CN102942363B - Method for preparing AZO target by powdery slurry pouring - Google Patents
Method for preparing AZO target by powdery slurry pouring Download PDFInfo
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Abstract
The invention relates to a method for preparing an AZO target by powdery slurry pouring. The method includes firstly mixing an AZO coprecipitation powder or a mixed powder of zinc oxide and aluminum oxide with deionized water, a dispersing agent and an adhesion agent in a ball-milling mode to obtain a mixture, injecting the mixture into a die to be formed, drying, degreasing, and sintering to process the mixture to a finished product of the AZO target with required size. According to the method for preparing the AZO target by the powdery slurry pouring, the prepared AZO target is high in consistency and good in structure uniformity, the large-size AZO target is easy to prepare, the formed green body is good in uniformity, and during the later sintering process, the green body is uniform in contraction and free of deformation and cracking. The method is simple in processing operation, easy to control and suitable for industrial production.
Description
Technical field
The present invention relates to photoelectric functional material field, more particularly relate to a kind of use slurry casting to prepare AZO(Al-doped in Zinc Oxide) method of target.
Background technology
Along with the fast development in the fields such as semi-conductor, computer, sun power, transparent conductive oxide (TCO) film is owing to having good electroconductibility and high-transmission rate concurrently, the high-resolution flat-panel monitors such as transparency electrode, liquid-crystal display (LCD), plasma display (PDP), Organic Light Emitting Diode (OLED) can be widely used in, in solar cell and various optoelectronic device.Present industrial most widely used transparent conductive film is ITO(Tin doped Indium Oxide) film, but it has expensive, under high temperature, transmitance reduces rapidly, and is easily reduced in hydrogen plasma, is applied in solar cell the shortcomings such as the efficiency reduction making battery; And ZnO is cheap, abundant raw material, stablizes than ITO in hydrogen ion atmosphere, can not only make good semi-conductor and piezoelectric membrane, also make good transparent conductive film by doping, in ZnO, mix optics and electric property that Ga, Al, In or F ion can improve ZnO film.Wherein, AZO(Al-doped in Zinc Oxide) film research the most extensively and the most deep, in thin-film solar cells, obtain certain applications at present.AZO target as sputter film is known as one of the most promising thin-film material at present.
AZO target is one of important sources of preparation AZO film.The quality good or not of target directly decides the quality of film.The technical problem underlying that current AZO sputtering target material faces has: how big area prepares AZO sputters ceramic target.Keep the large-scale development owing to preparing film, corresponding ceramic target size also will increase considerably.Problems faced is: 1) how to guarantee the microtexture of large size ceramic sputtering target material and the homogeneity of tissue, avoids producing defect; 2) ceramic sputtering target material density how is improved; 3) explore Financial cost lower, the preparation technology that production efficiency is higher is the striving direction of ceramic target manufacture from now on.
In current AZO target process of producing product, dry-pressing formed, cold isostatic compaction is ceramic powder molding mode conventional at present.The dry-pressing formed preparation to the larger base substrate of size has certain difficulty, and forming mould loss is comparatively large, and moulding process is complicated, and the density skewness of finished base substrate, sintering process cloth uniform shrinkage easily causes the phenomenons such as cracking, layering.The molding blank density that isostatic cool pressing is prepared is high, good uniformity, and cost is low, be also one of the most frequently used forming method, but this forming method requires high to forming mould, and Mold Making difficulty is comparatively large, and is only applicable to the shaping of simple shape.
Forming method up-to-date is at present gel casting forming, as patent CN102351526 A mentions, by AZO powder and premixed liquid, shaping slurry is obtained after the mixing such as dispersion agent, again initiator, catalyzer are evenly added after in slurry, pour mould into, be cured at a certain temperature, after solidification, green compact are put into organic solvent and carry out binder removal, carry out drying after binder removal at a certain temperature and obtain biscuit; Sintered sample is obtained by certain sintering schedule sintering; AZO target article is obtained after processing.The method equipment requirements is simple, and technique is convenient, and cost is low, but the AZO target product density prepared is not high, and production process not easy operation control.
