CN104944964B - A kind of method that reduction sintering condition prepares high-density ITO targe material - Google Patents
A kind of method that reduction sintering condition prepares high-density ITO targe material Download PDFInfo
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- CN104944964B CN104944964B CN201510360593.7A CN201510360593A CN104944964B CN 104944964 B CN104944964 B CN 104944964B CN 201510360593 A CN201510360593 A CN 201510360593A CN 104944964 B CN104944964 B CN 104944964B
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Abstract
A kind of method that reduction sintering condition prepares high-density ITO targe material,Need first to prepare the first premixed liquid in the method preparation of ITO slurry in the early stage and use ball mill,Prepare to baking oven used in secondary material in low temperature drying,Ball mill is needed first to prepare the second premixed liquid and is reused in the preparation of ITO slurry,Slip casting is employed in the processing and forming of ITO base substrate and with compressed air as transmission medium,Normobaric oxygen atmospheric condition is employed in the sintering processing of ITO base substrate,The ITO slurry of high solid loading is to prepare one of necessary condition of high density ITO base substrate,The ITO base substrate for preparing measures its relative density up to 74 ~ 76% by arranging mercury method,And the ball milling of secondary material makes the solid concentration of ITO slurry reach 89 ~ 91%,Preferably viscosity flow and relatively low sintering temperature can prepare the high-density ITO targe material of relative density up to 99.50 ~ 99.67%.
Description
Technical field
The invention belongs to ITO target technical field is prepared, it is related specifically to a kind of sintering condition that reduces and prepares high density ITO
The method of target.
Background technology
ITO is the abbreviation title of Tin-doped Indium Oxide, and the implication of ITO refers to a kind of indium tin oxide material
Material, ITO target is the sintered body being made up of indium tin oxide.
High-density ITO targe material is mainly prepared by sintering process under condition of normal pressure, is selected with sintering activity during sintering
Material powder or add sintering aid realizing.
Patent CN201010597008 discloses a kind of method of preparing ITO target material by oxygen atmosphere pressureless sintering process, by excellent
Change sintering process, sinter out the ITO target that relative density is 99.4% when oxygen flow is for 20L/min, but sintering temperature 1600
DEG C higher, temperature retention time 60h is partially long.
Patent CN200910227780 discloses a kind of method that control grain size manufactures ITO target, using normal pressure-sintered
Technology, is incubated 8h at 1550 DEG C in embodiment, and the most high-density of target is that 7.11g/cm3 i.e. relative density are about
99.44%.
Patent CN201210424320 discloses a kind of preparation method of indium-tin oxide target material, using gel injection-moulding work
Skill, sinters and is obtained the ITO target that relative density reaches 99.5% under the conditions of 1 ~ 2 times of oxygen pressure, but need in material powder
Middle one or more conducts that adds in bismuth oxide, antimony oxide, zinc oxide, niobium oxide, titanium oxide, lead oxide powder
Sintering aid.
In above-mentioned patent, according to sintering activity raw material or the method by strict control sintering process, its former
The range of choice of raw material is limited, its latter is harsh to the control accuracy requirement of sintering process parameter, it is difficult to ensure the steady of product
Qualitative or need expensive high-performance equipment to improve product stability, cost is very high.Method according to sintering aid is added,
Then other impurities can be introduced in ITO target, so as to affect ITO target quality, the purity for being also unsatisfactory for high-end ITO target will
Ask.
Content of the invention
For solving the above problems, the invention provides a kind of reduce the method that sintering condition prepares high-density ITO targe material, should
In normal pressure atmosphere, under the conditions of less than nominal sintering temperatures, sintering prepares high-density ITO targe material to method, so as to reduce sintering
Cost and the purpose of equipment investment cost.
