CN102191465A - Indium-doped zinc oxide target material and preparation method of transparent conducting film - Google Patents
Indium-doped zinc oxide target material and preparation method of transparent conducting film Download PDFInfo
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- CN102191465A CN102191465A CN2010101275817A CN201010127581A CN102191465A CN 102191465 A CN102191465 A CN 102191465A CN 2010101275817 A CN2010101275817 A CN 2010101275817A CN 201010127581 A CN201010127581 A CN 201010127581A CN 102191465 A CN102191465 A CN 102191465A
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Abstract
The invention relates to an indium-doped zinc oxide target material and a preparation method of a transparent conducting film. Indium-doped zinc oxide powder is prepared by the liquid phase method or the solid phase method; the high-purity indium-doped zinc oxide ceramic target material is obtained by performing isostatic pressing, vacuum sintering and atmosphere annealing on the indium-doped zinc oxide powder; and the transparent conducting film is prepared from the target material through the sputtering method. The mass content of indium oxide is 0.5 to 10 percent; the purity of the target material is not less than 99.9 percent; and the relative density of the target material is not less than 95 percent and can be up to 99.5 percent. The transparent conducting film prepared from the target material through the sputtering method has high photoelectric property; the resistivity can be 7*10<-4> Omega cm at most; and in a visible light range (400 to 800nm), the highest transmissivity can be up to 92 percent and the average transmissivity is not less than 84 percent. Therefore, the transparent conducting film can be applied to fields of solar cells, light-emitting diodes, panels, liquid crystal displays and the like.
Description
Technical field
The present invention relates to the preparation method of a kind of indium doping zinc-oxide sputtering target material and nesa coating thereof, belong to technical field of optoelectronic functional materials.
Background technology
Transparent conductive oxide (transparent conductive oxide is called for short TCO) is a kind of important optoelectronic functional materials, and it has very high transmitance to visible light, and infrared light is had very high reflectivity, has good conductivity simultaneously.Therefore, TCO is widely used in fields such as solar cell, flat board and liquid-crystal display, photodiode and thermal radiation speculum.Tin-doped indium oxide (Indium Tin Oxide is called for short ITO) is a current application nesa coating the most widely, and the mass content of Indium sesquioxide reaches 90% in this film.As everyone knows, indium metal is the content rareness in the earth's crust, is scarce resource, costs an arm and a leg; And ITO is unstable in hydrogen plasma.Therefore, low indium content nesa coating that must development of new substitutes ITO.The crude zinc oxide materials source is abundant, and low price is nontoxic, has good stability in hydrogen plasma; Be a kind of wide bandgap semiconductor, visible light is had high permeability, realize that easily the n type mixes, and nesa coating conductivity and ITO after the n type mixes are approaching.Therefore, be that matrix carries out adulterated nesa coating and become current research emphasis with zinc oxide, in a lot of fields the development trend that progressively replaces ITO is arranged.
Sputtering method is the main method of preparation TCO, and the quality of sputtering target material will directly have influence on the quality of TCO film.The preparation technology of ITO target is very ripe at present, and the research of zno-based nesa coating target has also obtained certain progress.Chinese patent prospectus CN 1413947A discloses a kind of preparation method who adopts zinc oxide and Indium sesquioxide mixed powder through the zinc indium oxide ceramic target of coldmoulding and the normal atmosphere sintering preparation of normal pressure, and the mass content of its Indium sesquioxide is 2-7%.Chinese patent prospectus CN101208452A, 101208453A and 101326304A disclose the preparation method of the indium zinc oxide target through adding the preparation of micro-zirconium white or aluminum oxide.Chinese patent prospectus CN 101440470A discloses and has a kind ofly prepared the preparation method that zinc oxide aluminum powder and hot pressed sintering prepare AZO target material through liquid phase method, and prepared target relative density is not less than 95%.Chinese patent prospectus CN 1289128A discloses and has a kind ofly gone out aluminium-doped zinc oxide (AZO) target that aluminum oxide total mass content is 1-6% (or pure aluminium powder 0.5-3%) by oxide powder and zinc and aluminum oxide (or pure aluminium powder) intermingling sintering, and the target relative density can reach more than 94%.The preparation method of the AZO ceramic target that it is 1at-10at% that Chinese patent prospectus CN 101285164A discloses a kind of aluminium element content.It is the Indium sesquioxide of 90-99% and Indium sesquioxide and the zinc oxide agglomerating InGaZn of 1-10% by mass content that Chinese patent prospectus CN 1558962A discloses a kind of
7O
10Target, the indium content of this target is the same with ITO, all greater than 90%.From present disclosed patent, also do not adopt the zno-based nesa coating target of vacuum sintering preparation.
The present invention adopts liquid phase or solid phase method to prepare indium doping zinc-oxide powder, obtains indium doping zinc-oxide ceramic target through cold isostatic compaction, vacuum sintering and atmosphere annealing, and uses this target to prepare nesa coating through sputtering method.The nesa coating of this method preparation has good photoelectric properties, and technology is simple, and is with low cost, is expected to substitute ITO.
Summary of the invention
The present invention proposes the method for preparing indium doping zinc-oxide target, and proposed to adopt this target to prepare the method for nesa coating.This method can be prepared high-density, highly purified indium doping zinc-oxide target easily and have excellent conductive performance and the nesa coating of high permeability.
The present invention adopts following technical scheme:
1. indium doping zinc-oxide target, it is characterized in that: this target is formed through sintering by zinc, indium oxide powder; Wherein the mass content of Indium sesquioxide is 0.5-10%; The purity of target is not less than 99.9%; The relative density of target is not less than 95%, reaches as high as 99.5%.
