CN103325859B - A kind of preparation method of ito thin film - Google Patents

A kind of preparation method of ito thin film Download PDF

Info

Publication number
CN103325859B
CN103325859B CN201310260388.4A CN201310260388A CN103325859B CN 103325859 B CN103325859 B CN 103325859B CN 201310260388 A CN201310260388 A CN 201310260388A CN 103325859 B CN103325859 B CN 103325859B
Authority
CN
China
Prior art keywords
thin film
ito
preparation
ito thin
colloidal sol
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201310260388.4A
Other languages
Chinese (zh)
Other versions
CN103325859A (en
Inventor
徐东
***
石佳光
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Xu dong
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to CN201310260388.4A priority Critical patent/CN103325859B/en
Publication of CN103325859A publication Critical patent/CN103325859A/en
Application granted granted Critical
Publication of CN103325859B publication Critical patent/CN103325859B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

Abstract

The present invention is applicable to field of photovoltaic materials, it is provided that the preparation method of a kind of ito thin film, and the method comprises the following steps: preparation ITO colloidal sol;Prepare ito thin film.The ito thin film surfacing, the granule that are prepared by said method are fine and close, and the mean transmissivity in visible region is up to 90%, and resistivity reaches 10-4Level, work function reaches 4.9eV, it is possible to meet the application in the field such as LCD, solar film battery.

