CN107352996A - A kind of preparation method of tin antimony oxide ceramic sputtering target material - Google Patents
A kind of preparation method of tin antimony oxide ceramic sputtering target material Download PDFInfo
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Abstract
The invention provides a kind of preparation method of tin antimony oxide ceramic sputtering target material, preparation method processing step provided by the present invention is easy, and using the method for gel casting forming, shaping can be stood in atmospheric conditions, the preparation tin antimony oxide ceramic sputtering target material suitable for industrially scalable.Meanwhile the tin-antiomony oxide film layer that the tin antimony oxide ceramic sputtering target material as made from the inventive method is prepared through magnetron sputtering membrane process has the advantages that visible light transmissivity is high, film layer resistance is high, is adapted as photoelectric device substrate applications.
Description
Technical field
The present invention relates to field of photoelectric devices, in particular to a kind of tin-antiomony oxide (hereinafter referred to as：ATO) ceramics splash
Shoot at the target the preparation method of material.
Background technology
With the rapid development of semiconductor, FPD and opto-electronics, transparent conductive oxide film is as the sector
Basic material have been obtained for being widely applied, and there is vast potential for future development.Transparent conductive oxide
(Transparent conductive oxide, abbreviation TCO) film because simultaneously have concurrently good electric conductivity (<10-3Ω.CM)
With high visible light transmissivity (＞ 80%), thus solar cell is widely used in, flat-panel display device, feature window applies
In the field of photoelectric devices such as layer.At present, the TCO films of most study mainly have three major controls：In2O3 bases, zno-based and SnO2 bases.
Wherein, it is most representative with ITO (Sn is adulterated in In2O3), AZO (Al is adulterated in ZnO), and ATO (Sb is adulterated in SnO2).
ITO is because electric conductivity and visible light permeability preferably turn into industrial most widely used TCO materials at present, so
And because the content in nature phosphide material is relatively low, thus the market demand can not be met, cause ITO prices high.Meanwhile indium
Material is poisonous, easily pollutes and environment and is detrimental to health, and is easily gone back when ITO is applied in the environment such as hydrogen plasma
Original, it is unstable.It is then desired to find a kind of aboundresources, cheap, nontoxic, stable performance transparent conductive oxide is thin
Film replaces ito thin film.
Zno-based and SnO2 sills are all the focuses of research in recent years.But for ZnO, SnO2 materials have more
Wide bandwidth (＞ 3.6eV), so that prepare thin-film material by it is more than 90% in the transmitance of visible-range.Together
When, SnO2 is also equipped with the chemical stability more stablized and heat endurance, although the resistivity of pure SnO2 thin-film materials is up to 106
Ω .CM, but the electrical property of SnO2 thin-film materials can effectively be changed and to its photopermeability by appropriate doping (such as ATO)
Influence little.Therefore, ATO films are one of most potential substitution ito thin film materials.
The research and development of high-performance ATO films, also become the place of study hotspot, such as prior art (CN103739282A,
Publication date：On April 23rd, 2014) a kind of mistake cold isostatic pressing method is disclosed, and it is empty using SPS sintering process and normal pressure
Gas atmosphere sintering method, the ATO targets that relative density is higher, conducts electricity very well are prepared in laboratory.But in this method, it is first
First mist projection granulating is carried out to powder, cold isostatic compaction processing is also carried out under 200~400MPa ultra-high pressure conditions, not only
Complex process, and high is required to equipment performance, it is not the optimal method of industrial-scale production ATO targets.
In view of this, it is special to propose the present invention.
The content of the invention
The first object of the present invention is to provide a kind of preparation method of tin antimony oxide ceramic sputtering target material, of the invention to be carried
The preparation method processing step of confession is easy, and using the method for gel casting forming, can stand shaping in atmospheric conditions, fit
In the preparation ATO target materials of industrially scalable.
