CN108109722A - Ito thin film preparation method - Google Patents
Ito thin film preparation method Download PDFInfo
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- CN108109722A CN108109722A CN201711336814.2A CN201711336814A CN108109722A CN 108109722 A CN108109722 A CN 108109722A CN 201711336814 A CN201711336814 A CN 201711336814A CN 108109722 A CN108109722 A CN 108109722A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/02—Oxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
- H01B1/08—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances oxides
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Abstract
The invention discloses a kind of ito thin film preparation methods, comprise the following steps：Aqueous slkali is added in into the mixed aqueous solution containing indium salts, pink salt, the pH value of mixed aqueous solution is adjusted to 68, indium salts, pink salt is separately converted to the indium hydroxide to precipitate, tin hydroxide；Separation of solid and liquid is carried out to mixed aqueous solution, indium hydroxide and tin hydroxide are cleaned multiple times using deionized water, obtain the presoma of indium hydroxide and tin hydroxide；The presoma of indium hydroxide and tin hydroxide is placed in 50 70 DEG C and is dried, and is placed on 5 20min of microwave sintering in 650 750 DEG C, obtains ITO nano particles；ITO nano particles are dispersed in formation ITO nanoparticulate dispersions in ITO colloidal sols；By ITO nanoparticulate dispersion spin-coating films, and ito thin film is obtained after carrying out drying process and annealing；Ito thin film is prepared using the method that sol-gel precursor method and nanometer crystallization combine, annealing obtains ito thin film at low temperature；This method is simple and effective, and product has high conductivity.
Description
Technical field
The present invention relates to technical field of film preparation, and in particular to a kind of ito thin film preparation method.
Background technology
Tin-doped indium oxide（Abbreviation ITO）Because of it with conductivity is high, visible light transmittance is high, chemical stability is good and
With its matrix associativity it is good the advantages that and be mainly used in transparent conducting glass, film etc..
In the prior art, it is the new method that a kind of cost is relatively low, simple for process that solwution method, which prepares ito thin film,.It is usually molten
Liquid method is divided into two kinds：Sol-gel precursor method and nanometer crystallization.Sol-gel precursor method would generally with inorganic indium salts and
Pink salt mixes in water phase or organic phase, and by high-temperature heat treatment after film forming, oxide is formed by chemical change；It is but molten
Ito thin film prepared by glue gel precursor process largely needs to be made annealing treatment by being subsequently higher than 300 DEG C of high temperature.And it receives
Meter Jing Fa is then to be just using after opposite route, the crystallized complete ITO nanocrystal solutions of use, therefore film
ITO crystal films, it is only necessary to organic solvent be removed by subsequent heat treatment, promote electric conductivity；But prepared by nanocrystalline method
Film cause consistency not high due to the natural interstitia that spherical particles generate during solid matter, affect the conductive energy of film
Power.
Therefore, now need to provide a kind of simple and effective can be made the ITO with certain high conductivity ito thin film at low temperature
Method for manufacturing thin film.
The content of the invention
For this purpose, the present invention provides a kind of ito thin film preparation methods, comprise the following steps：
Step 1: adding in aqueous slkali into the mixed aqueous solution containing indium salts, pink salt, the pH value of mixed aqueous solution is adjusted to 6-8, it will
Indium salts, pink salt are separately converted to the indium hydroxide to precipitate, tin hydroxide；
Step 2: carrying out separation of solid and liquid to the mixed aqueous solution after step 1, indium hydroxide is cleaned multiple times using deionized water
With tin hydroxide, the presoma of acquisition indium hydroxide and tin hydroxide；
It is dried Step 3: indium hydroxide and the presoma of tin hydroxide that step 2 is obtained are placed in 50-70 DEG C, and
Microwave sintering 5-20min in 650-750 DEG C is placed on, obtains ITO nano particles；
Step 4: the ITO nano particles that step 3 is obtained are dispersed in formation ITO nanoparticulate dispersions in ITO colloidal sols；
Step 5: by the ITO nanoparticulate dispersion spin-coating films obtained by step 4, and after carrying out drying process and annealing
Obtain ito thin film.
