CN105523579A - Preparation method for indium tin oxide powder - Google Patents
Preparation method for indium tin oxide powder Download PDFInfo
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- CN105523579A CN105523579A CN201510876519.0A CN201510876519A CN105523579A CN 105523579 A CN105523579 A CN 105523579A CN 201510876519 A CN201510876519 A CN 201510876519A CN 105523579 A CN105523579 A CN 105523579A
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- C01—INORGANIC CHEMISTRY
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- C01G19/00—Compounds of tin
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- 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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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The invention relates to a preparation method for indium tin oxide powder. The preparation method comprises the following steps: providing a microporous membrane, wherein the microporous membrane has an upper surface and a lower surface facing the upper surface and comprises a plurality of micropores, and the micropores penetrate the upper and lower surfaces of the microporous membrane; introducing an aqueous indium tin solution and allowing the aqueous indium tin solution to flow from upper surface of microporous membrane to lower surface of microporous membrane via the micropores; introducing an aqueous ammonia solution and allowing the aqueous ammonia solution to flow along the lower surface of microporous membrane, wherein the aqueous ammonia solution is mixed and reacts with the aqueous indium tin solution flowing to the lower surface of microporous membrane so as to form a mixture; introducing the mixture into a water-bath container for ageing, carrying out filtering after ageing so as obtain a solid precipitate and subjecting the solid precipitate to washing and drying; and roasting the dried solid so as to obtain indium tin oxide powder.
Description
Technical field
The present invention relates to a kind of method preparing indium-tin oxide powder, particularly a kind of method preparing indium-tin oxide powder based on microreactor.
Background technology
Tin indium oxide (ITO) is a kind of n-type semiconductor, possesses excellent photoelectric properties.The resistivity (about 10 that the thin film obtained with ITO sputtering of materials is standby very low
-4Ω cm), good through performance is possessed for visible ray simultaneously.Therefore, ito thin film is widely used in the fields such as liquid crystal display, Organic Light Emitting Diode, touch-screen, solar cell.At present, in the consumption of global indium resource, ITO industry occupies 85%.Along with the development of current flat panel display industry, the requirement for ito thin film also develops towards maximization, high-compactness, high purity.The character of ito thin film is fundamentally decided by the character of ito powder, and therefore in order to meet industry development requirement, ito powder preparation process needs further to optimize.
Common tin indium oxide preparation method comprises chemical coprecipitation, sol-gel method, hydrothermal method, spray pyrolysis etc.Wherein, chemical coprecipitation is considered to simple, the most economic method, has a wide range of applications in experimental study and industrial production.But the method for traditional chemical coprecipitation exists microcosmic, and mixing is poor, reacts uneven, easily occurs dephasign, the problems such as partial over saturation degree is low, and preparation process is wayward in system.
Summary of the invention
In view of this, necessaryly a kind of preparation method reacting evenly, prepare the indium-tin oxide powder of size tunable is provided.
A kind of preparation method of indium-tin oxide powder, it comprises the following steps: provide a microporous membrane, described microporous membrane has the upper surface lower surface relative with described upper surface with, and described microporous membrane comprises multiple micropore, and multiple described micropore is through two surfaces up and down of this microporous membrane; Pass into an indium tin aqueous solution, make the described indium tin aqueous solution flow into the lower surface of microporous membrane through described micropore from the upper surface of described microporous membrane; Pass into an ammonia soln, described ammonia soln flowed along the lower surface direction of described microporous membrane, described ammonia soln with flow to the indium tin aqueous solution of described microporous membrane lower surface and react, form a mixture; Passed into by mixture in a water bath containers aging, aging rear filtering mixt obtains solid precipitation, then solid precipitation is carried out wash, dry; And dried solid is carried out roasting, obtain indium-tin oxide powder.
Relative to prior art, the preparation method of tin indium oxide provided by the invention, by adopting microporous membrane, and in conjunction with the micropore dispersion that fluid cross-flow is sheared, make the indium tin aqueous solution dispersed by microporous membrane, realize with ammonia soln fully within the Millisecond time, Homogeneous phase mixing, thus formed precipitation from homogeneous solution, the indium tin oxide particles prepared is also more even.
Accompanying drawing explanation
Fig. 1 is the preparation flow figure of indium-tin oxide powder provided by the invention.
