CN102351526A - 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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- CN102351526A CN102351526A CN2011101664260A CN201110166426A CN102351526A CN 102351526 A CN102351526 A CN 102351526A CN 2011101664260 A CN2011101664260 A CN 2011101664260A CN 201110166426 A CN201110166426 A CN 201110166426A CN 102351526 A CN102351526 A CN 102351526A
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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 for preparing the AZO target with gel casting forming.
Background technology
Magnetron sputtering prepare the zno-based film be all preparations study at most in film process, 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 the industrial production, technical maturity, technical application are extensive.
The selection of AZO target is played crucial 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 influences its quality of forming film easily because oxidation is poisoned.The manufacturing of ceramic target, moulding, processing inconvenience, thus cost is higher, but ceramic target still is widely used in actual industrial production owing to its good performance.
In magnetron sputtering technique, performances such as the purity of ceramic target, density, resistivity are bigger to the performance impact of its goods, generally speaking, have only 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 to the ceramic target Effect on 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, show as the base substrate density uneven, shrink unevenly, be easy to generate defectives such as layering, cracking.Cold isostatic compaction has characteristics such as blank density is high and even, but the Mold Making difficulty is bigger, and only is fit to the moulding of simple shape goods.In addition, external (like 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 composition and the even problem of density unevenness, influences the target use properties.
At present, owing to prepare film to large scale development, corresponding ceramic target size also need increase considerably.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 new requirement to the target cost, it is lower to explore Financial cost, and the higher preparation technology of production efficiency 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, technology is convenient and swift, the moulding sample strength is high, a kind of method for preparing the AZO target with gel casting forming that economy and practicality are good.
The objective of the invention is to realize like this: gel casting forming prepares the method for AZO target; May further comprise the steps: take by weighing zinc oxide aluminum powder and premixed liquid; Adding dispersion agent mixes; Obtain the moulding slurry after the mixing; After evenly adding initiator, catalyzer in the slurry, pour mould into, be cured at a certain temperature; After the curing green compact are put into organic solvent and carry out binder removal, carry out drying behind the binder removal at a certain temperature and obtain biscuit; Obtain sintered sample by certain sintering schedule sintering; Obtain AZO target goods after the 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, the methacrylic acid a kind of; Used linking agent can be N, a kind of in N '-methylene-bisacrylamide, the polydimethyl vinylformic acid; To account for the premixed liquid massfraction be 5～20% to monomeric content in the premixed liquid, and it is 1～15% that linking agent accounts for the premixed liquid massfraction, and wherein the content of linking agent is less than monomeric content;
Said 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 the ball milling time is 0.5～48h;
The initiator that moulding slurry behind the described ball milling adds can be in ammonium persulphate, Potassium Persulphate, ydrogen peroxide 50 or the 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 ℃;
Said curing back sample carries out binder removal in organic solution, organic solution can for a kind of in polyoxyethylene glycol, the ethanol or they arbitrarily than mixture, the binder removal time is 4～48h; To carry out drying temperature be 20～200 ℃ to green compact behind the said binder removal;
Said dry back base substrate carries out sintering, and sintering temperature is 1300～1600 ℃.
Beneficial effect and advantage:
(1) the AZO target distributed components of the present invention preparation, density 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 density is even, the blank sintering process samples is indeformable, do not ftracture, and yield rate is high.
(3) simple with gel injection prepared AZO ceramic target to equipment requirements, moulding process is convenient and swift, is convenient to the specification that rapid adjustment in the production process is produced product, the industrial production cost is lower.
(4) this method prepares that AZO ceramic target moulding sample strength is high, economy and practicality be good.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Following examples are used to illustrate the present invention, but are not used for limiting scope of the present invention.
Embodiment 1: takes by weighing 150 gram deionized waters, adds 30 gram acrylamides and 20 gram N, and N '-methylene-bisacrylamide, thorough mixing is mixed with premixed liquid.Adding aluminum oxide quality mark is 1.5% zinc oxide aluminum powder 1000 grams in premixed liquid, adds 3 milliliters of AN-2000 again as dispersion agent.On ball mill, carry out ball mill mixing, ball milling made the slurry thorough mixing even in 20 hours.
In slurry, add 3 milliliters of Tetramethyl Ethylene Diamines as catalyzer, add 12 milliliters of ammonium persulphates, pour in the mould after mixing as initiator.Place 80 ℃ of baking ovens to be cured, solidify after 5 minutes and take out.
To solidify the back base substrate and place polyglycol solution to carry out binder removal, the binder removal time is 20h, and base substrate carries out drying behind the taking-up binder removal, and drying temperature is 80 ℃, makes the biscuit body.The biscuit body is carried out sintering under 1450 ℃, make required AZO target after the processing.Prepared AZO target color even, density is 5.42g/cm
3
Embodiment 2: takes by weighing 850 gram deionized waters, adds 100 gram acrylamides and 50 gram N, and N '-methylene-bisacrylamide, thorough mixing is mixed with premixed liquid.Adding aluminum oxide quality mark is 3% zinc oxide aluminum powder 2500 grams in premixed liquid, and adds 30 milliliters of AN-2000 as dispersion agent.On ball mill, carry out ball mill mixing, ball milling made the slurry thorough mixing even in 15 hours.
In slurry, add 20 milliliters of Tetramethyl Ethylene Diamines as catalyzer, add 80 milliliters of ammonium persulphates, pour in the mould after mixing as initiator.Place 60 ℃ of baking ovens to be cured, solidify after 10 minutes and take out.