In step 4, the molar concentration of ITO nano particles is 0.06-0.24mol/L in ITO nanoparticulate dispersions.
In step 1, containing indium salts, pink salt mixed aqueous solution in the amount of substance of tin element account for indium, tin element total material
The sum of amount 5-12%.
Indium salts in mixed aqueous solution include one kind in inidum chloride, inidum chloride hydrate, indium nitrate, indium nitrate hydrate
Or it is a variety of, the pink salt in mixed aqueous solution includes one or two kinds of in butter of tin, its hydrate.
Aqueous slkali in step 1 is set to the aqueous solution of sodium hydroxide, ammonia.
In step 2, separation of solid and liquid is carried out using centrifugation；During centrifugation, the rotating speed of centrifugal separator is 3000-
3500r/min, centrifugation time 5-10min.
In step 5, the temperature of drying process is 150-250 DEG C, and the time of drying process is 1-3h.
In step 5, the temperature of annealing is 250-300 DEG C, and the time of annealing is 5-10min；Wherein, move back
The mode of fire processing for microwave sintering, the protective gas in processing procedure be set to nitrogen, hydrogen, argon gas it is a kind of or more
Kind.
The preparation method of ITO colloidal sols in step 3 is：Indium salts will be contained, tin (II) salt is dissolved in organic solvent, in 60-80
DEG C reflux 3h, obtain the ITO colloidal sols.
The organic solvent includes any one in ethyl alcohol, ethylene glycol, dimethylbenzene, propyl alcohol, isopropanol or a variety of.
The present invention has the following advantages that part compared with the prior art：
In the present invention, ito thin film is prepared using the method that sol-gel precursor method and nanometer crystallization combine, obtained low
The lower annealing of temperature still has the ito thin film of certain high conductivity；The preparation method is simple and effective, and obtained after testing
Ito thin film meets high conductivity requirement.
Specific embodiment
Technical scheme is clearly and completely described below, it is clear that described embodiment is this hair
Bright part of the embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art exist
All other embodiments obtained under the premise of creative work are not made, belong to the scope of protection of the invention.
As long as in addition, technical characteristic involved in invention described below different embodiments non-structure each other
It can be combined with each other into conflict.
Embodiment 1
A kind of ito thin film preparation method is present embodiments provided, is comprised the following steps：
Step 1: adding in aqueous slkali into the mixed aqueous solution containing indium salts, pink salt, the pH value of mixed aqueous solution is adjusted to 6-8, it will
Indium salts, pink salt are separately converted to the indium hydroxide to precipitate, tin hydroxide；
Step 2: carrying out separation of solid and liquid to the mixed aqueous solution after step 1, indium hydroxide is cleaned multiple times using deionized water
With tin hydroxide, the presoma of acquisition indium hydroxide and tin hydroxide；
It is dried Step 3: indium hydroxide and the presoma of tin hydroxide that step 2 is obtained are placed in 50-70 DEG C, and
Microwave sintering 5-20min in 650-750 DEG C is placed on, obtains ITO nano particles；
Step 4: the ITO nano particles that step 3 is obtained are dispersed in formation ITO nanoparticulate dispersions in ITO colloidal sols；
Step 5: by the ITO nanoparticulate dispersion spin-coating films obtained by step 4, and after carrying out drying process and annealing
Obtain ito thin film.
During the present embodiment preferred steps four, the molar concentration of ITO nano particles is 0.06- in ITO nanoparticulate dispersions
0.24mol/L。
In the present embodiment, ito thin film is prepared using the method that sol-gel precursor method and nanometer crystallization combine, obtained
Making annealing treatment at low temperature still has the ito thin film of certain high conductivity；The preparation method is simple and effective, and made after testing
The ito thin film obtained meets high conductivity requirement.