The second object of the present invention is that providing a kind of tin antimony oxide ceramic as made from preparation method of the present invention splashes
Shoot at the target material, the ATO films prepared using tin antimony oxide ceramic sputtering target material of the present invention have that translucency is good, film layer resistance is high and steady
Calmly, the advantages that being adapted as photoelectric device substrate applications.
Third object of the present invention is to provide a kind of phototube for including tin antimony oxide ceramic sputtering target material of the present invention
Part.
Fourth object of the present invention is to provide a kind of preparation method of photoelectric device.
In order to realize the above-mentioned purpose of the present invention, spy uses following technical scheme：
A kind of preparation method of tin antimony oxide ceramic sputtering target material, the preparation method comprise the following steps：By deionization
Water and dispersant, obtain premixed liquid；SnO is added into premixed liquid2Powder, ball milling mixing, then add sintering doping and change
Property agent, continue ball milling mixing, obtain slurry；Then, Organic adhesive and defoamer are added into slurry, again ball milling mixing,
Obtain aqueous gel solution；After aqueous gel solution is stirred into deaeration, mould is injected, stands at ambient pressure, obtains ceramic body；
After ceramic blank drying, the high temperature sintering under oxygen atmosphere, tin antimony oxide ceramic sputtering target material is obtained；Wherein, the sintering is mixed
Miscellaneous modifying agent is Sb2O3Powder and CuO powders.
Preferably, in the preparation method of tin antimony oxide ceramic sputtering target material of the present invention, the dosage of dispersant for go from
The 5~20% of sub- water quality；It is furthermore preferred that the dispersant is PAA, PAA-NH4 or citric acid.
Preferably, in the preparation method of tin antimony oxide ceramic sputtering target material of the present invention, SnO2The dosage of powder is pre-
1~5 times of mixed liquid quality, the time of ball milling mixing is 1~5h；It is furthermore preferred that SnO2The particle diameter of powder is 0.5~5 μm.
Preferably, in the preparation method of tin antimony oxide ceramic sputtering target material of the present invention, Sb2O3The dosage of powder is
SnO2The 1~5% of powder quality, and/or, the dosage of CuO powders is SnO2The 0~1% of powder quality；It is furthermore preferred that Sb2O3
The dosage of powder is SnO2The 2~4% of powder quality, and/or, the dosage of CuO powders is SnO2The 0.1 of powder quality~
0.3%.
Preferably, in the preparation method of tin antimony oxide ceramic sputtering target material of the present invention, the dosage of Organic adhesive is
The 0.5~1% of stock quality, and/or, the dosage of defoamer is the 0.2~0.5% of stock quality；It is it is furthermore preferred that described organic
Adhesive is B-1000, B-1002, PEG or PVA, and the defoamer is polyether-type defoaming or foam inhibitor.
Preferably, in the preparation method of tin antimony oxide ceramic sputtering target material of the present invention, the temperature of the standing is 25
~30 DEG C, the time of standing is 20~24h.
Preferably, in the preparation method of tin antimony oxide ceramic sputtering target material of the present invention, the temperature of the high temperature sintering
For 1200~1350 DEG C, the time of sintering is 3~5h；It is furthermore preferred that the high temperature sintering is carried out under elevated pressure conditions；Enter
One step is preferable, and the condition of high voltage is 0.3~0.5MPa.
Meanwhile the present invention also provides a kind of tin antimony oxide ceramic sputtering target material as made from preparation method of the present invention.
Further, present invention also offers the photoelectric device for including tin antimony oxide ceramic sputtering target material of the present invention.
Likewise, present invention provides a kind of preparation method of photoelectric device, the present invention is included in the preparation method
The preparation method of tin antimony oxide ceramic sputtering target material.
Compared with prior art, beneficial effects of the present invention are：
(1) preparation method simple process of the present invention, the requirement for equipment is low and production efficiency is high, is advised suitable for industrialization
The production of mould；
(2) in the inventive method, by the composition to doping vario-property agent and the selection of dosage and adjustment, so as to enter one
Step optimization and improve as the tin antimony oxide ceramic sputtering target material prepared by the inventive method performance, make its meet different condition and
Use demand under environment.
Embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the present invention.It is unreceipted specific in embodiment
Condition person, the condition suggested according to normal condition or manufacturer are carried out.Agents useful for same or the unreceipted production firm person of instrument, it is
The conventional products that can be obtained by commercially available purchase.
In view of requirement of the method for production equipment and operating condition etc. in currently available technology is higher, it is not suitable for work
The production ATO targets of industry, mass, spy of the present invention provide a kind of relatively low for equipment requirement, and simple process, production effect
The high method of rate, and then realize prepared by extensive, the industrialized production of high-performance ATO targets.
Specifically, preparation method provided by the present invention comprises the following steps：
(a) by deionized water and dispersant, it is preferred that the dosage of dispersant is the 5~20% of ion water quality, more
Preferably, the dosage of dispersant is the 10~15% of deionized water quality；
Meanwhile dispersant used is preferably PAA (polyacrylic acid), PAA, PAA-NH4 or citric acid etc.；
And the mixing can preferably be carried out in ball mill, and this is also allowed for itself and metal-oxide powder further
Ball milling mixing, the time control of mixing obtain premixed liquid in 1~2h；
(b) SnO is added into premixed liquid2Powder, SnO2The dosage of powder is preferably 1~4 times of premixed liquid quality, more
Preferably, it is 3~4 times of premixed liquid quality；
Likewise it is preferred that, SnO used2The particle diameter of powder is 0.5~5 μm, such as can be, but be not limited to 1,1.5,2,
2.5th, 3,3.5,4, or 4.5 μm etc.；
SnO is added in premixed liquid2After powder, ball milling mixing is carried out, it is preferred that the time control of mixing is in 2~4h, so
Sintering doping vario-property agent is added afterwards；
By sintering doping vario-property agent, the optically and electrically performance of product ATO targets can be effectively adjusted, is more suitable for it
The practical application in the opto-electronic device as base material；
Preferably, sintering doping vario-property agent used in the present invention is Sb2O3Powder and CuO powders, both sintering are mixed
Miscellaneous modifying agent can be added sequentially, or by the two mix after add；
It is furthermore preferred that Sb2O3The dosage of powder is SnO2The 1~5% of powder quality, such as can be, but be not limited to 2,
2.5th, 3,3.5,4, or 4.5%；It is further preferred that Sb2O3The dosage of powder is SnO2The 2~4% of powder quality；More enter
One step is preferable, Sb2O3The dosage of powder is SnO2The 2~3% of powder quality；
It is furthermore preferred that the dosage of CuO powders is SnO2The 0~1% of powder quality, such as can be, but be not limited to 0.05,
0.1st, 0.2,0.3,0.4,0.5,0.6,0.7,0.8, or 0.9%；It is further preferred that the dosage of CuO powders is SnO2Powder
The 0.05~0.5% of weight；Still more preferably, the dosage of CuO powders is SnO2The 0.1~0.3% of powder quality；
And by the adjustment and optimization to sintering doping vario-property agent dosage, it is also beneficial to further improve product ATO targets
Electric conductivity, while be also beneficial to improve product relative density, improve its actual performance；
Sintering doping vario-property agent is added, continues ball milling mixing, the time of ball milling is preferably controlled in 15~20h, so that
Obtaining different powder granules can be sufficiently mixed uniformly, while by ball milling, it is also possible that different powder granules can fully be ground
Gall broken, the particle diameter of powder granule is reached 10~200nm particle size range, as slurry；
In the step, mill ball used is preferably zirconium oxide abrasive ball in mechanical milling process, meanwhile, in mechanical milling process,
The dosage of mill ball is preferably 1~1.5 times of metal-oxide powder quality (or Multimetal oxide powder gross mass)；
The rotating speed of ball milling is controlled in 35r/min or so；
(c) Organic adhesive and defoamer are added into slurry obtained by step (b)；
Preferably, the dosage of Organic adhesive is the 0.5~1% of stock quality, such as can be, but be not limited to 0.6,
0.7th, 0.8, or 0.9% etc.；Likewise it is preferred that, Organic adhesive used is B-1000, B-1002, PEG or PVA, used to disappear
