CN104909723B - High-density ITO target preparation method - Google Patents
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Abstract
The invention relates to a high-density ITO target preparation method, which is characterized in that indium-tin oxide powder prepared through a chemical co-precipitation method is adopted as a raw material, a sintering agent comprising a metal oxide, a phosphoric acid compound or phosphorus oxide and nanometer SiO2 is added, a pressure filtration molding method is used to prepare a billet, and sintering is performed at a temperature of 1450-1550 DEG C in an oxygen atmosphere to obtain the ITO target with the relative density of 98.6-99.6% and the bending strength of 112-158 MPa, wherein the thermal insulation time is 3-10 h. With the method of the present invention, the problems of small strength, poor uniformity, easy deformation and easy cracking of the current ITO are solved, and the method is suitable for preparation of the large-size and high-density ITO target.
Description
Technical field
The present invention relates to a kind of preparation method of high-density ITO targe material, belongs to optoelectronic materials technology.
Background technology
ITO target is the important source material for preparing ITO electro-conductive glass, is widely used in liquid crystal display (LCD) panel and is permitted
In the preparation of polyelectron product, such as touch screen, plasma scope (PDP), automobile solar heat protection antifog glass, organic light emission plane
Display (OLED), optical-electrical converter, solaode etc..The performance of ITO is to determine conductive glass product quality, production effect
Rate, the key factor of yield rate.Its main performance index includes composition, phase structure and density.High density just can guarantee that target has
There are relatively low resistivity, higher thermal conductivity and higher mechanical strength, therefore the relative density of high-quality ITO target should be greater than
99.5%.Up to the present, the technology of preparing of high-performance ITO target is mainly rested in Germany, Korea, Japan and other countries handss.
The production of ITO target mainly includes powder preparation, three key links of molding and sintering.Open within 80 years from eighties of last century
Beginning, foreign countries took the lead in preparing ITO powder body using liquid-phase coprecipitation.The method synthesis diameter of particle is little, narrowly distributing, structure and shape
Looks are controllable, and large-scale degree is high, low production cost, and this technology has become ripe.China carry out ITO ceramic target material research starting compared with
Evening, but in terms of powder technology of preparing, in particular by powder body prepared by liquid-phase coprecipitation, its powder characteristic has been close to foreign countries
Level.Patent both domestic and external such as Japan Patent JP193939/1993, JP29770/1995, JP68935/1994;Chinese patent CN
The A of 101830498 A, CN 102627454, CN 103274683A etc. prepare high density ITO to Co deposited synthesis ito powder
Technology have been reported that.In order to improve the density of ITO target, the nanorize of powder body and the control of structure are on one side.
On the premise of not affecting ITO target electric conductivity, addition agglutinant is to reduce sintering temperature, improves density and control microstructure
Another important channel.United States Patent (USP) US6,784,361, US6,288,325, US6,613,603 and Chinese patent CN
A of 102180653 A, CN 103232234 etc. is reported using high price, the metal-oxide of low melting point as ITO target
Agglutinant, can significantly reduce sintering temperature, improve target sintered density.The A of Chinese patent CN 103232234 describe to use
Ito powder (In prepared by coprecipitation2O3:SnO2=90:L 0wt%) as raw material, add mass ratio to be 1~5%
Y2O3, Dy2O3, B2O3, Li2One or several in O are used as agglutinant;After mix homogeneously, using compression molding, in oxygen atmosphere
Under at 1200~1600 DEG C sinter 4~10 hours.Target density by no added agglutinant 7.022g/cm3Improve to
7.13g/cm3.Document (Rare Metals Materials and engineering, 2006,36 (7), 1021~1024) also report and adopt chemical coprecipitation
Shallow lake method mixes Nb, in Ta, Bi to ITO material, when the quality incorporation of its metal-oxide is 1.0%~1.5%, and normobaric oxygen condition
Under, sintering temperature is 1450 DEG C~1500 DEG C, and ITO target relative densities can be made to improve to 97%~99%, and target resistivity can
Less than 30 × 10-4Ω·cm。
Raising of the moulding process to target consistency has the impact of no less important.The forming method master of current ITO target
There are two kinds:One kind is cold isostatic compaction (CIP) after first molding;Another kind is injection forming.United States Patent (USP) US5,531,948
Isostatic pressed or molding knot are reported with Chinese patent (A of CN 1528945A, CN 103787651, CN 103193262 A) etc.