Specifically, in step 1, containing indium salts, pink salt mixed aqueous solution in tin element substance amount account for indium, tin member
The 5-12% of the sum of the amount of plain total material；Wherein, the indium salts in mixed aqueous solution include inidum chloride, inidum chloride hydrate, nitric acid
One or more in indium, indium nitrate hydrate, the pink salt in mixed aqueous solution include one kind in butter of tin, its hydrate
Or two kinds；Meanwhile aqueous slkali is set to the aqueous solution of sodium hydroxide, ammonia.
As preferred embodiment, in step 2, separation of solid and liquid is carried out using centrifugation；During centrifugation, centrifugation point
The rotating speed disembarked is 3000-3500r/min, centrifugation time 5-10min.
Further, in step 5, the temperature of drying process is 150-250 DEG C, and the time of drying process is 1-3h；It moves back
The temperature of fire processing is 250-300 DEG C, and the time of annealing is 5-10min；Wherein, the mode of annealing is burnt for microwave
It ties, the protective gas in processing procedure is set to the one or more of nitrogen, hydrogen, argon gas.
On the basis of above-described embodiment, three the step of the present embodiment in the preparation methods of ITO colloidal sols be：Indium will be contained
Salt, tin (II) salt are dissolved in organic solvent, and flow back 3h at 60-80 DEG C, obtains the ITO colloidal sols；Wherein, the organic solvent bag
Include in ethyl alcohol, ethylene glycol, dimethylbenzene, propyl alcohol, isopropanol any one or it is a variety of.
Embodiment 2
On the basis of embodiment 1, the present embodiment further provides for a kind of specific embodiment：
Step 1: adding in aqueous slkali into the mixed aqueous solution containing indium salts, pink salt, the pH value for adjusting mixed aqueous solution is 6, by indium
Salt, pink salt are separately converted to the indium hydroxide to precipitate, tin hydroxide；In the present embodiment, containing indium salts, pink salt it is mixed
In Heshui solution the amount of the substance of tin element account for indium, tin element total material the sum of amount 5%；Indium salts bag in mixed aqueous solution
Include inidum chloride and its hydrate and/or indium nitrate and its hydrate, the pink salt in mixed aqueous solution includes butter of tin and/or four
Stannic chloride；Aqueous slkali is set to the aqueous solution of sodium hydroxide, ammonia.
Step 2: carrying out separation of solid and liquid to the mixed aqueous solution after step 1, indium hydrogen-oxygen is cleaned multiple times using deionized water
Compound and tin hydroxide obtain the presoma of indium hydroxide and tin hydroxide；In the present embodiment, as preferred reality
Mode is applied, separation of solid and liquid is carried out using centrifugation, during centrifugation, the rotating speed of centrifugal separator is 3000r/min, and centrifugation time is
5min；
It is dried Step 3: indium hydroxide and the presoma of tin hydroxide that step 2 is obtained are placed in 50 DEG C, then
Microwave sintering 5min in 650 DEG C is placed in, obtains ITO nano particles；
Step 4: the ITO nano particles that step 3 is obtained are dispersed in formation ITO nanoparticulate dispersions in ITO colloidal sols；
In the present embodiment, the preparation method of ITO colloidal sols is：Indium salts will be contained, tin (II) salt is dissolved in organic solvent, 60 DEG C flow back 3h,
Obtain the ITO colloidal sols；Wherein, the organic solvent includes ethyl alcohol；Meanwhile in the present embodiment, ITO nanoparticulate dispersions
The molar concentration of middle ITO nano particles is 0.06mol/L；
Step 5: by the ITO nanoparticulate dispersion spin-coating films obtained by step 4, and after carrying out drying process and annealing
Obtain ito thin film；In the present embodiment, the temperature of drying process is 150 DEG C, and the time of drying process is 1h；Annealing
Temperature is 250 DEG C, and the time of annealing is 5min；Wherein, the mode of annealing is microwave sintering, in processing procedure
Protective gas is set to nitrogen.