The sintering process of ceramic target mainly contains normal pressure-sintered, HIP sintering, hot pressed sintering, vacuum and protective atmosphere sintering etc.Because HIP sintering combines hot pressing advantage different from hot isostatic pressing, powder at high temperature thermoplasticity is better, and deformation resistance is little, can be shaping at lower pressure, thus sintering time is shorter, can suppress growing up of crystal grain very well, is one of common method of preparation super-high density ceramic target.Heat and other static pressuring processes cost is higher, and production process is technical comparatively strong, and target size limits by mould, also have impact on the application of technique.
The normal pressure-sintered method of pottery is the most frequently used sintering process; first the target of the certain density of dry-pressing formed preparation is adopted to mould base; under vacuum or certain protective atmosphere and sintering temperature, target powder base is sintered; by the setting of sintering schedule and the control of atmosphere; make the growth of target powder base crystal grain in certain limit; thus ensure that the density of target finished product is high, the features such as uniform crystal particles.Japan employing normal pressure-sintered ceramic in research comparatively early, input cost is high, has stronger technical superiority at present.Normal pressure-sintered method main advantage is that the target size prepared is comparatively large, and in industrial application, production efficiency is higher, equipment cost is low, finished product production cost is low and target quality better, to a certain degree can meet the needs of high-end field sputtering.
Vacuum hot-pressing effectively make use of the advantage of hot pressed sintering and vacuum atmosphere, can obtain purity good, the ceramic target that density is higher.This preparation technology is stressed effect decline sintering temperature and low and sintering time outside, but this technique exists that hot-press equipment volume is restricted and mould cost is high, and the shortcomings such as size is less, industrial application is less.
Summary of the invention
The object of the invention is to the defect overcoming above-mentioned prior art, a kind of biscuit that can be easy to prepare large-size target is provided, and target product density good uniformity, production process is simple, easy handling controls, production cost is low, the shaping method preparing AZO target of the slurry casting that production efficiency is high.
The present invention takes following technical proposals:
A kind of method using slurry casting to prepare AZO target, it is characterized in that: first the mixed powder of AZO co-precipitation powder or zinc oxide and aluminum oxide is carried out ball milling with deionized water, dispersion agent, binding agent and mix, inject in-mold molding, dry, degreasing, sintering post-treatment becomes the AZO target finished product of desired size.
In the mixed powder of above-mentioned AZO co-precipitation powder or zinc oxide and aluminum oxide, aluminum oxide accounts for 1 ~ 5wt% of powder total amount.
The add-on of above-mentioned deionized water is 0.3 ~ 1.5 times of the mixed powder quality of AZO co-precipitation powder or zinc oxide and aluminum oxide.
Above-mentioned dispersion agent is polymine or ammonium polyacrylate, and its add-on is 0.1 ~ 2.5wt% of powder total amount.
Above-mentioned binding agent is the combination of one or more in polyvinyl alcohol, polyethylene glycol or polymethyl acid alcohol, and its add-on is 0.5 ~ 3wt% of powder total amount.
Above-mentioned ball milling mixing adopts zirconia ball or resin balls, ball milling mixing time 3 ~ 48h.
Above-mentioned powder first filters before injection in-mold molding, and then add proper quantity of defoaming agent removing bubble, described defoamer is glycerine polyethenoxy ether, and add-on is 0.1 ~ 0.5wt% of slip total amount.
Above-mentioned drying means is: first at room temperature 20 ~ 35 DEG C by shaping biscuit drying 2 ~ 4 days, then place in baking oven and dry, oven temperature is 50 ~ 120 DEG C, dry 2 ~ 10h.
Above-mentioned degreasing carries out in debinding furnace, skimming temp 400 ~ 600 DEG C, temperature rise rate 3 ~ 15 DEG C/h.
Above-mentioned sintering refers under air atmosphere condition, under 1200 ~ 1500 DEG C of temperature ranges, and insulation 2 ~ 8h., technical solution of the present invention compared with prior art, there is following beneficial effect and advantage:
1. the AZO target density prepared by the present invention is high, and relative density can reach more than 96%, and microtexture, homogeneity of structure is good.