For achieving the above object, the present invention is adopted the following technical scheme that:
A kind of method that reduction sintering condition prepares high-density ITO targe material, ITO powder proportioning by weight is oxidation
Indium:Tin oxide=90:10, the method include the preparation of initial stage ITO slurry, low temperature drying prepare secondary material, the preparation of ITO slurry,
The sintering of the processing and forming of ITO base substrate and ITO base substrate processes five steps, needs in the early stage first to prepare in the preparation of ITO slurry
Go out the first premixed liquid and ball mill is used, prepare to baking oven used in secondary material, in the preparation of ITO slurry in low temperature drying
The second premixed liquid need to first be prepared and ball mill is reused, in the processing and forming of ITO base substrate, employ slip casting
And with compressed air as transmission medium, in the sintering processing of ITO base substrate, employ normobaric oxygen atmospheric condition, the feature of the present invention
As follows:
1. the preparation of initial stage ITO slurry:
Purity is taken more than the ITO powder 5000g that 99.99%, average grain diameter is 20 ~ 100nm, ITO powder in the first premixed liquid
Solid concentration require control 40 ~ 50%, weigh the water of 7500 ~ 5000g according to the requirement, in water add ammoniacal liquor mixing stir
Mix uniformly and the first premixed liquid is prepared, the addition of ammoniacal liquor is defined equal to 9 ~ 10 by the pH value of first premixed liquid, will be above-mentioned
ITO powder is all poured into stir in first premixed liquid and prepares initial stage ITO slurry, and initial stage ITO slurry is placed on ball
Ball milling is carried out in grinding machine, and the time of ball milling reaches 0.5 ~ 8 mPa s by the viscosity number of initial stage ITO slurry and is defined;
2. low temperature drying prepares secondary material:
Initial stage ITO slurry after above-mentioned 1. ball milling is poured in pallet and is dried, the cleaning oven temperature that drying is used
At 100 ~ 150 DEG C, drying time controlled at 1 ~ 2 day for control, and after drying, the water content of initial stage ITO slurry will be less than 0.5%, will contain
Secondary material standby is called by initial stage ITO slurry of the water yield less than 0.5%;
3. the preparation of ITO slurry:
Gross weight according to secondary material chooses 1.20 ~ 1.59% organic dispersing agent and 9.90 ~ 12.36% water respectively, will have
Machine dispersant is added to the water and adds ammoniacal liquor mixing and stirring to prepare the second premixed liquid, and the addition of ammoniacal liquor is with described second
The pH value of premixed liquid is defined equal to 9 ~ 10, second premixed liquid is all poured in ball mill and continues stirring, and secondary material is equal
Even be divided into three weight portions and in three batches secondary addition ball mill in carry out ball milling, per batch ball milling time control in 10 ~ 15h, three
Its viscosity number of ITO slurry that the total time control of batch ball milling is prepared after 30 ~ 45h, three batch ball millings reaches 910 ~ 1388
MPa s, carries out vacuumizing degassing to ITO slurry, and after degassing, the solid concentration of ITO slurry must reach 89 ~ 91%;
Above-mentioned organic dispersing agent is aliphatic acid Macrogol Ester, Merlon, any one in polyacrylic acid;
4. the processing and forming of ITO base substrate:
With compressed air as transmission medium and using slip casting process high density ITO base substrate, by above-mentioned 3. in ITO
Slurry is pressed into micropore mold and is molded, and the die cavity specifications control of micropore mold is in 150 × 200 × 10mm, the pressure of compressed air
In 1.1 ~ 1.5MPa, the time control of pressurize the demoulding immediately can prepare ITO base substrate after 50 ~ 90min, shaping, should for control
ITO base substrate surveys its relative density using row's mercury method after drying, and relative density must reach 74 ~ 76%;
5. the sintering processing of ITO base substrate:
By above-mentioned 4. in the ITO base substrate that obtains carry out degreasing, then under the conditions of normobaric oxygen atmosphere and at 1520 ~ 1535 DEG C
Temperature in sintering 10 ~ 15h prepare ITO target, the ITO target surveys its relative density with Archimedes's drainage, with respect to close
Degree can reach 99.50 ~ 99.67%.
Due to adopting techniques described above scheme, the present invention produces following good effect:
1st, the present invention selects nano level ITO powder, and initial stage ITO slurry first passes through deposition after first time ball milling depolymerization
Drying is converted into secondary material, then carries out second ball milling to secondary material, using feed way in three batches during second ball milling, permissible
The ITO base substrate that relative density reaches 74 ~ 76% is prepared, the relative density of this ITO base substrate is higher, and the ITO in which is described
Between powder particles, distance is closer to substantially increasing sintering power, be the highly dense of sintering processing relative density up to 99.50 ~ 99.67%
Degree ITO target is laid a good foundation.
2nd, the ITO slurry of high solid loading is to prepare one of high intensity, necessary condition of high density ITO base substrate, prepares
ITO base substrate by arrange mercury method measure its relative density up to 74 ~ 76%, the relative density be close to ITO powder theory pile up close
Degree, and second ball milling of secondary material can make the solid concentration of ITO slurry reach 89 ~ 91% by batch charging mode, preferably
Viscosity flow be especially suitable for ITO base substrate injection forming processing.
