CN105523579B - A kind of preparation method of indium-tin oxide powder - Google Patents
A kind of preparation method of indium-tin oxide powder Download PDFInfo
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- CN105523579B CN105523579B CN201510876519.0A CN201510876519A CN105523579B CN 105523579 B CN105523579 B CN 105523579B CN 201510876519 A CN201510876519 A CN 201510876519A CN 105523579 B CN105523579 B CN 105523579B
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- C01G19/00—Compounds of tin
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- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The present invention relates to a kind of preparation method of indium-tin oxide powder, comprises the following steps：A microporous membrane is provided, the microporous membrane has a upper surface and a lower surface relative with the upper surface, and the microporous membrane includes multiple micropores, up and down two surface of multiple micropores through the microporous membrane；It is passed through an indium stannum aqueous solution so that micropore described in upper surface Jing of the indium stannum aqueous solution from the microporous membrane flows into the lower surface of microporous membrane；It is passed through an ammonia spirit so that the ammonia spirit flows along the lower surface direction of the microporous membrane, and the ammonia spirit is with the indium stannum aqueous solution for flowing to the microporous membrane lower surface and reacts, forms a mixture；Mixture is passed through it is aging in a water bath containers, it is aging after filter mixture and obtain solid precipitation, then solid precipitation is carried out washing, is dried；And dried solid is carried out into roasting, obtain indium-tin oxide powder.
Description
Technical field
The present invention relates to a kind of method for preparing indium-tin oxide powder, more particularly to a kind of to prepare oxidation based on microreactor
The method of indium tin powder.
Background technology
Tin indium oxide（ITO）It is a kind of n-type semiconductor, possesses excellent photoelectric properties.Obtained with ITO sputtering of materials
Thin film possess very low resistivity（About 10-4Ω‧cm）, possess good through performance simultaneously for visible ray.Therefore, ITO
Thin film is widely used in the fields such as LCDs, Organic Light Emitting Diode, touch screen, solaode.At present, the whole world
In the consumption of indium resource, ITO industries occupy 85%.As current flat panel shows the development of industry, for the requirement of ito thin film
Also towards maximization, high-compactness, high-purity development.The property of ito thin film is fundamentally decided by the property of ito powder, because
, in order to meet industry development requirement, ito powder preparation process needs further optimization for this.
Common tin indium oxide preparation method includes chemical coprecipitation, sol-gel process, hydro-thermal method, spray pyrolysis
Deng.Wherein, chemical coprecipitation is considered as most simple, economic method, is had extensively in experimentation and commercial production
Application.But the method for traditional chemical coprecipitation has microcosmic, and mixing is poor, reacts uneven, easily occur miscellaneous in system
Phase, local degree of supersaturation are low, the problems such as preparation process is wayward.
The content of the invention
In view of this, it is necessory to provide, a kind of reaction is uniform, prepare the preparation side of the indium-tin oxide powder of size tunable
Method.
A kind of preparation method of indium-tin oxide powder, which comprises the following steps：A microporous membrane is provided, the microporous membrane has
One upper surface and a lower surface relative with the upper surface, the microporous membrane include multiple micropores, and multiple micropores run through
In two surface up and down of the microporous membrane；It is passed through an indium stannum aqueous solution so that upper table of the indium stannum aqueous solution from the microporous membrane
Micropore described in the Jing of face flows into the lower surface of microporous membrane；It is passed through an ammonia spirit so that the ammonia spirit is along the microporous membrane
Lower surface direction flowing, the ammonia spirit is with the indium stannum aqueous solution for flowing to the microporous membrane lower surface and reacts, shape
Into a mixture；Mixture is passed through it is aging in a water bath containers, it is aging after filter mixture and obtain solid precipitation, then by solid
Precipitation is carried out washing, is dried；And dried solid is carried out into roasting, obtain indium-tin oxide powder.
The preparation method of the tin indium oxide provided relative to prior art, the present invention, by adopting microporous membrane, and combines stream
The micropore dispersion of body cross-flow shearing so that indium stannum aqueous solution is dispersed by microporous membrane, within the Millisecond time and ammonia spirit
Realize fully, uniformly mixing, so as to form homogeneous precipitation, the indium tin oxide particles for preparing are also more uniform.
Description of the drawings
The preparation flow figure of the indium-tin oxide powder that Fig. 1 is provided for the present invention.
Indium stannum aqueous solution and the course of reaction schematic diagram of ammonia spirit that Fig. 2 is provided for the present invention.