2. the present invention adopts powder slurry casting, easily preparation large size AZO target, and molding blank good uniformity, in later stage sintering process base substrate shrink even, indeformable, do not ftracture.
3. the present invention is simple to operate in implementation process, is easy to control, and is applicable to suitability for industrialized production.
4. production cost of the present invention is low, remarkable in economical benefits.
Embodiment
Below specific embodiments of the invention, only as further illustrating of the present invention, not as limitation of the present invention; for those skilled in the art; under the prerequisite not departing from thinking of the present invention, done part is improved or change, all should belong to protection scope of the present invention.
Embodiment 1
By AZO co-precipitation powder 1000g, wherein aluminum oxide accounts for the 3wt% of AZO powder quality, add deionized water 1500g, zirconia ball 2400g, add polymine 1.0g again, polyvinyl alcohol 5.0g, mixing and ball milling 3h, after ball milling, slip is leached and add glycerine polyethenoxy ether 1.0g, carry out degasification froth breaking, slowly inject in gypsum mold shaping when slip bubble-free, gypsum mold squirts with a small amount of water before using in advance, cause biscuit defect too soon with absorb-free, molding biscuit to be placed at room temperature 28 DEG C dry 2 days.And then biscuit is put into loft drier dry 8 hours at 50 DEG C, finally dried biscuit is placed degreasing in debinding furnace, skimming temp is 500 DEG C, and temperature rise rate is 10 DEG C/h, top temperature insulation 5h.Sintered by biscuit after degreasing, sintering atmosphere is under air conditions, and sintering temperature is up to 1320 DEG C, and top temperature insulation 3.5h, finally obtain the sintered sample that relative density is 98.7%.
Embodiment 2
By AZO co-precipitation powder 1000g, wherein aluminum oxide accounts for the 1wt% of AZO powder quality, add deionized water 1000g, zirconia ball 2400g, add polymine 15g again, binding agent polyvinyl alcohol 15g, mixing and ball milling 10h, after ball milling, slip is leached and add glycerine polyethenoxy ether 3.0g and carry out froth breaking, degasification, slowly inject in gypsum mold shaping when slip bubble-free, gypsum mold squirts with a small amount of water before using in advance, causes biscuit defect too soon with absorb-free, molding biscuit to be placed at room temperature 20 DEG C dry 4 days.And then biscuit is put into loft drier dry 4 hours at 70 DEG C, finally dried biscuit is placed degreasing in debinding furnace, skimming temp is 600 DEG C, and temperature rise rate is 15 DEG C/h, top temperature insulation 2h.Sintered by biscuit after degreasing, sintering atmosphere is that under air conditions, sintering temperature is up to 1400.
Embodiment 3
By AZO co-precipitation powder 1500g, wherein aluminum oxide accounts for the 5wt% of AZO powder quality, add deionized water 450g, zirconia ball 3600g, add ammonium polyacrylate 37.5g again, binding agent polymethyl acid alcohol 45g, mixing and ball milling 38h, after ball milling, slip is leached and add glycerine polyethenoxy ether 9.0g and carry out froth breaking, degasification, slowly inject in gypsum mold shaping when slip bubble-free, gypsum mold squirts with a small amount of water before using in advance, causes biscuit defect too soon with absorb-free, molding biscuit to be placed at room temperature 30 DEG C dry 3 days.And then biscuit is put into loft drier dry 2 hours at 120 DEG C, finally dried biscuit is placed degreasing in debinding furnace, skimming temp is 600 DEG C, and temperature rise rate is 5 DEG C/h, top temperature insulation 10h.Sintered by biscuit after degreasing, sintering atmosphere is under air conditions, and sintering temperature is up to 1200 DEG C, and top temperature insulation 8h, finally obtain the sintered sample that relative density is 98.2%.
