CN102351526B - Method for preparing AZO target materials by adopting gel injection molding forming - Google Patents
Method for preparing AZO target materials by adopting gel injection molding forming Download PDFInfo
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- CN102351526B CN102351526B CN 201110166426 CN201110166426A CN102351526B CN 102351526 B CN102351526 B CN 102351526B CN 201110166426 CN201110166426 CN 201110166426 CN 201110166426 A CN201110166426 A CN 201110166426A CN 102351526 B CN102351526 B CN 102351526B
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Abstract
The invention relates to a method for preparing AZO target materials by adopting gel injection molding forming, which belongs to a preparation method of AZO target materials for sputtering ZnO base films. The method for preparing the AZO target materials by adopting the gel injection molding forming comprises the following steps of: weighing ZAO powder and premixing liquid, adding dispersing agents to be mixed, obtaining forming slurry after the mixing, uniformly adding initiating agents and catalysts into the slurry, pouring the mixture into a mold, curing the materials at a certain temperature, placing raw blanks into organic solvents for gel removing after the curing, drying the materials at a certain temperature after the gel removing to obtain biscuit, sintering the biscuit according to a certain sintering system to obtain sintering samples, and obtaining the AZO target products after the processing. The AZO ceramic target materials prepared by the method have simple equipment requirement, the forming is convenient and fast, the forming sample intensity is high, and the economy and the practicability are good. The ingredient distribution of the target materials prepared by the method is uniform, the density is high, and the use performance of the AZO target materials can be improved.
Description
Technical field
The present invention relates to the preparation method of the AZO target that a kind of sputter zno-based film uses, particularly relate to a kind of method with preparing AZO target materials by adopting gel injection molding forming.
Background technology
Magnetron sputtering making ZnO base film be study at most in the standby film process of the ownership system, the most ripe, and most widely used method.The magnetron sputtering technique rate of film build is high, and substrate temperature is low, and the adhesivity of film is good, and is easy to control, cost is low, can realize large-area coating film.Magnetron sputtering technique in industrial production, technical maturity, technology are widely used.
The selection of AZO target is played very important effect with the quality of making the magnetron sputtering product, and the AZO target both can use Zn and Al alloy, also can use ZnO/Al
2O
3Oxide ceramics.Metal targets is easily manufactured, purity is high, and sedimentation effect is high, but metal targets easily affects its quality of forming film because oxidation is poisoning.The manufacturing of ceramic target, moulding, processing inconvenience, thus cost is higher, but ceramic target is because its good performance still is widely used in actual industrial production.
In magnetron sputtering technique, the performances such as the purity of ceramic target, density, resistivity are larger to the performance impact of its goods, generally speaking, only have high-quality sputtering target material could prepare high-quality thin-film material.Therefore, the development of high-quality AZO target is played very crucial effect with exploitation to the application of zno-based thin-film material.
In the preparation process of ceramic target, using highly purified raw material is the prerequisite of the high-quality target of preparation, but the technological process of its preparation is most important equally on the impact of ceramic target performance.Moulding and sintering are exactly two important process procedures, especially moulding process link, and homogeneity of ingredients, goods final densities and the cost of manufacture of target all played a decisive role.That the sintering of AZO target usually adopts is normal pressure-sintered, hot pressed sintering and atmosphere sintering method, and normal pressure-sintered is the most frequently used sintering means; That forming method commonly used has is dry-pressing formed, cold isostatic compaction etc.Dry-pressing formed the large size base substrate is manufactured with difficulty, shows as the green density inequality, shrink unevenly, easily produce the defectives such as layering, cracking.Cold isostatic compaction has the characteristics such as blank density is high and even, but the Mold Making difficulty is larger, and only is fit to the moulding of simple shape goods.In addition, abroad (as the Tosoh company of Japan) adopts lower-cost slip-casting shaping process to make the large-size ceramic target, but there is the blank density gradient in grouting process, causes ceramic target to have the problem of composition and Density inhomogeneity, affects the target use properties.
At present, to large scale development, corresponding ceramic target size also needs to increase considerably due to the preparation film.The technical problem underlying that the AZO sputtering target material faces has: how to prepare big area AZO sputter ceramic target, how to guarantee the microtexture of large size ceramic sputtering target material and the homogeneity of tissue.In addition, along with the development of plated film industry, also can propose Secretary to the target cost, explore Financial cost lower, the preparation technology that production efficiency is higher is ceramic target research and the developing direction of producing.
