CN108002428A - It is a kind of that the preparation method with ITO particles and the ITO particles by this method preparation is deposited - Google Patents
It is a kind of that the preparation method with ITO particles and the ITO particles by this method preparation is deposited Download PDFInfo
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
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Abstract
The present invention provides a kind of preparation method being deposited with ITO particles, this method, which is included in non-pressure sintering furnace, carries out following steps：(1) by ITO base substrates in oxygen flowing environment, 180 240 DEG C are heated to the heating rate of 10~100 DEG C/h, then 400 600 DEG C are heated to the heating rate of 10~30 DEG C/h, 1~4h is kept the temperature after heating；(2) in oxygen flowing environment, 1300~1500 DEG C is heated to the heating rate of 100~200 DEG C/h and is carried out without pressure oxygen sintering, sintering time is 1~10h.The preparation method of the present invention, simplifies powder and prepares control condition, be conducive to individually control powder quality, and simplifies shaping, degreasing sintered technique, still belongs to first in ITO preparation method of granules at home.Present invention also offers a kind of ITO particles, which meets the technical requirement of vacuum vapour deposition, and even structure is not easy to crack.
Description
Technical field
The invention belongs to technical field of semiconductor material preparation, more particularly to for vapour deposition method to prepare electrically conducting transparent thin for one kind
The preparation method of the ITO particles of film and the ITO particles prepared by this method.
Background technology
The method of production transparent conductive film material has many kinds now, and wherein magnetron sputtering method is to apply most sides
Method.Magnetron sputtering method is mainly used in the manufacture of LCD and solar battery film material.Because in the production technology mistake of semiconductor
Cheng Zhong, can cause destruction to semiconductor surface than more serious, so preparing two pole of semiconductor light emitting using magnetron sputtering method
It is general to use when managing the transparent conductive film of (LED), Organic Light Emitting Diode (OLED), macromolecular LED diode (PLED)
The method of vacuum vapor plating.
Vacuum vapor plating, i.e., by heating evaporation, certain material makes it in the method for surface of solids deposition film forming.Earliest
Itd is proposed by M. faraday in 1857, be one of common coating technique now.Transparent lead is prepared using the method for vacuum evaporation
Conductive film, technique is relatively simple, and the film being prepared has is influenced higher excellent of smaller, film transmitance by sedimentary condition
Point.Nineteen ninety-five Y.H.Aliyu et al. has been reported to be sunk with the method for thermal evaporation deposition on AIGaInP epitaxial layers prepared by MOCVD
Product indium tin oxide (ITO) does the structure of current extending.
Indium tin oxide ITO is widely used in the transparency electrode field of photoelectric device.This is because indium tin oxide ITO
With high conductivity and visible light transmissivity, compared with other transparent conductive films, ito thin film also has good chemical stabilization
Property, heat endurance, there is good adhesion and good showing methods characteristic to substrate, be the ideal for making transparency electrode
Material.
At present semiconductor LED with its high electric light transformation efficiency, long lifespan, it is environmentally protective the advantages that, become the new of 2l centuries
Generation lighting source.Ito thin film in LED is mainly prepared using the method for electron beam heating, vacuum evaporation, that is, utilizes high energy electricity
Beamlet bombardment indium, tin-oxide mixed material surface, make its distillation, then deposit to the cold and ito film is formed on substrate.This side
Method needs the technological parameter that strictly controls less, and operation and control film growth are relatively easy, and the film of preparation will not produce very much
Uncontrollable impurity, the growth rate of film can be controlled strictly, can be adapted to large-scale industrial production.With the day of semiconductor technology
Become ripe, LED component is developed constantly to be developed to efficient and high brightness direction, and market application is more and more wider, to ITO evaporating particles
Demand is also more and more.Vacuum evaporation at the same time prepares ito thin film and also can be widely used to OLED (organic light emitting diode), PLED
(macromolecular LED diode) etc. field.