Description

A kind of preparation method of ito thin film
Technical field
The invention belongs to field of photovoltaic materials, particularly relate to the preparation method of a kind of ito thin film.
Background technology
Indium tin oxide (being called for short ITO) thin film is the sull of a kind of electrically conducting transparent, has conductivity High, visible light transmissivity high, chemical stability is good and with the advantage such as matrix is firmly combined with, be mainly used in Field of photoelectric devices, be mainly used in flat panel Liquid Crystal show (LCD), sensor, electroluminescent (ELD) and The aspects such as functional glass, in particular with developing rapidly of solar film battery in recent years, ito thin film is made For the necessary component of solaode, promote the market demand to ito thin film greatly.
Ito thin film main performance index in products application is presented as resistivity, transmitance and work function. At present, the preparation method of ito thin film mainly has magnetron sputtering method, reacting heat evaporation method, metallorganic Learn vapour deposition process, spray pyrolysis to send out and sol-gel process etc., in the most above-mentioned ito thin film preparation method, The most ripe and formation industrialization the method for development is magnetron sputtering method.But, cost is high, process conditions Harshness etc. becomes sputtering method and produces the major defect of ito thin film.
Summary of the invention
The purpose of the embodiment of the present invention is to provide the preparation method of a kind of ito thin film, it is intended to solve how to carry Problem for the ito thin film that a kind of low cost, technique component content simple, each can accurately control.
The embodiment of the present invention is achieved in that the preparation method of a kind of ito thin film, comprises the following steps:
To containing indium salts, pink salt mixed solution in add stabilizer, surfactant and carry out mixing, at ageing Reason, obtains ITO colloidal sol;
Described ITO colloidal sol is carried out on matrix dried after film at least one times, then carries out annealing treatment Reason, obtains ito thin film, and wherein, the method for described annealing is: by the base after dried coating film processes Body is at N2And H2It is incubated 1-2h, wherein, described N in 450-700 DEG C under mixed atmosphere2And H2In mixed atmosphere H2Volume fraction be 1~4%.
Embodiments providing a kind of method using preparation of ITO thin films by Sol-Gel process, the method makes Prepare mixed solution by solwution method, can control the content of each component in ito thin film more accurately, meanwhile, with Main flow production at present is prepared ito thin film method and is compared, and the method need not large-scale vapour deposition and magnetic control spatters Jet device, equipment cost is low, depreciation is little and present invention process is simple, it is possible to achieve large area is coated with continuously Film, feasibility is high.The ito thin film that the method prepares, purity is high, and resistivity is low, can reach 10-4 Level, transmitance is up to more than 90%, and work function is high, for 4.9eV, it is possible to meet solar film battery Requirement to thin-film electrode material.
Accompanying drawing explanation
Fig. 1 is the preparation technology flow chart of the ito thin film that the embodiment of the present invention 1 provides;
Fig. 2 is the change in resistance curve chart of the ito thin film that the embodiment of the present invention 2 provides;
Fig. 3 is the transmitance change curve of the ito thin film that the embodiment of the present invention 3 provides;
Fig. 4 is the Work function Change curve chart of the ito thin film that the embodiment of the present invention 4 provides.
Detailed description of the invention
In order to make the technical problem to be solved in the present invention, technical scheme and beneficial effect clearer, with Lower combination drawings and Examples, are further elaborated to the present invention.Should be appreciated that described herein Specific embodiment only in order to explain the present invention, be not intended to limit the present invention.
Embodiments provide the preparation method of a kind of ito thin film, comprise the following steps:
S01. prepare ITO colloidal sol: to containing indium salts, pink salt mixed solution in add stabilizer, surface activity Agent carries out mixing, ripening, obtains ITO colloidal sol;
S02. ito thin film is prepared: carry out described ITO colloidal sol on matrix being dried place after film at least one times Reason, then makes annealing treatment, obtains ito thin film, and wherein, the method for described annealing is: will be through Matrix after dried coating film process is at N2And H2It is incubated 1-2h, wherein, institute in 450-700 DEG C under mixed atmosphere State N2And H2H in mixed atmosphere2Volume fraction be 1~4%.
Specifically, in above-mentioned steps S01, the compound method of mixed solution is unrestricted, can be by indium salts After being dissolved in organic solvent, reflux at 55-70 DEG C agitating heating 1-3h, treats that it is cooled to room temperature, is specially When 20-30 DEG C, it is mixed with the organic solution of pink salt;Can also be indium salts is dissolved in organic solvent after, Reflux at 55-70 DEG C agitating heating 1-3h, treats that it cools down room temperature, when specially 20-30 DEG C, adds pink salt Mixed dissolution forms mixed solution.In the embodiment of the present invention, the mode of mixing is unrestricted, conventional mixing Method is used equally to prepare above-mentioned mixed solution.As the presently preferred embodiments, in order to realize above-mentioned indium salts and pink salt Being sufficiently mixed of mixed solution, needs to be stirred above-mentioned mixed liquor, wherein preferred magnetic agitation, Mixing time is 1-5h.In order to avoid Sn in mixed solution4+Produce flocculent deposit after hydrolysis to separate out and affect The quality of ito thin film, in this step S01 for dissolving indium salts, the organic solvent of pink salt is preferably anhydrous solvent. As specific embodiment, wherein, the above-mentioned organic solvent for dissolving indium salts be acetyl ethyl ketone, first isopropyl acetone, At least one in butanone, Ketohexamethylene;For dissolve the organic solvent of pink salt be ethanol, methanol, isopropanol, At least one in ethylene glycol monomethyl ether.It should be understood, of course, that can be used in this area dissolving above-mentioned indium salts Compound, pink salt compound organic solvent the most within the scope of the present invention.
