CN108975904A - A kind of high-densit ITO target of strong ultrasonic wave added method preparation even tissue - Google Patents
A kind of high-densit ITO target of strong ultrasonic wave added method preparation even tissue Download PDFInfo
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- CN108975904A CN108975904A CN201810729836.3A CN201810729836A CN108975904A CN 108975904 A CN108975904 A CN 108975904A CN 201810729836 A CN201810729836 A CN 201810729836A CN 108975904 A CN108975904 A CN 108975904A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
- C04B35/457—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates based on tin oxides or stannates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B3/00—Producing shaped articles from the material by using presses; Presses specially adapted therefor
- B28B3/003—Pressing by means acting upon the material via flexible mould wall parts, e.g. by means of inflatable cores, isostatic presses
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
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- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses a kind of preparation methods of the high-densit ITO target of even tissue, and the ITO (In2O3:SnO2=9:1, wt%) of 20~70nm of partial size, purity >=99.99% are passed through dry granulating machine, the fluffy particle of 15-20um or so size is made；The fluffy ITO particle by granulation is loaded in a mold again and is placed in calm pressure, the pressure of hydraulic press is adjusted, mould inside pressure is respectively set to 400MPa, 600MPa, 800MPa, 1000MPa, 1200MPa and 1500MPa；Introduce the biscuit sample that molding consistency under power P=3Kw ultrasonic vibration and calm pressure double action is up to 62.2 ± 0.2%.
Description
Technical field
The present invention relates to a kind of preparations of ITO material, and in particular to a kind of system of the high-densit ITO target of even tissue
It is standby.
Background technique
ITO refers to the abbreviation of Indium and Tin oxide.Ito thin film has to visible transparent and good electric conductivity,
Its transmitance >=95% to visible light, to absorptivity >=85% of ultraviolet light, to reflectivity >=70% of infrared ray, to microwave
Attenuation rate >=85%.Meanwhile the excellent machining performance of ito thin film, hardness height and wear-and corrosion-resistant, and be easy in acidic liquid
In etch fine figure.Thus ito thin film shows (LCD), electric color in thin film transistor (TFT) (TFT), flat panel Liquid Crystal in recent years
Layer window, the active and passive constituent element in photovoltaic device and infra-red radiation reflection heat mirror films etc. obtain extensively
Using being the particularly important electronic functional material of current era of knowledge-driven economy information industry.
ITO target is one of production extremely important material of transparent conductive film.ITO target is mainly splashed by magnetic control
ITO target is sputtered on glass or other substrates to form ito thin film by jet device.The theoretical density of ITO target is 7.15g/
Cm3, good finished product ITO target should have >=99% relative density, and such ITO target has low resistivity, higher
Thermal conductivity and higher mechanical strength.The preparation method of high-purity high-density degree ITO target comes with some shortcomings at present, for example, heat etc.
Static pressure equipment is expensive, operating cost is higher, causes production cost higher；The large-size ITO target material of hot pressing sintering method preparation is easy
Cracking, and the production cost is very high；The poor dispersion of obtained ITO target powder-product, easily generation agglomeration；Ceramics,
Density reaches 95%, but since sintering temperature is higher, material grains are grown up obviously, and performance is by a degree of influence.
Obtained ITO target mobility is bad, and the compactness of final ITO target is caused not reach requirement.
Summary of the invention
The object of the invention provides a kind of preparation method for the ITO target that microstructure is uniform, crystal grain is tiny.
The object of the invention is achieved through the following technical solutions:
A kind of preparation method of the high-densit ITO target of even tissue, it is characterised in that:
The ITO (In2O3:SnO2=9:1, wt%) of 20~70nm of partial size, purity >=99.99% are passed through into dry granulation
The fluffy particle of 15-20um or so size is made in machine.The fluffy ITO particle by granulation is loaded in a mold and placed again
In calm pressure.Adjust hydraulic press pressure, by mould inside pressure be respectively set to 400MPa, 600MPa, 800MPa,
1000MPa, 1200MPa and 1500MPa.It introduces under power P=3Kw ultrasonic vibration and calm pressure double action and forms consistency
Up to 62.2 ± 0.2% biscuit sample.Finally, 1550 DEG C at a temperature of sintering 2h be made.
The invention has the following beneficial effects:
Material density produced by the present invention is 99.3 ± 0.3%, the ITO target that microstructure is uniform, crystal grain is tiny.
Detailed description of the invention
Fig. 1: the calm pressure of difference introduces influence of the strong ultrasonic vibration to ITO forming of green body.
Fig. 2: the ITO target consistency curve of different time sintering.
Fig. 3: the microscopic appearance of the ITO target of different sintering times.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
A kind of preparation method of the high-densit ITO target of even tissue, by 20~70nm of partial size, purity >=99.99%
ITO (In2O3:SnO2=9:1, wt%) passes through dry granulating machine, and the fluffy particle of 15-20um or so size is made.It again will be through
The fluffy ITO particle for crossing granulation loads in a mold and is placed in calm pressure.The pressure for adjusting hydraulic press, by mould inside pressure
It is respectively set to 400MPa, 600MPa, 800MPa, 1000MPa, 1200MPa and 1500MPa by force.It is super to introduce power P=3Kw
The biscuit sample that molding consistency under pressure double action is up to 62.2 ± 0.2% is swung and cools down in acoustic shock.Finally, in 1550 DEG C of temperature
The lower sintering 2h of degree is made.