At present, the preparation method of ITO evaporating particles for normal pressure-sintered method and has pressure sintering process.The former uses common electrical heating
The high temperature sintering furnace of oxidizing gas can be led to, equipment is simple, but atmospheric oxygen content is unable to control or detected in sintering process, right
The product quality (such as oxygen loss rate) of ITO evaporating particles can not ensure that equipment controllable precision is poor；In addition normal pressure-sintered stove burner hearth
Larger, throughput is smaller, and in-furnace temperature differs greatly, and the density and microstructure (such as crystallite dimension) on ITO particles influence
It is larger, therefore common mass production of the normal pressure-sintered method to ITO particles brings hidden danger of quality.The latter can solve partial pressure of oxygen and ask
Topic, can also solve the problems, such as temperature uniformity, but be that sintering furnace carries pressure the problem of maximum, constitute a latent danger to production safety；
In addition it is big compared with normal pressure-sintered stove in terms of equipment investment, it is unfavorable for controlling production cost.Therefore, there is an urgent need for a kind of technique of research and design
Simply, securely and reliably, can ensure the evaporation preparation method of ITO particles of product quality.
The content of the invention
The technical problems to be solved by the invention are to overcome the shortcomings of to mention in background above technology and defect, there is provided one
Preparation method of the kind evaporation with ITO particles and the ITO particles by this method preparation.
To achieve the object of the present invention, the technical scheme is that：
A kind of preparation method being deposited with ITO particles, is included in non-pressure sintering furnace and carries out following steps：(1) by ITO bases
Body is heated to 180-240 DEG C, then the liter with 10~30 DEG C/h in oxygen flowing environment, with the heating rate of 10~100 DEG C/h
Warm speed is heated to 400-600 DEG C, and 1~4h is kept the temperature after heating；(2) in oxygen flowing environment, with 100~200 DEG C/h
Heating rate be heated to 1300~1500 DEG C carry out without pressure oxygen sintering, sintering time is 1~10h, obtains ITO particles.
The preparation method of the present invention, used pressureless sintering processing refers to, using with oxygen content monitor and pressure
The big flow atmosphere sintering furnace of power sensing detection table is sintered, and pressure gauge is shown as " 0 " during sintering.The process of step (1) is
Ungrease treatment process, 100 DEG C/h is not to be exceeded in order to which organic additive is removed clean and prevention particle fracture, heating rate,
Organic additive starts to decompose after 240 DEG C, can be removed completely substantially after 400 DEG C totally, therefore need to will heat up speed
Rate and soaking time control are within the scope of the invention.The process of step (2) is without pressure oxygen sintering processes process, due to having
Machine additive has removed totally, to prevent the ITO blank crackings after degreasing, makes base substrate center portion consistent with Outer shrink speed,
At the same time in view of powder sintering activity and the energy conservation and environmental protection of production process, speed and soaking time control need to be will heat up in this hair
In bright scope.
The preparation method of the present invention, carries out ungrease treatment, it is possible to reduce the consumption of gas, makes organic add under oxygen atmosphere
Agent is added more fully to decompose and react, ITO base substrate holes increase after avoiding degreasing, avoid in air access holes gap and quilt
Absorb, the nitrogen atom for causing since ITO particles belong to oxide in the air of absorption to contain in sintering lacks effective
Diffusion admittance, sintering when be difficult to eliminate, so as to can cause nitrogen impurity exceeded in vacuum coating.Also, the system of the present invention
Preparation Method, is degreasing to be carried out in same sintering furnace and without pressure oxygen sintering, further avoid in air access holes gap simultaneously
Absorbed the defects of caused.
The preparation method of above-mentioned evaporation ITO particles, it is preferred that in the step (1), with the liter of 60~100 DEG C/h
Warm speed is heated to 200-220 DEG C, then is heated to 500-600 DEG C with the heating rate of 10~30 DEG C/h, and 1 is kept the temperature after heating
~2h.
The preparation method of above-mentioned evaporation ITO particles, it is preferred that in the non-pressure sintering furnace oxygen flow for 5~
50L/min.Oxygen flux control within the scope of the invention, can further prevent base substrate from being opened in degreasing or sintering process
Split.
The preparation method of above-mentioned evaporation ITO particles, it is preferred that the ITO base substrates are by by In2O3Powder, SnO2
After slurry is made in powder mixing addition water and dispersant, successively after ball milling mixing, mist projection granulating, metal die are compressing
It is prepared.
