CN109231259A - A kind of method that indium metal and metallic tin prepare ultra-fine ITO powder - Google Patents
A kind of method that indium metal and metallic tin prepare ultra-fine ITO powder Download PDFInfo
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- CN109231259A CN109231259A CN201811187676.0A CN201811187676A CN109231259A CN 109231259 A CN109231259 A CN 109231259A CN 201811187676 A CN201811187676 A CN 201811187676A CN 109231259 A CN109231259 A CN 109231259A
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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
- C01G19/006—Compounds containing, besides tin, two or more other elements, with the exception of oxygen or hydrogen
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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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
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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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
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
The invention discloses a kind of methods for preparing ultra-fine ITO powder by indium metal and tin.Directly using indium metal ingot and tin slab as raw material, through composition design, after alloying fritting in hot-bulb grinding machine in 100~300 DEG C of temperature under conditions of carry out gas oxidation, generate indium oxide and tin oxide, make the indium oxide just generated and tin oxide from molten alloy droplets sur-face peeling using the ball action of ball mill simultaneously, and complete fine grinding, ITO powder is finally obtained, the even-grained ITO composite powder product of output after air current classifying.The present invention has many advantages, such as that reaction process is short, product granularity is thin, reagent consumption is few, solves the problems, such as that direct metal indium, tin generate oxidation film in oxidation process and causes to be difficult to further to be oxidized compared with traditional handicraft.
Description
Technical field
The invention belongs to material field of metallurgy, more particularly to a kind of mill oxidation of hot-bulb prepares the side of ultra-fine ito powder
Method.
Background technique
Indium tin oxide (Indium tin oxide, ITO) has high transparency, low-resistivity, film hardness high, good
The advantages that chemical stability and etching performance, is widely used in liquid crystal display, solar battery, thin film light emitting device, sensing
The tips such as device manufacturing field.Current preparation method is all indium oxide and tin oxide respectively at powder, forms, sinters into after remixing
ITO target, long flow path, powder processed are at high cost.And due to forming stable tin dioxide film after metallic tin oxidation, conventional acid is not dissolved in
And alkali, oxidation reaction further progress is hindered, thus putty powder is mostly used wet chemistry method preparation, common feature is in the solution
Pink salt presoma is synthesized, then obtains tin oxide by calcining or without calcining, main problem is that long flow path, wastewater flow rate are big.
Patent CN102923765A " a kind of indium tin oxide (ITO) nano-powder and its manufacturing method " can with indium and tin
Organic matter is added through conbustion synthesis ellipsoid indium oxide and putty powder in dissolved salt raw material；A kind of fuel of patent CN102417203 "
The method that synthetic method prepares ultra-fine ITO powder " equally using indium and tin nitrate as raw material, obtains ultra-fine ITO powder with reduction burning
Body, the consumption of such method reagent is big, product cost is high.Patent CN105540647A discloses that " a kind of thermal spraying prepares rotary target
With ITO powder and its production method and application ", the coprecipitated starch of ITO is obtained using one step of chemical coprecipitation, then be heat-treated to obtain
ITO powder, process is short, meets the production theory of short route, there are also hydro-thermal methods, sol-gal process for congenic method.And spray-oxidizing process
It is also a kind of direct synthesis method, and using indium metal and tin as raw material, process is further simplified, but spraying apparatus investment is big, work
Skill control requires high.
Consider from simple flow, indium metal and tin direct oxidation be prepare indium oxide and tin oxide most straightforward approach, but
Problem is that the passivation of oxidation film aoxidizes metal further to become difficult, especially metallic tin, once forming tin oxide film
The further progress of reaction can be obstructed afterwards, and only peelling off oxide layer in time can just make oxidation reaction constantly go on, and ball milling
It can reach this effect.Therefore, this patent proposes a kind of method for preparing ultra-fine ITO powder by indium metal and tin, in heated condition
It is lower that indium metal and tin are aoxidized using air, and synchronous progress ball milling, realize quick oxidation, the oxide skin(coating) stripping of indium and tin
It falls and refines, mixes with oxidation product, process economy is efficient, cleaning is high-quality, is expected to the ultra-fine ITO powder application field of further expansion.
Summary of the invention
The problem of for background technique, the invention proposes a kind of indium metals and metallic tin to prepare ultra-fine ITO powder
Method complete indium metal refinement synchronous with oxide with the Simultaneous Oxidation of tin, realization using hot-bulb grinding machine as consersion unit
The economical and efficient of ultra-fine indium oxide and glass putty, controllable steady production.
