CN101580384B - Yttrium-doped AZO target and preparation method thereof - Google Patents
Yttrium-doped AZO target and preparation method thereof Download PDFInfo
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- CN101580384B CN101580384B CN200910108040A CN200910108040A CN101580384B CN 101580384 B CN101580384 B CN 101580384B CN 200910108040 A CN200910108040 A CN 200910108040A CN 200910108040 A CN200910108040 A CN 200910108040A CN 101580384 B CN101580384 B CN 101580384B
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- yttrium
- oxide
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- zinc oxide
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- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000000843 powder Substances 0.000 claims abstract description 17
- 239000011787 zinc oxide Substances 0.000 claims abstract description 17
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 14
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 238000005245 sintering Methods 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims description 12
- 239000000758 substrate Substances 0.000 claims description 12
- 229910052727 yttrium Inorganic materials 0.000 claims description 12
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 11
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 8
- 238000004080 punching Methods 0.000 claims description 7
- 238000000462 isostatic pressing Methods 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 5
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 4
- -1 polyoxyethylene Polymers 0.000 claims description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000013077 target material Substances 0.000 abstract description 3
- 238000002834 transmittance Methods 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- 238000005303 weighing Methods 0.000 abstract description 2
- 239000011230 binding agent Substances 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 238000000465 moulding Methods 0.000 abstract 1
- 238000003825 pressing Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 18
- 239000000463 material Substances 0.000 description 8
- 229920002799 BoPET Polymers 0.000 description 4
- 239000005041 Mylar™ Substances 0.000 description 4
- JYMITAMFTJDTAE-UHFFFAOYSA-N aluminum zinc oxygen(2-) Chemical compound [O-2].[Al+3].[Zn+2] JYMITAMFTJDTAE-UHFFFAOYSA-N 0.000 description 4
- 239000012789 electroconductive film Substances 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 238000004544 sputter deposition Methods 0.000 description 4
- 150000001241 acetals Chemical class 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 150000003746 yttrium Chemical class 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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- Physical Vapour Deposition (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention relates to an yttrium-doped AZO target material, which comprises 1-10% of aluminum oxide, 0.1-5% of yttrium oxide and the balance of zinc oxide by weight percentage. The invention also provides a preparation method of the yttrium-doped AZO target, which comprises the following steps: s1, weighing the raw materials of zinc oxide, aluminum oxide and yttrium oxide powder according to a predetermined proportion, adding a binder, adding water and mixing uniformly; s2, drying the mixture, and then pressing and molding the powder to form a blank with a predetermined shape and strength; s3, sintering the blank under normal pressure and normal atmosphere, wherein the sintering temperature is 1200-1600 ℃. The transparent conductive film prepared by the target material provided by the invention has the characteristics of high light transmittance, low resistivity, good film adhesion, compactness, integrity, good stability and the like.
Description
[technical field]
The present invention relates to field of photovoltaic materials, relate in particular to adulterated AZO target of a kind of yttrium and preparation method thereof.
[background technology]
Along with the development of liquid-crystal display and solar cell, make transparent conductive film become one of key material in recent years, how reducing the transparent conductive film material cost is present primary goal with the performance that improves thin-film material.Transparent conductive oxide (Transparent Conductive Oxide; Abbreviation TCO) film mainly comprises oxide compound and the composite multi-component oxide film material thereof of In, Sn, Sb, Zn and Cd; Not only transparent but also performance conduction is able to widespread use because of it for photoelectric characteristic such as have that the forbidden band is wide, visible range optical transmittance height and resistivity are low, transparent conductive oxide film.
