CN106847365A - A kind of preparation method of the modified zinc sulphide conductive material of tin indium oxide - Google Patents
A kind of preparation method of the modified zinc sulphide conductive material of tin indium oxide Download PDFInfo
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- CN106847365A CN106847365A CN201611211736.9A CN201611211736A CN106847365A CN 106847365 A CN106847365 A CN 106847365A CN 201611211736 A CN201611211736 A CN 201611211736A CN 106847365 A CN106847365 A CN 106847365A
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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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- 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
- H01B1/10—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances sulfides
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- H—ELECTRICITY
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- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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Abstract
The invention discloses a kind of modified zinc sulphide conductive material preparation method of tin indium oxide, belong to electronic material preparing technical field.The present invention is first by indium stannum alloy drying and grinding into powder, the sodium hydroxide solution and peroxide SiClx solution hybrid reaction obtained with mixed in hydrochloric acid reaction obtain sodium silicate solution, add acetic acid zinc powder hybrid reaction, it is then placed in inidum chloride solution of tin, generation colloid, sodium hydroxide solution is added dropwise in inidum chloride solution of tin, colloidal solution is centrifuged again, drying and calcining, collect the powder after calcining, in addition acetic acid, stirring and dissolving, add sodium sulfide solution stirring reaction, staticly settle, it is separated by filtration, then washed respectively with deionized water and absolute ethyl alcohol, vacuum drying, can be prepared by a kind of modified zinc sulphide conductive material of tin indium oxide, the method of the present invention prepares simple, conductive layer is strong with the basic binding strength of glass, surface is not easily susceptible to cracking, and have good translucency and electric conductivity concurrently.
Description
Technical field
The invention discloses a kind of preparation method of the modified zinc sulphide conductive material of tin indium oxide, it is related to photoelectric material technology
Field.
Background technology
In recent years, with the high speed development of information technology, transparent conducting glass is used as flat-panel display device, solar-electricity
The basic material of pond, electroluminescent, liquid crystal display, sensor etc. is extremely paid attention to.Wherein, most representative transparent conducting glass
It is tin-doped indium oxide（ITO）Conductive glass.It not only has the characteristic of mechanically and chemically stable performance, and with excellent
Electric conductivity, transparent performance and electrode pattern etc. is readily formed with wet etching, is applied by many industrial circles.At present,
The method for preparing the transparent conducting glass of ito film mainly has physical vaporous deposition, chemical vapour deposition technique and sol-gal process.
No matter which kind of method, being intended to finished product ito film glass has less sheet resistance and the transparency higher.
Zinc sulfide nano-material has special photoelectric property, in the fields such as luminescent material, electrooptical device and LED materials
It is with a wide range of applications.Zinc sulphide is two or six compound semiconductors, is current topmost multispectral infrared optical material.
Zinc sulphide has an excellent fluorescent effect and electroluminescent function, nano-zinc sulfide with more unique photoelectric effect, electricity,
The fields such as magnetics, optics, mechanics and catalysis show many excellent performances, thus nano-zinc sulfide research cause it is more
The attention of people.Can be used to make pigment and glass, luminescent powder, rubber, plastics, luminous paint of white etc..Prepare zinc sulphide at present
Method have wet method, gas phase synthesis method, the single-step solid phase reaction method of room temperature one and elemental direct reaction method etc..At present, vapour deposition is used
Electro-conductive glass prepared by method has that process conditions are harsh, prepare material it is size-constrained processed the problems such as；And use collosol and gel legal system
Standby electro-conductive glass, although technics comparing is simple, can prepare transparent conducting glass of large-size etc., but there is sheet resistance greatly, table
Surface roughness is high, easy problems of crack.Therefore the conduction that a kind of process is simple is provided simultaneously with translucency and electric conductivity is developed
Material, has great importance.