The purpose of the present invention is achieved by the following technical programs:
A kind of method that indium metal and metallic tin prepare ultra-fine ITO powder, it is advanced using indium metal ingot and metal tin slab as raw material
The design of row composition and alloying fritting, in hot-bulb grinding machine in 100~300 DEG C of temperature and under conditions of be passed through oxidizing gas into
The mill oxidation of row hot-bulb, is oxidized indium metal and the metallic tin form of being in a liquid state, while carrying out ball milling, after the completion of hot-bulb mill oxidation
To ultra-fine ITO powder.
Hot-bulb grinding machine interior room reaction temperature of the present invention is 100~300 DEG C, and indium metal and Xi Yi system are oxidized by the air generation
Indium oxide and tin oxide, it is equal within the scope of 0~1000 DEG C from the gibbs free energy change value that can be seen that the reaction in attached drawing 3
In -300kJ/mol hereinafter, and increased as temperature increases, therefore reaction temperature is not easy excessively high, and wherein indium is oxidizable compared with tin.
But the indium oxide and tin oxide generated is covered on the surface of metal drop, hinders the further progress of oxidation reaction.
Sn+O2(g)=SnO2
2In+1.5O2(g)=In2O3
Reaction temperature in this method is 100~300 DEG C, and the fusing point of indium metal is 156.61 DEG C, and the fusing point of metallic tin is
231.89 DEG C, the fusing point of indium stannum alloy melt is lower, and there are 0~150 DEG C of the degrees of superheat for the method for the present invention, it is ensured that indium stannum alloy
Needed for the dynamics of oxidation reaction.The reaction simultaneously is exothermic reaction, and it is unfavorable that excessively high temperature improves degree of oxidation, and improves
Energy consumption.
Ultra-fine ITO powder is directly prepared by indium metal and metallic tin using hot-bulb mill oxidation reaction in technical solution of the present invention
End carries out ball milling refinement to newly-generated indium oxide and tin oxide with ball milling while oxidation, can peel off the oxidation on surface
Layer, and newly-generated indium oxide and stannic oxide powder are refined constantly by ball milling, the direct ultra-fine ito powder of output.
Preferably, the mass ratio of indium metal ingot and metal tin slab is 9.45:1 in composition design.
Preferably, the temperature of the alloying fritting is 250~300 DEG C, and indium metal ingot and metal tin slab are in temperature
Fritting is carried out at 250~300 DEG C, so that indium and tin form the alloy melt of uniform ingredients, to guarantee the uniform of oxidation reaction
Property, also guarantee the uniform distribution of final oxide；
Preferably, the oxidizing gas is air or oxygen.
Preferably, it is 0.1~2m/s that the oxidizing gas, which blasts linear velocity, forces blasting for oxidizing gas that can accelerate
The oxidation of indium and tin, while certain agitaion is played to molten alloy liquid, enhanced oxidation diffusion mass transfer can make indium and tin
It aoxidizes more abundant；The linear velocity that blasts is more preferably 0.5~1.5m/s.
Preferably, milling intensity is 30~120rpm in the hot mechanical milling process, and filling rate is 10~50%, and ratio of grinding media to material is
3~9, above-mentioned parameter both can guarantee grinding efficiency, also can guarantee production efficiency；It is further preferred that the filling rate be 20~
40%, ratio of grinding media to material is 5~8.
Of both ball milling can play the role of in the present invention, on the one hand produce the indium oxide on molten alloy droplets surface and tin
Nitride layer is constantly removed, and oxidation reaction is enable constantly to carry out, and on the other hand makes the indium oxide generated and tin oxide at once by ball
Mill oxidation, directly obtains ultra-fine indium oxide and tin oxide.But ball milling operation is high energy consumption process, therefore should not be turned using excessively high
Speed.
Ball material medium used in the preferably described ball milling is one of zirconium oxide, agate, hard alloy and corundum,
It is inertia material, it is ensured that high-temperature stability and product purity；Preferably zirconium oxide.
Preferably, the time of the described hot-bulb mill reaction process is 1~5h, it is ensured that indium and tin it is fully oxidized and thin
Mill；Further preferably 1~3h.