Embodiment 4
By the powder mix 1500g of zinc oxide and aluminum oxide, wherein aluminum oxide accounts for the 1wt% of mixed powder total amount, add deionized water 675g, zirconia ball 3600g, add polymine 27.0g again, binding agent polyvinyl alcohol 37.5g, mixing and ball milling 45h, after ball milling, slip is leached and add glycerine polyethenoxy ether 9.0g and carry out froth breaking, degasification, slowly inject in gypsum mold shaping when slip bubble-free, gypsum mold squirts with a small amount of water before using in advance, causes biscuit defect too soon with absorb-free, molding biscuit to be placed at room temperature 35 DEG C dry 3 days.And then biscuit is put into loft drier dry 3 hours at 60 DEG C, finally dried biscuit is placed degreasing in debinding furnace, skimming temp is 500 DEG C, and temperature rise rate is 5 DEG C/h, top temperature insulation 15h.Sintered by biscuit after degreasing, sintering atmosphere is under air conditions, and sintering temperature is up to 1500 DEG C, and top temperature insulation 2h, finally obtain the sintered sample that relative density is 98.8%.
Embodiment 5
By the powder mix 1500g of zinc oxide and aluminum oxide, wherein aluminum oxide accounts for the 3wt% of mixed powder total amount, add deionized water 720g, zirconia ball 3600g, add ammonium polyacrylate 22.5g again, binding agent polyvinyl alcohol 30.0g, mixing and ball milling 38h, after ball milling, slip is leached and add glycerine polyethenoxy ether 10.0g and carry out froth breaking, degasification, slowly inject in gypsum mold shaping when slip bubble-free, gypsum mold squirts with a small amount of water before using in advance, causes biscuit defect too soon with absorb-free, molding biscuit to be placed at room temperature 30 DEG C dry 3 days.And then biscuit is put into loft drier dry 2 hours at 120 DEG C, finally dried biscuit is placed degreasing in debinding furnace, skimming temp is 450 DEG C, and temperature rise rate is 3 DEG C/h, top temperature insulation 10h.Sintered by biscuit after degreasing, sintering atmosphere is under air conditions, and sintering temperature is up to 1350 DEG C, and top temperature insulation 4h, finally obtain the sintered sample that relative density is 97.8%.
Embodiment 6
By the powder mix 1500g of zinc oxide and aluminum oxide, wherein aluminum oxide accounts for the 5wt% of mixed powder total amount, add deionized water 1200g, zirconia ball 3600g, add polymine 4.5g again, binding agent polyvinyl alcohol 30.0g, mixing and ball milling 35h, after ball milling, slip is leached and add glycerine polyethenoxy ether 4.0g and carry out froth breaking, degasification, slowly inject in gypsum mold shaping when slip bubble-free, gypsum mold squirts with a small amount of water before using in advance, causes biscuit defect too soon with absorb-free, molding biscuit to be placed at room temperature 38 DEG C dry 2 days.And then biscuit is put into loft drier dry 5 hours at 60 DEG C, finally dried biscuit is placed degreasing in debinding furnace, skimming temp is 400 DEG C, and temperature rise rate is 3 DEG C/h, top temperature insulation 10h.Sintered by biscuit after degreasing, sintering atmosphere is under air conditions, and sintering temperature is up to 1250 DEG C, and top temperature insulation 5h, finally obtain the sintered sample that relative density is 99.2%.
Embodiment 7
By AZO powder 5000g, wherein aluminum oxide accounts for the 2wt% of AZO powder quality, add deionized water 3000g, zirconia ball 12000g, add dispersants ammonium polyacrylate 50g again, the mixture 100g of binding agent polyvinyl alcohol and polyethylene glycol, mixing and ball milling 48h, after ball milling, slip is leached and add defoamer, slowly inject in gypsum mold shaping when slip bubble-free, gypsum mold squirts with a small amount of water before using in advance, biscuit defect is caused too soon with absorb-free, molding biscuit to be placed under room temperature 30 DEG C of conditions dry 3 days, and then biscuit is put into loft drier dry 3 hours at 80 DEG C, finally dried biscuit is placed degreasing in debinding furnace, skimming temp is 500 DEG C, temperature rise rate is 10 DEG C/h, top temperature insulation 6h.Sintered by biscuit after degreasing, sintering atmosphere is under air conditions, and sintering temperature is up to 1380 DEG C, and top temperature insulation 5h, obtains the sintered sample that relative density is 98.9%.Sintered sample can obtain the AZO target being of a size of 300 × 270 × 10mm after processing grinding and polishing.