The content of the invention
Present invention mainly solves technical problem：Harsh for the existing process conditions that there is electro-conductive glass, sheet resistance is big, table
Surface roughness is high, easy problems of crack, there is provided a kind of preparation method of the modified zinc sulphide conductive material of tin indium oxide, this hair
The bright sodium hydroxide solution and peroxide SiClx solution for first by indium stannum alloy drying and grinding into powder, being obtained with mixed in hydrochloric acid reaction is mixed
Sodium silicate solution is reacted to obtain in conjunction, adds acetic acid zinc powder hybrid reaction, is then placed in inidum chloride solution of tin, generates colloid,
Sodium hydroxide solution is added dropwise in inidum chloride solution of tin, then colloidal solution is centrifuged, drying and calcining, after collecting calcining
Powder, add acetic acid in, stirring and dissolving, add sodium sulfide solution stirring reaction, staticly settle, be separated by filtration, then use
Deionized water and absolute ethyl alcohol are washed respectively, vacuum drying, you can a kind of modified zinc sulphide conductive material of tin indium oxide is obtained, this
Invention the method is prepared simply, and conductive layer is strong with the basic binding strength of glass, and surface is not easily susceptible to cracking, and has good printing opacity concurrently
Property and electric conductivity.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
（1）Weigh 500~800g indium stannum alloys to clean, spontaneously dry, 25~30min of mechanical lapping, collect indium tin powder, then
By solid-liquid mass ratio 1:10, the mixed in hydrochloric acid reaction that indium tin powder and mass concentration are 20~30% surpasses under 200~300W
Sound 20~30min of decentralized processing, is prepared into inidum chloride solution of tin, standby；
（2）Count by weight, 20~24 parts of sodium hydroxide solutions and 10~12 parts of peroxide SiClx hybrid reactions are weighed respectively, obtain
Sodium silicate solution, adds 25~35 parts of acetic acid zinc powders and mixes, and obtains mixed solution；
（3）The mixed solution of above-mentioned preparation is put into 35~65 parts of steps（1）In the inidum chloride solution of tin of preparation, with 200~
The rotating speed stirring reaction of 300r/min, until generation colloidal precipitation；
（4）In the solution of above-mentioned generation colloidal precipitation, the sodium hydroxide solution that mass fraction is 20~25% is added dropwise, is reached to pH
To 8~9, then opposite carries out the centrifugation that speed is 4000~6000rmp into the solution of colloidal precipitation, takes filter cake, is put into 50
Dried at~60 DEG C, placed into the calcining furnace at 600~700 DEG C, collect the powder after calcining；
（5）By the powder after the calcining of above-mentioned preparation in mass ratio 1：During 5~10 addition mass fractions are 17~25% acetic acid,
Stirring adds the sodium sulfide solution stirring reaction of 0.1~0.5mol/L to being completely dissolved, and staticly settles 2~3min, filtering point
From, filter cake is taken, then washed respectively 3~5 times with deionized water and absolute ethyl alcohol, 2~5h is vacuum dried at 80~100 DEG C,
Can be prepared by a kind of modified zinc sulphide conductive material of tin indium oxide.
Application process of the invention：The resistance of the conductive material of the modified zinc sulphide of tin indium oxide of the invention obtained for 60~
80 Ω, pyroconductivity be 0.272~0.294W/cmK, light transmittance be 71.8~72.6%, elastic modelling quantity be 74.8~
76.2GPa, light transmittance improves 10~12%, and resistance value excellent in stability.
Compared with other method, Advantageous Effects are the present invention：
（1）The present invention is prepared simply, and conductive layer is strong with the basic binding strength of glass, and surface is not easily susceptible to cracking；
（2）The present invention has good translucency and electric conductivity.
Specific embodiment
Weigh 500~800g indium stannum alloys to clean, spontaneously dry, 25~30min of mechanical lapping, collect indium tin powder, with
Solid-liquid mass ratio 1 is pressed afterwards:10, by the mixed in hydrochloric acid reaction that indium tin powder and mass concentration are 20~30%, under 200~300W
Ultrasonic disperse processes 20~30min, is prepared into inidum chloride solution of tin, standby, counts by weight, and 20~24 parts of hydrogen are weighed respectively
Sodium hydroxide solution and 10~12 parts of peroxide SiClx hybrid reactions, obtain sodium silicate solution, add 25~35 parts of acetic acid zinc powders and mix
Stirring is closed, mixed solution is obtained, the mixed solution of above-mentioned preparation is put into 35~65 parts of inidum chloride solution of tin of preparation, with 200
The rotating speed stirring reaction of~300r/min, until generation colloidal precipitation, in the solution of above-mentioned generation colloidal precipitation, is added dropwise quality
Fraction is 20~25% sodium hydroxide solution, and 8~9 are reached to pH, then it is 4000 that opposite carries out speed into the solution of colloidal precipitation
The centrifugation of~6000rmp, takes filter cake, is dried at being put into 50~60 DEG C, places into the calcining furnace at 600~700 DEG C, receives
Powder after collection calcining, by the powder after the calcining of above-mentioned preparation in mass ratio 1：5~10 addition mass fractions are 17~25%
In acetic acid, stirring adds the sodium sulfide solution stirring reaction of 0.1~0.5mol/L to being completely dissolved, staticly settle 2~
3min, is separated by filtration, and takes filter cake, is then washed respectively 3~5 times with deionized water and absolute ethyl alcohol, the vacuum at 80~100 DEG C
Dry 2~5h, you can a kind of modified zinc sulphide conductive material of tin indium oxide is obtained.