The method that indium metal of the present invention and metallic tin prepare ultra-fine ITO powder, specifically includes the following steps:
S1. composition design: take indium metal ingot and metal tin slab by certain mass ratio be precise；
S2. alloying fritting: load weighted indium metal ingot and metal tin slab carry out fritting at being 250~300 DEG C in temperature,
Indium and tin is set to form the alloy melt of uniform ingredients；
S3. alloy molten: alloy melt obtained by step S2 is added in hot-bulb grinding machine, is opened electric heating, is made ball mill inner cavity
Temperature reaches 100~300 DEG C；
S4. hot-bulb mill oxidation: opening rotating device, start hot ball-milling reaction, maintain certain revolving speed, while from air inlet
Oxidizing gas is blasted into inner cavity, starts oxidation reaction and ball milling；Hot-bulb is ground in oxidation process, and the flue gas of combustion chamber is from fuel
The exhanst gas outlet of room is discharged, and reacts smoke filtration of the flue gas in inner cavity through being installed in reaction chamber and exports discharge, filtering mouth dress
There is ceramic filter plate, the material in ball mill can be prevented to be carried over；
S5. cooling discharging: reaction stops heating, ball milling and drum oxidizing gas after a certain period of time, opens discharge port and releases
Product I TO powder, puts loading feed bin after being completely cooled down to greenhouse, and classification obtains varigrained ITO product.
Compared with the prior art, the beneficial effects of the present invention are:
(1) the method for the present invention creativeness is replaced using indium metal and metal tin alloy fritting-liquid phase Low Temperature Thermal ball milling oxidation
The prevailing technology of existing precursor preparation-calcining and decomposing, greatly improves productivity, simple flow, and unique auxiliary material oxidant uses
Clean air or oxygen reduce reagent consumption, significantly reduce production cost, realize green, low-carbon, efficiently ultra-fine
Ito powder preparation.
(2) the method for the present invention aoxidizes at low temperature, and oxidizing temperature only has 100~300 DEG C, is used compared with the existing technology
High temperature oxidation process, equipment requirement is reduced using the method for the present invention, the consumption of the energy is reduced, while reducing and being produced into
This.
(3) the method for the present invention collects the oxidation of indium metal tin, the removing of oxidation product, refinement are completed in process, process is short,
Clean and effective, solve has kept oxidation reaction difficult in conventional oxidation process with the generation of indium oxide and tin oxide film carries out down
The shortcomings that going.
(4) present invention realizes indium tin Simultaneous Oxidation, and shortening indium oxide and tin oxide in prior art, powder processed produces respectively
The process of ultra-fine ito powder out.
Detailed description of the invention
Attached drawing 1 is the process flow diagram for the method that indium metal of the present invention and metallic tin prepare ultra-fine ITO powder.
Attached drawing 2 is the XRD diagram of 1 gained ito powder of the embodiment of the present invention.
Attached drawing 3 is the Δ G of metallic tin and indium oxidation reactionθT relationship figure.
Specific embodiment
To facilitate the understanding of the present invention, the present invention is made below in conjunction with Figure of description and preferred embodiment more complete
Face meticulously describes, but the protection scope of the present invention is not limited to the following specific embodiments.
Unless otherwise defined, all technical terms used hereinafter and the normally understood meaning of those skilled in the art
It is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, it is no intended to limit of the invention
Protection scope.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment 1
As in the indium metal ingot of raw material: In > 99.99%, total impurities < 0.01%；In metal tin slab: Sn >
99.99%, total impurities < 0.01%.
The present embodiment provides a kind of method that indium metal and metallic tin prepare ultra-fine ITO powder, process flow chart such as attached drawings 1
It is shown, the specific steps are as follows:
S1. indium metal ingot and metal tin slab 9.45:1 precise in mass ratio, nominal amount 1000g composition design: are taken；
S2. alloying fritting: load weighted indium metal ingot and metal tin slab carry out pre- in crucible at being 280 DEG C in temperature
It is molten, so that indium and tin is formed the alloy melt of uniform ingredients, and stir for several times；
S3. alloy molten: alloy melt obtained by step S2 is added in hot-bulb grinding machine, is 5 to be put into respective counts by ratio of grinding media to material
The zirconia ball of amount opens electric heating, ball mill inner cavity temperature is made to reach 200 DEG C；
S4. hot-bulb mill oxidation: opening rotating device, start hot ball-milling reaction, maintains revolving speed 100rpm, while from air inlet
Linear velocity into inner cavity with 0.5m/s blasts air, starts oxidation reaction and ball milling；Hot-bulb is ground in oxidation process, combustion chamber
Flue gas is discharged from the exhanst gas outlet of fuel chambers, reacts smoke filtration of the flue gas in inner cavity through being installed in reaction chamber and exports row
Out, filtering mouth is equipped with ceramic filter plate, and the material in ball mill can be prevented to be carried over；
S5. cooling discharging: stopping heating, ball milling and drum air, open discharge port and release product I TO powder after reaction 2h, from
Loading feed bin is put after being so cooled to greenhouse.
