CN104944964A - Method for preparing high-density ITO target on conditions of reducing sintering temperature - Google Patents
Method for preparing high-density ITO target on conditions of reducing sintering temperature Download PDFInfo
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Abstract
Provided is a method for preparing a high-density ITO target on conditions of reducing sintering temperature. According to the method, in preparation of ITO slurry during the initial period, first premixing liquid needs to be prepared first and a ball mill is used; an oven is used in low-temperature drying preparation of a secondary material; in preparation of the ITO slurry, second premixing liquid needs to be prepared first and the ball mill is used again, a grouting forming method is adopted in the forming processing of ITO blank and compressed air serves as a pressure transmitting medium, and normal pressure oxygen atmosphere conditions are adopted in the sintering processing of the ITO blank. The ITO slurry with a high solid phase content is one requirement for preparing the high-density ITO blank, the relative density of the prepared ITO blank can be as high as 74-76% through measurement in a mercury emission method, the solid content of the ITO slurry is 89-91% through ball milling of the secondary material, and the high-density ITO target with the relative density as high as 99.50-99.67% can be prepared through good viscosity mobility and the low sintering temperature.
Description
Technical field
The invention belongs to preparation ITO target technical field, be related specifically to a kind of method reducing sintering condition and prepare high-density ITO targe material.
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, and ITO target is the sintered compact be made up of indium tin oxide.
High-density ITO targe material is prepared mainly through sintering process under condition of normal pressure, selects the raw material powder with sintering activity or add sintering aid to realize during sintering.
Patent CN201010597008 discloses a kind of method of preparing ITO target material by oxygen atmosphere pressureless sintering process, by optimizing sintering process, sinter out the ITO target that relative density is 99.4% when oxygen flow is 20L/min, but sintering temperature 1600 DEG C is higher, soaking time 60h is partially long.
Patent CN200910227780 discloses a kind of method controlling grain size to produce ITO target, adopts normal pressure-sintered technology, and at 1550 DEG C of insulation 8h in embodiment, 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, use Gel-casting process, sinter under 1 ~ 2 times of oxygen pressure condition and obtain the ITO target that relative density reaches 99.5%, but need add in material powder in bismuthous oxide bismuth trioxide, antimonous oxide, zinc oxide, niobium oxides, titanium oxide, lead oxide powder one or more as sintering aid.
In above-mentioned patent, according to sintering activity raw material or by the strict method controlling sintering process, it former limit the range of choice of raw material, its the latter requires harsh to the control accuracy of sintering process parameter, the high-performance equipment of the stability or needs costliness that are difficult to guarantee product is to improve product stability, and cost is very high.According to the method for adding sintering aid, then can introduce other impurity in ITO target, thus affect ITO target quality, also not meet the purity requirement of high-end ITO target.
Summary of the invention
For solving the problem, the invention provides a kind of method reducing sintering condition and prepare high-density ITO targe material, the method normal pressure atmosphere, lower than nominal sintering temperatures condition under sintering prepare high-density ITO targe material, thus reach and reduce sintering cost and the object of equipment investment cost.
For achieving the above object, the present invention adopts following technical scheme:
A kind of method reducing sintering condition and prepare high-density ITO targe material, ITO powder proportioning is by weight Indium sesquioxide: stannic oxide=90:10, the method comprises the preparation of initial stage ITO slurry, secondary material is prepared in cryodrying, the preparation of ITO slurry, the forming process of ITO base substrate and the sintering processing five steps of ITO base substrate, need first prepare the first premixed liquid and use ball mill in the preparation of ITO slurry in the early stage, prepare in secondary material in cryodrying and use baking oven, need first prepare the second premixed liquid and reuse ball mill in the preparation of ITO slurry, in the forming process of ITO base substrate, have employed slip casting and be transmission medium with pressurized air, normobaric oxygen atmospheric condition is have employed in the sintering processing of ITO base substrate, feature of the present invention is as follows:
1. the preparation of initial stage ITO slurry:
Get purity and be greater than 99.99%, median size is the ITO powder 5000g of 20 ~ 100nm, in first premixed liquid, the solid load of ITO powder requires to control 40 ~ 50%, the water of 7500 ~ 5000g is taken according to this requirement, in water, add ammoniacal liquor mixing and stirring prepare the first premixed liquid, the add-on of ammoniacal liquor equals 9 ~ 10 with the pH value of described first premixed liquid and is as the criterion, all being poured into by above-mentioned ITO powder in described first premixed liquid stirs prepares initial stage ITO slurry, initial stage ITO slurry is placed in ball mill and carries out ball milling, the time of ball milling reaches 0.5 ~ 8 mPas with the viscosity number of initial stage ITO slurry and is as the criterion,