In a preferred embodiment, the indium salts in this step S01 is Indium-111 chloride, trichloride hydrate indium (InCl3·xH2O) at least one, in indium acetate, Indium Tris acetylacetonate, indium nitrate, indium hydroxide, its In, trichloride hydrate indium (InCl3·xH2O) in, preferably x=3.5 or 4.Pink salt be anhydrous stannic chloride, At least one in tin acetate, five water stannic chlorides, stannous chloride dihydrate.Described containing indium salts, the mixing of pink salt Solution is containing Indium-111 chloride, trichloride hydrate indium (InCl3·xH2O), indium acetate, Indium Tris acetylacetonate, At least one in indium nitrate, indium hydroxide and anhydrous stannic chloride, tin acetate, five water stannic chlorides, two water chlorine Change the mixed solution of at least one in stannous.Above-mentioned mixing is can be used in of course it is to be understood that this area Indium salts prepared by solution, pink salt and combinations thereof are the most within the scope of the present invention.In order to farthest drop The content of impurity in the low ito thin film finally given, this indium salts, pink salt Analysis about Selection are pure, the most more preferably With chromatographically pure, as selected the purity indium salts more than 99.99%, pink salt.
As the presently preferred embodiments, above-mentioned preparation containing indium salts, the mixed solution of pink salt, its concentration with under The thickness stating ito thin film prepared by step S02 has direct relation, when mixed solution concentration is bigger, preparation Monolayer ito thin film is thicker.Therefore, in order to obtain the monolayer ito thin film that thickness is suitable, be evenly distributed, above-mentioned In in mixed solution3+With Sn4+Total concentration is 0.1-0.5mol/L.Additionally, described in above-mentioned S01 containing indium salts, In the mixed solution of pink salt, the ratio of each component has certain impact, the especially ratio of indium to the performance of thin film Relatively big on the electric conductivity of ito thin film and the impact of work function, the content of indium is different, the conduction of thin-film material Performance and work function are different.In the embodiment of the present invention, use In in ito thin film commonly used in the art3+With Sn4+'s Concentration and Sn thereof4+Account for In3+With Sn4+The ratio of total concentration is used equally to realize above-mentioned containing indium salts, the mixing of pink salt The preparation of solution.Wherein, Sn is worked as4+Account for In3+With Sn4+During the 5-12at% of total concentration, the ITO prepared is thin The electric conductivity of membrane material is preferable, and work function is bigger.
In this step S01, adding stabilizer in the mixed solution containing indium salts and pink salt is so that indium salts It is uniformly dispersed in mixed solution with pink salt, and makes the stable system of mixed solution.That commonly uses in this area is steady Determine agent and consumption is used equally to the embodiment of the present invention.In a preferred embodiment, alcamines selected by this stabilizer Compound, in further preferred embodiments, this stabilizer selects monoethanolamine, diethanolamine, three ethanol At least one in amine, the most preferably monoethanolamine.
In above-mentioned steps S01, in order to improve the filming performance of colloidal sol and make the sol particles of formation be evenly distributed, The ITO colloidal sol of preparation needs to add a certain amount of surfactant.After adding surfactant, preparation During ito thin film, ITO colloidal sol is more preferable with the wettability of matrix, and film forming is more uniform;It addition, to annealed place Ito thin film after reason, it is more preferable to add the crystalline property after surfactant, and does not adds surfactant Comparing, add the ito thin film electric conductivity after surfactant and improve a lot, resistivity substantially reduces. In a preferred embodiment, in order to form stable, finely dispersed ITO colloidal sol, obtain simultaneously electric conductivity high, The ito thin film that resistivity is low, the consumption of described surfactant is the 0.5-3% for colloidal sol total volume fraction. As specific embodiment, this surfactant is fatty acid ethylene glycol ether, polyethenoxy sorbitan list oil Acid esters, ethylene oxide/propylene oxide block copolymer, fatty monoethanol amide, fatty diglycollic amide, In single hard fatty acids glyceride, sodium n-alkylbenzenesulfonate, polyoxyethylenated alcohol sodium sulfate at least one Kind.In of course it is to be understood that this area, other can be used for solving the surfactant of the problems referred to above also at this In the protection domain of invention.When surfactant is grouped into by two groups or two or more one-tenth, its each composition Mass ratio is unrestricted.
In order to form uniform and stable ITO colloidal sol, through above-mentioned process containing indium salts, the mixed solution of pink salt Needing to carry out ripening, digestion time is preferably 3-5h, specifically includes 3h, 3.5h, 4h, 4.5h, 5h etc..
Film matrix described in above-mentioned steps S02 does not limit, and can be used for what ito thin film was smeared in this area Matrix is all in the range of the embodiment of the present invention.As particular preferred embodiment, owing to following step uses height Warm processes and is dried ito thin film and makes annealing treatment, therefore, the selection of above-mentioned film matrix is high temperature resistant, The quartz glass substrate that chemical stability is good.As specific embodiment, the preparation method of quartz glass substrate is: First by after quartz glass ultrasonic cleaning 10-30min, with deionized water rinsing several times, put into and acetone boils 10-30 Min, alternately rinses several times with methanol, deionized water, it is thus achieved that the matrix of clean surface, last nitrogen the most successively The 60-120 DEG C of drying in an oven of air-blowing wind is stand-by.