The transmission electron microscope picture of the indium-tin oxide powder that Fig. 3 is prepared for the embodiment 1 that the present invention is provided.
The transmission electron microscope picture of indium-tin oxide powder prepared by the embodiment 3 that Fig. 4 present invention is provided.
Main element symbol description
| 100 | Microporous membrane |
| 200 | Indium stannum aqueous solution |
| 300 | Ammonia spirit |
| 400 | Coil pipe |
Specific examples below will further illustrate the present invention with reference to above-mentioned accompanying drawing.
Specific embodiment
Below in conjunction with specific embodiment, the preparation method of the indium-tin oxide powder provided to the present invention is made further in detail
Explanation.
Fig. 1 is referred to, the present invention provides a kind of preparation method of indium-tin oxide powder, and the preparation method specifically includes following
Step：
S1 a, there is provided microporous membrane 100, the microporous membrane 100 have a upper surface and one it is relative with the upper surface under
Surface, the microporous membrane 100 include multiple micropores, up and down two surface of the plurality of micropore through the microporous membrane 100；
S2, is passed through an indium stannum aqueous solution 200 so that upper surface Jing of the indium stannum aqueous solution 200 from the microporous membrane 100
The micropore flows into the lower surface of microporous membrane 100；
S3, is passed through an ammonia spirit 300 so that the ammonia spirit 300 is flowed along the lower surface direction of the microporous membrane 100
Dynamic, the ammonia spirit 300 mixes and reacts with the indium stannum aqueous solution 200 for flowing to 100 lower surface of the microporous membrane, forms one and mixes
Compound；
S4, mixture is passed through it is aging in a water bath containers, it is aging after filter mixture and obtain solid precipitation, then by solid
Precipitation is carried out washing, is dried；And
Dried solid is carried out roasting, obtains indium-tin oxide powder by S5.
In step sl, the material of the microporous membrane 100 for not with 300 generationization of indium stannum aqueous solution 200 and ammonia spirit
The material of reaction is learned, can be macromolecular material, be applied the metal material or other composites of matcoveredn.Fig. 2 is referred to, it is described
A diameter of 1 micron -5 microns of micropore in microporous membrane 100.It is appreciated that when the diameter of micropore is less than 1 micron, producing in reaction
Raw solid sediment is easily blocking microporous；When the diameter of micropore is excessive, when such as more than 5 microns, reactant mixing is not enough filled
Point, cause the particle diameter of final product excessive.In the present embodiment, the microporous membrane 100 is polychloroethylene film.
In step s 2, the indium stannum aqueous solution 200 is the mixed solution containing indium ion and tin ion.Specifically, institute
State indium stannum aqueous solution 200 to form by the water soluble salt containing indium, stanniferous water soluble salt and water mixed preparing.Wherein, containing indium
Water soluble salt can be for indium chloride, indium nitrate, indium sulfate etc.；Stanniferous water soluble salt can be stannic chloride, nitric acid stannum, STANNOUS SULPHATE CRYSTALLINE
Deng.The concentration of the indium ion in the indium stannum aqueous solution 200 is 0.45 mol/L-2.25 mol/L, and the concentration of tin ion is
0.05 mol/L-0.25 mol/L.In the present embodiment, the indium stannum aqueous solution 200 is by InCl3‧4H2O and SnCl4‧5H2O is molten
Formed in water.
Up and down two surface of the micropore in the microporous membrane 100 through microporous membrane 100, forms multiple micro channels.
The indium stannum aqueous solution 200 flows to the lower surface of microporous membrane 100 from the upper surface of microporous membrane 100 along micro channel.