In using the present invention2O3Powder and SnO2The mode of powder mixing prepares ITO base substrates, on the one hand can be very convenient
Ground adjustment indium, the component ratio of tin, avoid preparing the ITO particulate component ratios produced in ITO powder process using coprecipitation
Fluctuation is big, so that the problem of reducing evaporation ito thin film electrical property；On the other hand, In (OH) can be overcome3With Sn (OH)4Two kinds of hydrogen
The problem of oxide acid-base value required in precipitation reaction differs greatly；By preparing In respectively2O3Powder and SnO2Powder
Body, can individually control the grain growth of powder, base substrate particle size range needed for conveniently regulating and controlling production, it is good to obtain suitable sintering activity
Base substrate.
The preparation method of above-mentioned evaporation ITO particles, it is preferred that the In2O3The BET specific surface area of powder is 4m2/g
~40m2/ g, average grain diameter are 20~200nm；The SnO2The BET specific surface area of powder is 2m2/ g~20m2/ g, average grain diameter
For 40~400nm.Principal component due to preparing ITO particles is In2O3Powder and SnO2Powder, In2O3The sintering activity of powder is determined
Determine the sintering temperature of particle, and SnO2The addition of powder may insure the density after ITO particles sintering, therefore need to be by In2O3Powder
And SnO2BET specific surface area and the average grain diameter control of powder are within the scope of the invention.
The preparation method of above-mentioned evaporation ITO particles, it is preferred that the In2O3The BET specific surface area of powder is 12m2/
G~14m2/ g, the SnO2The BET specific surface area of powder is 10m2/ g~12m2/g。
The preparation method of above-mentioned evaporation ITO particles, it is preferred that the In2O3Powder and SnO2The mass ratio of powder is
(85~98)：(15~2), the solid content of the slurry is 30~75wt%, and ZrO is used in the mechanical milling process2Ball is used as and grinds
Grinding media carries out ball milling mixing, controls slurry and ZrO2The mass ratio of ball is 1:(1~5), 10~100 turns/min of rotational speed of ball-mill,
1~20h of milling time.In order to make In2O3Powder and SnO2Powder can be uniformly mixed, while ensure ZrO2The service life of ball,
Avoid causing the Zr contents of ITO particles exceeded, need to be by the process regulation of ball-milling treatment within the scope of the invention.
The preparation method of above-mentioned evaporation ITO particles, it is preferred that ITO base substrates are carried out using punching block or sintered carbide die
It is compressing, mould diameter is 8~34mm, and briquetting pressure is 10~30MPa, and the dwell time is 0.5~2min.Due to vacuum
Filming equipment there are certain requirements the size of ITO particles, and due to ITO particles, in sintering, shrinking percentage is 11~13%, is needed
By mould diameter and the process regulation of compression process within the scope of the invention, it just can guarantee that to obtain a diameter of 7~
The ITO target of 30mm.
The preparation method of above-mentioned evaporation ITO particles, it is preferred that the dispersant is the aqueous solution of polyacrylate,
Its mass fraction is 10~80wt%；The mist projection granulating is granulated for atomizer or injecting type spraying, the mist projection granulating
During need add binding agent, the binding agent be polyvinyl alcohol aqueous solution, its mass fraction is 2~20wt%.Through spraying
After granulation, powder granule is smooth, spherical, and the particle diameter of powder spheric granules is 15~105 μm, wherein 30~70 μm of contents exist
More than 60%.
The inventive concept total as one, the present invention also provides a kind of ITO being prepared according to above-mentioned preparation method
Particle, the ITO particles have indium oxide phase structure, and tin is solid-solubilized in indium oxide lattice completely, the crystal grain of the ITO particles
Size is 5 μm~15 μm, wherein 5 μm~10 μm of particle accounts for more than 80%, relative density is 55~65%, purity for 99% with
On.