In the present embodiment, ito thin film is prepared using the method that sol-gel precursor method and nanometer crystallization combine, obtained
Making annealing treatment at low temperature still has the ito thin film of certain high conductivity；The preparation method is simple and effective, and this reality after testing
The sheet resistance of ito thin film made from example is applied as 243 Ω/sq, meets high conductivity requirement.
Embodiment 3
On the basis of embodiment 1, the present embodiment further provides for a kind of specific embodiment：
Step 1: adding in aqueous slkali into the mixed aqueous solution containing indium salts, pink salt, the pH value for adjusting mixed aqueous solution is 8, by indium
Salt, pink salt are separately converted to the indium hydroxide to precipitate, tin hydroxide；In the present embodiment, containing indium salts, pink salt it is mixed
In Heshui solution the amount of the substance of tin element account for indium, tin element total material the sum of amount 12%；Indium salts bag in mixed aqueous solution
Include inidum chloride and its hydrate and/or indium nitrate and its hydrate, the pink salt in mixed aqueous solution includes butter of tin and/or four
Stannic chloride；Aqueous slkali is set to the aqueous solution of sodium hydroxide, ammonia.
Step 2: carrying out separation of solid and liquid to the mixed aqueous solution after step 1, indium hydrogen-oxygen is cleaned multiple times using deionized water
Compound and tin hydroxide obtain the presoma of indium hydroxide and tin hydroxide；In the present embodiment, as preferred reality
Mode is applied, separation of solid and liquid is carried out using centrifugation, during centrifugation, the rotating speed of centrifugal separator is 3500r/min, and centrifugation time is
10min；
It is dried Step 3: indium hydroxide and the presoma of tin hydroxide that step 2 is obtained are placed in 70 DEG C, then
Microwave sintering 20min in 750 DEG C is placed in, obtains ITO nano particles；
Step 4: the ITO nano particles that step 3 is obtained are dispersed in formation ITO nanoparticulate dispersions in ITO colloidal sols；
In the present embodiment, the preparation method of ITO colloidal sols is：Indium salts will be contained, tin (II) salt is dissolved in organic solvent, 80 DEG C flow back 3h,
Obtain the ITO colloidal sols；Wherein, the organic solvent includes isopropanol；Meanwhile in the present embodiment, ITO nano particles disperse
The molar concentration of ITO nano particles is 0.24mol/L in liquid；
Step 5: by the ITO nanoparticulate dispersion spin-coating films obtained by step 4, and after carrying out drying process and annealing
Obtain ito thin film；In the present embodiment, the temperature of drying process is 250 DEG C, and the time of drying process is 3h；Annealing
Temperature is 350 DEG C, and the time of annealing is 10min；Wherein, the mode of annealing is microwave sintering, in processing procedure
Protective gas be set to hydrogen.
In the present embodiment, ito thin film is prepared using the method that sol-gel precursor method and nanometer crystallization combine, obtained
Making annealing treatment at low temperature still has the ito thin film of certain high conductivity；The preparation method is simple and effective, and this reality after testing
The sheet resistance of ito thin film made from example is applied as 184 Ω/sq, meets high conductivity requirement.
Embodiment 4
On the basis of embodiment 1, the present embodiment further provides for a kind of specific embodiment：
Step 1: adding in aqueous slkali into the mixed aqueous solution containing indium salts, pink salt, the pH value for adjusting mixed aqueous solution is 7, by indium
Salt, pink salt are separately converted to the indium hydroxide to precipitate, tin hydroxide；In the present embodiment, containing indium salts, pink salt it is mixed
In Heshui solution the amount of the substance of tin element account for indium, tin element total material the sum of amount 8%；Indium salts bag in mixed aqueous solution
Include inidum chloride and its hydrate and/or indium nitrate and its hydrate, the pink salt in mixed aqueous solution includes butter of tin and/or four
Stannic chloride；Aqueous slkali is set to the aqueous solution of sodium hydroxide, ammonia.