In step s3, the indium stannum aqueous solution 200 is mixed with ammonia spirit 300 in the lower surface of microporous membrane 100, the indium
Stannum aqueous solution 200 and ammonia spirit 300 can regard continuous phase and dispersion phase as respectively according to the difference of flow, and ensure continuous phase with
The flow ratio of dispersion phase meets：Continuous phase:Dispersion phase=3:2-4:1.It is appreciated that working as indium stannum aqueous solution 200 and ammonia spirit
When 300 flow-rate ratio meets above-mentioned condition, then indium stannum aqueous solution 200 can regard continuous phase as, and ammonia spirit 300 is dispersion phase；When
When the flow-rate ratio of ammonia spirit 300 and indium stannum aqueous solution 200 meets above-mentioned condition, then indium stannum aqueous solution 200 can regard dispersion phase as,
Ammonia spirit 300 is continuous phase.By continuous phase constantly shear dispersion phase be capable of achieving it is biphase it is quick, be sufficiently mixed, and carry out
Coprecipitation reaction, so as to produce the precipitation granule of uniform particle sizes.The continuous phase need to meet above-mentioned with the flow ratio of dispersion phase
Condition, can cause two kinds of solution to have good mixed effect, and have suitable particle diameter yardstick after mixing, and then can improve
The production rate of final product.It is appreciated that when the continuous phase is less with the ratio of dispersion phase, such as less than 3:When 2, dispersion phase is not
Can be sheared by continuous phase in time, mixed effect is poor, after causing mixing, drop yardstick is larger, so as to the solid precipitation granule for being formed
Also it is larger, cause final product grain diameter larger；When the continuous phase it is larger with the ratio of dispersion phase, such as larger than 4:1, easily
When causing dispersion phase with continuously mixing, the flow resistance of dispersion phase is big, so that the mixed process of dispersion phase and continuous phase
It is suppressed, the product of coprecipitation reaction is less, causes the production rate of final product to reduce.The indium stannum aqueous solution 200 and ammonia
The flow velocity of aqueous solution 300 can be according to above-mentioned continuous phase with dispersion phase flow ratio be adjusted.It is appreciated that the mixture
It is made up of mixed liquor and solid sediment, the solid sediment is the indium hydroxide and hydroxide generated by coprecipitation reaction
The mixture of stannum.
Further, the indium stannum aqueous solution 200 is carried out at normal temperatures with the mixing and reaction of ammonia spirit 300, generally
20 DEG C -25 DEG C, the concentration of the ammonia 300 is 2 mol/L-10 mol/L, the indium stannum aqueous solution 200 and ammonia spirit 300
In hybrid reaction, the concentration of indium stannum aqueous solution 200 and ammonia spirit 300 is bigger, and the precipitation granule produced after reaction is more intensive, most
The particle diameter of end-product is also less.Further, the proportionate relationship by controlling continuous phase and dispersion phase can reach the control mixing
The pH value of mixed liquor in thing, the pH of mixed liquor described in the present embodiment can cause reaction between 6-9 in this pH value range
Solution can be reacted after uniform mixing completely.It is appreciated that when the pH value of mixed liquor exceeds suitable scope, working as mixed liquor
PH value it is too little, when such as less than 6, easily cause the precipitation in mixed liquor incomplete；When the pH value of mixed liquor is more than 9, finally
The particle diameter of product will not change with the change of pH value, cause ammonia luxus consumption.Further, when the mixed liquor
When pH value is maintained in above-mentioned suitable scope, the control to particle size can be realized by the size of control ph.With pH
The reduction of value, the particle diameter of product gradually increase, and this is to reduce the reduction for then representing ammonia concn due to pH value, and degree of supersaturation subtracts
Little, particle size is in increase；Conversely, with the increase of pH value, the particle diameter of product is gradually reduced.Specifically, as the pH of mixed liquor
Be worth for 6.5 when, the particle diameter of the product can reach 100 nanometers；When the pH value of mixed liquor is 8.5, the particle diameter of the product can
Reach 18 nanometers.
Further, the indium stannum aqueous solution 200 is passed into a coil pipe with the mixture after 300 hybrid reaction of ammonia spirit
Circulate in 400, the mixture continues reaction in coil pipe 400, further to promote indium stannum aqueous solution 200 and ammonia spirit 300
Between the extent of reaction.It is appreciated that the precipitate produced in above-mentioned reaction is less due to granule, can be under the drive of mixed liquor
Flowed in coil pipe 400 together.Specifically, Single port of the mixture from the coil pipe 400 is flowed into, and from coil pipe 400
Flow out another port.The length of the coil pipe 400 is 1.5 meters -2 meters, and the time that the mixture circulates in coil pipe 400 is 30
- 1 minute second, so that the mixture can be fully reacted in coil pipe 400.
In step s 4, the temperature of the water-bath is 50 DEG C -55 DEG C, and ageing time is -12 hours 11 hours, so that instead
The precipitation granule homogenization that should be generated.After the completion of aging, mixture is filtered, and by the solid precipitation deionization being filtrated to get
Water and ethanol are washed twice respectively, are vacuum dried 24 hours gained solid precipitation again, with abundant after the completion of washing at 55 DEG C
Removal moisture content.