Summary of the invention
The purpose of this invention is to provide that a kind of equipment requirements is simple, technique is convenient and swift, the moulding sample strength is high, a kind of method with preparing AZO target materials by adopting gel injection molding forming that economy and practicality are good.
The object of the present invention is achieved like this: the method for preparing AZO target materials by adopting gel injection molding forming, comprise the following steps: take zinc oxide aluminum powder and premixed liquid, add dispersion agent to mix, obtain the moulding slurry after mixing, after evenly adding initiator, catalyzer in slurry, pour mould into, be cured at a certain temperature, after curing, green compact are put into organic solvent and carried out binder removal, carry out at a certain temperature drying after binder removal and obtain biscuit; Obtain sintered sample by certain sintering schedule sintering; Obtain AZO target goods after processing;
Wherein said zinc oxide aluminum powder is the powder that contains zinc oxide and aluminum oxide, perhaps contains the powder of zinc oxide and aluminium, and the shared massfraction of zinc oxide is 90.0～99.9%, and all the other are aluminum oxide or are aluminium;
Wherein said premixed liquid is the mixed aqueous solution of monomer, linking agent, monomer can be in acrylamide, Methacrylamide, methoxyl group-polymethyl acrylic acid, methacrylic acid a kind of, linking agent used can be N, a kind of in N '-methylene-bisacrylamide, polydimethyl vinylformic acid; In premixed liquid, to account for the premixed liquid massfraction be 5～20% to the content of monomer, and it is 1～15% that linking agent accounts for the premixed liquid massfraction, and wherein the content of linking agent is less than the content of monomer;
Described with premixed liquid, when the zinc oxide aluminum powder mixes, the zinc oxide aluminum powder accounts for slurry volume mark 25～60%; The massfraction that dispersion agent accounts for slurry is 0～5%, mixes and adopts ball milling method, and Ball-milling Time is 0.5～48h;
The initiator that moulding slurry after described ball milling adds can be in ammonium persulphate, Potassium Persulphate, hydrogen peroxide or hydrochloric acid azo a kind of; Described catalyzer can be Tetramethyl Ethylene Diamine; Be cured after adding initiator and catalyzer, solidification value is 20～150 ℃;
After described curing, sample carries out binder removal in organic solution, organic solution can for a kind of in polyoxyethylene glycol, ethanol or they arbitrarily than mixture, the binder removal time is 4～48h; After described binder removal, to carry out drying temperature be 20～200 ℃ to green compact;
After described drying, base substrate carries out sintering, and sintering temperature is 1300～1600 ℃.
Beneficial effect and advantage:
(1) AZO target distributed components, the density of the present invention's preparation are high, have improved the use properties of AZO target.
(2) compared with prior art, high with the blank density of gel casting forming, and each position even density, blank sintering process sample is indeformable, do not ftracture, and yield rate is high.
(3) prepare with gel injection technique that the AZO ceramic target is simple to equipment requirements, moulding process is convenient and swift, be convenient to the specification that in production process, rapid adjustment is produced product, the industrial production cost is lower.
(4) the method prepare that AZO ceramic target moulding sample strength is high, economy and practicality good.
Description of drawings
Fig. 1 is process flow sheet of the present invention.
Embodiment
Following examples are used for explanation the present invention, but are not used for limiting the scope of the invention.
Embodiment 1: take 150 gram deionized waters, add 30 gram acrylamides and 20 gram N, N '-methylene-bisacrylamide fully is hybridly prepared into premixed liquid.Adding the quality of alumina mark in premixed liquid is 1.5% zinc oxide aluminum powder 1000 grams, then adds 3 milliliters of AN-2000 as dispersion agent.Carry out ball milling and mix on ball mill, ball milling fully mixed slurry in 20 hours.
Add 3 milliliters of Tetramethyl Ethylene Diamines as catalyzer in slurry, add 12 milliliters of ammonium persulphates as initiator, pour in mould after mixing.Be placed in 80 ℃ of baking ovens and be cured, solidify after 5 minutes and take out.