Oxygen content analysis test is carried out to product I TO composite powder, obtains indium tin oxidizability (In2O3+SnO2) > 96.9%,
It is between 0.40~8.4 μm that laser particle analyzer, which measures its particle size range, and average particle size is 4.33 μm, wherein -5.0 μm account for 76%.
Its XRD diagram is as shown in Fig. 2, as can be seen from the figure ITO composite powder diffraction peak intensity height, good crystallinity；Product purity is high, entirely
Portion is oxide indium and tin oxide.
Embodiment 2
Indium metal ingot and metal tin slab as raw material is the same as embodiment 1.
The present embodiment provides a kind of method that indium metal and metallic tin prepare ultra-fine ITO powder, process flow chart such as attached drawings 1
It is shown, the specific steps are as follows:
S1. indium metal ingot and metal tin slab 9.45:1 precise in mass ratio, nominal amount 1000g composition design: are taken；
S2. alloying fritting: load weighted indium metal ingot and metal tin slab carry out pre- in crucible at being 300 DEG C in temperature
It is molten, so that indium and tin is formed the alloy melt of uniform ingredients, and stir for several times；
S3. alloy molten: alloy melt obtained by step S2 is added in hot-bulb grinding machine, is 9 to be put into respective counts by ratio of grinding media to material
The corundum ball of amount opens electric heating, ball mill inner cavity temperature is made to reach 120 DEG C；
S4. hot-bulb mill oxidation: opening rotating device, start hot ball-milling reaction, maintains revolving speed 120rpm, while from air inlet
Linear velocity into inner cavity with 1.0m/s blasts air, starts oxidation reaction and ball milling；Hot-bulb is ground in oxidation process, combustion chamber
Flue gas is discharged from the exhanst gas outlet of fuel chambers, reacts smoke filtration of the flue gas in inner cavity through being installed in reaction chamber and exports row
Out, filtering mouth is equipped with ceramic filter plate, and the material in ball mill can be prevented to be carried over；
S5. cooling discharging: stopping heating, ball milling and drum air, open discharge port and release product I TO powder after reaction 1h, from
Loading feed bin is put after being so cooled to greenhouse.
Oxygen content analysis test is carried out to product I TO composite powder, obtains indium tin oxidizability (In2O3+SnO2) > 99.86%,
It is between 0.58~10.2 μm that laser particle analyzer, which measures its particle size range, and average particle size is 5.18 μm, wherein -5.0 μm account for 63%.
Embodiment 3
Indium metal ingot and metal tin slab as raw material is the same as embodiment 1.
The present embodiment provides a kind of method that indium metal and metallic tin prepare ultra-fine ITO powder, process flow chart such as attached drawings 1
It is shown, the specific steps are as follows:
S1. indium metal ingot and metal tin slab 9.45:1 precise in mass ratio, nominal amount 1000g composition design: are taken；
S2. alloying fritting: load weighted indium metal ingot and metal tin slab carry out pre- in crucible at being 250 DEG C in temperature
It is molten, so that indium and tin is formed the alloy melt of uniform ingredients, and stir for several times；
S3. alloy molten: alloy melt obtained by step S2 is added in hot-bulb grinding machine, is 3 to be put into respective counts by ratio of grinding media to material
The zirconia ball of amount opens electric heating, ball mill inner cavity temperature is made to reach 280 DEG C；
S4. hot-bulb mill oxidation: opening rotating device, start hot ball-milling reaction, maintains revolving speed 40rpm, while from air inlet
Linear velocity into inner cavity with 0.4m/s blasts air, starts oxidation reaction and ball milling；Hot-bulb is ground in oxidation process, combustion chamber
Flue gas is discharged from the exhanst gas outlet of fuel chambers, reacts smoke filtration of the flue gas in inner cavity through being installed in reaction chamber and exports row
Out, filtering mouth is equipped with ceramic filter plate, and the material in ball mill can be prevented to be carried over；
S5. cooling discharging: stopping heating, ball milling and drum air, open discharge port and release product I TO powder after reaction 3h, from
Loading feed bin is put after being so cooled to greenhouse.
