.
5, ATO solution is lifted on the sample of preparation using method of pulling up, pull rate 5mm/min is kept the temperature at 50 DEG C
30min, lifting number are 1 time.
6, the sample after coating is first placed in 40 DEG C of heat preservation 40min to be dried, then is placed in Muffle furnace and is calcined,
5 DEG C/min of heating rate, keeps the temperature 30min, then Temperature fall at 500 DEG C.
Embodiment 3:
1, Sn:In is prepared using sol-gel method2O3=2:1, partial size 10nm, square resistance are 90 Ω/, quality point
The ITO ethyl alcohol phase colloidal sol that number is 5.0%.
2, with 1500rpm on ITO electro-conductive glass, time 20s spin coating ITO colloidal sol, spin coating number is 2 times.
3, the sample after coating is first placed in 50 DEG C of heat preservation 50min to be dried, then is placed in Muffle furnace and is calcined,
5 DEG C/min of heating rate, keeps the temperature 30min, then Temperature fall at 450 DEG C.
4, using tin oxalate as tin source, indium trichloride is indium source, Sn:In2O3It is that 2mM ATO water phase is molten that=1:1, which prepares concentration,
Glue.
5, ITO solution is lifted on the sample of preparation using method of pulling up, pull rate 10mm/min is kept the temperature at 40 DEG C
30min, lifting number are 1 time
6, the sample after coating is first placed in 50 DEG C of heat preservation 40min to be dried, then is placed in Muffle furnace and is calcined,
5 DEG C/min of heating rate, keeps the temperature 30min, then Temperature fall at 450 DEG C.
Embodiment 4:
1, Al:ZnO=4:1, partial size 20nm are prepared using sol-gel method, square resistance is 100 Ω/, quality point
The ITO ethyl alcohol phase colloidal sol that number is 4.0%.
2, with 3000rpm on AZO electro-conductive glass, time 30s spin coating AZO colloidal sol, spin coating number is 2 times.
3, the sample after coating is first placed in 40 DEG C of heat preservation 50min to be dried, then is placed in Muffle furnace and is calcined,
5 DEG C/min of heating rate, keeps the temperature 30min, then Temperature fall at 500 DEG C.
4, using aluminium chloride as silicon source, zinc sulfate is zinc source, and it is 1.5mM AZO aqueous solution that Al:ZnO=2:1, which prepares concentration,.
5, ATO solution is lifted on the sample of preparation using method of pulling up, pull rate 10mm/min is kept the temperature at 30 DEG C
30min, lifting number are 2 times.
6, the sample after coating is first placed in 50 DEG C of heat preservation 50min to be dried, then is placed in Muffle furnace and is calcined,
5 DEG C/min of heating rate, keeps the temperature 30min, then Temperature fall at 450 DEG C.
Case study on implementation described above is not to limit to the scope of the patents of the invention, but the present invention is not limited to above-mentioned implementations
Example, can make a variety of variations with the purpose of innovation and creation according to the present invention, and the spirit of all technical solutions according to the present invention is real
The change made under matter and principle substitution, combines, is reduced to equivalent substitute mode, as long as meeting goal of the invention of the invention, all
It belongs to the scope of protection of the present invention.
Claims (10)
1. a kind of method of enhancing electro-conductive glass permeability and electric conductivity, which is characterized in that brilliant by coating transparent conductive nano
Colloidal sol and its precursor solution fill conductive glass surface bumps defect, effectively improve electro-conductive glass translucency and electric conductivity, wrap
Include following steps:
A. electrically conducting transparent colloidal sol is coated in conductive glass surface first, then calcined；
B. precursor solution is coated again, is calcined again；
C. calcining step are as follows: the sample after coating is first placed in 40-80 DEG C of heat preservation 20-50min and is dried, then is placed in Muffle
It is calcined in furnace, 5-15 DEG C of heating rate/min, then in 350-500 DEG C of heat preservation 20-50min, Temperature fall obtains sample；
Wherein, the electro-conductive glass is FTO, ATO, ITO or AZO；
The electrically conducting transparent colloidal sol is SnO2、In2O3, ZnO and F, Sb element doping SnO2Colloidal sol, Sn element doping
In2O3Colloidal sol, the ZnO colloidal sol of Al element doping；
The precursor solution is that villiaumite adulterates stanniferous inorganic salts or organic salt, antimonic salt adulterate stanniferous inorganic salts or organic salt, tin
Salt dopping inorganic salts containing indium or organic salt, aluminium salt doping inorganic salts containing zinc or organic salt are one of, wherein the substance of F and Sn
Amount ratio be 0.01~4: 1, Sb and Sn the mass ratio of the material be 0.01~4: 1, Sn and In the mass ratio of the material be 0.01~4:
The mass ratio of the material of 1, Al and Zn is 0.01~8: 1, and solvent is one kind of ethyl alcohol, isopropanol or water, and concentration is 0.01~6mM.