Step 2: carrying out separation of solid and liquid to the mixed aqueous solution after step 1, indium hydrogen-oxygen is cleaned multiple times using deionized water
Compound and tin hydroxide obtain the presoma of indium hydroxide and tin hydroxide；In the present embodiment, as preferred reality
Mode is applied, separation of solid and liquid is carried out using centrifugation, during centrifugation, the rotating speed of centrifugal separator is 3200r/min, and centrifugation time is
8min；
It is dried Step 3: indium hydroxide and the presoma of tin hydroxide that step 2 is obtained are placed in 60 DEG C, then
Microwave sintering 15min in 700 DEG C is placed in, obtains ITO nano particles；
Step 4: the ITO nano particles that step 3 is obtained are dispersed in formation ITO nanoparticulate dispersions in ITO colloidal sols；
In the present embodiment, the preparation method of ITO colloidal sols is：Indium salts will be contained, tin (II) salt is dissolved in organic solvent, 70 DEG C flow back 3h,
Obtain the ITO colloidal sols；Wherein, the organic solvent includes dimethylbenzene；Meanwhile in the present embodiment, ITO nano particles disperse
The molar concentration of ITO nano particles is 0.15mol/L in liquid；
Step 5: by the ITO nanoparticulate dispersion spin-coating films obtained by step 4, and after carrying out drying process and annealing
Obtain ito thin film；In the present embodiment, the temperature of drying process is 200 DEG C, and the time of drying process is 2h；Annealing
Temperature is 280 DEG C, and the time of annealing is 8min；Wherein, the mode of annealing is microwave sintering, in processing procedure
Protective gas is set to argon gas.
In the present embodiment, ito thin film is prepared using the method that sol-gel precursor method and nanometer crystallization combine, obtained
Making annealing treatment at low temperature still has the ito thin film of certain high conductivity；The preparation method is simple and effective, and this reality after testing
The sheet resistance of ito thin film made from example is applied as 262 Ω/sq, meets high conductivity requirement.
Obviously, the above embodiments are merely examples for clarifying the description, and is not intended to limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And the obvious variation thus extended out or
Among changing still in the protection domain of the invention.
Claims (10)
1.ITO method for manufacturing thin film, it is characterised in that：It comprises the following steps：
Step 1: adding in aqueous slkali into the mixed aqueous solution containing indium salts, pink salt, the pH value of mixed aqueous solution is adjusted to 6-8, it will
Indium salts, pink salt are separately converted to the indium hydroxide to precipitate, tin hydroxide；
Step 2: carrying out separation of solid and liquid to the mixed aqueous solution after step 1, indium hydroxide is cleaned multiple times using deionized water
With tin hydroxide, the presoma of acquisition indium hydroxide and tin hydroxide；
It is dried Step 3: indium hydroxide and the presoma of tin hydroxide that step 2 is obtained are placed in 50-70 DEG C, and
Microwave sintering 5-20min in 650-750 DEG C is placed on, obtains ITO nano particles；
Step 4: the ITO nano particles that step 3 is obtained are dispersed in formation ITO nanoparticulate dispersions in ITO colloidal sols；
Step 5: by the ITO nanoparticulate dispersion spin-coating films obtained by step 4, and after carrying out drying process and annealing
Obtain ito thin film.
2. ito thin film preparation method according to claim 1, it is characterised in that：In step 4, ITO nano particles point
The molar concentration of ITO nano particles is 0.06-0.24mol/L in dispersion liquid.
3. ito thin film preparation method according to claim 1 or 2, it is characterised in that：In step 1, containing indium salts, pink salt
Mixed aqueous solution in tin element substance amount account for indium, tin element total material the sum of amount 5-12%.