3rd, the present invention only sinters 10 ~ 15h in 1520 ~ 1535 DEG C of temperature under the conditions of normobaric oxygen atmosphere and can just be obtained relatively
ITO target of the density more than 99.5%, lower than nominal sintering temperatures 15 ~ 80 DEG C, the reduction of sintering temperature can reduce and sinter into
Sheet and equipment loss, increase chamber design size, it is ensured that yield rate.
Specific embodiment
The present invention is a kind of method that reduction sintering condition prepares high-density ITO targe material, under the conditions of normobaric oxygen atmosphere only
10 ~ 15h is sintered in 1520 ~ 1535 DEG C of temperature and just ITO target of the relative density more than 99.5% can be obtained, than normal sintering temperature
Degree is low 15 ~ 80 DEG C, and the reduction of sintering temperature can reduce sintering cost and equipment loss, increase chamber design size, protect
Card yield rate.
The present invention using ITO powder proportioning by weight be indium oxide:Tin oxide=90:10.
The present invention includes that the preparation of initial stage ITO slurry, low temperature drying prepare secondary material, the preparation of ITO slurry, ITO base substrate
Processing and forming and the sintering of ITO base substrate process five steps, need in the early stage first to prepare first in the preparation of ITO slurry pre-
Mixed liquid simultaneously uses ball mill, prepares to baking oven used in secondary material in low temperature drying, needs first to prepare in the preparation of ITO slurry
Go out the second premixed liquid and ball mill is reused, slip casting is employed in the processing and forming of ITO base substrate and with compression
Air is transmission medium, employs normobaric oxygen atmospheric condition, it can be seen that the present invention is borrowed in the sintering processing of ITO base substrate
Some routine techniques above-mentioned.
The following is according to above-mentioned general rule and for two embodiments, the invention is not limited in two embodiments, two
The not described content of individual embodiment is all defined by technical scheme.
Embodiment 1
Purity is taken more than the ITO powder 5000g that 99.99%, average grain diameter is 40nm, ITO powder consolidates in the first premixed liquid
Phase content requirement controls 40%, weighs the water of 7500g according to the requirement, adds ammoniacal liquor mixing and stirring to prepare in water
First premixed liquid, the addition of ammoniacal liquor are equal to 9 with the pH value of first premixed liquid, above-mentioned ITO powder are all poured into described
Stir in first premixed liquid and initial stage ITO slurry is prepared, initial stage ITO slurry is placed in ball mill carries out ball milling, ball milling
Time 0.9 mPa s is reached with the viscosity number of initial stage ITO slurry.Initial stage ITO slurry after ball milling is poured in pallet to be carried out
Dry, at 100 DEG C, drying time controlled at 1 day the cleaning oven temperature control that drying is used, and water content is first less than 0.5%
Secondary material standby is called by phase ITO slurry.Gross weight according to secondary material chooses 1.20% ammonium polyacrylate and 12.36% respectively
Water, through calculate water be about 618g, ammonium polyacrylate machine is added to the water and is added ammoniacal liquor mixing and stirring to prepare second
Premixed liquid, the addition of ammoniacal liquor are equal to 9 with the pH value of second premixed liquid, and second premixed liquid is all poured into ball mill
Interior continuation stirring, secondary material is uniformly divided into three weight portions and secondary in three batches addition in ball mill carries out ball milling, per batch ball milling
Time control in 10h, its viscosity of ITO slurry that the total time control of three batch ball millings is prepared after 30h, three batch ball millings
Value reaches 958 mPa s, and ITO slurry is carried out vacuumizing degassing, and after degassing, the solid concentration of ITO slurry reaches 89%.With pressure
Contracting air is transmission medium and processes high density ITO base substrate using slip casting, ITO slurry press-in micropore mold is formed
Type, the die cavity specifications control of micropore mold in 150 × 200 × 10mm, the Stress control of compressed air in 1.1MPa, pressurize when
Between control after 60min, shaping and the demoulding immediately ITO base substrate can be prepared, the ITO base substrate surveys which using row's mercury method after drying
Relative density, relative density must reach 75%.ITO base substrate is carried out degreasing, then under the conditions of normobaric oxygen atmosphere and 1530
DEG C temperature in sintering 10 prepare ITO target, the ITO target surveys its relative density, relative density with Archimedes's drainage
99.59% can be reached.