In this S02 step, ITO colloidal sol is prepared from matrix by ito thin film by using physical method. The present invention uses antivacuum physical method, not only need not the equipment of costliness, decreases cost of investment, and Simple to operate, it is simple to large-scale industrial production.As particular preferred embodiment, described physical method is preferably One in knife coating, spin-coating method, czochralski method, drop-coating, silk screen print method.Of course it is to be understood that In this area other to be used for the physical method of ITO colloidal sol film the most within the scope of the present invention.In order to Obtain thickness uniformly suitable monolayer ito thin film, the embodiment of the present invention selected dip-coating method carry out film, The rate of pulling is 5-20cm/min.
Every time after film, need ito film layer is dried process.Owing to ITO colloidal sol is the most normal With temperature such as 100-400 DEG C dry time, matrix is thin with the ITO of the combination defective tightness of ITO colloidal sol, formation Membrane crystallization is not sufficiently stable, thus causes the part thin film when film again of ito thin film after drying the most molten On the one hand in ITO colloidal sol, therefore, have impact on the quality of ito thin film and electric conductivity thereof and work function; On the other hand, it is unfavorable for accurately controlling the thickness of film.In order to solve the problems referred to above, thus it is effectively improved height The adhesion of temperature dried ito thin film crystallization and matrix, when avoiding again film, part thin film is dissolved in molten simultaneously Glue, finally give conduct electricity very well, ito thin film that work function is high, in the embodiment of the present invention, described be dried Temperature is preferably 500~600 DEG C, and drying time is 10-30min.In order to improve drying efficiency, it is dried and sets Standby preferably tube furnace.
In S02 step, in order to obtain the Ag doping ito thin film of suitable thickness, need to carry out more than at least one times Dried coating film process.Wherein, the standard of number of repetition is to meet the thickness of described ito thin film at 20-300nm It is advisable.The embodiment of the present invention be use single to be dried, the mode of film repeatedly to change the thickness of thin film, and When coating times is too much, film thickness is excessive, cause in annealing process due to the stress between different film layers Difference is excessive causes thin film easily to ftracture in change, and defect increases, and crystal boundary scattering strengthens, and film resiativity increases, Thus cause the electric conductivity of ito thin film to be deteriorated;When film thickness is too small, in Thin-film anneal processing procedure In be unfavorable for promoting thin film crystallization, the integrity of lattice structure is poor, and defect is more, to the trapping of carrier with Scattering process is greatly enhanced, and makes carrier concentration and mobility relatively low, and the resistivity of ito thin film increases.Warp Inventor studies discovery repeatedly, when the thickness of Ag doping ito thin film is at 20-300nm, and described Ag doping ITO Conducting electricity very well of thin film, and resistivity is low, can reach 10-4Level.
In this S02 step, in order to promote the growth of film particles, reduce crystal boundary scattering, accelerate crystal boundary passivation, Obtain surfacing, resistivity ground, thin film that electric conductivity is strong, meanwhile, prevent ito thin film from aoxidizing, Described ito thin film carries out quick thermal annealing process under reducing atmosphere.As particular preferred embodiment, described The method of annealing is: by film-dried matrix at N2And H2In 450-700 DEG C of guarantor under mixed atmosphere Temperature 1-2h, wherein, described N2And H2H in mixed atmosphere2Volume fraction be 1-4%.Certainly, it should reason Solve, other noble gases, such as Ar, also can use as protective gas in above-mentioned annealing.
The sol-gel technique that the present invention uses ionic liquid phase to adulterate prepares ito thin film, each former in ito thin film Son is interconnected to form network structure, and the transmission for electronics provides effective path, it is possible to reduce thin film Resistivity, improves the electric conductivity of thin film.The ito thin film surfacing of preparation, granule densification, visible Light district transmitance reaches more than 85%, and resistivity reaches 10-4Level, it is possible to meet flat pannel display, solar energy thin The needs in the fields such as film battery.
The present invention uses sol-gel technique to prepare ito thin film, and preparation method is simple, uses ionic liquid phase to mix Miscellaneous method can accurately control ions dosage, makes Sn/ (Sn+In)=5-12at% in the ITO colloidal sol of preparation, from And the electric conductivity that improves ito thin film is preferable;Secondly, during preparation ITO colloidal sol, with the addition of surface to live Property agent, modified to Sol-Modified, uniform in matrix surface film forming during film, the ito thin film electric conductivity obtained Energy is high, resistivity is low;Again, the embodiment of the present invention prepares ito thin film, reducing gases after high-temperature heat treatment Annealing under atmosphere, the ito thin film granule of preparation is relatively big, arranges finer and close, and the ito thin film obtained conducts electricity very well, There is higher work function.The ito thin film surface compact prepared through above-mentioned process is smooth, it is seen that light Transmitance reaches 90%, and resistivity is low reaches 10-4, work function is more than 4.9eV, can meet LCD, solar energy The requirement to ito thin film performance of the hull cell field.
The present invention will be further illustrated by the examples that follow.
The preparation method of one one kinds of ito thin films of embodiment
The preparation of ITO colloidal sol: Indium-111 chloride is dissolved in acetylacetone,2,4-pentanedione 55 DEG C and is heated at reflux 1h, two hydration dichloros Change stannum to be dissolved in a small amount of dehydrated alcohol, then will mix under two kinds of solution room temperatures, wherein in mixed solution Sn/ (Sn+In)=5%, continues stirring 1h, then after adding a small amount of monoethanolamine, single hard fatty acids glyceride ITO colloidal sol is obtained after ageing 3h.