In step s 5, dry solid is placed in Muffle furnace carries out roasting, and the temperature of the roasting is 400 DEG C -600
DEG C, the time of roasting is -2 hours 1 hour.After the completion of roasting, lurid indium-tin oxide powder is obtained.In the present embodiment, institute
The particle diameter of the indium-tin oxide powder for obtaining is between 13 nanometers -100 nanometers.Refer to Fig. 3 and Fig. 4 and prepare different for the present invention
The transmission electron microscope photo of the indium-tin oxide powder obtained under parameter, it can be seen that the Indium sesquioxide. that the present invention is prepared
The granule of tin powder is between 13 nanometers -100 nanometers.
The preparation method of the tin indium oxide that the present invention is provided, by using microporous membrane 100, and with reference to fluid cross-flow shearing
Micropore dispersion so that indium stannum aqueous solution 200 is dispersed by microporous membrane 100, using suitable continuous phase and the ratio of dispersion phase,
Realize with ammonia spirit 300 within the Millisecond time it is abundant, uniform mix, so as to form homogeneous precipitation, the oxidation for preparing
Indium tin particles are also more uniform；By using microporous membrane 100, at the same further after control mixing the pH value of solution scope, from
And realize the controllable standby to indium tin oxide particles particle diameter so that particle diameter can regulate and control in 13 nanometer of -100 nanometer range；Coil pipe
400 setting makes reaction more fully carry out, and the production rate that improve final product can enable reaction by arranging coil pipe 400
Fully carry out so that the production rate of the final product of reaction is improved.
The present invention is further illustrated below by way of specific embodiment, but is not limited to the scope of the present invention.
Embodiment 1
Weigh InCl3‧4H2O and SnCl4‧5H2O crystal, is dissolved in deionized water, obtains indium stannum aqueous solution, wherein, InCl3's
Concentration is 1.8mol/L, In:Sn=9:1.Compound concentration is the ammonia spirit of 8 mol/L, at normal temperatures, using microporous membrane to indium
Stannum aqueous solution and ammonia spirit are mixed and are reacted, and wherein indium stannum aqueous solution is dispersion phase, and ammonia is continuous phase, by continuous
Mutually constantly shear dispersion phase and realize biphase quick mixing, and carry out coprecipitation reaction, continuous phase：Dispersion phase=2：1.Will mixing
Mixture afterwards continues reaction by a length of 1.5 meters of coil pipe, and reacted mixture flows into beaker and continues stirring.By in beaker
Mixture be placed in aging 12 hours in water-bath, bath temperature be 50 DEG C.Filter after aging, the solid for obtaining is utilized into deionization
Water and ethanol are vacuum dried 24 hours after washing twice respectively at 55 DEG C.Dried solid is placed in Muffle furnace and is roasted
Burn 1 hour, sintering temperature is 500 degree, obtains lurid indium-tin oxide powder, and the indium tin oxide particles particle diameter for preparing is
14 nanometers.Such as the transmission electron microscope picture that Fig. 3 is the indium tin oxide particles, wherein, Fig. 3 (a)-(c) is respectively scale yardstick and exists
Image under the conditions of 20nm, 50nm, 100nm.
Embodiment 2
Weigh InCl3‧4H2O and SnCl4‧5H2O crystal, is dissolved in deionized water, obtains indium stannum aqueous solution, wherein, InCl3's
Concentration is 0.45mol/L, In:Sn=9:1.Compound concentration is the ammonia spirit of 4 mol/L, at normal temperatures, using microporous membrane to indium
Stannum aqueous solution and ammonia spirit are mixed and are reacted, and wherein ammonia is dispersion phase, and indium stannum aqueous solution is continuous phase, by continuous
Mutually constantly shear dispersion phase and realize biphase quick mixing, and carry out coprecipitation reaction, continuous phase：Dispersion phase=3：1.Will mixing
Thing continues reaction by a length of 1.5 meters of coil pipe, and reacted mixture flows into beaker and continues stirring.By the mixture in beaker
It is placed in aging 12 hours in water-bath, bath temperature is 50 DEG C.Filter after aging, the solid for obtaining is utilized into deionized water and ethanol
It is vacuum dried 24 hours at 55 DEG C after washing twice respectively.Dried solid is placed in Muffle furnace carries out roasting 1 hour,
Sintering temperature is 500 degree, obtains lurid indium-tin oxide powder, and the indium tin oxide particles particle diameter for preparing is 100 nanometers.