Embodiment 2
Purity is taken more than the ITO powder 5000g that 99.99%, average grain diameter is 65nm, ITO powder consolidates in the first premixed liquid
Phase content requirement controls 50%, weighs the water of 5000g according to the requirement, adds ammoniacal liquor mixing and stirring to prepare in water
First premixed liquid, the addition of ammoniacal liquor are equal to 10 with the pH value of first premixed liquid, above-mentioned ITO powder are all poured into described
Stir in first premixed liquid and initial stage ITO slurry is prepared, initial stage ITO slurry is placed in ball mill carries out ball milling, ball milling
Time be about 10h, its viscosity number reaches 5.5mPa s.Initial stage ITO slurry after ball milling is poured in pallet and is dried,
At 120 DEG C, drying time controlled at 1 day the cleaning oven temperature control that drying is used, by initial stage ITO of the water content less than 0.5%
Secondary material standby is called by slurry.Gross weight according to secondary material chooses 1.59% Merlon and 9.90% water, warp respectively
Measuring and calculating water is about 495g, ammonium polyacrylate machine is added to the water and is added ammoniacal liquor mixing and stirring to prepare the second premixed liquid,
The addition of ammoniacal liquor is equal to 10 with the pH value of second premixed liquid, second premixed liquid is all poured in ball mill and is continued
Stirring, secondary material is uniformly divided into three weight portions and secondary in three batches addition in ball mill carries out ball milling, the time per batch ball milling
Control is reached in 15h, its viscosity number of ITO slurry that the total time control of three batch ball millings is prepared after 45h, three batch ball millings
1388 mPa s, carry out vacuumizing degassing to ITO slurry, and after degassing, the solid concentration of ITO slurry reaches 91%.With compressed air
High density ITO base substrate is processed for transmission medium and using slip casting, ITO slurry press-in micropore mold is molded, micropore
, in 150 × 200 × 10mm, the Stress control of compressed air is in 1.5MPa, the time control of pressurize for the die cavity specifications control of mould
The demoulding immediately ITO base substrate can be prepared after 90min, shaping, it is relatively close that the ITO base substrate surveys which using row's mercury method after drying
Degree, relative density reach 76%.ITO base substrate is carried out degreasing, then under the conditions of normobaric oxygen atmosphere and in 1520 DEG C of temperature
Sintering 15 prepares ITO target, and the ITO target surveys its relative density with Archimedes's drainage, and relative density can reach
99.63%.
Above-mentioned two embodiment has absolutely proved the good effect that the present invention is produced, and this is obvious to this area.
Claims (1)
1. a kind of method that reduction sintering condition prepares high-density ITO targe material, ITO powder proportioning by weight is indium oxide:
Tin oxide=90:10, the method includes that the preparation of initial stage ITO slurry, low temperature drying prepare secondary material, the preparation of ITO slurry, ITO
The sintering of the processing and forming of base substrate and ITO base substrate processes five steps, needs first to prepare in the preparation of ITO slurry the in the early stage
One premixed liquid simultaneously uses ball mill, prepares to baking oven used in secondary material in low temperature drying, needs elder generation in the preparation of ITO slurry
Prepare the second premixed liquid and reuse ball mill, employ in the processing and forming of ITO base substrate slip casting and with
Compressed air is transmission medium, employs normobaric oxygen atmospheric condition, it is characterized in that in the sintering processing of ITO base substrate:
1. the preparation of initial stage ITO slurry:
The water of 7500 ~ 5000g is weighed, in water, adds ammoniacal liquor mixing and stirring to prepare the first premixed liquid, the addition of ammoniacal liquor
Amount is defined equal to 9 ~ 10 by the pH value of first premixed liquid, by purity more than the ITO that 99.99%, average grain diameter is 20 ~ 100nm
Powder 5000g is all poured into stir in first premixed liquid and is prepared initial stage ITO slurry, ITO powder in initial stage ITO slurry
The solid concentration of body requires control 40 ~ 50%, and initial stage ITO slurry is placed in ball mill carries out ball milling, and the time of ball milling is with first
The viscosity number of phase ITO slurry reaches 0.5 ~ 8 mPa s and is defined;