Matrix processes: quartz glass ultrasonic cleaning 10min, deionized water rinsing is put in acetone the most afterwards and boiled 10min, the most successively with nitrogen blowing 70 DEG C of drying in an oven after methanol, deionized water rinsing.
Lifting film: Best-Effort request prepares ito thin film, and quartz glass substrate is dipped vertically into 20s in gel, At the uniform velocity lift with 5cm/min, obtain uniform dissolved glue film.
Heat treatment: dissolved glue film, at 500 DEG C of heat treatment 10min, then repeats film according to thickness requirement, finally N in tube furnace2And H2The lower 500 DEG C of annealing 1h of mixed atmosphere, quickly cooling obtains ito thin film.
The preparation technology flow chart of this ito thin film is as shown in Figure 1.
The preparation method of 21 kinds of ito thin films of embodiment
Prepared by colloidal sol: four water indium chloride being dissolved in acetylacetone,2,4-pentanedione 65 DEG C and is heated at reflux 2h, anhydrous stannic chloride is dissolved in In a small amount of dehydrated alcohol, then will mix under two kinds of solution room temperatures, wherein in mixed solution Sn/ (Sn+In)=5-12%, continues stirring after adding diethanolamine, polyoxyethylene sorbitan monooleate dehydration 2h, then obtains ITO colloidal sol after ageing 4h.
Matrix processes: quartz glass ultrasonic cleaning 20min, deionized water rinsing is put in acetone the most afterwards and boiled 15min, the most successively with nitrogen blowing 80 DEG C of drying in an oven after methanol, deionized water rinsing.
Lifting film: Best-Effort request prepares ito thin film, and quartz glass substrate is dipped vertically into 10s in gel, At the uniform velocity lift with 10cm/min, obtain uniform dissolved glue film.
Heat treatment: dissolved glue film, at 500 DEG C of heat treatment 10min, then repeats film according to thickness requirement, finally N in tube furnace2And H2The lower 550 DEG C of annealing 1h of mixed atmosphere, and furnace cooling to obtain ITO to room temperature thin Film.
The ito thin film prepared is carried out resistivity properties test, and its result is as shown in Figure 2.
The preparation method of 31 kinds of ito thin films of embodiment
Prepared by colloidal sol: Indium Tris acetylacetonate being dissolved in acetylacetone,2,4-pentanedione 70 DEG C and is heated at reflux 2.5h, five water stannic chlorides are molten In a small amount of dehydrated alcohol, then will mix under two kinds of solution room temperatures, wherein in mixed solution Sn/ (Sn+In)=10%, continues to stir after adding a small amount of monoethanolamine, polyoxyethylene sorbitan monooleate dehydration Mix 3h, then obtain ITO colloidal sol after ageing 5h.
Matrix processes: quartz glass ultrasonic cleaning 20min, deionized water rinsing is put in acetone the most afterwards and boiled 30min, the most successively with nitrogen blowing 90 DEG C of drying in an oven after methanol, deionized water rinsing.
Lifting film: Best-Effort request prepares ito thin film, and quartz glass substrate is dipped vertically into 1min in gel, At the uniform velocity lift with 15cm/min, obtain uniform dissolved glue film.
Heat treatment: dissolved glue film, at 500 DEG C of heat treatment 30min, then repeats film according to thickness requirement, finally N in tube furnace2And H2The lower 550 DEG C of annealing 2h of mixed atmosphere, and furnace cooling to obtain ITO to room temperature thin Film.
The ito thin film prepared is carried out light transmittance properties test, and its result is as shown in Figure 3.
The preparation method of 41 kinds of ito thin films of embodiment
Prepared by colloidal sol: indium chloride being dissolved in acetylacetone,2,4-pentanedione 60 DEG C and is heated at reflux 1h, five water stannic chlorides are dissolved on a small quantity Dehydrated alcohol in, then will under two kinds of solution room temperatures mix, wherein Sn/ (Sn+In)=9% in mixed solution, Continue stirring 3h after adding monoethanolamine, fatty acid ethylene glycol ether, then obtain ITO colloidal sol after ageing 5h.
Matrix processes: quartz glass ultrasonic cleaning 20min, deionized water rinsing is put in acetone the most afterwards and boiled 30min, the most successively with nitrogen blowing 80 DEG C of drying in an oven after methanol, deionized water rinsing.
Lifting film: Best-Effort request prepares ito thin film, and quartz glass substrate is dipped vertically into 10s in gel, At the uniform velocity lift with 15cm/min, obtain uniform dissolved glue film.
Heat treatment: dissolved glue film, at 500 DEG C of heat treatment 30min, then repeats film according to thickness requirement, finally N in tube furnace2And H2Under mixed atmosphere, 450-650 DEG C makes annealing treatment 2h, and furnace cooling obtains ITO to room temperature Thin film.
The ito thin film prepared is carried out work function performance test, and its result is as shown in Figure 4.
The preparation method of 51 kinds of ito thin films of embodiment
Prepared by colloidal sol: indium acetate is dissolved in acetylacetone,2,4-pentanedione 70 DEG C and is heated at reflux 1.5h, and anhydrous stannic chloride is dissolved in few In the dehydrated alcohol of amount, then will mix under two kinds of solution room temperatures, wherein in mixed solution Sn/ (Sn+In)=10%, adds monoethanolamine, sodium n-alkylbenzenesulfonate and fatty monoethanol amide follow-up Continuous stirring 3h, then obtains ITO colloidal sol after ageing 5h.
Matrix processes: quartz glass ultrasonic cleaning 20min, deionized water rinsing is put in acetone the most afterwards and boiled 30min, the most successively with nitrogen blowing 90 DEG C of drying in an oven after methanol, deionized water rinsing.
Lifting film: Best-Effort request prepares ito thin film, quartz glass substrate be dipped vertically in gel 15s with 15cm/min at the uniform velocity lifts, and obtains uniform dissolved glue film.
Heat treatment: dissolved glue film, at 500 DEG C of heat treatment 30min, then repeats film according to thickness requirement, finally N in tube furnace2And H2The lower 550 DEG C of annealing 2h of mixed atmosphere, and furnace cooling to obtain ITO to room temperature thin Film.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all at this Any amendment, equivalent and the improvement etc. made within bright spirit and principle, should be included in the present invention Protection domain within.