Infusion is polyether-type defoaming or foam inhibitor；
Preferably, the dosage of the defoamer is the 0.2~0.5% of stock quality, such as can be, but is not limited to 0.3,
Or 0.4% etc.；
After adding Organic adhesive and defoamer into slurry, ball milling mixing is carried out again, the time of ball milling is preferably 1
~2h, that is, obtain the stable aqueous gel solution of even density, suspendability；
In this step, the dosage of adhesive and defoamer is for ceramic body Forming Quality and further product tin oxide
The quality of antimony ceramic sputtering target material also suffers from large effect, thus, by the adjustment for both auxiliary dosages and excellent
Change, can also effectively improve the intensity of base substrate, reduce the spoilage in base substrate knockout course, improve yield rate, at the same it is also favourable
Regulate and control in the density to product tin antimony oxide ceramic sputtering target material；
(d) after aqueous gel solution being stirred into deaeration, it is preferred that stirring is carried out under vacuum, the pressure of vacuum
Power control is preferably controlled in 0.5~1h in 0.5Pa or so, the time of stirring；
Then, will stir in the aqueous gel solution injection mould after de- robe is handled, preferable mould therefor is plaster mold
Tool, its size can carry out free regulation and dismounting as needed；
Then, stood at ambient pressure (preferably under atmospheric pressure), the environment temperature of standing is preferably 25~30
DEG C, the time of standing is preferably 20~24h, after removing mould, that is, obtains ceramic body；
In the present invention, in atmospheric conditions stand can access ceramic body, this compared to prior art method and
Speech, treatment conditions are clearly more gentle, and the requirement for equipment is also lower, and operation is also more simple, and this also causes the present invention
Method is more suitable for industrialized expanding production and used；
(e) after ceramic blank drying, can preferably be dried by the way of air-drying, it is (preferable in oxygen atmosphere
Realize oxygen stream to take offence in atmosphere to be sintered, high temperature sintering 99.5%) oxygen concentration is preferably more than under, it is preferred that sintering
0.3~0.5MPa of environmental pressure position, temperature is 1200~1350 DEG C, and 3~5h of heat preservation sintering under the temperature conditionss, is produced
To tin antimony oxide ceramic sputtering target material；
Due to the conversion (Sb of Sb ionic valence conditions occurring in sintering process3+→Sb5+) and Sb2O3Volatilization, also to try one's best
The content of Lacking oxygen in material is reduced, thus needs that the temperature of sintering is adjusted and optimized；Meanwhile also require sintering reaction
Carried out under pure oxygen pressure atmosphere, to reduce the content for burning till Lacking oxygen in rear product, and effectively improve later stage target in plated film
The stability of film layer resistance afterwards.
By the selection and optimization for raw material, preparation flow technique and reaction condition etc., also cause by the inventive method
Obtained tin antimony oxide ceramic sputtering target material has good photoelectric properties, is adapted as the base material of photoelectric device and uses.
Meanwhile (size can reach (300-400) × (400-600) to tin antimony oxide ceramic sputtering target material size provided by the present invention greatly
× (10-25) mm), density is high, flatness is high, without obvious buckling deformation and cracking.
And on this basis, the present invention equally also provides a kind of light for including tin antimony oxide ceramic sputtering target material of the present invention
Electrical part, such as after can tin antimony oxide ceramic sputtering target material of the present invention be processed further, it is used further to solar cell, flat board
In the preparation of the photoelectric device such as display or feature window coating.
And the preparation method of such photoelectric device can also include the step of tin antimony oxide ceramic sputtering target material, i.e. first
Tin antimony oxide ceramic sputtering target material is prepared according to the inventive method, then these targets are processed, then it is corresponding to prepare
Photoelectric device.