Example 1
Weigh 500g indium stannum alloys to clean, spontaneously dry, mechanical lapping 25min, collect indium tin powder, then press solid-liquid quality
Than 1:10, by the mixed in hydrochloric acid reaction that indium tin powder and mass concentration are 20%, ultrasonic disperse treatment 20min, prepares under 200W
Inidum chloride solution of tin is obtained, it is standby, count by weight, 20 parts of sodium hydroxide solutions are weighed respectively and 10 parts of peroxide SiClxs mixing are anti-
Should, sodium silicate solution is obtained, add 25 parts of acetic acid zinc powders and mix, mixed solution is obtained, by the mixed solution of above-mentioned preparation
It is put into 35 parts of inidum chloride solution of tin of preparation, with the rotating speed stirring reaction of 200r/min, until colloidal precipitation is generated, above-mentioned
Generate in the solution of colloidal precipitation, the sodium hydroxide solution that mass fraction is 20% is added dropwise, 8 are reached to pH, then opposite is sunk into colloid
The solution in shallow lake carries out the centrifugation that speed is 4000rmp, takes filter cake, is dried at being put into 50 DEG C, places into the calcining at 600 DEG C
In stove, the powder after calcining is collected, by the powder after the calcining of above-mentioned preparation in mass ratio 1：5 addition mass fractions are 17%
In acetic acid, stirring adds the sodium sulfide solution stirring reaction of 0.1mol/L to being completely dissolved, and staticly settles 2min, filtering point
From, filter cake is taken, then washed respectively 3 times with deionized water and absolute ethyl alcohol, it is vacuum dried 2h at 80 DEG C, you can one kind is obtained
The modified zinc sulphide conductive material of tin indium oxide.
The resistance of the conductive material of the modified zinc sulphide of obtained tin indium oxide of the invention is 60 Ω, and pyroconductivity is
0.272W/cmK, light transmittance is 71.8%, and elastic modelling quantity is 74.8GPa, and light transmittance improves 10%, and resistance value stability is excellent
It is different.
Example 2
Weigh 650g indium stannum alloys to clean, spontaneously dry, mechanical lapping 27min, indium tin powder is collected, then by solid-liquid mass ratio
1:10, by the mixed in hydrochloric acid reaction that indium tin powder and mass concentration are 25%, ultrasonic disperse treatment 25min, is prepared under 250W
Inidum chloride solution of tin, it is standby, count by weight, 22 parts of sodium hydroxide solutions are weighed respectively and 11 parts of peroxide SiClx mixing are anti-
Should, sodium silicate solution is obtained, add 30 parts of acetic acid zinc powders and mix, mixed solution is obtained, by the mixed solution of above-mentioned preparation
It is put into 40 parts of inidum chloride solution of tin of preparation, with the rotating speed stirring reaction of 250r/min, until colloidal precipitation is generated, above-mentioned
Generate in the solution of colloidal precipitation, the sodium hydroxide solution that mass fraction is 22% is added dropwise, 8.5 are reached to pH, then opposite is into colloid
The solution of precipitation carries out the centrifugation that speed is 5000rmp, takes filter cake, is dried at being put into 55 DEG C, places into forging at 650 DEG C
Burn in stove, the powder after calcining is collected, by the powder after the calcining of above-mentioned preparation in mass ratio 1：7 addition mass fractions are 21%
Acetic acid in, stirring adds the sodium sulfide solution stirring reaction of 0.3mol/L to being completely dissolved, and staticly settles 2.5min, mistake
Filter is separated, and takes filter cake, is then washed respectively 4 times with deionized water and absolute ethyl alcohol, and 3.5h is vacuum dried at 90 DEG C, you can system
Obtain a kind of modified zinc sulphide conductive material of tin indium oxide.
The resistance of the conductive material of the modified zinc sulphide of obtained tin indium oxide of the invention is 70 Ω, and pyroconductivity is
0.283W/cmK, light transmittance is 72.2%, and elastic modelling quantity is 75.5GPa, and light transmittance improves 11%, and resistance value stability is excellent
It is different.
Example 3
Weigh 800g indium stannum alloys to clean, spontaneously dry, mechanical lapping 30min, indium tin powder is collected, then by solid-liquid mass ratio
1:10, by the mixed in hydrochloric acid reaction that indium tin powder and mass concentration are 30%, ultrasonic disperse treatment 30min, is prepared under 300W
Inidum chloride solution of tin, it is standby, count by weight, 24 parts of sodium hydroxide solutions are weighed respectively and 12 parts of peroxide SiClx mixing are anti-
Should, sodium silicate solution is obtained, add 35 parts of acetic acid zinc powders and mix, mixed solution is obtained, by the mixed solution of above-mentioned preparation
It is put into 65 parts of inidum chloride solution of tin of preparation, with the rotating speed stirring reaction of 300r/min, until colloidal precipitation is generated, above-mentioned
Generate in the solution of colloidal precipitation, the sodium hydroxide solution that mass fraction is 25% is added dropwise, 9 are reached to pH, then opposite is sunk into colloid
The solution in shallow lake carries out the centrifugation that speed is 6000rmp, takes filter cake, is dried at being put into 60 DEG C, places into the calcining at 700 DEG C
In stove, the powder after calcining is collected, by the powder after the calcining of above-mentioned preparation in mass ratio 1：10 addition mass fractions are 25%
In acetic acid, stirring adds the sodium sulfide solution stirring reaction of 0.5mol/L to being completely dissolved, and staticly settles 3min, filtering point
From, filter cake is taken, then washed respectively 5 times with deionized water and absolute ethyl alcohol, it is vacuum dried 5h at 100 DEG C, you can be obtained one
Plant the modified zinc sulphide conductive material of tin indium oxide.