The characteristics of isostatic pressing is closed for high-density ITO targe material.The green density of CIP shapings is uniform, is easier to obtain density height after sintering
ITO target.But CIP is formed with the limitation of its own, the yield rate that such as large-size target shapes is low, stability is poor, easily goes out
Now layering and the phenomenon such as crackle, it is impossible to shape the target of complicated shape, require mould and press higher, and equipment investment is larger.
Another forming technique, i.e. casting technology are general using without press-powder slurry cast preparation high density in combination with isostatic pressing technology
ITO target.Japan Patent (JP1117136/88, JP117137/88, JP117138/88) report, by oxidation plug with molten metal with stannum oxide with
In slurry injection water absorbing porous mold by made by Gypsum Fibrosum or macromolecular material that water containing dispersant and binding agent blendes together;
Further increase green density through the demoulding, drying, then Jing isostatic cool pressings.Then sinter at 1300-1400 DEG C, obtained
ITO target density is more than 95%, but is still below 99.5%.It is high that the A of Chinese patent CN 103044021 report a kind of injection forming
The preparation method of density high intensity ITO target base substrate, using density after ITO body dryings prepared by this patent up to 4.29~
4.65g/cm3, relative density is 60-~65%, and after 1590 DEG C of sintering, the relative density of ITO is up to 99.3~99.6%.It is beautiful
State's patent US8,778,234 and US 6,033,620 are respectively adopted injection forming and the method for pressure prepares ITO targets
Material, its density reaches more than 99.5%.United States Patent (USP) US8,778,234 highlights slip casting powder composition and agglutinant to promoting
The importance of sintering.From the trend analysis of photoelectric material and product, high density, high uniformity and large-size ITO target material
Preparation is developing direction from now on, compares other biscuit manufacturing process, and slip casting method has obviously advantage.
At present for large scale, the preparation of high density target biscuit, foreign countries are used in combination using casting with compressing.It is general
All over the mould using special plastic material, the grouting pressure that different companies uses is different.Injection forming technology is by day
The companies such as this day ore deposit, Japan east Cao, Korea's SCP generally adopt, the high-density ITO targe material international market of technology production
Occupation rate is up to more than 95%.So far, casting technology is not yet applied at home in the production of ITO target.Therefore
Prepare large scale, high-density ITO targe material, it is necessary to take into full account that powder body is constituted and performance and molding and the matching of sintering method.
The content of the invention
It is an object of the invention to provide a kind of preparation method of high-density ITO targe material, according to ITO biscuits prepared by the method
Intensity is big, and uniformity is good, is unlikely to deform and ftractures, and is suitable to the production of large-size target.The structure of the ITO target that the present invention is obtained
Uniformly, relative density is more than 99.5%, and comprcssive strength is more than 112 ± 12MPa.
The present invention is realized by the following technical programs:A kind of preparation method of high-density ITO targe material, its feature
It is:In-Sn oxide powder with chemical coprecipitation preparation adds by metal-oxide, phosphate cpd or phosphorus oxygen as raw material
Compound and Nano-meter SiO_22The agglutinant of composition, using the method for pressure filtration molding base substrate is prepared, in 1450~1550 under oxygen atmosphere
DEG C sintering, temperature retention time be 3~10 hours, obtain relative density be 98.6~99.6%, bending strength is 112~158MPa's
ITO target.
Step in detail below is taken to prepare:
(1) In-Sn oxide powder with chemical coprecipitation preparation is as raw material preparing raw material powder body, oxygen in material powder
The mass content for changing stannum is 5~20%, and the mass content of Indium sesquioxide. is 80~95%, and powder purity is not less than 99.99%, powder body
Particle size range is 0.02~1.0 μm;
(2) the agglutinant mixing of certain mass ratio is added in the material powder in step (1), in the mixed powder body
In add containing accounting for the polyacrylic binding agent and 0.1~0.7% methyl that material powder mass ratio is 0.05~0.2%
In the aqueous solution of acrylic amine dispersant, pH value is adjusted to 9~11 with ammonia;The slurry being uniformly mixed after ball milling, then
Stirring, evacuation 10~30 minutes removes the bubble in slurry, in slurry material powder account for solid phase mass content for 80~
90%;
(3) in the slurry injection porous mold for preparing step (2), grouting pressure is 0.8~2.0MPa, and mould is resin
Material, with gradient pore size distribution, from inside to outside aperture increases successively;Lay filter cloth in resin die surface;In grouting pressure effect
It is lower to discharge moisture by mould micropore, until volume no longer changes substantially;
(4) demoulding is dried, and baking temperature is 20~80 DEG C, and the relative density of the base substrate of acquisition is 59.2~64.8%;It is dry
Base substrate after dry is sintered under normal pressure pure oxygen atmosphere, and temperature is 1450~1550 DEG C, and temperature retention time is 3~10 hours, obtains phase
It is 98.6~99.6% to density, bending strength is the ITO target of 112~158MPa.