Embodiment 1
It is prepared as follows tin antimony oxide ceramic sputtering target material
(a) the dispersion machine PAA of appropriate amount of deionized water and deionized water quality 10% is weighed, adds in tumbling ball mill
Row mixing 1-2 hours, obtain premixed liquid；
(b) SnO of 4 times of quality is added into premixed liquid2Powder, add SnO2The particle diameter of powder is 0.5~5 μm, and ball
Grind 3h；
Then, SnO is added2The Sb of powder quality 2%2O3Powder (0.5~5 μm of particle diameter) and SnO2Powder quality 0.2%
CuO powders, and continue ball milling 20h, obtain slurry；
(c) Organic adhesive of slurry gross mass 0.6% and the defoamer of slurry gross mass 0.2% are added into slurry,
Continue ball milling 2h, obtain aqueous gel solution；
(d) under vacuum (pressure 0.5Pa or so), aqueous gel solution is stirred into deaeration 1h in agitator tank, so
Inject afterwards in mould, and under the conditions of 25 DEG C, stand 24h, the demoulding, obtain ceramic body；
(e) after ceramic body is air-dried, in oxygen stream takes offence atmosphere (oxygen concentration is more than 99.5%), 0.5MPa is forced into,
The heat preservation sintering 5h under the conditions of 1300 DEG C, obtains tin antimony oxide ceramic sputtering target material.
(300-400) × (400-600) can be reached as the tin antimony oxide ceramic sputtering target material size prepared by embodiment 1
× (10-25) mm, and flatness it is high, without obvious buckling deformation and cracking.The size of target crystalline grains can reach 5~15 μm, crystalline substance
It is mutually ZnO fibre ore structures.
Embodiment 2
Tin antimony oxide ceramic sputtering target material is prepared according to the method for embodiment 1, the tin antimony oxide ceramic of as embodiment 2 is splashed
Shoot at the target material；
Wherein, in embodiment 2, the dosage of CuO powders is SnO2The 0.1% of powder quality.
Embodiment 3
Tin antimony oxide ceramic sputtering target material is prepared according to the method for embodiment 1, the tin antimony oxide ceramic of as embodiment 3 is splashed
Shoot at the target material；
Wherein, in embodiment 3, the dosage of CuO powders is SnO2The 0.5% of powder quality.
Comparative example 1
The method of reference implementation example 1 prepares tin antimony oxide ceramic sputtering target material, and the tin antimony oxide ceramic of as comparative example 1 is splashed
Shoot at the target material；
Wherein, in comparative example 1, CuO powders are replaced with into equivalent Sb2O3Powder (0.5~5 μm of particle diameter), i.e., in comparative example 1
With SnO2The Sb of powder quality 2.2%2O3Powder is doping vario-property auxiliary agent.
Comparative example 2
The method of reference implementation example 1 prepares tin antimony oxide ceramic sputtering target material, and the tin antimony oxide ceramic of as comparative example 2 is splashed
Shoot at the target material；
Wherein, in comparative example 2, CuO powders are replaced with into equivalent SiO2Powder.
Comparative example 3
The method of reference implementation example 1 prepares tin antimony oxide ceramic sputtering target material, and the tin antimony oxide ceramic of as comparative example 3 is splashed
Shoot at the target material；
Wherein, in comparative example 3, CuO powders are replaced with into equivalent MnO2Powder.
Comparative example 4
Tin antimony oxide ceramic sputtering target material is prepared with reference to the method for embodiment 1, the tin antimony oxide ceramic of as comparative example 4 is splashed
Shoot at the target material；
Wherein, in comparative example 4, the dosage of Organic adhesive is the 0.4% of slurry gross mass.
Comparative example 5
Tin antimony oxide ceramic sputtering target material is prepared with reference to the method for embodiment 1, the tin antimony oxide ceramic of as comparative example 5 is splashed
Shoot at the target material；
Wherein, in comparative example 5, the dosage of Organic adhesive is the 1.2% of slurry gross mass.