Claims (5)

1. a preparation method for ito thin film, comprises the following steps:
To containing indium salts, pink salt mixed solution in add stabilizer, surfactant and carry out mixing, at ageing Reason, obtains ITO colloidal sol, described containing indium salts, pink salt mixed solution in, In3+With Sn4+Total concentration is 0.1-0.5 Mol/L, wherein, Sn4+Account for In3+With Sn4+The 5-12at% of total concentration;In described ITO colloidal sol, described table Face activating agent consumption is the 0.5-3% of described ITO colloidal sol total volume fraction, and described surfactant is fatty acid Glycol ether, polyoxyethylene sorbitan monooleate dehydration, ethylene oxide/propylene oxide block copolymer, fat Fat acid single ethanol amide, fatty diglycollic amide, single hard fatty acids glyceride, sodium n-alkylbenzenesulfonate, At least one in polyoxyethylenated alcohol sodium sulfate;
Described ITO colloidal sol is carried out on matrix dried after film at least one times, then carries out annealing treatment Reason, obtains ito thin film, and wherein, the method for described annealing is: by the base after dried coating film processes Body is at N2And H2It is incubated 1-2h, wherein, described N in 450-700 DEG C under mixed atmosphere2And H2Gaseous mixture H in atmosphere2Volume fraction be 1~4%;
In the step of described ito thin film, the temperature of described dried is 500-600 DEG C, and the time is 10-30 min。
2. the preparation method of ito thin film as claimed in claim 1, it is characterised in that: described in preparation In the step of ITO colloidal sol, described indium salts is in Indium-111 chloride, indium acetate, Indium Tris acetylacetonate, indium nitrate At least one.
3. the preparation method of ito thin film as claimed in claim 1 or 2, it is characterised in that: in preparation In the step of described ITO colloidal sol, described pink salt is anhydrous stannic chloride, five water stannic chlorides, tin acetate, two water At least one in stannous chloride.
4. the preparation method of ito thin film as claimed in claim 1 or 2, it is characterised in that: in preparation In the step of described ITO colloidal sol, described stabilizer is alcamine compound.
5. the preparation method of ito thin film as claimed in claim 1 or 2, it is characterised in that: in preparation In the step of described ITO colloidal sol, described digestion time is 3~5h.
CN201310260388.4A 2013-06-26 2013-06-26 A kind of preparation method of ito thin film Active CN103325859B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201310260388.4A CN103325859B (en) 2013-06-26 2013-06-26 A kind of preparation method of ito thin film