The resistance of the conductive material of the modified zinc sulphide of obtained tin indium oxide of the invention is 80 Ω, and pyroconductivity is
0.294W/cmK, light transmittance is 72.6%, and elastic modelling quantity is 76.2GPa, and light transmittance improves 12%, and resistance value stability is excellent
It is different.
Claims (1)
1. the preparation method of the modified zinc sulphide conductive material of a kind of tin indium oxide, it is characterised in that specific preparation process is：
（1）Weigh 500~800g indium stannum alloys to clean, spontaneously dry, 25~30min of mechanical lapping, collect indium tin powder, then
By solid-liquid mass ratio 1:10, the mixed in hydrochloric acid reaction that indium tin powder and mass concentration are 20~30% surpasses under 200~300W
Sound 20~30min of decentralized processing, is prepared into inidum chloride solution of tin, standby；
（2）Count by weight, 20~24 parts of sodium hydroxide solutions and 10~12 parts of peroxide SiClx hybrid reactions are weighed respectively, obtain
Sodium silicate solution, adds 25~35 parts of acetic acid zinc powders and mixes, and obtains mixed solution；
（3）The mixed solution of above-mentioned preparation is put into 35~65 parts of steps（1）In the inidum chloride solution of tin of preparation, with 200~
The rotating speed stirring reaction of 300r/min, until generation colloidal precipitation；
（4）In the solution of above-mentioned generation colloidal precipitation, the sodium hydroxide solution that mass fraction is 20~25% is added dropwise, is reached to pH
To 8~9, then opposite carries out the centrifugation that speed is 4000~6000rmp into the solution of colloidal precipitation, takes filter cake, is put into 50
Dried at~60 DEG C, placed into the calcining furnace at 600~700 DEG C, collect the powder after calcining；
（5）By the powder after the calcining of above-mentioned preparation in mass ratio 1：During 5~10 addition mass fractions are 17~25% acetic acid,
Stirring adds the sodium sulfide solution stirring reaction of 0.1~0.5mol/L to being completely dissolved, and staticly settles 2~3min, filtering point
From, filter cake is taken, then washed respectively 3~5 times with deionized water and absolute ethyl alcohol, 2~5h is vacuum dried at 80~100 DEG C,
Can be prepared by a kind of modified zinc sulphide conductive material of tin indium oxide.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112592607A (en) * | 2020-12-29 | 2021-04-02 | 成都芙涵麟涂料科技有限公司 | Preparation method of filler for conductive coating |
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| CN103346269A (en) * | 2013-07-15 | 2013-10-09 | 广州新视界光电科技有限公司 | Semi-transparent electrode and organic light-emitting device comprising same |
| US20140252316A1 (en) * | 2011-10-04 | 2014-09-11 | Hao Yan | Quantum dots, rods, wires, sheets, and ribbons, and uses thereof |
| CN105731521A (en) * | 2016-02-04 | 2016-07-06 | 常州可赛成功塑胶材料有限公司 | Preparation method of indium tin oxide-modified highly-dispersive light-transmitting infrared zinc sulfide |
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2016
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Patent Citations (4)
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| CN102194904A (en) * | 2010-03-17 | 2011-09-21 | 绿阳光电股份有限公司 | Thin film solar structure and manufacturing method thereof |
| US20140252316A1 (en) * | 2011-10-04 | 2014-09-11 | Hao Yan | Quantum dots, rods, wires, sheets, and ribbons, and uses thereof |
| CN103346269A (en) * | 2013-07-15 | 2013-10-09 | 广州新视界光电科技有限公司 | Semi-transparent electrode and organic light-emitting device comprising same |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112592607A (en) * | 2020-12-29 | 2021-04-02 | 成都芙涵麟涂料科技有限公司 | Preparation method of filler for conductive coating |
| CN112592607B (en) * | 2020-12-29 | 2022-01-11 | 惠州市七点光电科技有限公司 | Preparation method of filler for conductive coating |
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Application publication date: 20170613 |