Comparative example 6
Tin antimony oxide ceramic sputtering target material is prepared with reference to the method for embodiment 1, the tin antimony oxide ceramic of as comparative example 6 is splashed
Shoot at the target material；
Wherein, in comparative example 6, the dosage of defoamer is the 0.1% of slurry gross mass.
Comparative example 7
Tin antimony oxide ceramic sputtering target material is prepared with reference to the method for embodiment 1, the tin antimony oxide ceramic of as comparative example 7 is splashed
Shoot at the target material；
Wherein, in comparative example 7, the dosage of defoamer is the 0.6% of slurry gross mass.
Comparative example 8
Tin antimony oxide ceramic sputtering target material is prepared with reference to the method for embodiment 1, the tin antimony oxide ceramic of as comparative example 8 is splashed
Shoot at the target material；
In comparative example 8, the temperature of sintering is 1100 DEG C, and heat preservation sintering 5h.
Comparative example 9
Tin antimony oxide ceramic sputtering target material is prepared with reference to the method for embodiment 1, the tin antimony oxide ceramic of as comparative example 9 is splashed
Shoot at the target material；
In comparative example 9, the temperature of sintering is 1450 DEG C, and heat preservation sintering 5h.
Experimental example 1
(1) influence of the doping vario-property agent for product ATO target performances is sintered
Prepare 100 pieces of corresponding tin antimony oxide ceramic sputtering targets respectively according to embodiment 1-3 and comparative example 1-3 method
Material, carry out density measurement；Then, after each group target is sputtered on substrate, translucency and electrical performance testing are carried out；
Translucency and electrical performance test method are as follows：Using glass as substrate, will be prepared respectively by different embodiment methods
Tin antimony oxide ceramic sputtering target material on substrate direct current control sputter coating, thickness 0.2nm.Then, respectively to each group plated film after
Glass substrate carries out visible ray and near infrared light transmission measurement, while carries out resistance test, in each test group, randomly selects
5 pieces of complete finished products of tin antimony oxide ceramic sputtering target material are tested, and calculate the average value of indices, as a result such as following table institute
Show：
From the contrast test data of upper table, with Sb2O3And CuO powders are that doping vario-property auxiliary agent can be effectively improved
The light transmission of product ATO targets, while the relative density of product can be also effectively improved, and target body resistivity drops, make it
It is more suitable for making photoelectric device base material.
(2) influence of organic adhesive and defoamer to base substrate yield rate and product tin antimony oxide ceramic sputtering target material performance
Respectively corresponding tin antimony oxide ceramic sputtering target material, Mei Geshi are prepared according to the method for embodiment 1, comparative example 4-7
The parallel repetition of group 200 times is tested, and counts and calculate the spoilage after each experimental group ceramic body demoulding respectively；Meanwhile from each reality
Test in the complete finished product tin antimony oxide ceramic sputtering target material of group, randomly select 5 progress density measurements, it is as a result as shown in the table：
From as above correction data, the dosage of Organic adhesive and defoamer is stripped spoilage and product for base substrate
Tin antimony oxide ceramic sputtering target material density has large effect.And use Organic adhesive and defoaming according to ratio of the present invention
Agent, the spoilage of the base substrate demoulding can not only be effectively reduced, improve yield rate；Meanwhile it can also effectively improve the relative of product
Density, so as to improve its performance.