Oxygen content analysis test is carried out to product I TO composite powder, obtains indium tin oxidizability (In2O3+SnO2) > 92.10%,
It is between 1.43~18.27 μm that laser particle analyzer, which measures its particle size range, and average particle size is 8.06 μm, wherein -5.0 μm account for
34%.
Embodiment 4
Indium metal ingot and metal tin slab as raw material is the same as embodiment 1.
The present embodiment provides a kind of method that indium metal and metallic tin prepare ultra-fine ITO powder, process flow chart such as attached drawings 1
It is shown, the specific steps are as follows:
S1. indium metal ingot and metal tin slab 9.45:1 precise in mass ratio, nominal amount 1000g composition design: are taken；
S2. alloying fritting: load weighted indium metal ingot and metal tin slab carry out pre- in crucible at being 270 DEG C in temperature
It is molten, so that indium and tin is formed the alloy melt of uniform ingredients, and stir for several times；
S3. alloy molten: alloy melt obtained by step S2 is added in hot-bulb grinding machine, is 7 to be put into respective counts by ratio of grinding media to material
The agate ball of amount opens electric heating, ball mill inner cavity temperature is made to reach 250 DEG C；
S4. hot-bulb mill oxidation: opening rotating device, start hot ball-milling reaction, maintains revolving speed 120rpm, while from air inlet
Linear velocity into inner cavity with 1.0m/s blasts air, starts oxidation reaction and ball milling；Hot-bulb is ground in oxidation process, combustion chamber
Flue gas is discharged from the exhanst gas outlet of fuel chambers, reacts smoke filtration of the flue gas in inner cavity through being installed in reaction chamber and exports row
Out, filtering mouth is equipped with ceramic filter plate, and the material in ball mill can be prevented to be carried over；
S5. cooling discharging: stopping heating, ball milling and drum air, open discharge port and release product I TO powder after reaction 2h, from
Loading feed bin is put after being so cooled to greenhouse.
Oxygen content analysis test is carried out to product I TO composite powder, obtains indium tin oxidizability (In2O3+SnO2) > 99.80%,
It is between 0.02~4.6 μm that laser particle analyzer, which measures its particle size range, and average particle size is 1.37 μm, wherein -5.0 μm account for 100%.
Embodiment 5
Indium metal ingot and metal tin slab as raw material is the same as embodiment 1.
The present embodiment provides a kind of method that indium metal and metallic tin prepare ultra-fine ITO powder, process flow chart such as attached drawings 1
It is shown, the specific steps are as follows:
S1. indium metal ingot and metal tin slab 9.45:1 precise in mass ratio, nominal amount 5000g composition design: are taken；
S2. alloying fritting: load weighted indium metal ingot and metal tin slab carry out pre- in crucible at being 300 DEG C in temperature
It is molten, so that indium and tin is formed the alloy melt of uniform ingredients, and stir for several times；
S3. alloy molten: alloy melt obtained by step S2 is added in hot-bulb grinding machine, is 7 to be put into respective counts by ratio of grinding media to material
The zirconia ball of amount opens electric heating, ball mill inner cavity temperature is made to reach 220 DEG C；
S4. hot-bulb mill oxidation: opening rotating device, start hot ball-milling reaction, maintains revolving speed 90rpm, while from air inlet
Linear velocity into inner cavity with 0.7m/s blasts air, starts oxidation reaction and ball milling；Hot-bulb is ground in oxidation process, combustion chamber
Flue gas is discharged from the exhanst gas outlet of fuel chambers, reacts smoke filtration of the flue gas in inner cavity through being installed in reaction chamber and exports row
Out, filtering mouth is equipped with ceramic filter plate, and the material in ball mill can be prevented to be carried over；
S5. cooling discharging: stopping heating, ball milling and drum air, open discharge port and release product I TO powder after reaction 2.5h,
Loading feed bin is put after naturally cooling to greenhouse.
Oxygen content analysis test is carried out to product I TO composite powder, obtains indium tin oxidizability (In2O3+SnO2) > 99.20%,
It is between 0.35~9.42 μm that laser particle analyzer, which measures its particle size range, and average particle size is 4.72 μm, wherein -5.0 μm account for 69%.
Claims (10)
1. a kind of method that indium metal and metallic tin prepare ultra-fine ITO powder, which is characterized in that be with indium metal ingot and metal tin slab
Raw material first carries out composition design and alloying fritting, in 100~300 DEG C of temperature and is passed through oxidizing gas in hot-bulb grinding machine
Under conditions of carry out hot-bulb mill oxidation, be oxidized indium metal and the metallic tin form of being in a liquid state, while carrying out ball milling, hot-bulb grind oxygen
Ultra-fine ITO powder is obtained after the completion of changing.