The TCO film of zno-based has characteristics such as cost is low, nontoxic, stable height.Pure ZnO is the broad stopband direct band-gap semicondictor, has the resistivity of 0.1-10 Ω cm.In order to improve the conductivity of ZnO, adopt doped with Al unit usually to improve the carrier concentration of ZnO material usually and improve conductivity.The film that is doped with the ZnO material of Al and processes is the AZO film, has conductivity preferably, but loses efficacy owing to the unstable AZO film that causes of conductivity can appear in the AZO film after using the long period.In order to improve AZO adhesion of thin film and the electroconductibility that further improves film, normal employing improves its performance to the mode that the AZO film carries out further doping vario-property.For preparing this film, this just need provide the AZO target of corresponding other element doping.
[summary of the invention]
The purpose of this invention is to provide the adulterated AZO target material of a kind of yttrium, to be used to prepare the adulterated AZO nesa coating of yttrium.
For reaching the foregoing invention purpose, the present invention provides a kind of yttrium adulterated AZO target, and containing weight percent in this target is the aluminum oxide of 1-10%, the yttrium oxide of 0.1-5%, and the zinc oxide of surplus.
The present invention also provides the preparation method of the adulterated AZO target of this yttrium, may further comprise the steps:
S1 adds sticker in confirming that in advance good ratio takes by weighing raw material zinc oxide, aluminum oxide, yttrium oxide powder respectively, adds water to mix;
After the S2 mixture drying, powder is pressed, forms the base substrate of predetermined shape and intensity;
S3 is carrying out sintering with base substrate under normal pressure, normal atmosphere, sintering temperature is 1200-1600 ℃.
Among the above-mentioned preparation method provided by the present invention, in step S1, the weight percent between said zinc oxide, aluminum oxide, the yttrium oxide is that aluminum oxide 1-10%, yttrium oxide 0.1-5%, surplus are zinc oxide.
Among the above-mentioned preparation method, in step S1, said sticker is to be selected from Z 150PH, polyoxyethylene glycol or polyvinyl butyral acetal.
Among the above-mentioned preparation method, in step S1, in step S1, the addition of said sticker is the 0.5-2% of the gross weight of raw material zinc oxide, aluminum oxide, yttrium oxide.
Among the above-mentioned preparation method, in step S1, said zinc oxide, aluminum oxide, yttrium oxide powder are nanoscale powder, and granularity is the 20-200 nanometer.
Among the above-mentioned preparation method, the drying among the said step S2 is to adopt spray-drying process.
Among the above-mentioned preparation method; Compacting to mixture among the said step S2 comprises static pressure compactings such as punching block compacting and wet type; At first powder is carried out the punching block press forming; Form the base substrate of predetermined shape and intensity, then carry out the wet type isostatic pressing, the processing parameter of static pressure such as wet type is 100-160MPa.
Among the above-mentioned preparation method, also be included in the sintering of step S3 before, according to the dimensional requirement behind compacting back idiosome size and the sintering, the compacting idiosome is carried out mechanical workout.
Among the above-mentioned preparation method, also be included in the sintering of step S3 after, sintered compact is carried out mechanical workout, make it to become the target finished product that is suitable for using.
Can find out that from above technical scheme the adulterated AZO target of yttrium provided by the present invention is compared with traditional AZO target; Has following advantage: adopt the transmittance of nesa coating of this target preparation high, resistivity is low; Adhesive force is good, compact and complete, good stability.Can pass through the add-on of adjustment yttrium oxide and aluminum oxide, and then the carrier concentration and the energy gap of regulating film, improve electroconductibility and can meet transmitance.
The preparation method of target provided by the present invention is compared to AZO target preparation method of the prior art, and have following advantage: production technique is simple, and production cost is low; Can make the product of demands of different through the simple adjustment of processing parameter; Can make complex-shaped product; The utilization ratio of material is high.
[embodiment]
Embodiment 1
Get purity and be 99.95%, granularity is powder aluminum oxide 10g, yttrium oxide 5g, the zinc oxide 85g of 20-200 nanometer, adds 2 gram Z 150PH again, and add in the entry and mix; Then mixture is carried out spraying drying; Subsequently, dried powder is carried out the punching block press forming, form the base substrate of desired shape and intensity, then carry out the wet type isostatic pressing with 100MPa.Idiosome after the compacting sinters the block that density is theoretical density 96% at 1200 ℃ after being machined to suitable sintering, carry out mechanical workout once more, promptly processes standard-sized target.