(3) influence of the sintering temperature for tin antimony oxide ceramic sputtering target material performance
Prepare 100 pieces of corresponding tin antimony oxide ceramic sputtering targets respectively according to embodiment 1- and comparative example 8-9 method
Material, and randomly select 5 pieces of complete finished products of ATO targets in each experimental group and tested, it is as a result as shown in the table：
| Experimental group | Target performance |
| Embodiment 1 | Relative density 95.3%, the Ω of bulk resistor 45 |
| Comparative example 8 | Relative density 74.4%, the Ω of bulk resistor 58 |
| Comparative example 9 | Relative density 96.2%, the Ω of bulk resistor 613 |
From comparative example data as above, for the method for comparative example, it is sintered according to the inventive method,
The relative density of gained finished product tin antimony oxide ceramic sputtering target material is higher, and ensures that target bulk resistor is relatively low, meets magnetron sputtering
Use technique.Target density is relatively low made from comparative example 8, and the easy dry linting of target, influences coating effects in sputter procedure；Comparative example
Although 9 can also obtain higher relative density, target bulk resistor is higher, and electric conductivity is poor, can not meet magnetron sputtering plating
Technique.
Although illustrate and describing the present invention with specific embodiment, but will be appreciated that without departing substantially from the present invention's
Many other change and modification can be made in the case of spirit and scope.It is, therefore, intended that in the following claims
Including belonging to all such changes and modifications in the scope of the invention.
Claims (10)
1. a kind of preparation method of tin antimony oxide ceramic sputtering target material, it is characterised in that the preparation method comprises the following steps：
By deionized water and dispersant, premixed liquid is obtained；
SnO is added into premixed liquid2Powder, ball milling mixing, sintering doping vario-property agent is then added, continues ball milling mixing, is starched
Material；
Then, Organic adhesive and defoamer are added into slurry, ball milling mixing, obtains aqueous gel solution again；
After aqueous gel solution is stirred into deaeration, mould is injected, stands at ambient pressure, obtains ceramic body；
After ceramic blank drying, the high temperature sintering under oxygen atmosphere, tin antimony oxide ceramic sputtering target material is obtained；
Wherein, the sintering doping vario-property agent is Sb2O3Powder and CuO powders.
2. preparation method according to claim 1, it is characterised in that the dosage of dispersant for deionized water quality 5~
20%；
Preferably, the dispersant is PAA, PAA-NH4 or citric acid.
3. preparation method according to claim 1, it is characterised in that SnO2The dosage of powder is the 1~5 of premixed liquid quality
Times, the time of ball milling mixing is 1~5h；
Preferably, SnO2The particle diameter of powder is 0.5~5 μm.
4. preparation method according to claim 1, it is characterised in that Sb2O3The dosage of powder is SnO2The 1 of powder quality
~5%, and/or, the dosage of CuO powders is SnO2The 0~1% of powder quality；
Preferably, Sb2O3The dosage of powder is SnO2The 2~4% of powder quality, and/or, the dosage of CuO powders is SnO2Powder
The 0.05~0.5% of quality.
5. preparation method according to claim 1, it is characterised in that the dosage of Organic adhesive is the 0.5 of stock quality
~1%, and/or, the dosage of defoamer is the 0.2~0.5% of stock quality；
Preferably, the Organic adhesive is B-1000, B-1002, PEG or PVA, and the defoamer is that polyether-type is defoamed or pressed down
Infusion.
6. preparation method according to claim 1, it is characterised in that the temperature of the standing is 25~30 DEG C, standing
Time is 20~24h.
7. preparation method according to claim 1, it is characterised in that the temperature of the high temperature sintering is 1200~1350
DEG C, the time of sintering is 3~5h；
Preferably, the high temperature sintering is carried out under elevated pressure conditions；
It is furthermore preferred that the condition of high voltage is 0.3~0.5MPa.
8. tin antimony oxide ceramic sputtering target material made from the preparation method as any one of claim 1-7.
9. include the photoelectric device of tin antimony oxide ceramic sputtering target material described in claim 8.
10. a kind of preparation method of photoelectric device, it is characterised in that methods described includes any one of claim 1-7 institutes
The preparation method stated.
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Cited By (2)
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| CN113461420A (en) * | 2021-06-21 | 2021-10-01 | 桂林电子科技大学 | Preparation method of high-density ITO target material |
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Application publication date: 20171117 |