Compared with prior art, the advantage of the invention is that：
The method of the present invention, is different from traditional preparation methods, in same equipment, using degreasing sintered integration side
Formula, make ITO base substrates after degreasing need not movement can directly heat up sintering, avoid the ITO base substrates after degreasing in moving process
In cause to damage, occur sintering cracking, lack corner phenomena such as.Using without pressure oxygen sintering, also it is different from common normal pressure or has
Pressure sintering, requirement of the pressureless sintering to equipment is relatively low, can effectively control ITO oxide particles to decompose, and controls oxygen loss rate, stablizes control
Make pellet relative density, the technical indicator such as crystallite dimension, and can complete monitoring in production process, it is ensured that ITO particle manufacture quality
Stability.
In general, the ITO preparation method of granules in the present invention, simplifies powder and prepares control condition, be conducive to individually
Powder quality is controlled, and simplifies shaping, degreasing sintered technique, still belongs in ITO preparation method of granules at home first, fits
For industrialized production.And the ITO particles being prepared by the method for the present invention, the technical indicator for meeting vacuum vapour deposition will
Ask, even structure is not easy to crack.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is attached drawing needed in technology description to be briefly described, it should be apparent that, drawings in the following description are the present invention
Some embodiments, for those of ordinary skill in the art, without creative efforts, can also basis
These attached drawings obtain other attached drawings.
Fig. 1 is that process flow chart of the evaporation with ITO particles is prepared in the embodiment of the present invention 1；
Fig. 2 is the shape appearance figure of the evaporation ITO powder granules prepared in the embodiment of the present invention 1；
Fig. 3 is the phase structure XRD diagram of the evaporation ITO particles prepared in the embodiment of the present invention 1；
Fig. 4 is profile scanning Electronic Speculum (SEM) figure of the evaporation ITO particles prepared in the embodiment of the present invention 1.
Embodiment
For the ease of understanding the present invention, below in conjunction with Figure of description and preferred embodiment to invent herein do it is more complete
Face, meticulously describe, but protection scope of the present invention is not limited to specific examples below.
Unless otherwise defined, all technical terms used hereinafter are generally understood that implication phase with those skilled in the art
Together.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention's
Protection domain.
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.
The distribution of ITO powder granularities uses 3000 Analyzer testing results of Mastersizer, the crystalline substance of ITO particles in the present invention
Granularity is detected using scanning electron microscope, and phase structure is detected using X-ray diffractometer, and size uses miking.
Comparative example 1：
Weigh 9500 grams of In2O3Powder, 500 grams of SnO2Powder, 3586 grams of pure water and 200 grams of dispersants are fitted into ball mill,
It is 1 by the mass ratio of slurry and ball:2 load ZrO2Ball, rolls rotating speed 50 turns/min, Ball-milling Time 12h；Add 600 grams of bondings
Mist projection granulating is carried out after agent stirring 60min；ITO powders are fitted into the punching block or sintered carbide die of a diameter of 27.5mm,
Pressurize 1min is pressed into disc-shaped ITO base substrates under the pressure of 25MPa；Be fitted into without pressure oxygen atmosphere sintering stove in first with the liter of 60 DEG C/h
Warm speed is heated to 600 DEG C of progress dumpings, and 1h, oxygen flow 20L/min are kept the temperature after heating；Again with the liter of 200 DEG C/h
Warm speed is heated to 1500 DEG C and carries out without pressure oxygen sintering, sintering time 5h, oxygen flow 20L/min；Finally obtain
ITO particle fractures, color is dark green, and relative density 74.7% is obtained by size method.Detected by XRD, phase structure is oxidation
Indium phase structure, section SEM show 5~15 μm of crystallite dimension.
Comparative example 2：
The preparation of ITO base substrates with comparative example 1, by ITO base substrates be fitted into without in pressure oxygen atmosphere sintering stove first with the liter of 60 DEG C/h
Warm speed is heated to 400 DEG C, then is heated to 600 DEG C of insulations 1h, oxygen flow 20L/min with the heating rate of 30 DEG C/h；So
1450 DEG C of insulations 5h, oxygen flow 20L/min are heated to the heating rate of 200 DEG C/h afterwards；The ITO particles finally obtained are opened
Split, color obtains relative density 63.5% in green by size method.Being detected by XRD, phase structure is indium oxide phase structure,
Section SEM shows 5~15 μm of crystallite dimension.