2. secondary material is prepared in cryodrying:
Initial stage ITO slurry after above-mentioned 1. ball milling is poured in pallet and carries out drying, the cleaning oven temperature of Dryly use controls at 100 ~ 150 DEG C, control time of drying at 1 ~ 2 day, after dry, the water content of initial stage ITO slurry will lower than 0.5%, by water content lower than 0.5% initial stage ITO slurry be called secondary material and for subsequent use;
3. the preparation of ITO slurry:
The organic dispersing agent of 1.20 ~ 1.59% and the water of 9.90 ~ 12.36% is chosen respectively according to the gross weight of secondary material, organic dispersing agent is added to the water and adds ammoniacal liquor mixing and stirring and prepare the second premixed liquid, the add-on of ammoniacal liquor equals 9 ~ 10 with the pH value of described second premixed liquid and is as the criterion, described second premixed liquid is all poured in ball mill and continue to stir, secondary material be evenly divided into three weight parts and carry out ball milling secondary adding in ball mill in three batches, the time controling of every batch of ball milling is at 10 ~ 15h, controlling total time at 30 ~ 45h of three batches of ball millings, its viscosity number of ITO slurry prepared after three batches of ball millings reaches 910 ~ 1388 mPas, vacuumize degassing is carried out to ITO slurry, the solid load of degassed rear ITO slurry must reach 89 ~ 91%,
Above-mentioned organic dispersing agent is any one in lipid acid Macrogol Ester, polycarbonate, polyacrylic acid;
4. the forming process of ITO base substrate:
Be transmission medium with pressurized air and adopt slip casting to process high density ITO base substrate, by above-mentioned 3. in ITO slurry press-in micropore mold and shaping, the die cavity specifications control of micropore mold is at 150 × 200 × 10mm, compressed-air actuated pressure-controlling is at 1.1 ~ 1.5MPa, the time controling of pressurize is at 50 ~ 90min, can the demoulding immediately prepare ITO base substrate after shaping, this ITO base substrate after drying row's of use mercury method surveys its relative density, 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 normobaric oxygen atmospheric condition and in the temperature of 1520 ~ 1535 DEG C, sinter 10 ~ 15h prepare ITO target, this ITO target Archimedes's drainage surveys its relative density, and relative density can reach 99.50 ~ 99.67%.
Owing to adopting technical scheme described above, the present invention produces following positively effect:
1, the present invention selects nano level ITO powder, initial stage ITO slurry is after first time ball milling depolymerization, first be converted into secondary material by deposition drying, again second time ball milling is carried out to secondary material, feed way is in three batches adopted during second time ball milling, the ITO base substrate that relative density reaches 74 ~ 76% can be prepared, the relative density of this ITO base substrate is higher, illustrate that the ITO powder particles spacing in it is nearer, substantially increase sintering power, for sintering processing relative density up to 99.50 ~ 99.67% high-density ITO targe material lay a good foundation.
2, the ITO slurry of high solid loading is one of the prerequisite of preparation high strength, high density ITO base substrate, the ITO base substrate prepared measures its relative density by row's mercury method can reach 74 ~ 76%, this relative density is close to the theoretical tap density of ITO powder, and the second time ball milling of secondary material can make the solid load of ITO slurry reach 89 ~ 91% by batch charging mode, good viscosity flow is applicable to the injection forming processing of ITO base substrate very much.
3, the present invention only sinters 10 ~ 15h and just can obtain the ITO target of relative density more than 99.5% under normobaric oxygen atmospheric condition in 1520 ~ 1535 DEG C of temperature, lower than nominal sintering temperatures 15 ~ 80 DEG C, the reduction of sintering temperature can reduce sintering cost and equipment loss, increase chamber design size, ensure yield rate.
Embodiment
The present invention is a kind of method reducing sintering condition and prepare high-density ITO targe material, under normobaric oxygen atmospheric condition, in 1520 ~ 1535 DEG C of temperature, only sinter 10 ~ 15h just can obtain the ITO target of relative density more than 99.5%, lower than nominal sintering temperatures 15 ~ 80 DEG C, the reduction of sintering temperature can reduce sintering cost and equipment loss, increase chamber design size, ensure yield rate.
The ITO powder proportioning by weight that the present invention uses is Indium sesquioxide: stannic oxide=90:10.
The present invention includes the preparation of initial stage ITO slurry, secondary material is prepared in cryodrying, the preparation of ITO slurry, the forming process of ITO base substrate and the sintering processing five steps of ITO base substrate, need first prepare the first premixed liquid and use ball mill in the preparation of ITO slurry in the early stage, prepare in secondary material in cryodrying and use baking oven, need first prepare the second premixed liquid and reuse ball mill in the preparation of ITO slurry, in the forming process of ITO base substrate, have employed slip casting and be transmission medium with pressurized air, normobaric oxygen atmospheric condition is have employed in the sintering processing of ITO base substrate, can find out that the present invention has used some routine techniques above-mentioned.