Use this target, adopt the sedimentary method of radio-frequency sputtering on mylar or glass substrate, to deposit the zinc oxide aluminum transparent electroconductive film that contains yttrium, gained film thickness 900-1000nm, resistivity 0.5 * 10
-3Ω cm, the visible light transmissivity 86% under the 550nm wavelength.
Embodiment 2
Get purity and be 99.95%, granularity is powder aluminum oxide 1g, yttrium oxide 0.5g, the zinc oxide 98.5g of 20-200 nanometer, adds 0.5 gram polyoxyethylene glycol again, and add in the entry and mix; Then mixture is carried out spraying drying: EAT 180-270 ℃, air outlet temperature 100-125 ℃, rotary atomizer rotating speed 6000-12000 per hour changes; Subsequently, dried powder is carried out the punching block press forming, form the base substrate of desired shape and intensity, then carry out the wet type isostatic pressing with 160MPa.Idiosome after the compacting sinters the block that density is theoretical density 96% at 1600 ℃ after being machined to suitable sintering, carry out mechanical workout once more, promptly processes standard-sized target.
Use this target, adopt the sedimentary method of radio-frequency sputtering on mylar or glass substrate, to deposit the zinc oxide aluminum transparent electroconductive film that contains yttrium, gained film thickness 500-600nm, resistivity 1.6 * 10
-3Ω cm, the visible light transmissivity 95% under the 550nm wavelength.
Embodiment 3
Get purity and be 99.95%, granularity is powder aluminum oxide 5g, yttrium oxide 1.5g, the zinc oxide 93 .5g of 20-200 nanometer, adds 1.0 gram polyvinyl butyral acetals again, and add in the entry and mix; Then mixture is carried out spraying drying: EAT 180-270 ℃, air outlet temperature 100-125 ℃, rotary atomizer rotating speed 6000-12000 per hour changes; Subsequently, dried powder is carried out the punching block press forming, form the base substrate of desired shape and intensity, then carry out the wet type isostatic pressing with 130MPa.Idiosome after the compacting sinters the block that density is theoretical density 96% at 1300 ℃ after being machined to suitable sintering, carry out mechanical workout once more, promptly processes standard-sized target.
Use this target, adopt the sedimentary method of radio-frequency sputtering on mylar or glass substrate, to deposit the zinc oxide aluminum transparent electroconductive film that contains yttrium, gained film thickness 700-800nm, resistivity 0.9 * 10
-3Ω cm, the visible light transmissivity 89% under the 550nm wavelength.
Embodiment 4
Get purity and be 99.95%, granularity is powder aluminum oxide 3.5g, yttrium oxide 1.5g, the zinc oxide 96g of 20-200 nanometer, adds 1.2 gram polyoxyethylene glycol again, and add in the entry and mix; Then mixture is carried out spraying drying: EAT 180-270 ℃, air outlet temperature 100-125 ℃, rotary atomizer rotating speed 6000-12000 per hour changes; Subsequently, dried powder is carried out the punching block press forming, form the base substrate of desired shape and intensity, then carry out the wet type isostatic pressing with 150MPa.Idiosome after the compacting sinters the block that density is theoretical density 96% at 1380 ℃ after being machined to suitable sintering, carry out mechanical workout once more, promptly processes standard-sized target.
Use this target, adopt the sedimentary method of radio-frequency sputtering on mylar or glass substrate, to deposit the zinc oxide aluminum transparent electroconductive film that contains yttrium, gained film thickness 600-700nm, resistivity 1.2 * 10
-3Ω cm, the visible light transmissivity 92% under the 550nm wavelength.
The above embodiment has only expressed several kinds of embodiments of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to claim of the present invention.Should be pointed out that for the person of ordinary skill of the art under the prerequisite that does not break away from the present invention's design, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with accompanying claims.