2. low temperature drying prepares secondary material:
Initial stage ITO slurry after above-mentioned 1. ball milling is poured in pallet and is dried, the cleaning oven temperature control that drying is used
At 100 ~ 150 DEG C, drying time controlled at 1 ~ 2 day, and after drying, the water content of initial stage ITO slurry will be less than 0.5%, by water content
Secondary material standby is called by initial stage ITO slurry less than 0.5%;
3. the preparation of ITO slurry:
Gross weight according to secondary material chooses 1.20 ~ 1.59% organic dispersing agent and 9.90 ~ 12.36% water respectively, by organic point
Powder is added to the water and adds ammoniacal liquor mixing and stirring to prepare the second premixed liquid, and the addition of ammoniacal liquor is with the described second premix
The pH value of liquid is defined equal to 9 ~ 10, second premixed liquid is all poured in ball mill and continues stirring, secondary material is uniformly divided
For three weight portions and in three batches carry out ball milling in secondary addition ball mill, the time control per batch ball milling in 10 ~ 15h, three batches
Its viscosity number of ITO slurry that the total time control of ball milling is prepared after 30 ~ 45h, three batch ball millings reaches 910 ~ 1388
MPa s, carries out vacuumizing degassing to ITO slurry, and after degassing, the solid concentration of ITO slurry must reach 89 ~ 91%;
Above-mentioned organic dispersing agent is fatty acid polyethylene glycol ester, Merlon, any one in polyacrylic acid;
4. the processing and forming of ITO base substrate:
With compressed air as transmission medium and using slip casting process high density ITO base substrate, by above-mentioned 3. in ITO slurry
It is pressed into micropore mold and is molded, the die cavity specifications control of micropore mold is in 150 × 200 × 10mm, the Stress control of compressed air
In 1.1 ~ 1.5MPa, the time control of pressurize the demoulding immediately prepares ITO base substrate after 50 ~ 90min, shaping, the ITO base substrate
Its relative density is surveyed after drying using row's mercury method, relative density must reach 74 ~ 76%;
5. the sintering processing of ITO base substrate:
By above-mentioned 4. in the ITO base substrate that obtains carry out degreasing, then under the conditions of normobaric oxygen atmosphere and in 1520 ~ 1535 DEG C of temperature
In degree, 10 ~ 15h of sintering prepares ITO target, and the ITO target surveys its relative density with Archimedes's drainage, and relative density can
To reach 99.50 ~ 99.67%.
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CN106045496B (en) * | 2016-05-27 | 2018-06-19 | 洛阳瑞德材料技术服务有限公司 | A kind of method that ITO target is prepared using negative pressure of vacuum injection forming technology |
CN111592339A (en) * | 2020-06-03 | 2020-08-28 | 福建阿石创新材料股份有限公司 | ITO target material and preparation method thereof |
CN113699492A (en) * | 2021-08-25 | 2021-11-26 | 蔡精敏 | Process for preparing high-density tin-doped indium oxide green body |
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CN103044021A (en) * | 2012-12-28 | 2013-04-17 | 中国船舶重工集团公司第七二五研究所 | Preparation method of slip-casting high-density and high-strength ITO target green body |
CN103787650A (en) * | 2014-02-27 | 2014-05-14 | 中国船舶重工集团公司第七二五研究所 | Method for preparing ITO (Indium Tin Oxide) target |
CN104058729A (en) * | 2014-06-30 | 2014-09-24 | 中国船舶重工集团公司第七二五研究所 | Method for preparing large-specification ITO (indium tin oxide) target material |
CN104355610A (en) * | 2014-09-28 | 2015-02-18 | 中国船舶重工集团公司第七二五研究所 | Method for preparing large-scale ITO (Indium Tin Oxide) target material by using automatic slip casting technology |
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JP2005075648A (en) * | 2003-08-29 | 2005-03-24 | Tosoh Corp | Method of manufacturing indium tin oxide sintered compact |
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CN103044021A (en) * | 2012-12-28 | 2013-04-17 | 中国船舶重工集团公司第七二五研究所 | Preparation method of slip-casting high-density and high-strength ITO target green body |
CN103787650A (en) * | 2014-02-27 | 2014-05-14 | 中国船舶重工集团公司第七二五研究所 | Method for preparing ITO (Indium Tin Oxide) target |
CN104058729A (en) * | 2014-06-30 | 2014-09-24 | 中国船舶重工集团公司第七二五研究所 | Method for preparing large-specification ITO (indium tin oxide) target material |
CN104355610A (en) * | 2014-09-28 | 2015-02-18 | 中国船舶重工集团公司第七二五研究所 | Method for preparing large-scale ITO (Indium Tin Oxide) target material by using automatic slip casting technology |
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