Be below according to above-mentioned general rule for two embodiments, the present invention is not limited to two embodiments, and the content of not stating of two embodiments is all as the criterion with technical scheme.
embodiment 1
Get the ITO powder 5000g that purity is greater than 99.99%, median size is 40nm, in first premixed liquid, the solid load of ITO powder requires to control 40%, the water of 7500g is taken according to this requirement, in water, add ammoniacal liquor mixing and stirring prepare the first premixed liquid, the add-on of ammoniacal liquor equals 9 with the pH value of described first premixed liquid, all being poured into by above-mentioned ITO powder in described first premixed liquid stirs prepares initial stage ITO slurry, be placed in ball mill by initial stage ITO slurry and carry out ball milling, the time of ball milling reaches 0.9 mPas with the viscosity number of initial stage ITO slurry.Poured in pallet by initial stage ITO slurry after ball milling and carry out drying, the cleaning oven temperature of Dryly use controls at 100 DEG C, controls time of drying at 1 day, by water content lower than 0.5% initial stage ITO slurry be called secondary material and for subsequent use.The ammonium polyacrylate of 1.20% and the water of 12.36% is chosen respectively according to the gross weight of secondary material, 618g is about through measuring and calculating water, ammonium polyacrylate machine is added to the water and adds ammoniacal liquor mixing and stirring and prepare the second premixed liquid, the add-on of ammoniacal liquor equals 9 with the pH value of described second premixed liquid, described second premixed liquid is all poured in ball mill and continue to stir, secondary material be evenly divided into three weight parts and carry out ball milling secondary adding in ball mill in three batches, the time controling of every batch of ball milling is at 10h, controlling total time at 30h of three batches of ball millings, its viscosity number of ITO slurry prepared after three batches of ball millings reaches 958 mPas, vacuumize degassing is carried out to ITO slurry, the solid load of degassed rear ITO slurry reaches 89%.Be transmission medium with pressurized air and adopt slip casting to process high density ITO base substrate, ITO slurry press-in micropore mold is shaping, the die cavity specifications control of micropore mold is at 150 × 200 × 10mm, compressed-air actuated pressure-controlling is at 1.1MPa, the time controling of pressurize is at 60min, can the demoulding immediately prepare ITO base substrate after shaping, this ITO base substrate after drying row's of use mercury method surveys its relative density, and relative density must reach 75%.ITO base substrate is carried out degreasing, and under normobaric oxygen atmospheric condition and in the temperature of 1530 DEG C, then sinter 10 prepare ITO target, this ITO target Archimedes's drainage surveys its relative density, and relative density can reach 99.59%.
embodiment 2
Get the ITO powder 5000g that purity is greater than 99.99%, median size is 65nm, in first premixed liquid, the solid load of ITO powder requires to control 50%, the water of 5000g is taken according to this requirement, in water, add ammoniacal liquor mixing and stirring prepare the first premixed liquid, the add-on of ammoniacal liquor equals 10 with the pH value of described first premixed liquid, all being poured into by above-mentioned ITO powder in described first premixed liquid stirs prepares initial stage ITO slurry, initial stage ITO slurry is placed in ball mill and carries out ball milling, the time of ball milling is about 10h, and its viscosity number reaches 5.5mPas.Poured in pallet by initial stage ITO slurry after ball milling and carry out drying, the cleaning oven temperature of Dryly use controls at 120 DEG C, controls time of drying at 1 day, by water content lower than 0.5% initial stage ITO slurry be called secondary material and for subsequent use.The polycarbonate of 1.59% and the water of 9.90% is chosen respectively according to the gross weight of secondary material, 495g is about through measuring and calculating water, ammonium polyacrylate machine is added to the water and adds ammoniacal liquor mixing and stirring and prepare the second premixed liquid, the add-on of ammoniacal liquor equals 10 with the pH value of described second premixed liquid, described second premixed liquid is all poured in ball mill and continue to stir, secondary material be evenly divided into three weight parts and carry out ball milling secondary adding in ball mill in three batches, the time controling of every batch of ball milling is at 15h, controlling total time at 45h of three batches of ball millings, its viscosity number of ITO slurry prepared after three batches of ball millings reaches 1388 mPas, vacuumize degassing is carried out to ITO slurry, the solid load of degassed rear ITO slurry reaches 91%.Be transmission medium with pressurized air and adopt slip casting to process high density ITO base substrate, ITO slurry press-in micropore mold is shaping, the die cavity specifications control of micropore mold is at 150 × 200 × 10mm, compressed-air actuated pressure-controlling is at 1.5MPa, the time controling of pressurize is at 90min, can the demoulding immediately prepare ITO base substrate after shaping, this ITO base substrate after drying row's of use mercury method surveys its relative density, and relative density reaches 76%.ITO base substrate is carried out degreasing, and under normobaric oxygen atmospheric condition and in the temperature of 1520 DEG C, then sinter 15 prepare ITO target, this ITO target Archimedes's drainage surveys its relative density, and relative density can reach 99.63%.