To solidify the back base substrate and place polyglycol solution to carry out binder removal, the binder removal time is 24h, and base substrate carries out drying behind the taking-up binder removal, and drying temperature is 90 ℃, makes the biscuit body.The biscuit body is carried out sintering under 1500 ℃, make required AZO target after the processing.Prepared AZO target color even, density is 5.40g/cm
3
Embodiment 3: takes by weighing 750 gram deionized waters, adds 150 gram polyacrylamides and 100 gram N, and N '-methylene-bisacrylamide, thorough mixing is mixed with premixed liquid.Adding aluminum oxide quality mark is 2% zinc oxide aluminum powder 3600 grams in premixed liquid, and adds 25 milliliters of AN-2000 as dispersion agent.On ball mill, carry out ball mill mixing, ball milling made the slurry thorough mixing even in 20 hours.
In slurry, add 18 milliliters of Tetramethyl Ethylene Diamines as catalyzer, add 72 milliliters of ammonium persulphates, pour in the mould after mixing as initiator.Place 60 ℃ of baking ovens to be cured, solidify after 5 minutes and take out.
To solidify the back base substrate and place polyglycol solution to carry out binder removal, the binder removal time is 20h, and base substrate carries out drying behind the taking-up binder removal, and drying temperature is 80 ℃, makes the biscuit body.The biscuit body is carried out sintering under 1450 ℃, make required AZO target after the processing.Prepared AZO target color even, density is 5.45g/cm
3
Embodiment 4: take by weighing 400 gram deionized waters, add 70 gram methacrylic acids and 30 gram polydimethyl vinylformic acid, thorough mixing is mixed with premixed liquid.Adding aluminum oxide quality mark is 0.5% zinc oxide aluminum powder 2000 grams in premixed liquid, and adds 15 milliliters of AN-2000 as dispersion agent.On ball mill, carry out ball mill mixing, ball milling made the slurry thorough mixing even in 24 hours.
In slurry, add 11 milliliters of Tetramethyl Ethylene Diamines as catalyzer, add 44 milliliters of ammonium persulphates, pour in the mould after mixing as initiator.Place 80 ℃ of baking ovens to be cured, solidify after 15 minutes and take out.
To solidify the back base substrate and place polyglycol solution to carry out binder removal, the binder removal time is 15h, and base substrate carries out drying behind the taking-up binder removal, and drying temperature is 80 ℃, makes the biscuit body.The biscuit body is carried out sintering under 1400 ℃, make required AZO target after the processing.Prepared AZO target color even, density is 5.38g/cm
3
Claims (1)
1. method for preparing the AZO target with gel casting forming; It is characterized in that: gel casting forming prepares the method for AZO target; May further comprise the steps: take by weighing zinc oxide aluminum powder and premixed liquid; Add dispersion agent and mix, obtain the moulding slurry after the mixing, evenly add initiator, catalyzer in the slurry after; Pour mould into; Be cured at a certain temperature, after the curing green compact put into organic solvent and carry out binder removal, carry out drying behind the binder removal at a certain temperature and obtain biscuit; Obtain sintered sample by certain sintering schedule sintering; Obtain AZO target goods after the 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, the methacrylic acid a kind of; Used linking agent can be N, a kind of in N '-methylene-bisacrylamide, the polydimethyl vinylformic acid; To account for the premixed liquid massfraction be 5～20% to monomeric content in the premixed liquid, and it is 1～15% that linking agent accounts for the premixed liquid massfraction, and wherein the content of linking agent is less than monomeric content;
Said 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 the ball milling time is 0.5～48h;
The initiator that moulding slurry behind the described ball milling adds can be in ammonium persulphate, Potassium Persulphate, ydrogen peroxide 50 or the 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 ℃;
Said curing back sample carries out binder removal in organic solution, organic solution can for a kind of in polyoxyethylene glycol, the ethanol or they arbitrarily than mixture, the binder removal time is 4～48h; To carry out drying temperature be 20～200 ℃ to green compact behind the said binder removal;
Said dry back base substrate carries out sintering, and sintering temperature is 1300～1600 ℃.
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Cited By (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 |
| CN102942363A (en) * | 2012-11-22 | 2013-02-27 | 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 |
| CN103936425A (en) * | 2014-01-20 | 2014-07-23 | 清华大学 | Preparation method of ceramic plate |
| CN104152853A (en) * | 2014-07-08 | 2014-11-19 | 中国人民解放军国防科学技术大学 | Glass ceramic target material and preparation method thereof |
| CN105272209A (en) * | 2015-11-11 | 2016-01-27 | 攀枝花学院 | Preparation method of aluminum and titanium doped zinc oxide target material |
| CN105392444A (en) * | 2013-07-22 | 2016-03-09 | 义获嘉伟瓦登特公司 | Controlling of sintering kinetics of oxide 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 |
| 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 |
| 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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| 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)
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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 |
Cited By (15)
| 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 |
| CN102942363A (en) * | 2012-11-22 | 2013-02-27 | 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 |
| 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 |
| CN105392444B (en) * | 2013-07-22 | 2017-10-31 | 义获嘉伟瓦登特公司 | The control of the sintering kinetics of oxide ceramics |
| CN105392444A (en) * | 2013-07-22 | 2016-03-09 | 义获嘉伟瓦登特公司 | Controlling of sintering kinetics of oxide ceramics |
| CN103936425A (en) * | 2014-01-20 | 2014-07-23 | 清华大学 | Preparation method of ceramic plate |
| CN103936425B (en) * | 2014-01-20 | 2015-08-12 | 清华大学 | A kind of preparation method of ceramic plate |
| CN104152853A (en) * | 2014-07-08 | 2014-11-19 | 中国人民解放军国防科学技术大学 | Glass ceramic target material 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 |
| 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 |
| 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 |
| CN105272209A (en) * | 2015-11-11 | 2016-01-27 | 攀枝花学院 | Preparation method of aluminum and titanium doped zinc oxide target material |
| 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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