Metal-oxide, phosphate cpd or phosphorous oxides and Nano-meter SiO_2 in described agglutinant2Composition mass ratio
For:The mass content of metal-oxide is the 0.5~3% of material powder, phosphate cpd or phosphorous oxides and Nano-meter SiO_22Two
Person's gross mass content is the 0.01~1% of material powder.
Phosphate cpd in described agglutinant composition is indium phosphate, phosphoric acid stannum, yttrium phosphate or niobium phosphate, phosphorous oxides
It is phosphorus pentoxide.
Metal-oxide in described agglutinant composition is Dy2O3、Nb2O5、Ta2O5、Y2O3One or more group therein
Into.
The demoulding in described step (4) is dried, and baking temperature is 20~80 DEG C, can be divided into two stages:Base after the demoulding
Body is first dried 22h in room temperature state, and then at 80 DEG C 28h is dried.
The relative density of ITO target prepared by the present invention is 98.6~99.6%, and bending strength is 112~158MPa.This
The advantage of invention is to add agglutinant in In-Sn oxide powder by synthesizing in coprecipitation method, in sintering process
Lower temperature can play a part of solid solution and liquid-phase sintering.In addition, even structure, density can be obtained by pressure filtration molding method
High biscuit.1450~1550 DEG C of sintering under the conditions of pure oxygen, can obtain relative density height, the ITO target of even structure.This
It is bright suitable for large scale, the preparation of high-density ITO targe material.
Specific embodiment
A kind of preparation method of high-density ITO targe material is high using slurry pressure filtration molding and oxygen atmosphere by adding agglutinant
Warm sintering prepares high-density ITO targe material;Comprise the following steps successively:
(1), as raw material, the mass content of stannum oxide is equal in powder body for the In-Sn oxide powder with chemical coprecipitation preparation
For 5~20%, the mass content of Indium sesquioxide. is 80~95%, and powder purity is not less than 99.99%, and diameter of particle scope is
0.02~1.0 μm.
(2) agglutinant of certain mass ratio will be added in the ITO powder body in step (1), this mixed powder is added and accounts for powder
Body mass ratio is the aqueous solution of 0.05~0.2% acrylic adhesive and 0.1~0.7% methacrylic acid amine dispersant
In, with ammonia pH value is adjusted to 9~11;The slurry being uniformly mixed after ball milling, then stirs, evacuation 10~30 minutes,
The bubble in slurry is removed, it is 80~90% that material powder accounts for the solid phase mass content of slurry.
(3) in the slurry injection porous mold for preparing step (2), grouting pressure is 0.8~2.0MPa, and mould is resin
Material, with gradient pore size distribution, from inside to outside aperture increases successively;Lay filter cloth in resin die surface;Foundation grouting pressure will
Moisture is discharged by mould micropore, until volume no longer changes substantially.
(4) demoulding is dried, and biscuit baking temperature is 20~80 DEG C, and the relative density of the base substrate of acquisition is 59.2~
64.8%.Dry base substrate is sintered under normal pressure pure oxygen atmosphere, and temperature is 1450~1550 DEG C, and temperature retention time is 3~10 hours.
(5) composition of the agglutinant added when preparing mixed-powder in step (2) includes MxOy, phosphate compoundss simultaneously
Or oxide and Nano-meter SiO_22;The mass content of MxOy is the 0.5~3% of material powder ITO, phosphate compoundss and nanometer
SiO2Gross mass content for material powder 0.01~1%.
(6) agglutinant component MxOy added when preparing mixed-powder in step (2) is Dy2O3, Nb2O5, Ta2O5, Y2O3,
Can be one or more therein composition.
Embodiment 1
The ITO powder body of lkg is accurately weighed, the Dy of 0.5wt% is added in ITO powder body2O3, the P of 0.002wt%2O5,
The Nano-meter SiO_2 of 0.008wt%2, and a certain amount of deionized water is weighed for 80% by solid concentration mass ratio, with above-mentioned composite powder
Body configuration premix slurry;Add simultaneously and account for the polyacrylic binding agent and 0.1% metering system that powder quality ratio is 0.05%
Acid amide dispersant, by compound mix grinding 4 hours in Ball-stirring mill are inserted, and obtain the slurry of pressure filtration molding needs.