4. ito thin film preparation method according to claim 3, it is characterised in that：Indium salts in mixed aqueous solution include chlorine
Change indium, inidum chloride hydrate, indium nitrate, the one or more in indium nitrate hydrate, the pink salt in mixed aqueous solution includes four
It is one or two kinds of in stannic chloride, its hydrate.
5. the ito thin film preparation method according to any one of claim 1-4, it is characterised in that：Alkali soluble in step 1
Liquid is set to the aqueous solution of sodium hydroxide, ammonia.
6. the ito thin film preparation method according to any one of claim 1-5, it is characterised in that：In step 2, use
Centrifugation carries out separation of solid and liquid；During centrifugation, the rotating speed of centrifugal separator is 3000-3500r/min, centrifugation time 5-
10min。
7. the ito thin film preparation method according to any one of claim 1-6, it is characterised in that：It is dry in step 5
The temperature of processing is 150-250 DEG C, and the time of drying process is 1-3h.
8. the ito thin film preparation method according to any one of claim 1-7, it is characterised in that：In step 5, annealing
The temperature of processing is 250-300 DEG C, and the time of annealing is 5-10min；Wherein, the mode of annealing is microwave sintering,
Protective gas in its processing procedure is set to the one or more of nitrogen, hydrogen, argon gas.
9. the ito thin film preparation method according to any one of claim 1-8, it is characterised in that：ITO in step 3 is molten
The preparation method of glue is：Indium salts will be contained, tin (II) salt is dissolved in organic solvent, 60-80 DEG C flow back 3h, it is molten to obtain the ITO
Glue.
10. ito thin film preparation method according to claim 9, it is characterised in that：The organic solvent includes ethyl alcohol, second
In glycol, dimethylbenzene, propyl alcohol, isopropanol any one or it is a variety of.
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| CN201711336814.2A CN108109722A (en) | 2017-12-14 | 2017-12-14 | Ito thin film preparation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108083322A (en) * | 2018-01-29 | 2018-05-29 | 首凯汽车零部件（江苏）有限公司 | The preparation method of ZnO nano crystalline substance solution and its film forming coherent condition regulation and control method |
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| CN103693678A (en) * | 2012-09-27 | 2014-04-02 | 三菱综合材料株式会社 | Ito powder and method of producing same, dispersion liquid and method of ito film |
| CN104692452B (en) * | 2013-12-10 | 2016-04-27 | 中国科学院苏州纳米技术与纳米仿生研究所 | The preparation method that a kind of tin indium oxide is nanocrystalline |
| CN105776321A (en) * | 2014-12-23 | 2016-07-20 | 中国科学院苏州纳米技术与纳米仿生研究所 | An indium tin oxide nanometer crystal composite solution, and a preparing method and applications thereof |
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| CN103693678A (en) * | 2012-09-27 | 2014-04-02 | 三菱综合材料株式会社 | Ito powder and method of producing same, dispersion liquid and method of ito film |
| CN103325859A (en) * | 2013-06-26 | 2013-09-25 | 深圳市亚太兴实业有限公司 | Preparation method of ITO thin film |
| CN104692452B (en) * | 2013-12-10 | 2016-04-27 | 中国科学院苏州纳米技术与纳米仿生研究所 | The preparation method that a kind of tin indium oxide is nanocrystalline |
| CN105776321A (en) * | 2014-12-23 | 2016-07-20 | 中国科学院苏州纳米技术与纳米仿生研究所 | An indium tin oxide nanometer crystal composite solution, and a preparing method and applications thereof |
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| CN108083322A (en) * | 2018-01-29 | 2018-05-29 | 首凯汽车零部件（江苏）有限公司 | The preparation method of ZnO nano crystalline substance solution and its film forming coherent condition regulation and control method |
| CN108083322B (en) * | 2018-01-29 | 2020-03-27 | 首凯汽车零部件（江苏）有限公司 | Preparation method of ZnO nanocrystalline solution and film-forming aggregation state regulation method thereof |
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Application publication date: 20180601 |