Above-mentioned two embodiments have absolutely proved the positively effect that the present invention produces, and this is apparent to this area.
Claims (1)
1. the method reducing sintering condition and prepare high-density ITO targe material, ITO powder proportioning is by weight Indium sesquioxide: stannic oxide=90:10, the method comprises the preparation of initial stage ITO slurry, secondary material is prepared in cryodrying, the preparation of ITO slurry, the forming process of ITO base substrate and the sintering processing five steps of ITO base substrate, need first prepare the first premixed liquid and use ball mill in the preparation of ITO slurry in the early stage, prepare in secondary material in cryodrying and use baking oven, need first prepare the second premixed liquid and reuse ball mill in the preparation of ITO slurry, in the forming process of ITO base substrate, have employed slip casting and be transmission medium with pressurized air, normobaric oxygen atmospheric condition is have employed in the sintering processing of ITO base substrate, it is characterized in that:
1. the preparation of initial stage ITO slurry:
Get purity and be greater than 99.99%, median size is the ITO powder 5000g of 20 ~ 100nm, in first premixed liquid, the solid load of ITO powder requires to control 40 ~ 50%, the water of 7500 ~ 5000g is taken according to this requirement, in water, add ammoniacal liquor mixing and stirring prepare the first premixed liquid, the add-on of ammoniacal liquor equals 9 ~ 10 with the pH value of described first premixed liquid and is as the criterion, all being poured into by above-mentioned ITO powder in described first premixed liquid stirs prepares initial stage ITO slurry, initial stage ITO slurry is placed in ball mill and carries out ball milling, the time of ball milling reaches 0.5 ~ 8 mPas with the viscosity number of initial stage ITO slurry and is as the criterion,
2. secondary material is prepared in cryodrying:
Initial stage ITO slurry after above-mentioned 1. ball milling is poured in pallet and carries out drying, the cleaning oven temperature of Dryly use controls at 100 ~ 150 DEG C, control time of drying at 1 ~ 2 day, after dry, the water content of initial stage ITO slurry will lower than 0.5%, by water content lower than 0.5% initial stage ITO slurry be called secondary material and for subsequent use;
3. the preparation of ITO slurry:
The organic dispersing agent of 1.20 ~ 1.59% and the water of 9.90 ~ 12.36% is chosen respectively according to the gross weight of secondary material, organic dispersing agent is added to the water and adds ammoniacal liquor mixing and stirring and prepare the second premixed liquid, the add-on of ammoniacal liquor equals 9 ~ 10 with the pH value of described second premixed liquid and is as the criterion, described second premixed liquid is all poured in ball mill and continue to stir, secondary material be evenly divided into three weight parts and carry out ball milling secondary adding in ball mill in three batches, the time controling of every batch of ball milling is at 10 ~ 15h, controlling total time at 30 ~ 45h of three batches of ball millings, its viscosity number of ITO slurry prepared after three batches of ball millings reaches 910 ~ 1388 mPas, vacuumize degassing is carried out to ITO slurry, the solid load of degassed rear ITO slurry must reach 89 ~ 91%,
Above-mentioned organic dispersing agent is any one in lipid acid Macrogol Ester, polycarbonate, polyacrylic acid;
4. the forming process of ITO base substrate:
Be transmission medium with pressurized air and adopt slip casting to process high density ITO base substrate, by above-mentioned 3. in ITO slurry press-in micropore mold and shaping, the die cavity specifications control of micropore mold is at 150 × 200 × 10mm, compressed-air actuated pressure-controlling is at 1.1 ~ 1.5MPa, the time controling of pressurize is at 50 ~ 90min, can the demoulding immediately prepare ITO base substrate after shaping, this ITO base substrate after drying row's of use mercury method surveys its relative density, 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 normobaric oxygen atmospheric condition and in the temperature of 1520 ~ 1535 DEG C, sinter 10 ~ 15h prepare ITO target, this ITO target Archimedes's drainage surveys its relative density, and relative density can reach 99.50 ~ 99.67%.
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Cited By (3)
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| CN106045496A (en) * | 2016-05-27 | 2016-10-26 | 洛阳瑞德材料技术服务有限公司 | Method using vacuum negative-pressure slip casting technology to prepare ITO target material |
| 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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