Embodiment 1：
According to technological process as shown in Figure 1,9500 grams of In are weighed2O3Powder (average grain diameter 65nm, BET 12.80m2/
G), 500 grams of SnO2Powder (average grain diameter 70nm, BET 12.50m2/ g), make after 3586 grams of pure water and 200 grams of dispersants
Slurry is obtained, dispersant is the aqueous solution of polyacrylate, its mass fraction is 40wt%；Slurry is fitted into ball mill, by material
The mass ratio of slurry and ball is 1:2 load ZrO2Ball, rolls rotating speed 50 turns/min, Ball-milling Time 12h；600 grams of binding agents are added to stir
Mist projection granulating is carried out after mixing 60min, binding agent is the aqueous solution of polyvinyl alcohol, its mass fraction is 10wt%；ITO powders are filled
In the punching block or sintered carbide die that enter a diameter of 27.5mm, pressurize 1min is pressed into disc-shaped ITO bases under the pressure of 25MPa
Body；ITO base substrates are fitted into without in pressure oxygen atmosphere sintering stove, are first heated to 200 DEG C with the heating rate of 60 DEG C/h, then with 30 DEG C/h
Heating rate be heated to 600 DEG C, keep the temperature 1h, oxygen flow 20L/min；Then it is heated to the heating rate of 120 DEG C/h
1430 DEG C carry out without pressure oxygen sintering, and sintering time 5h, oxygen flow 20L/min, obtains ITO particles；The ITO particles are complete
It is good, there is appearance structure as shown in Figure 2, color is in light green color, purity 99.99%, and relative density is obtained by size method
60.8%；The phase structure XRD diagram of the ITO particles is as shown in figure 3, as seen from the figure, its phase structure is indium oxide phase structure；Should
Profile scanning Electronic Speculum (SEM) figure of ITO particles is as shown in figure 4, as seen from the figure, its crystallite dimension is 5~10 μm.
Embodiment 2：
ITO base substrates are fitted into without pressing in oxygen atmosphere sintering stove, first with 100 DEG C/h's by the preparation of ITO base substrates with embodiment 1
Heating rate is heated to 200 DEG C, then is heated to 600 DEG C of insulations 1h, oxygen flow 50L/min with the heating rate of 30 DEG C/h；
Then it is heated to 1400 DEG C with the heating rate of 200 DEG C/h sinter without pressure oxygen, sintering time 5h, oxygen flow is
50L/min；The ITO particles finally obtained are intact, and color is in light green color, and purity 99.99%, relative density is obtained by size method
55.8%.Detected by XRD, phase structure is indium oxide phase structure, and section SEM shows 5~10 μm of crystallite dimension.
Embodiment 3：
Weigh 9800 grams of In2O3Powder (average grain diameter 60nm, BET 13.60m2/ g), 200 grams of SnO2Powder (average grain
Footpath 85nm, BET 10.35m2/ g), 3586 grams of pure water and 200 grams of dispersants be fitted into ball mill, by the ball milling in embodiment 1
ITO base substrates are made in mixing, granulation, forming method, and ITO base substrates are fitted into without pressing in oxygen atmosphere sintering stove, by de- in embodiment 1
Fat sintering method is sintered.Obtained ITO particles are intact, and color is in light green color, and purity 99.99%, phase is obtained by size method
To density 61.7%.Detected by XRD, phase structure is indium oxide phase structure, and section SEM shows 5~8 μm of crystallite dimension.
Embodiment 4：
Weigh 9000 grams of In2O3Powder (average grain diameter 67nm, BET 12.54m2/ g), 1000 grams of SnO2Powder (average grain
Footpath 70nm, BET 12.48m2/ g), 3586 grams of pure water and 200 grams of dispersants be fitted into ball mill, by the ball milling in embodiment 1
ITO base substrates are made in mixing, granulation, forming method, are fitted into without pressing in oxygen atmosphere sintering stove, by the degreasing sintered side in embodiment 1
Method is sintered.Obtained ITO particles are intact, and color is in light green color, and purity 99.99%, relative density is obtained by size method
62.3%.Detected by XRD, phase structure is indium oxide phase structure, and section SEM shows 5~10 μm of crystallite dimension.