Claims (1)
1. the preparation method of the adulterated AZO target of yttrium is characterized in that, comprises following steps:
Get purity and be 99.95%, granularity is powder aluminum oxide 1g, yttrium oxide 0.5g, the zinc oxide 98.5g of 20-200 nanometer, adds 0.5 gram polyoxyethylene glycol again, and add in the entry and mix; Then mixture is carried out spraying drying: EAT 180-270 ℃, air outlet temperature 100-125 ℃, rotary atomizer rotating speed 6000-12000 per hour changes; Subsequently; Dried powder is carried out the punching block press forming, form the base substrate of desired shape and intensity, then carry out the wet type isostatic pressing with 160MPa; Idiosome after the compacting is after being machined to suitable sintering; Sinter the block that density is theoretical density 96% at 1600 ℃, carry out mechanical workout once more, promptly process standard-sized target.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN200910108040A CN101580384B (en) | 2009-06-10 | 2009-06-10 | Yttrium-doped AZO target and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910108040A CN101580384B (en) | 2009-06-10 | 2009-06-10 | Yttrium-doped AZO target and preparation method thereof |
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| Publication Number | Publication Date |
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| CN101580384A CN101580384A (en) | 2009-11-18 |
| CN101580384B true CN101580384B (en) | 2012-09-26 |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153352B (en) * | 2010-12-17 | 2015-05-20 | 西北稀有金属材料研究院 | Composite adhesive and application thereof in preparation of sintering target |
| CN102351434B (en) * | 2011-07-08 | 2013-07-24 | 华南理工大学 | Preparation method of cerium-aluminum codoped zinc oxide film |
| CN102311671B (en) * | 2011-08-30 | 2014-07-30 | 河南华美新材料科技有限公司 | AZO transparent conductive film paint, glass plated with the paint and preparation method thereof |
| CN105573004A (en) * | 2016-01-21 | 2016-05-11 | 内蒙古坤瑞玻璃股份有限公司 | Electrochromism bulletproof and explosion-proof glass and preparation method thereof |
| CN105601125A (en) * | 2016-01-21 | 2016-05-25 | 内蒙古坤瑞玻璃股份有限公司 | Transparent electroconductive glass for electrochromic glass and preparation method of transparent electroconductive glass |
| CN106187151A (en) * | 2016-07-20 | 2016-12-07 | 浙江舒玛新材料有限公司 | A kind of aluminum doped yttrium zinc oxide ceramic target and preparation method thereof |
| 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 |
| CN111018515A (en) * | 2019-12-26 | 2020-04-17 | 广州市尤特新材料有限公司 | Method for manufacturing target material and target material |
| 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 |
| CN116102346B (en) * | 2023-04-04 | 2023-06-30 | 广州市尤特新材料有限公司 | Metal-doped AZO target and preparation method thereof |
| CN116751048A (en) * | 2023-06-05 | 2023-09-15 | 洛阳晶联光电材料有限责任公司 | Gallium-aluminum doped zinc oxide target material and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1063317B1 (en) * | 1998-03-05 | 2003-07-30 | Asahi Glass Company Ltd. | Sputtering target, transparent conductive film, and method for producing the same |
| CN101333644A (en) * | 2007-06-28 | 2008-12-31 | 三星康宁精密琉璃株式会社 | Zinc oxide analog amorphous film sputtering target and its manufacture method |
-
2009
- 2009-06-10 CN CN200910108040A patent/CN101580384B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1063317B1 (en) * | 1998-03-05 | 2003-07-30 | Asahi Glass Company Ltd. | Sputtering target, transparent conductive film, and method for producing the same |
| CN101333644A (en) * | 2007-06-28 | 2008-12-31 | 三星康宁精密琉璃株式会社 | Zinc oxide analog amorphous film sputtering target and its manufacture method |
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| CN101580384A (en) | 2009-11-18 |
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