Embodiment 8
By AZO powder 5000g, wherein aluminum oxide accounts for the 5wt% of AZO powder quality, add deionized water 4000g, zirconia ball 12000g, add polyethylene of dispersing agent imines 40g again, the mixture 120g of binding agent polyvinyl alcohol and polyethylene glycol, mixing and ball milling 48h, after ball milling, slip is leached and add defoamer, slowly inject in gypsum mold shaping when slip bubble-free, gypsum mold squirts with a small amount of water before using in advance, biscuit defect is caused too soon with absorb-free, molding biscuit to be placed under room temperature 30 DEG C of conditions dry 3 days, and then biscuit is put into loft drier dry 3 hours at 80 DEG C, finally dried biscuit is placed degreasing in debinding furnace, skimming temp is 500 DEG C, temperature rise rate is 10 DEG C/h, top temperature insulation 6h.Sintered by biscuit after degreasing, sintering atmosphere is under air conditions, and sintering temperature is up to 1350 DEG C, and top temperature insulation 5h, obtains the sintered sample that relative density is 99.6%.Sintered sample can obtain the AZO target being of a size of 300 × 270 × 10mm after processing grinding and polishing.
Embodiment 9
By the mixed powder 5000g of zinc oxide and aluminum oxide, wherein aluminum oxide accounts for the 2.5wt% of AZO powder quality, add deionized water 2500g, zirconia ball 12000g, add dispersants ammonium polyacrylate 50g again, the mixture 125g of binding agent polyvinyl alcohol and polyethylene glycol, mixing and ball milling 48h, after ball milling, slip is leached and add defoamer, slowly inject in gypsum mold shaping when slip bubble-free, gypsum mold squirts with a small amount of water before using in advance, biscuit defect is caused too soon with absorb-free, molding biscuit to be placed under room temperature 30 DEG C of conditions dry 3 days, and then biscuit is put into loft drier dry 8 hours at 60 DEG C, finally dried biscuit is placed degreasing in debinding furnace, skimming temp is 600 DEG C, temperature rise rate is 10 DEG C/h, top temperature insulation 4h.Sintered by biscuit after degreasing, sintering atmosphere is under air conditions, and sintering temperature is up to 1400 DEG C, and top temperature insulation 5h, obtains the sintered sample that relative density is 99.1%.Sintered sample can obtain the AZO target being of a size of 300 × 270 × 10mm after processing grinding and polishing.
Claims (2)
1. the method using slurry casting to prepare AZO target, it is characterized in that: first the mixed powder of AZO co-precipitation powder or zinc oxide and aluminum oxide is carried out ball milling with deionized water, dispersion agent, binding agent and mix, filter, add proper quantity of defoaming agent removing bubble, described defoamer is glycerine polyethenoxy ether, and add-on is 0.1 ~ 0.5wt% of slip total amount, then in-mold molding is injected, drying, degreasing, sintering post-treatment becomes the AZO target finished product of desired size;
In the mixed powder of above-mentioned AZO co-precipitation powder or zinc oxide and aluminum oxide, aluminum oxide accounts for 1 ~ 5wt% of powder total amount;
The add-on of above-mentioned deionized water is 0.3 ~ 1.5 times of the mixed powder quality of AZO co-precipitation powder or zinc oxide and aluminum oxide;
Above-mentioned dispersion agent is polymine or ammonium polyacrylate, and its add-on is 0.1 ~ 2.5wt% of powder total amount;
Above-mentioned binding agent is the combination of one or more in polyvinyl alcohol or polyethylene glycol, and its add-on is 0.5 ~ 3wt% of powder total amount;
Above-mentioned drying means is: first at room temperature 20 ~ 35 DEG C by shaping biscuit drying 2 ~ 4 days, then place in baking oven and dry, oven temperature is 50 ~ 120 DEG C, dry 2 ~ 10h;
Above-mentioned degreasing carries out in debinding furnace, skimming temp 400 ~ 600 DEG C, temperature rise rate 3 ~ 15 DEG C/h;
Above-mentioned sintering refers under air atmosphere condition, under 1200 ~ 1500 DEG C of temperature ranges, and insulation 2 ~ 8h.