Fig. 2 is the reaction process schematic diagram of the indium tin aqueous solution provided by the invention and ammonia soln.
Fig. 3 is the transmission electron microscope picture of the indium-tin oxide powder of embodiment 1 provided by the invention preparation.
The transmission electron microscope picture of indium-tin oxide powder prepared by Fig. 4 embodiment 3 provided by the invention.
Main element nomenclature
| 100 | Microporous membrane |
| 200 | The indium tin aqueous solution |
| 300 | Ammonia soln |
| 400 | Coil pipe |
Following specific embodiment will further illustrate the present invention in conjunction with above-mentioned accompanying drawing.
Embodiment
Below in conjunction with specific embodiment, the preparation method of indium-tin oxide powder provided by the invention is described in further detail.
Refer to Fig. 1, the invention provides a kind of preparation method of indium-tin oxide powder, this preparation method specifically comprises the following steps:
S1, provides a microporous membrane 100, and described microporous membrane 100 has the upper surface lower surface relative with described upper surface with, and described microporous membrane 100 comprises multiple micropore, and described multiple micropore is through two surfaces up and down of this microporous membrane 100;
S2, passes into an indium tin aqueous solution 200, makes the described indium tin aqueous solution 200 flow into the lower surface of microporous membrane 100 through described micropore from the upper surface of described microporous membrane 100;
S3, passes into an ammonia soln 300, and described ammonia soln 300 is flowed along the lower surface direction of described microporous membrane 100, and described ammonia soln 300 mixes with the indium tin aqueous solution 200 flowing to described microporous membrane 100 lower surface and reacts, and forms a mixture;
S4, passes in a water bath containers aging by mixture, aging rear filtering mixt obtains solid precipitation, then solid precipitation is carried out wash, dry; And
S5, carries out roasting by dried solid, obtains indium-tin oxide powder.
In step sl, the material of described microporous membrane 100 is with the indium tin aqueous solution 200 and ammonia soln 300, the material of chemical reaction does not occur, and can be macromolecular material, the metallic substance being coated with matcoveredn or other matrix material.Refer to Fig. 2, in described microporous membrane 100, the diameter of micropore is 1 micron-5 microns.Be appreciated that the solid sediment produced in reaction is easily blocking microporous when the diameter of micropore is less than 1 micron; When the diameter of micropore is excessive, when being such as greater than 5 microns, reactant mixing is abundant not, causes the particle diameter of final product excessive.In the present embodiment, described microporous membrane 100 is polychloroethylene film.
In step s 2, the described indium tin aqueous solution 200 is the mixing solutions containing indium ion and tin ion.Particularly, the described indium tin aqueous solution 200 is by forming containing the water-soluble salt of indium, stanniferous water-soluble salt and water mixed preparing.Wherein, the water-soluble salt containing indium can be indium chloride, indium nitrate, indium sulfate etc.; Stanniferous water-soluble salt can be tin chloride, nitric acid tin, tin sulphate etc.The concentration of the indium ion in the described indium tin aqueous solution 200 is 0.45mol/L-2.25mol/L, and the concentration of tin ion is 0.05mol/L-0.25mol/L.In the present embodiment, the described indium tin aqueous solution 200 is by InCl
34H
2o and SnCl
45H
2the water-soluble formation of O.