After solidifying, base substrate is placed in polyglycol solution and carries out binder removal, and the binder removal time is 20h, take out binder removal after base substrate carry out drying, drying temperature is 80 ℃, makes the biscuit body.The biscuit body is carried out sintering under 1450 ℃, make required AZO target after processing.Prepared AZO target color even, density is 5.42g/cm
3
Embodiment 2: take 850 gram deionized waters, add 100 gram acrylamides and 50 gram N, N '-methylene-bisacrylamide fully is hybridly prepared into premixed liquid.Adding the quality of alumina mark in premixed liquid is 3% zinc oxide aluminum powder 2500 grams, and adds 30 milliliters of AN-2000 as dispersion agent.Carry out ball milling and mix on ball mill, ball milling fully mixed slurry in 15 hours.
Add 20 milliliters of Tetramethyl Ethylene Diamines as catalyzer in slurry, add 80 milliliters of ammonium persulphates as initiator, pour in mould after mixing.Be placed in 60 ℃ of baking ovens and be cured, solidify after 10 minutes and take out.
After solidifying, base substrate is placed in polyglycol solution and carries out binder removal, and the binder removal time is 24h, take out binder removal after base substrate carry out drying, drying temperature is 90 ℃, makes the biscuit body.The biscuit body is carried out sintering under 1500 ℃, make required AZO target after processing.Prepared AZO target color even, density is 5.40g/cm
3
Embodiment 3: take 750 gram deionized waters, add 150 gram polyacrylamides and 100 gram N, N '-methylene-bisacrylamide fully is hybridly prepared into premixed liquid.Adding the quality of alumina mark in premixed liquid is 2% zinc oxide aluminum powder 3600 grams, and adds 25 milliliters of AN-2000 as dispersion agent.Carry out ball milling and mix on ball mill, ball milling fully mixed slurry in 20 hours.
Add 18 milliliters of Tetramethyl Ethylene Diamines as catalyzer in slurry, add 72 milliliters of ammonium persulphates as initiator, pour in mould after mixing.Be placed in 60 ℃ of baking ovens and be cured, solidify after 5 minutes and take out.
After solidifying, base substrate is placed in polyglycol solution and carries out binder removal, and the binder removal time is 20h, take out binder removal after base substrate carry out drying, drying temperature is 80 ℃, makes the biscuit body.The biscuit body is carried out sintering under 1450 ℃, make required AZO target after processing.Prepared AZO target color even, density is 5.45g/cm
3
Embodiment 4: take 400 gram deionized waters, add 70 gram methacrylic acids and 30 gram polydimethyl vinylformic acid, fully be hybridly prepared into premixed liquid.Adding the quality of alumina mark in premixed liquid is 0.5% zinc oxide aluminum powder 2000 grams, and adds 15 milliliters of AN-2000 as dispersion agent.Carry out ball milling and mix on ball mill, ball milling fully mixed slurry in 24 hours.
Add 11 milliliters of Tetramethyl Ethylene Diamines as catalyzer in slurry, add 44 milliliters of ammonium persulphates as initiator, pour in mould after mixing.Be placed in 80 ℃ of baking ovens and be cured, solidify after 15 minutes and take out.
After solidifying, base substrate is placed in polyglycol solution and carries out binder removal, and the binder removal time is 15h, take out binder removal after base substrate carry out drying, drying temperature is 80 ℃, makes the biscuit body.The biscuit body is carried out sintering under 1400 ℃, make required AZO target after processing.Prepared AZO target color even, density is 5.38g/cm
3
Claims (1)
1. method with preparing AZO target materials by adopting gel injection molding forming, it is characterized in that: the method for preparing AZO target materials by adopting gel injection molding forming, comprise the following steps: take zinc oxide aluminum powder and premixed liquid, add dispersion agent to mix, obtain the moulding slurry after mixing, after evenly adding initiator, catalyzer in slurry, pour mould into, be cured at a certain temperature, after curing, green compact put into organic solvent and carried out binder removal, carry out at a certain temperature drying after binder removal and obtain biscuit; Obtain sintered sample by certain sintering schedule sintering; Obtain AZO target goods after processing;
Described zinc oxide aluminum powder is the powder that contains zinc oxide and aluminum oxide, perhaps contains the powder of zinc oxide and aluminium, and the shared massfraction of zinc oxide is 90.0～99.9%, and all the other are aluminum oxide or are aluminium;
Described premixed liquid is the mixed aqueous solution of monomer, linking agent, monomer can be in acrylamide, Methacrylamide, methoxyl group-polymethyl acrylic acid, methacrylic acid a kind of, linking agent used can be N, a kind of in N '-methylene-bisacrylamide, polydimethyl vinylformic acid; In premixed liquid, to account for the premixed liquid massfraction be 5～20% to the content of monomer, and it is 1～15% that linking agent accounts for the premixed liquid massfraction, and wherein the content of linking agent is less than the content of monomer;
Described with premixed liquid, when the zinc oxide aluminum powder mixes, the zinc oxide aluminum powder accounts for slurry volume mark 25～60%; The massfraction that dispersion agent accounts for slurry is 0～5%, mixes and adopts ball milling method, and Ball-milling Time is 0.5～48h;
The initiator that moulding slurry after described ball milling adds can be in ammonium persulphate, Potassium Persulphate, hydrogen peroxide or hydrochloric acid azo a kind of; Described catalyzer can be Tetramethyl Ethylene Diamine; Be cured after adding initiator and catalyzer, solidification value is 20～150 ℃;
After described curing, sample carries out binder removal in organic solution, organic solution can for a kind of in polyoxyethylene glycol, ethanol or they arbitrarily than mixture, the binder removal time is 4～48h; After described binder removal, to carry out drying temperature be 20～200 ℃ to green compact;
After described drying, base substrate carries out sintering, and sintering temperature is 1300～1600 ℃.