Slurry is entered after holding vessel and evacuated degassing, and surface laying filter cloth, size are poured under 0.8MPa pressure
In for the resin porous mold of 500mm × 500mm, the liquid medium in slip is made through the outage row of filter cloth and resin die
Go out, form uniformly densely base substrate, stand the demoulding after 4h.Base substrate after the demoulding is dried in room temperature state (i.e. under normal temperature and pressure)
22h, then at 80 DEG C 28h is dried, and obtains high density ITO base substrate.Base substrate obtains relative density and reaches Jing after 1550 DEG C sinter 10h
98.6% ITO target.The average bending strength of respective material is 112 ± 12MPa.
Embodiment 2
The ITO powder body of lkg is accurately weighed, the Ta of 2.0wt% is added in ITO powder body2O3, the P of 0.05wt%2O5,
The Nano-meter SiO_2 of 0.5wt%2, and a certain amount of deionized water is weighed for 85% by solid concentration mass ratio, with above-mentioned composite granule
Configuration premix slurry;Add simultaneously and account for the polyacrylic binding agent and 0.4% methacrylic acid amino that powder quality ratio is 0.1%
Dispersant, by compound mix grinding 4 hours in Ball-stirring mill are inserted, and obtain the slurry of pressure filtration molding needs.
Slurry is entered after holding vessel and evacuated degassing, and surface laying filter cloth, size are poured under 1.5MPa pressure
In for the resin porous mold of 500mm × 500mm, the liquid medium in slip is made through the outage row of filter cloth and resin die
Go out, form uniformly densely base substrate, stand the demoulding after 4h.Base substrate after the demoulding is dried 22h in room temperature state, then at 80 DEG C of dryings
28h, obtains high density ITO base substrate.Base substrate obtains the ITO target that relative density is up to 99.4% Jing after 1510 DEG C sinter 10h.It is right
The average bending strength for answering material is 149 ± 13MPa.
Embodiment 3
The ITO powder body of lkg is accurately weighed, the Y of 0.50wt% is added in ITO powder body2O3With the Ta of 2.0wt%2O3,
The P of 0.05wt%2O5, the Nano-meter SiO_2 of 0.8wt%2, and a certain amount of deionized water is weighed for 85% by solid concentration mass ratio,
With above-mentioned composite granule configuration premix slurry;Add simultaneously account for polyacrylic binding agent that powder quality ratio is 0.1% and
0.4% methacrylic acid amine dispersant, by compound mix grinding 4 hours in Ball-stirring mill are inserted, and obtain the slurry of pressure filtration molding needs.
Slurry is entered after holding vessel and evacuated degassing, and surface laying filter cloth, size are poured under 1.5MPa pressure
In for the resin porous mold of 500mm × 500mm, the liquid medium in slip is made through the outage row of filter cloth and resin die
Go out, form uniformly densely base substrate, stand the demoulding after 4h.Base substrate after the demoulding is dried 22h in room temperature state, then at 80 DEG C of dryings
28h, obtains high density ITO base substrate.Base substrate obtains the ITO target that relative density is up to 99.6% Jing after 1510 DEG C sinter 10h.It is right
The average bending strength for answering material is 158 ± 15MPa.
Embodiment 4
Comparative example:Without agglutinant
The ITO powder body of lkg is accurately weighed, a certain amount of deionized water is weighed for 80% by solid concentration mass ratio, it is and upper
State composite granule configuration premix slurry;Add simultaneously and account for the polyacrylic binding agent and 0.1% that powder quality ratio is 0.05%
Methacrylic acid amine dispersant, by compound mix grinding 4 hours in Ball-stirring mill are inserted, and obtain the slurry of pressure filtration molding needs.
Slurry is entered after holding vessel and evacuated degassing, and surface laying filter cloth, size are poured under 2.0MPa pressure
In for the resin porous mold of 500mm × 500mm, the liquid medium in slip is made through the outage row of filter cloth and resin die
Go out, form uniformly densely base substrate, stand the demoulding after 4h.Base substrate after the demoulding is dried 22h in room temperature state, then at 80 DEG C of dryings
28h, obtains high density ITO base substrate.Base substrate obtains the ITO target that relative density is up to 96.7% Jing after 1600 DEG C sinter 10h.It is right
The average bending strength for answering material is 103 ± 15MPa.
Embodiment 5 (comparative example 3)
Comparative example:Common gypsum mould slip casting method
The ITO powder body of lkg is accurately weighed, the Y of 0.50wt% is added in ITO powder body2O3With the Ta of 2.0wt%2O3,
The P of 0.05wt%2O5, the Nano-meter SiO_2 of 0.8wt%2, and a certain amount of deionized water is weighed for 85% by solid concentration mass ratio,
With above-mentioned composite granule configuration premix slurry;Add simultaneously account for polyacrylic binding agent that powder quality ratio is 0.1% and
0.4% methacrylic acid amine dispersant, by compound mix grinding 4 hours in Ball-stirring mill are inserted, and obtain the slurry of pressure filtration molding needs.