Micropore in described microporous membrane 100, through two surfaces up and down of microporous membrane 100, forms multiple micro channel.The described indium tin 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 described indium tin aqueous solution 200 mixes with ammonia soln 300 at the lower surface of microporous membrane 100, this indium tin aqueous solution 200 and ammonia soln 300 can regard external phase and disperse phase as respectively according to the difference of flow, and ensure that the flow ratio of external phase and disperse phase meets: external phase: disperse phase=3:2-4:1.Be appreciated that then the indium tin aqueous solution 200 can regard external phase as, and ammonia soln 300 is disperse phase when the throughput ratio of the indium tin aqueous solution 200 and ammonia soln 300 meets above-mentioned condition; When the throughput ratio of ammonia soln 300 and the indium tin aqueous solution 200 meets above-mentioned condition, then the indium tin aqueous solution 200 can regard disperse phase as, and ammonia soln 300 is external phase.By external phase constantly shear disperse phase can realize two-phase quick, fully mix, and carry out coprecipitation reaction, thus produce the deposit seeds of uniform particle sizes.The flow ratio of described external phase and disperse phase need meet above-mentioned condition, and two kinds of solution can be made to have good mixed effect, and has suitable particle diameter yardstick after mixing, and then can improve the production rate of final product.Be appreciated that the ratio when described external phase and disperse phase is less, during as being less than 3:2, disperse phase can not be sheared by external phase in time, and mixed effect is poor, and after causing mixing, drop yardstick is larger, thus the solid precipitation particle formed is also comparatively large, causes final product grain diameter larger; When the ratio of described external phase and disperse phase is comparatively large, as being greater than 4:1, when easily causing disperse phase to mix with external phase, the resistance to flow of disperse phase is large, thus the mixing process of disperse phase and external phase is suppressed, the product of coprecipitation reaction is less, causes the production rate of final product to reduce.The flow velocity of the described indium tin aqueous solution 200 and ammonia soln 300 can regulate according to the flow ratio of above-mentioned external phase and disperse phase.Be appreciated that described mixture is made up of mixed solution and solid sediment, described solid sediment is the mixture of indium hydroxide and the stannic hydroxide generated by coprecipitation reaction.
Further, mixing and reacting of the described indium tin aqueous solution 200 and ammonia soln 300 is carried out at normal temperatures, be generally 20 DEG C-25 DEG C, the concentration of described ammoniacal liquor 300 is 2mol/L-10mol/L, the described indium tin aqueous solution 200 is with ammonia soln 300 hybrid reaction, the concentration of the indium tin aqueous solution 200 and ammonia soln 300 is larger, and the deposit seeds produced after reaction is more intensive, and the particle diameter of final product is also less.Further, the pH value controlling mixed solution in described mixture can be reached by the proportionlity controlling external phase and disperse phase, the pH of mixed solution described in the present embodiment, between 6-9, can make reaction soln after Homogeneous phase mixing in this pH value range, can complete reaction.When being appreciated that the pH value of mixed solution exceeds suitable scope, when the pH value of mixed solution is too little, during as being less than 6, easily make the precipitation in mixed solution incomplete; When the pH value of mixed solution is greater than 9, the particle diameter of final product can not change along with the change of pH value, causes ammoniacal liquor luxus consumption.Further, when the pH value of described mixed solution remains in above-mentioned suitable scope, by the size of control ph, the control to particle size is realized.Along with the reduction of pH value, the particle diameter of product increases gradually, and this is that degree of supersaturation reduces because pH value reduces then to represent the reduction of ammonia concn, and particle size is in increase; Otherwise along with the increase of pH value, the particle diameter of product reduces gradually.Particularly, when the pH value of mixed solution is 6.5, the particle diameter of described product can reach 100 nanometers; When the pH value of mixed solution is 8.5, the particle diameter of described product can reach 18 nanometers.
Further, the mixture after the described indium tin aqueous solution 200 and ammonia soln 300 hybrid reaction is passed in a coil pipe 400 and circulate, and this mixture continues to react, to promote the level of response between the indium tin aqueous solution 200 and ammonia soln 300 further in coil pipe 400.Be appreciated that the throw out produced in above-mentioned reaction is less due to particle, can flow into together in coil pipe 400 under the drive of mixed solution.Particularly, described mixture flows into from the Single port described coil pipe 400, and flows out from the another port of coil pipe 400.The length of described coil pipe 400 is 1.5 meters-2 meters, and the time that this mixture circulates in coil pipe 400 is 30 seconds-1 minute, fully can react to make this mixture in coil pipe 400.
In step s 4 which, the temperature of described water-bath is 50 DEG C-55 DEG C, and digestion time is 11 hours-12 hours, to make to react the deposit seeds homogenizing generated.Aging complete after, mixture is filtered, and will the solid precipitation deionized water that obtains be filtered and ethanol washes twice respectively, again by the vacuum-drying 24 hours at 55 DEG C of gained solid precipitation after having washed, to remove moisture content fully.