Embodiment 3
Weigh InCl3‧4H2O and SnCl4‧5H2O crystal, is dissolved in deionized water, obtains indium stannum aqueous solution, wherein, InCl3's
Concentration is 2.03mol/L, In:Sn=9:1.Compound concentration is the ammonia spirit of 9 mol/L, at normal temperatures, using microporous membrane to indium
Stannum aqueous solution and ammonia spirit are mixed and are reacted, and wherein indium stannum aqueous solution is dispersion phase, and ammonia is continuous phase, by continuous
Mutually constantly shear dispersion phase and realize biphase quick mixing, and carry out coprecipitation reaction, continuous phase：Dispersion phase=2：1.Will mixing
Thing continues reaction by a length of 1.5 meters of coil pipe, and reacted mixture flows into beaker and continues stirring.By the mixture in beaker
It is placed in aging 12 hours in water-bath, bath temperature is 50 DEG C.Filter after aging, the solid for obtaining is utilized into deionized water and ethanol
It is vacuum dried 24 hours at 55 DEG C after washing twice respectively.Dried solid is placed in Muffle furnace carries out roasting 1 hour,
Sintering temperature is 500 degree, obtains lurid indium-tin oxide powder, and the indium tin oxide particles particle diameter for preparing is 13 nanometers.
Such as the transmission electron microscope picture that Fig. 4 is the indium tin oxide particles, wherein, Fig. 3 (a)-(c) is respectively scale yardstick in 20nm, 50nm,
Image under the conditions of 100nm.
In addition, those skilled in the art can also make other changes in spirit of the invention, these are according to present invention essence certainly
The change made by god, should all be included in scope of the present invention.
Claims (6)
1. a kind of preparation method of indium-tin oxide powder, its step is：
A microporous membrane is provided, the microporous membrane has a upper surface and a lower surface relative with the upper surface, the micropore
Film includes multiple micropores, up and down two surface of multiple micropores through the microporous membrane；
It is passed through an indium stannum aqueous solution so that micropore described in upper surface Jing of the indium stannum aqueous solution from the microporous membrane flows into micro-
The lower surface of pore membrane；
It is passed through an ammonia spirit so that the ammonia spirit flows along the lower surface direction of the microporous membrane, the ammonia spirit
With the indium stannum aqueous solution for flowing to the microporous membrane lower surface and react, form a mixture；
Mixture is passed through it is aging in a water bath containers, it is aging after filter mixture and obtain solid precipitation, then solid precipitation is entered
Row is washed, is dried；And
Dried solid precipitation is carried out into roasting, indium-tin oxide powder is obtained；
The mixture is made up of mixed liquor and solid sediment, and the pH value of the mixed liquor is 6-9；
The taking a step forward the mixture is passed through in a coil pipe of the mixture ageing is circulated, time of circulation be 30 seconds -1 point
Clock；
The temperature of the water-bath is 50 DEG C -55 DEG C, and ageing time is -12 hours 11 hours.
2. the preparation method of indium-tin oxide powder as claimed in claim 1, it is characterised in that micropore is straight in the microporous membrane
Footpath is 1 micron -5 microns.
3. the preparation method of indium-tin oxide powder as claimed in claim 1, it is characterised in that the indium in the indium stannum aqueous solution
The concentration of ion is 0.45mol/L-2.25mol/L, and the concentration of tin ion is 0.05mol/L-0.25mol/L.
4. the preparation method of indium-tin oxide powder as claimed in claim 1, it is characterised in that the concentration of the ammonia is
2mol/L-10mol/L。
5. the preparation method of indium-tin oxide powder as claimed in claim 1, it is characterised in that the indium stannum aqueous solution and ammonia
Solution is divided into dispersion phase and continuous phase according to flow difference, and continuous phase is met with the flow ratio of dispersion phase：Continuous phase：Dispersion phase
=3:2-4:1.
6. the preparation method of indium-tin oxide powder as claimed in claim 1, it is characterised in that the grain of the indium-tin oxide powder
Footpath is 13 nanometers -100 nanometers.
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| CN109205659B (en) * | 2018-11-01 | 2019-08-06 | 清华大学 | A kind of preparation method for the indium oxide that crystal form is controllable |
| CN109607598B (en) * | 2019-01-22 | 2019-11-19 | 清华大学 | A kind of preparation method of big partial size indium oxide |
| CN115140760A (en) * | 2022-07-22 | 2022-10-04 | 昆明理工大学 | Preparation method of indium tin oxide nano powder based on microfluid rapid precipitation |
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| KR101092520B1 (en) * | 2009-11-24 | 2011-12-13 | 인하대학교 산학협력단 | Preparation method of indium-tin oxide nano powder using thermal plasma |
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