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310260388.4A CN103325859B (en) 2013-06-26 2013-06-26 A kind of preparation method of ito thin film

Publications (2)

Publication Number Publication Date
CN103325859A CN103325859A (en) 2013-09-25
CN103325859B true CN103325859B (en) 2016-08-10

Family

ID=49194510

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201310260388.4A Active CN103325859B (en) 2013-06-26 2013-06-26 A kind of preparation method of ito thin film

Country Status (1)

Country Link
CN (1) CN103325859B (en)

Families Citing this family (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103872089B (en) * 2014-02-28 2016-11-02 京东方科技集团股份有限公司 A kind of display floater and preparation method thereof, display device
CN104318983A (en) * 2014-10-31 2015-01-28 徐东 Preparation method of ITO thin film
CN105140312B (en) * 2015-08-28 2017-04-12 中国电子科技集团公司第四十八研究所 Composite TCO film and preparation method thereof
FR3061210B1 (en) * 2016-12-22 2021-12-24 Electricite De France SOL-GEL PROCESS FOR MANUFACTURING AN ANTICORROSION COATING ON METALLIC SUBSTRATE
CN107093495A (en) * 2017-03-22 2017-08-25 合肥仁德电子科技有限公司 A kind of preparation method of ito thin film for touch-screen
CN108109722A (en) * 2017-12-14 2018-06-01 湖南兴威新材料有限公司 Ito thin film preparation method
CN113816615B (en) * 2021-08-31 2023-06-16 西安理工大学 Ultrahigh transparent conductive ITO film and preparation method thereof
CN114242338B (en) * 2021-12-16 2024-02-06 长春博信光电子有限公司 Method for improving resistance value of ITO film
CN117275830B (en) * 2023-09-04 2024-03-29 冷水江市京科电子科技有限公司 Preparation method of capacitive touch screen ITO film

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1476021A (en) * 2002-06-28 2004-02-18 日亚化学工业株式会社 Composition, solution and method for forming transparent conductive film
CN102646759A (en) * 2012-05-04 2012-08-22 深圳市科聚新材料有限公司 Preparing method for transparent conductive oxide film

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1476021A (en) * 2002-06-28 2004-02-18 日亚化学工业株式会社 Composition, solution and method for forming transparent conductive film
CN102646759A (en) * 2012-05-04 2012-08-22 深圳市科聚新材料有限公司 Preparing method for transparent conductive oxide film