In step s 5, the solid of drying is placed in retort furnace and carries out roasting, the temperature of described roasting is 400 DEG C-600 DEG C, and the time of roasting is 1 hour-2 hours.After roasting completes, obtain lurid indium-tin oxide powder.In the present embodiment, the particle diameter of the indium-tin oxide powder obtained is between 13 nanometer-100 nanometers.Refer to the transmission electron microscope photo that Fig. 3 and Fig. 4 is the indium-tin oxide powder that the present invention obtains under different preparation parameter, as can be seen from the figure, the particle of the indium-tin oxide powder that the present invention prepares is all between 13 nanometer-100 nanometers.
The preparation method of tin indium oxide provided by the invention, by adopting microporous membrane 100, and in conjunction with the micropore dispersion that fluid cross-flow is sheared, make the indium tin aqueous solution 200 dispersed by microporous membrane 100, adopt the ratio of suitable external phase and disperse phase, realize with ammonia soln 300 fully within the Millisecond time, Homogeneous phase mixing, thus formed precipitation from homogeneous solution, the indium tin oxide particles prepared is also more even; By adopting microporous membrane 100, controlling the scope of the pH value of solution after mixing simultaneously further, thus realizing the controlled synthesis to indium tin oxide particles particle diameter, particle diameter can be regulated and controled in 13 nanometer-100 nanometer range; The setting of coil pipe 400 makes reaction more fully carry out, and the production rate that improve final product can make reaction fully to carry out by arranging coil pipe 400, and the production rate of the final product reacted is improved.
Further illustrate the present invention below by way of specific embodiment, but be not used for limiting the scope of the invention.
Embodiment 1
Take InCl
34H
2o and SnCl
45H
2o crystal, is dissolved in deionized water, obtains the indium tin aqueous solution, wherein, and InCl
3concentration be 1.8mol/L, In:Sn=9:1.Compound concentration is the ammonia soln of 8mol/L, at normal temperatures, microporous membrane is utilized to mix the indium tin aqueous solution and ammonia soln and react, wherein the indium tin aqueous solution is disperse phase, ammoniacal liquor is external phase, constantly shear by external phase the short mix that disperse phase realizes two-phase, and carry out coprecipitation reaction, external phase: disperse phase=2:1.Mixed mixture is continued reaction by the coil pipe that length is 1.5 meters, and reacted mixture flows into beaker to be continued to stir.Mixture in beaker is placed in water-bath aging 12 hours, bath temperature is 50 DEG C.Aging rear filtration, vacuum-drying 24 hours at 55 DEG C after utilizing deionized water and ethanol to wash twice respectively the solid obtained.Dried solid is placed in retort furnace and carries out roasting 1 hour, maturing temperature is 500 degree, obtains lurid indium-tin oxide powder, and the indium tin oxide particles particle diameter prepared is 14 nanometers.As Fig. 3 be as described in the transmission electron microscope picture of indium tin oxide particles, wherein, Fig. 3 (a)-(c) is respectively the image of scale yardstick under 20nm, 50nm, 100nm condition.
Embodiment 2
Take InCl
34H
2o and SnCl
45H
2o crystal, is dissolved in deionized water, obtains the indium tin aqueous solution, wherein, and InCl
3concentration be 0.45mol/L, In:Sn=9:1.Compound concentration is the ammonia soln of 4mol/L, at normal temperatures, microporous membrane is utilized to mix the indium tin aqueous solution and ammonia soln and react, wherein ammoniacal liquor is disperse phase, the indium tin aqueous solution is external phase, constantly shear by external phase the short mix that disperse phase realizes two-phase, and carry out coprecipitation reaction, external phase: disperse phase=3:1.Mixture is continued reaction by the coil pipe that length is 1.5 meters, and reacted mixture flows into beaker to be continued to stir.Mixture in beaker is placed in water-bath aging 12 hours, bath temperature is 50 DEG C.Aging rear filtration, vacuum-drying 24 hours at 55 DEG C after utilizing deionized water and ethanol to wash twice respectively the solid obtained.Dried solid is placed in retort furnace and carries out roasting 1 hour, maturing temperature is 500 degree, obtains lurid indium-tin oxide powder, and the indium tin oxide particles particle diameter prepared is 100 nanometers.