2. enhancing the method for electro-conductive glass permeability and electric conductivity according to claim 1, which is characterized in that described transparent to lead
Electrosol solvent is one kind of ethyl alcohol, isopropanol or water, and aerosol particle size is 2~20nm, by the square resistance < after powder tabletting
100 Ω/, mass fraction are 0.1~10.0%, wherein the mass ratio of the material of F and Sn is the substance of 0.01~4: 1, Sb and Sn
Amount ratio be 0.01~4: 1, Sn and In the mass ratio of the material be the mass ratio of the material of 0.01~4:1, Al and Zn be 0.01~8:
1。
3. enhancing the method for electro-conductive glass permeability and electric conductivity according to claim 1, which is characterized in that the villiaumite is
Sodium fluoride, potassium fluoride or ammonium fluoride are one of.
4. enhancing the method for electro-conductive glass permeability and electric conductivity according to claim 1, which is characterized in that the stanniferous nothing
Machine salt or organic salt are that stannous chloride, tin tetrachloride or stannous oxalate are one of.
5. enhancing the method for electro-conductive glass permeability and electric conductivity according to claim 1, which is characterized in that the antimonic salt is
Antimony trichloride or Antimony pentachloride are one of.
6. enhancing the method for electro-conductive glass permeability and electric conductivity according to claim 1, which is characterized in that it is described containing indium without
Machine salt or organic salt are that indium trichloride, indium sulfate or indium nitrate are one of.
7. enhancing the method for electro-conductive glass permeability and electric conductivity according to claim 1, which is characterized in that the aluminium salt is
Alchlor or aluminum sulfate are one of.
8. enhancing the method for electro-conductive glass permeability and electric conductivity according to claim 1, which is characterized in that the zinc is inorganic
Salt or organic salt are that zinc sulfate, zinc nitrate or zinc chloride are one of.
9. enhancing the method for electro-conductive glass permeability and electric conductivity according to claim 1, it is characterised in that: the coating side
Method is spin-coating method or czochralski method；When using spin-coating method film, revolving speed 1000-3000rpm, time 5-30s, spin coating number
It is 1-3 times；When using czochralski method film, pull rate 5-15mm/min, in 30-50 DEG C of heat preservation 30-50min, lifting time
Number is 1-3 times.
10. enhancing the method for electro-conductive glass permeability and electric conductivity according to claim 1, it is characterised in that: the conduction
Transmitance and electric conductivity improve 5% or more after glass-modified.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101103653A (en) * | 2002-09-03 | 2008-01-09 | 康宁股份有限公司 | Material for use in the manufacturing of luminous display devices |
| KR100804003B1 (en) * | 2006-09-08 | 2008-02-18 | 한국과학기술연구원 | Process for preparing indium tin oxide film |
| CN101337773A (en) * | 2008-08-14 | 2009-01-07 | 浙江理工大学 | Method for preparing ITO film with high conductivity |
| CN102067243A (en) * | 2008-06-24 | 2011-05-18 | 日本曹达株式会社 | Transparent conductive film having FTO/ITO multilayer body |
| CN103508406A (en) * | 2012-06-29 | 2014-01-15 | 无锡华润上华半导体有限公司 | AZO thin film, preparing method and MEMS device comprising AZO thin film |
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2016
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101103653A (en) * | 2002-09-03 | 2008-01-09 | 康宁股份有限公司 | Material for use in the manufacturing of luminous display devices |
| KR100804003B1 (en) * | 2006-09-08 | 2008-02-18 | 한국과학기술연구원 | Process for preparing indium tin oxide film |
| CN102067243A (en) * | 2008-06-24 | 2011-05-18 | 日本曹达株式会社 | Transparent conductive film having FTO/ITO multilayer body |
| CN101337773A (en) * | 2008-08-14 | 2009-01-07 | 浙江理工大学 | Method for preparing ITO film with high conductivity |
| CN103508406A (en) * | 2012-06-29 | 2014-01-15 | 无锡华润上华半导体有限公司 | AZO thin film, preparing method and MEMS device comprising AZO thin film |
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