Slurry is entered after holding vessel and evacuated degassing, and in being poured into the gypsum mold of 500mm × 500mm, slurry is poured
Note completes to stand the demoulding after 6h in gypsum mold.Base substrate after the demoulding is dried 26h in room temperature state, then at 100 DEG C of dryings
24h, obtains ITO base substrates.Base substrate obtains the ITO target that relative density is up to 96.3% Jing after 1550 DEG C sinter 10h.Respective material
Average bending strength be 98 ± 12MPa.
Claims (7)
1. a kind of preparation method of high-density ITO targe material, is characterized in that:With In-Sn oxide powder prepared by chemical coprecipitation
For raw material, add by metal-oxide, phosphate cpd or phosphorous oxides and Nano-meter SiO_22The agglutinant of composition, using filter pressing into
The method of type prepares base substrate, and in 1450~1550 DEG C of sintering under oxygen atmosphere, temperature retention time is 3~10 hours, is obtained relatively close
Spend for 98.6~99.6%, bending strength is the ITO target of 112~158MPa;
Step in detail below is taken to prepare:
(1) In-Sn oxide powder with chemical coprecipitation preparation is as raw material preparing raw material powder body, stannum oxide in material powder
Mass content be 5~20%, the mass content of Indium sesquioxide. is 80~95%, and powder purity is not less than 99.99%, diameter of particle
Scope is 0.02~1.0 μm;
(2) the agglutinant mixing of certain mass ratio is added in the material powder in step (1), in the mixed powder body again
Add to contain and account for the polyacrylic binding agent and 0.1~0.7% metering system that material powder mass ratio is 0.05~0.2%
In the aqueous solution of acid amide dispersant, pH value is adjusted to 9~11 with ammonia;The slurry being uniformly mixed after ball milling, then stirs,
Evacuation 10~30 minutes, removes the bubble in slurry, and material powder accounts for solid phase mass content for 80~90% in slurry;
(3) in the slurry injection porous mold for preparing step (2), grouting pressure is 0.8~2.0MPa, and mould is resinous wood
Material, with gradient pore size distribution, from inside to outside aperture increases successively;Lay filter cloth in resin die surface;Under grouting pressure effect
Moisture is discharged by mould micropore, until volume no longer changes substantially;
(4) demoulding is dried, and baking temperature is 20~80 DEG C, and the relative density of the base substrate of acquisition is 59.2~64.8%;After drying
Base substrate sinter under normal pressure pure oxygen atmosphere, temperature be 1450~1550 DEG C, temperature retention time be 3~10 hours, obtain it is relatively close
Spend for 98.6~99.6%, bending strength is the ITO target of 112~158MPa.
2. the preparation method of high-density ITO targe material according to claim 1, is characterized in that:Metal in described agglutinant
Oxide, phosphate cpd or phosphorous oxides and Nano-meter SiO_22Constituting mass ratio is:The mass content of metal-oxide is original
The 0.5~3% of feed powder body, phosphate cpd or phosphorous oxides and Nano-meter SiO_22The two gross mass content is the 0.01 of material powder
~1%.
3. the preparation method of high-density ITO targe material according to claim 1, is characterized in that:In described agglutinant composition
Phosphate cpd be indium phosphate, phosphoric acid stannum, yttrium phosphate or niobium phosphate, phosphorous oxides is phosphorus pentoxide.
4. the preparation method of high-density ITO targe material according to claim 1, is characterized in that:In described agglutinant composition
Metal-oxide be Dy2O3、Nb2O5、Ta2O5、Y2O3One or more composition therein.
5. the preparation method of high-density ITO targe material according to claim 2, is characterized in that:In described agglutinant composition
Phosphate cpd be indium phosphate, phosphoric acid stannum, yttrium phosphate or niobium phosphate, phosphorous oxides is phosphorus pentoxide.
6. the preparation method of high-density ITO targe material according to claim 5, is characterized in that:In described agglutinant composition
Metal-oxide be Dy2O3、Nb2O5、Ta2O5、Y2O3One or more composition therein.
7. the preparation method of high-density ITO targe material according to claim 1, is characterized in that:The demoulding in step (4) is dried,
Baking temperature is 20~80 DEG C, is divided into two stages:Base substrate after the demoulding is first dried 22h in room temperature state, then at 80 DEG C of dryings
28h。
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