Embodiment 3
Take InCl
34H
2o and SnCl
45H
2o crystal, is dissolved in deionized water, obtains the indium tin aqueous solution, wherein, and InCl
3concentration be 2.03mol/L, In:Sn=9:1.Compound concentration is the ammonia soln of 9mol/L, at normal temperatures, microporous membrane is utilized to mix the indium tin aqueous solution and ammonia soln and react, wherein the indium tin aqueous solution is disperse phase, ammoniacal liquor is external phase, constantly shear by external phase the short mix that disperse phase realizes two-phase, and carry out coprecipitation reaction, external phase: disperse phase=2:1.Mixture is continued reaction by the coil pipe that length is 1.5 meters, and reacted mixture flows into beaker to be continued to stir.Mixture in beaker is placed in water-bath aging 12 hours, bath temperature is 50 DEG C.Aging rear filtration, vacuum-drying 24 hours at 55 DEG C after utilizing deionized water and ethanol to wash twice respectively the solid obtained.Dried solid is placed in retort furnace and carries out roasting 1 hour, maturing temperature is 500 degree, obtains lurid indium-tin oxide powder, and the indium tin oxide particles particle diameter prepared is 13 nanometers.As Fig. 4 be as described in the transmission electron microscope picture of indium tin oxide particles, wherein, Fig. 3 (a)-(c) is respectively the image of scale yardstick under 20nm, 50nm, 100nm condition.
In addition, those skilled in the art also can do other change in spirit of the present invention, and these changes done according to the present invention's spirit, all should be included in the present invention's scope required for protection certainly.
Claims (10)
1. a preparation method for indium-tin oxide powder, it comprises the following steps:
There is provided a microporous membrane, described microporous membrane has the upper surface lower surface relative with described upper surface with, and described microporous membrane comprises multiple micropore, and multiple described micropore is through two surfaces up and down of this microporous membrane;
Pass into an indium tin aqueous solution, make the described indium tin aqueous solution flow into the lower surface of microporous membrane through described micropore from the upper surface of described microporous membrane;
Pass into an ammonia soln, described ammonia soln flowed along the lower surface direction of described microporous membrane, described ammonia soln with flow to the indium tin aqueous solution of described microporous membrane lower surface and react, form a mixture;
Passed into by mixture in a water bath containers aging, aging rear filtering mixt obtains solid precipitation, then solid precipitation is carried out wash, dry; And
Dried solid precipitation is carried out roasting, obtains indium-tin oxide powder.
2. the preparation method of indium-tin oxide powder as claimed in claim 1, it is characterized in that, in described microporous membrane, the diameter of micropore is 1 micron-5 microns.
3. the preparation method of indium-tin oxide powder as claimed in claim 1, it is characterized in that, the concentration of the indium ion in the described indium tin aqueous solution 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 characterized in that, the concentration of described ammoniacal liquor is 2mol/L-10mol/L.
5. the preparation method of indium-tin oxide powder as claimed in claim 1, it is characterized in that, the described indium tin aqueous solution is divided into disperse phase and external phase with ammonia soln according to flow is different, and the flow ratio of external phase and disperse phase meets: external phase: disperse phase=3:2-4:1.
6. the preparation method of indium-tin oxide powder as claimed in claim 1, it is characterized in that, described mixture is made up of mixed solution and solid sediment, and the pH value of this mixed solution is 6-9.
7. the preparation method of indium-tin oxide powder as claimed in claim 1, is characterized in that, taking a step forward mixture ageing to comprise this mixture to pass in a coil pipe and circulate.
8. the preparation method of indium-tin oxide powder as claimed in claim 7, it is characterized in that, the time that described mixture circulates in coils is 30 seconds-1 minute.
9. the preparation method of indium-tin oxide powder as claimed in claim 1, it is characterized in that, the temperature of described water-bath is 50 DEG C-55 DEG C, and digestion time is 11 hours-12 hours.
10. the preparation method of indium-tin oxide powder as claimed in claim 1, it is characterized in that, the particle diameter of described indium-tin oxide powder is 13 nanometer-100 nanometers.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109205659A (en) * | 2018-11-01 | 2019-01-15 | 清华大学 | A kind of preparation method for the indium oxide that crystal form is controllable |
| CN109607598A (en) * | 2019-01-22 | 2019-04-12 | 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109205659A (en) * | 2018-11-01 | 2019-01-15 | 清华大学 | A kind of preparation method for the indium oxide that crystal form is controllable |
| CN109607598A (en) * | 2019-01-22 | 2019-04-12 | 清华大学 | A kind of preparation method of big partial size indium oxide |
| 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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