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102924077A (en) * | 2012-11-20 | 2013-02-13 | 中国科学院上海硅酸盐研究所 | Method for preparing large-size zinc-oxide based target by casting through novel low-toxicity gel |
| CN102942363B (en) * | 2012-11-22 | 2015-06-17 | 国家钽铌特种金属材料工程技术研究中心 | Method for preparing AZO target by powdery slurry pouring |
| EP2829251B1 (en) * | 2013-07-22 | 2019-04-10 | Ivoclar Vivadent AG | Controlling of sintering kinetics of oxide ceramics |
| CN103936425B (en) * | 2014-01-20 | 2015-08-12 | 清华大学 | A kind of preparation method of ceramic plate |
| CN104152853B (en) * | 2014-07-08 | 2017-01-04 | 中国人民解放军国防科学技术大学 | Glass ceramics target and preparation method thereof |
| CN106145927A (en) * | 2015-04-17 | 2016-11-23 | 汉能新材料科技有限公司 | A kind of manufacture method of gallium doped zinc oxide target |
| CN106145928A (en) * | 2015-04-17 | 2016-11-23 | 汉能新材料科技有限公司 | A kind of manufacture method of tubular ZnO electronic ceramics |
| CN106145926A (en) * | 2015-04-17 | 2016-11-23 | 汉能新材料科技有限公司 | A kind of manufacture method of zinc oxide electronic ceramics |
| CN105272209B (en) * | 2015-11-11 | 2017-12-12 | 攀枝花学院 | Mix the preparation method of aluminium titanium zinc oxide target |
| CN112374887A (en) * | 2020-11-13 | 2021-02-19 | 北京航大微纳科技有限公司 | Gel injection molding preparation method of tungsten oxide-based ceramic target material |
| CN113354393A (en) * | 2021-07-13 | 2021-09-07 | 江苏迪丞光电材料有限公司 | Preparation method for preparing IGZO (indium gallium zinc oxide) rotary target material by gel casting |
| CN114804854A (en) * | 2022-05-11 | 2022-07-29 | 株洲火炬安泰新材料有限公司 | AZO target and preparation method thereof |
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| CN101073939A (en) * | 2007-06-18 | 2007-11-21 | 湖南华联特种陶瓷有限公司 | Toughened alumina ceramic overlapping curved pipe of high-performance zirconium oxide and its production |
| CN101319307A (en) * | 2008-07-14 | 2008-12-10 | 王悦林 | Method of manufacturing tin indium oxide target material |
| CN101851739A (en) * | 2009-04-02 | 2010-10-06 | 宜兴佰伦光电材料科技有限公司 | AZO sputtering target for high-stability transparent conductive film and manufacturing method |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101073939A (en) * | 2007-06-18 | 2007-11-21 | 湖南华联特种陶瓷有限公司 | Toughened alumina ceramic overlapping curved pipe of high-performance zirconium oxide and its production |
| CN101319307A (en) * | 2008-07-14 | 2008-12-10 | 王悦林 | Method of manufacturing tin indium oxide target material |
| CN101851739A (en) * | 2009-04-02 | 2010-10-06 | 宜兴佰伦光电材料科技有限公司 | AZO sputtering target for high-stability transparent conductive film and manufacturing method |
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