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
"基于溶胶凝胶法ITO薄膜材料的制备与表征";宣鑫科 等;《齐齐哈尔大学学报》;20100531;第26卷(第3期);全文 *
"溶胶-凝胶法制备ITO薄膜及其光电性能的研究";袁红梅 等;《电子器件》;20100228;第33卷;第5页右栏第1段至第9页左栏最后一段 *
"溶胶-凝胶法制备ITO薄膜研究进展";张学骜 等;《材料科学与工艺》;20070430;第15卷(第2期);全文 *
"溶胶凝胶法制备ITO透明导电薄膜的工艺研究";李芝华 等;《材料科学与工艺》;20060430;第14卷(第2期);全文 *
"热处理时间对溶胶-凝胶法制备ITO薄膜结构、形貌和性质的影响";高美珍 等;《材料导报:研究篇》;20090131;第23卷(第1期);第87页右栏第1段至90页左栏第2段 *

Also Published As

Publication number Publication date
CN103325859A (en) 2013-09-25

Similar Documents

Publication Publication Date Title
CN103325859B (en) A kind of preparation method of ito thin film
CN102646759B (en) Preparing method for transparent conductive oxide film
CN104318983A (en) Preparation method of ITO thin film
CN110518125A (en) A kind of preparation method of cation doping perovskite solar battery
WO2018028244A1 (en) Transparent conductive film, preparation method therefor and application thereof
CN105118919A (en) Perovskite solar cell composed of orderly-arranged small titanium dioxide balls and preparation method thereof
JP2008078113A (en) Device for manufacturing transparent conductive substrate
CN106158997B (en) A kind of preparation method of doped tin oxide transparent conductive film
CN106590618B (en) A kind of NiO/rGO laminated film and preparation method thereof with clad structure
CN111540807B (en) All-inorganic perovskite solar cell with high open-circuit voltage and preparation method thereof
CN103938210A (en) Method for preparing AZO transparent conductive film
CN102222575A (en) Preparation method for photoanode of dye-sensitized solar cell
CN105420696B (en) A kind of preparation method of tin oxide base thin film material
CN104726851B (en) A kind of method that sol-gal process prepares p-type SnO 2 thin film material
CN103343335B (en) The preparation method of boron-doping zinc-oxide film
CN103345977B (en) A kind of preparation method of Ag doping ito thin film
CN108374162A (en) A kind of preparation method of aluminum-doped zinc oxide transparent conductive film
JPWO2008117605A1 (en) Large-area transparent conductive film and method for producing the same
CN106119971B (en) A kind of preparation and its application of organic and inorganic perovskite spike crystal
CN103803809A (en) Method for producing zinc oxide-based transparent conductive coating glass
CN113816615A (en) Ultrahigh-transparency conductive ITO film and preparation method thereof
CN105603400A (en) Preparation method of ZnO transparent conductive film
CN104593758A (en) Preparation method of ZnO/Ag/ZnO composite transparent conducting thin film
CN108218246A (en) A kind of preparation method of transparent conducting film glass
CN109896743B (en) Conductive glass

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
ASS Succession or assignment of patent right

Owner name: XU DONG

Free format text: FORMER OWNER: SHENZHEN YATAIXING INDUSTRY LTD.

Effective date: 20150323

C41 Transfer of patent application or patent right or utility model
COR Change of bibliographic data

Free format text: CORRECT: ADDRESS; FROM: 518103 SHENZHEN, GUANGDONG PROVINCE TO: 518000 SHENZHEN, GUANGDONG PROVINCE

TA01 Transfer of patent application right

Effective date of registration: 20150323

Address after: 518000 Baoan District, Shenzhen, Baoan District, the people of the first district of the square building, the first floor of the building on the ground floor, building 13,

Applicant after: Xu Dong

Address before: 518103, Guangdong Province, Shenzhen, Baoan District Baoan district nine District Road Plaza, building 13, building

Applicant before: Shenzhen Yataixing Industry Ltd.

C14 Grant of patent or utility model
GR01 Patent grant