Embodiment 5：
Weigh 8500 grams of In2O3Powder (average grain diameter 65nm, BET 12.60m2/ g), 1500 grams of SnO2Powder (average grain
Footpath 82nm, BET 10.60m2/ g), 3586 grams of pure water and 200 grams of dispersants be fitted into ball mill, by the ball milling in embodiment 1
Mixing, be granulated, forming method ITO base substrates are made, be fitted into without pressure oxygen atmosphere sintering stove in by the degreasing sintered method in embodiment 1
It is sintered.Obtained ITO particles are intact, and color is in light green color, and purity 99.99%, relative density is obtained by size method
58.2%.Detected by XRD, phase structure is indium oxide phase structure, and section SEM shows 5~10 μm of crystallite dimension.
The performance indicator contrast for the ITO particles being prepared in above-mentioned comparative example 1~2 and embodiment 1~5 is as shown in table 1,
As shown in Table 1, the even structure for the ITO particles that preparation method of the invention is prepared, it is not easy to crack, meet vacuum vapour deposition
Technical requirement.
The performance indicator contrast for the ITO particles being prepared in 1 comparative example 1~2 of table and embodiment 1~5
Claims (10)
1. a kind of preparation method being deposited with ITO particles, it is characterised in that be included in non-pressure sintering furnace and carry out following steps：
(1) by ITO base substrates in oxygen flowing environment, 180-240 DEG C is heated to the heating rate of 10~100 DEG C/h, then with 10~
The heating rate of 30 DEG C/h is heated to 400-600 DEG C, and 1~4h is kept the temperature after heating；(2) in oxygen flowing environment, with 100
The heating rate of~200 DEG C/h is heated to 1300~1500 DEG C and carries out without pressure oxygen sintering, and sintering time is 1~10h, is obtained
ITO particles.
2. the preparation method of evaporation ITO particles according to claim 1, it is characterised in that in the step (1), with
The heating rate of 60~100 DEG C/h is heated to 200-220 DEG C, then is heated to 500-600 DEG C with the heating rate of 10~30 DEG C/h,
1~2h is kept the temperature after heating.
3. the preparation method of evaporation ITO particles according to claim 1, it is characterised in that in the non-pressure sintering furnace
Oxygen flow is 5~50L/min.
4. the preparation method of evaporation ITO particles according to claim 1, it is characterised in that the ITO base substrates are to pass through
By In2O3Powder, SnO2After slurry is made in powder mixing addition water and dispersant, successively by ball milling mixing, mist projection granulating, gold
It is prepared after category mould is compressing.
5. the preparation method of evaporation ITO particles according to claim 4, it is characterised in that the In2O3The BET of powder
Specific surface area is 4m2/ g~40m2/ g, average grain diameter are 20~200nm；The SnO2The BET specific surface area of powder is 2m2/ g~
20m2/ g, average grain diameter are 40~400nm.
6. the preparation method of evaporation ITO particles according to claim 5, it is characterised in that the In2O3The BET of powder
Specific surface area is 12m2/ g~14m2/ g, the SnO2The BET specific surface area of powder is 10m2/ g~12m2/g。
7. the preparation method of evaporation ITO particles according to claim 4, it is characterised in that the In2O3Powder with
SnO2The mass ratio of powder is (85~98)：(15~2), the solid content of the slurry are 30~75wt%, the mechanical milling process
It is middle to use ZrO2Ball carries out ball milling mixing as abrasive media, controls slurry and ZrO2The mass ratio of ball is 1:(1~5), ball milling turn
Speed 10~100 turns/min, 1~20h of milling time.
8. the preparation method of evaporation ITO particles according to claim 4, it is characterised in that closed using punching block or hard
Jin Mo carries out the compressing of ITO base substrates, and mould diameter is 8~34mm, and briquetting pressure is 10~30MPa, the dwell time 0.5
~2min.