2. prepare the method for AZO target according to use slurry casting according to claim 1, it is characterized in that: above-mentioned ball milling mixing adopts zirconia ball or resin balls, ball milling mixing time 3 ~ 48h.
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Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103205707B (en) * | 2013-04-24 | 2015-11-04 | 研创应用材料（赣州）有限公司 | The preparation method of a kind of conductive oxide target and conductive oxide film |
| CN103332929B (en) * | 2013-07-17 | 2016-01-13 | 国家纳米技术与工程研究院 | A kind of moulding process of high-compactness large size AZO target material blank body |
| CN104416160B (en) * | 2013-09-11 | 2017-04-19 | 安泰科技股份有限公司 | High-density zinc oxide based target and preparation method thereof |
| CN103510059B (en) * | 2013-10-21 | 2016-08-17 | 研创应用材料（赣州）股份有限公司 | A kind of method preparing Novel copper alloy protective layer material and thin film stack |
| CN103708819B (en) * | 2013-12-20 | 2016-06-15 | 福建省诺希新材料科技有限公司 | A kind of residual target of zinc oxide aluminum utilizing recovery prepares the method for the residual target powder of zinc oxide aluminum and the application of this powder |
| CN107032781A (en) * | 2017-05-26 | 2017-08-11 | 安徽拓吉泰新型陶瓷科技有限公司 | A kind of preparation method of injection forming high density AZO targets |
| CN107140972A (en) * | 2017-06-12 | 2017-09-08 | 安徽拓吉泰新型陶瓷科技有限公司 | A kind of preparation method of high density, low-resistivity AZO targets |
| CN107522483A (en) * | 2017-06-26 | 2017-12-29 | 广西新未来信息产业股份有限公司 | A kind of preparation method of AZO targets |
| CN109280877A (en) * | 2018-11-13 | 2019-01-29 | 江苏迪丞光电材料有限公司 | The preparation method and AZO target of AZO target |
| CN111440000B (en) * | 2020-04-24 | 2022-04-29 | 河北恒博新材料科技股份有限公司 | Preparation method of large-size rotary ceramic target |
| CN113213913A (en) * | 2021-04-16 | 2021-08-06 | 先导薄膜材料（广东）有限公司 | Preparation method of zinc aluminum oxide target material |
| CN113788669A (en) * | 2021-10-20 | 2021-12-14 | 南宁西桂微电子有限公司 | Preparation method of ITO sputtering target material |
| CN114230332A (en) * | 2022-01-15 | 2022-03-25 | 郑州大学 | AZO target and preparation method thereof |
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| CN102212781A (en) * | 2011-05-10 | 2011-10-12 | 孔伟华 | Method for manufacturing high-density and low-cost zinc oxide aluminum sputtering target |
| CN102351526A (en) * | 2011-06-11 | 2012-02-15 | 江苏尚易新材料科技有限公司 | Method for preparing AZO target materials by adopting gel injection molding forming |
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| CN102747334B (en) * | 2012-07-30 | 2014-03-12 | 中国科学院宁波材料技术与工程研究所 | Zinc-oxide-based transparent conductive film and preparation method thereof |
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| CN102212781A (en) * | 2011-05-10 | 2011-10-12 | 孔伟华 | Method for manufacturing high-density and low-cost zinc oxide aluminum sputtering target |
| CN102351526A (en) * | 2011-06-11 | 2012-02-15 | 江苏尚易新材料科技有限公司 | Method for preparing AZO target materials by adopting gel injection molding forming |
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Effective date of registration: 20180726 Address after: 753000 No. 119 metallurgical Road, Dawukou District, Shizuishan, the Ningxia Hui Autonomous Region Patentee after: Ningxia medium color new materials Co., Ltd. Address before: 753000 No. 119 metallurgical Road, Dawukou District, Shizuishan, the Ningxia Hui Autonomous Region Patentee before: National Special Metal Materials Engineering Research Center of Tantalum and Niobium |