As shown in Figure 1, as the consistency of the raising biscuit of pressure is also gradually increased, but increase trend and gradually weaken.Draw
Enter after strong ultrasonic vibration under identical pressure, the consistency of biscuit significantly improves, and when pressure reaches 1000MPa, consistency is
62.2 ± 0.2%, continue to increase with pressure, the consistency rate of biscuit is very slow, therefore it is we that pressure, which is 1000MPa,
The optimal pressure conditions of method.The influence that different time is sintered ITO target is calm to Pf=1000MPa to depress, if introduces Pw
The ITO biscuit of=3Kw ultrasonic vibration production is sintered at 1550 DEG C, and the ITO target consistency of different time sintering is as schemed
2.Direct extruding is apparently higher than by high temperature sintering production ITO target consistency as shown in Fig. 2, introducing ultrasonic wave added molding biscuit
Molding biscuit high temperature sintering makes ITO target.Ultrasonic wave added molding biscuit sample is introduced into 1550 DEG C of high temperature, is sintered
120min obtains highest consistency, reaches 99.3 ± 0.3%.And directly extrusion forming biscuit is sintered after 4h just in 1550 DEG C
Obtain 96.2 ± 0.2% consistency.As shown in figure 3, being the calm pressure of pressure Pf=1000MPa, the shake of Pw=3Kw ultrasound is introduced
The ITO biscuit for swinging production, in the microscopic appearance figure of the ITO target of 60min, 100min, 120min and 140min sintering.From figure
It can be seen that ITO particle is in 1-2um or so in 60min.Consistency is not very good between particle, has obvious hole to occur, with
After sintering time extends to 120min, have been combined very close between particle, hole and gap etc. disappear, and consistency reaches
To 99.3 ± 0.3%.As sintering time continues to extend, particle continues to grow up, and when sintering time is 140min, particle is had reached
7-10um, target consistency is 99.3 ± 0.2%, without significant change.
Claims (2)
1. a kind of preparation method of the high-densit ITO target of even tissue, it is characterised in that:
20~70nm of partial size, the ITO (In2O3:SnO2=9:1, wt%) of purity >=99.99% are passed through into dry granulating machine, system
At the fluffy particle of 15-20um or so size；The fluffy ITO particle by granulation is loaded in a mold and is placed in calm again
Pressure, adjust the pressure of hydraulic press, by mould inside pressure be respectively set to 400MPa, 600MPa, 800MPa, 1000MPa,
1200MPa and 1500MPa；It introduces molding consistency under power P=3Kw ultrasonic vibration and calm pressure double action and is up to 62.2
± 0.2% biscuit sample.
2. the preparation method of high-densit ITO target as described in claim 1, it is characterised in that: by the biscuit sample obtained
Product 1550 DEG C at a temperature of sintering 2h be made.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810729836.3A CN108975904A (en) | 2018-07-05 | 2018-07-05 | A kind of high-densit ITO target of strong ultrasonic wave added method preparation even tissue |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810729836.3A CN108975904A (en) | 2018-07-05 | 2018-07-05 | A kind of high-densit ITO target of strong ultrasonic wave added method preparation even tissue |
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| CN108975904A true CN108975904A (en) | 2018-12-11 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112301252A (en) * | 2020-09-16 | 2021-02-02 | 河南科技大学 | Preparation method of nano copper-based composite material |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106977179A (en) * | 2017-04-07 | 2017-07-25 | 中国船舶重工集团公司第七二五研究所 | A kind of method that two steps multi-steps sintering method prepares high fine and close ITO target |
| CN107244911A (en) * | 2017-01-13 | 2017-10-13 | 昆明理工大学 | A kind of preparation method of ITO tubular targets |
| CN108002815A (en) * | 2017-11-29 | 2018-05-08 | 株洲冶炼集团股份有限公司 | A kind of preparation method of tubulose ITO target |
-
2018
- 2018-07-05 CN CN201810729836.3A patent/CN108975904A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107244911A (en) * | 2017-01-13 | 2017-10-13 | 昆明理工大学 | A kind of preparation method of ITO tubular targets |
| CN106977179A (en) * | 2017-04-07 | 2017-07-25 | 中国船舶重工集团公司第七二五研究所 | A kind of method that two steps multi-steps sintering method prepares high fine and close ITO target |
| CN108002815A (en) * | 2017-11-29 | 2018-05-08 | 株洲冶炼集团股份有限公司 | A kind of preparation method of tubulose ITO target |
Non-Patent Citations (1)
| Title |
|---|
| 张明杰等: "不同冷等静压压力对ITO靶材性能影响的研究", 《化工新型材料》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112301252A (en) * | 2020-09-16 | 2021-02-02 | 河南科技大学 | Preparation method of nano copper-based composite material |
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