9. the preparation method of evaporation ITO particles according to claim 4, it is characterised in that the dispersant is poly- third
The aqueous solution of olefin(e) acid ester, its mass fraction are 10~80wt%；Need to add binding agent, the bonding during the mist projection granulating
Agent is the aqueous solution of polyvinyl alcohol, its mass fraction is 2~20wt%.
ITO that 10. the evaporation according to any one in claim 1~9 is prepared with the preparation method of ITO particles
Grain, it is characterised in that the ITO particles have indium oxide phase structure, and tin is solid-solubilized in indium oxide lattice completely, the ITO
The crystallite dimension of particle is 5 μm~15 μm, wherein 5 μm~10 μm of particle accounts for more than 80%, relative density is 55~65%, pure
Spend for more than 99%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711228577.8A CN108002428B (en) | 2017-11-29 | 2017-11-29 | Preparation method of ITO (indium tin oxide) particles for evaporation and ITO particles prepared by method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711228577.8A CN108002428B (en) | 2017-11-29 | 2017-11-29 | Preparation method of ITO (indium tin oxide) particles for evaporation and ITO particles prepared by method |
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| CN108002428A true CN108002428A (en) | 2018-05-08 |
| CN108002428B CN108002428B (en) | 2020-06-09 |
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| CN108516820A (en) * | 2018-07-04 | 2018-09-11 | 郑州大学 | A kind of short route sintering process of tin indium oxide target material |
| CN108947520A (en) * | 2018-06-26 | 2018-12-07 | 株洲冶炼集团股份有限公司 | A kind of preparation method of ITO sintering target |
| CN109231259A (en) * | 2018-10-09 | 2019-01-18 | 湖南工业大学 | A kind of method that indium metal and metallic tin prepare ultra-fine ITO powder |
| CN111606704A (en) * | 2020-06-03 | 2020-09-01 | 福建阿石创新材料股份有限公司 | ITO evaporation material and preparation method thereof |
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| CN102167597A (en) * | 2010-12-20 | 2011-08-31 | 昆明理工大学 | Method of preparing ITO target material by oxygen atmosphere pressureless sintering process |
| CN102731067A (en) * | 2012-07-04 | 2012-10-17 | 韶关西格玛技术有限公司 | Preparation method of high-density ITO (indium tin oxide) evaporation target |
| CN106966700A (en) * | 2017-03-09 | 2017-07-21 | 郑州大学 | A kind of short route preparation technology of tin indium oxide sintered body |
| CN107010940A (en) * | 2017-04-07 | 2017-08-04 | 中国船舶重工集团公司第七二五研究所 | A kind of control oxygen content prepares methods of the TFT LCD with ITO sputtering targets |
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| CN102167597A (en) * | 2010-12-20 | 2011-08-31 | 昆明理工大学 | Method of preparing ITO target material by oxygen atmosphere pressureless sintering process |
| CN102731067A (en) * | 2012-07-04 | 2012-10-17 | 韶关西格玛技术有限公司 | Preparation method of high-density ITO (indium tin oxide) evaporation target |
| CN106966700A (en) * | 2017-03-09 | 2017-07-21 | 郑州大学 | A kind of short route preparation technology of tin indium oxide sintered body |
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| CN108947520A (en) * | 2018-06-26 | 2018-12-07 | 株洲冶炼集团股份有限公司 | A kind of preparation method of ITO sintering target |
| CN108947520B (en) * | 2018-06-26 | 2021-06-11 | 株洲冶炼集团股份有限公司 | Preparation method of ITO (indium tin oxide) sintered target material |
| CN108516820A (en) * | 2018-07-04 | 2018-09-11 | 郑州大学 | A kind of short route sintering process of tin indium oxide target material |
| CN109231259A (en) * | 2018-10-09 | 2019-01-18 | 湖南工业大学 | A kind of method that indium metal and metallic tin prepare ultra-fine ITO powder |
| CN109231259B (en) * | 2018-10-09 | 2020-11-13 | 湖南工业大学 | Method for preparing ultrafine ITO powder from metal indium and metal tin |
| CN111606704A (en) * | 2020-06-03 | 2020-09-01 | 福建阿石创新材料股份有限公司 | ITO evaporation material and preparation method thereof |
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| CN108002428B (en) | 2020-06-09 |
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