2. the method that indium metal and metallic tin prepare ultra-fine ITO powder according to claim 1, which is characterized in that the group
It is 9.45:1 at the mass ratio of indium metal ingot and metal tin slab in design.
3. the method that indium metal and metallic tin prepare ultra-fine ITO powder according to claim 1, which is characterized in that the conjunction
The temperature of aurification fritting is 250~300 DEG C.
4. the method that indium metal and metallic tin prepare ultra-fine ITO powder according to claim 1, which is characterized in that the oxidation
Property gas be air or oxygen.
5. the method that indium metal and metallic tin prepare ultra-fine ITO powder according to claim 1, which is characterized in that the oxidation
Property atmosphere blast linear velocity be 0.1~2m/s, preferably 0.5~1.5m/s.
6. the method that indium metal and metallic tin prepare ultra-fine ITO powder according to claim 1, which is characterized in that the heat
Milling intensity is 30~120rpm in mechanical milling process, and filling rate is 10~50%, and ratio of grinding media to material is 3~9.
7. the method that indium metal and metallic tin prepare ultra-fine ITO powder according to claim 6, which is characterized in that the filling
Rate is 20~40%, and ratio of grinding media to material is 5~8.
8. the method that indium metal and metallic tin prepare ultra-fine ITO powder according to claim 1, which is characterized in that the ball milling
Ball material medium used is one of zirconia ball, corundum ball and agate ball；Preferably zirconium oxide.
9. the method that indium metal and metallic tin prepare ultra-fine ITO powder according to claim 1, which is characterized in that the heat
The time of ball-milling reaction process is 1~5h, preferably 1~3h.
10. the method that any one indium metal and metallic tin prepare ultra-fine ITO powder, feature exist according to claim 1~9
In, specifically includes the following steps:
S1. composition design: take indium metal ingot and metal tin slab in certain mass ratio precise；
S2. alloying fritting: load weighted indium metal ingot and metal tin slab carry out fritting at being 250~300 DEG C in temperature, make indium
The alloy melt of uniform ingredients is formed with tin；
S3. alloy molten: alloy melt obtained by step S2 is added in hot-bulb grinding machine, is opened electric heating, is made ball mill inner cavity temperature
Reach 100~300 DEG C；
S4. hot-bulb mill oxidation: rotating device is opened, starts hot ball-milling reaction, maintains certain revolving speed, while inside from air inlet
Oxidizing gas is blasted in chamber, starts oxidation reaction and ball milling；
S5. cooling discharging: reaction stops heating, ball milling and drum oxidizing gas after a certain period of time, opens discharge port and releases product
ITO powder, puts loading feed bin after being completely cooled down to greenhouse, and classification obtains varigrained ito powder.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114702311A (en) * | 2022-04-20 | 2022-07-05 | 江苏迪丞光电材料有限公司 | TZO ceramic target preparation method and processing device |
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| JPS6018737B2 (en) * | 1979-04-06 | 1985-05-11 | 松下電器産業株式会社 | electrical contact materials |
| CN103590072A (en) * | 2013-10-17 | 2014-02-19 | 清远先导材料有限公司 | Preparation method of high-purity indium |
| CN104496473A (en) * | 2014-12-30 | 2015-04-08 | 山东昊轩电子陶瓷材料有限公司 | Production method of high-density conductive niobium oxide target |
| CN107794389A (en) * | 2017-10-20 | 2018-03-13 | 温州宏丰电工合金股份有限公司 | A kind of silver-tin oxide or indium oxide contact material and preparation method thereof |
| CN108002428A (en) * | 2017-11-29 | 2018-05-08 | 株洲冶炼集团股份有限公司 | It is a kind of that the preparation method with ITO particles and the ITO particles by this method preparation is deposited |
| CN108557770A (en) * | 2018-06-21 | 2018-09-21 | 常熟理工学院 | A method of preparing nanometer metal oxide powder |
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| CN114702311A (en) * | 2022-04-20 | 2022-07-05 | 江苏迪丞光电材料有限公司 | TZO ceramic target preparation method and processing device |
| CN114702311B (en) * | 2022-04-20 | 2023-01-17 | 江苏迪丞光电材料有限公司 | TZO ceramic target preparation method and processing device |
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