2. the preparation method of 1 described indium doping zinc-oxide target, it is characterized in that: the preparation process of this target may further comprise the steps:
(1). the zinc for preparing, indium oxide powder are at first pressed pre-molding at stainless steel mould through 1～50Mpa single shaft, again through 100～300MPa cold isostatic compaction, the block after the moulding is dried down at 70-150 ℃ remove forming agent then.
(2). the block after the oven dry is sintering under vacuum state, and sintering temperature is 900-1500 ℃.
(3). the target germule behind the sintering placed carry out anneal under the purity oxygen atmosphere, annealing temperature is 800-1200 ℃.
(4). the target germule cutting after the anneal, polishing and installation backboard.
3. the preparation method of 2 described indium doping zinc-oxide targets, it is characterized in that: the employed zinc of this target of sintering, indium oxide powder are by coprecipitation method, sol-gel method, hydrolysis method, hydrothermal method, microemulsion method or solid phase Prepared by Ball Milling; Having added mass content in the process of preparation zinc, indium oxide powder is the dispersion agent of 0-5%, and dispersion agent comprises polyvinyl alcohol, polyoxyethylene glycol, polyvinyl butyral acetal, dioctyl sodium sulfosuccinate, Sodium dodecylbenzene sulfonate, Sodium glycocholate and tween etc.; Under air atmosphere or oxygen atmosphere, through 400-800 ℃ of presintering, carry out granulation then, sieving has promptly obtained zinc, indium oxide powder after zinc, the indium oxide presoma drying.
4. indium adulterated zinc oxide transparent conductive film is characterized in that: this nesa coating is to adopt 1 a described indium doping zinc-oxide target to prepare through sputtering method.
5. 4 described indium adulterated zinc oxide transparent conductive films, it is characterized in that: this nesa coating is the hexagonal wurtzite phase structure, and resistivity reaches 10
-4Ω cm, lowest resistivity 7 * 10
-4Ω cm, at the high permeability 92% of visible-range 400～800nm, average transmittances is not less than 84%.
6. the preparation method of 4 described indium adulterated zinc oxide transparent conductive films is characterized in that: in the sputter coating process, and working gas pure argon mixings 0-20% oxygen composition, pressure is 0.1～2.0Pa, underlayer temperature is room temperature～700 ℃.
The present invention uses above-mentioned target to adopt sputtering method to prepare the indium adulterated zinc oxide transparent conductive film.In the sputter coating process, working gas pure argon mixing 0-20% oxygen is formed, and pressure is 0.1～2.0Pa, and underlayer temperature is room temperature～700 ℃.Prepared indium adulterated zinc oxide transparent conductive film is the hexagonal wurtzite phase structure, and resistivity can reach 10
-4Ω cm, resistivity is minimum to reach 7 * 10
-4Ω cm, (400～800nm) high permeabilities can reach 92%, and average transmittances is not less than 84% at visible-range.
The indium doping zinc-oxide target and the nesa coating thereof of the present invention preparation be with low cost, have good broadcasting and TV performance, be expected to substitute a large amount of at present ITO target and nesa coatings thereof that use, save a large amount of noble metal indiums, significantly reduce the cost of nesa coating simultaneously.
Description of drawings
Fig. 1 is the transmitance of the indium adulterated zinc oxide transparent conductive film for preparing on the silica glass substrate.
Fig. 2 is the X-ray diffraction spectrum of the indium adulterated zinc oxide transparent conductive film for preparing on the silica glass substrate.
Embodiment
Further specify embodiments of the present invention below by example, purpose is to help further to understand the present invention rather than restriction the present invention, that is the present invention never is limited to following example.
Embodiment 1: the preparation of indium doping zinc-oxide target
At first adopt solid phase Prepared by Ball Milling zinc, indium oxide powder.According to In
2O
3/ (ZnO+In
2O
3) mass ratio is 5% to take by weighing zinc oxide (purity is 99.99%) powder and Indium sesquioxide (purity is 99.99%) powder, takes by weighing the polyoxyethylene glycol that accounts for powder total mass 1%, takes by weighing the abrading-ball that is three times in powder quality; Load weighted powder, polyoxyethylene glycol and abrading-ball are put in the ball grinder, added a certain amount of dehydrated alcohol then, ball grinder is sealingly fastened on the ball mill, then with 200 rev/mins speed ball milling 20 hours.After ball milling is finished slurry is poured out, 80 ℃ of down oven dry 5 hours,, after presintering is finished powder is sieved, granulation promptly obtained can be used for target agglomerating zinc, indium oxide powder then with powder presintering 5 hours under 700 ℃ and high purity oxygen gas.
Add an amount of dehydrated alcohol and put into to above-mentioned zinc, indium oxide powder and install mould in the stainless steel mould, pre-molding under the uniaxial tension of 20MPa, then through 200MPa isostatic cool pressing 10 minutes, subsequently the block after the moulding is placed on 90 ℃ of oven dry 4 hours down; After treating the block oven dry, it is transferred in the vacuum sintering furnace, be evacuated to and be warmed up to 1100 ℃ of sintering 20 hours after pressure is lower than 0.1Pa; After sintering is finished furnace temperature is dropped to 950 ℃, in sintering oven, feed high purity oxygen gas then and keep pressure-fired to carry out anneal 20 hours; Treat after anneal is finished furnace temperature drop to room temperature take out ceramic block and on request size carry out mechanical workout and the indium doping zinc-oxide target that backboard just can obtain being used for sputter coating be installed.The density of measuring this target through Archimedes's method reaches 5.4g/cm
3
Embodiment 2: the preparation of indium adulterated zinc oxide transparent conductive film
Adopt example 1 prepared indium doping zinc-oxide target to prepare nesa coating with magnetron sputtering method.Target is installed on the magnetic controlling target rifle correspondence position, is evacuated to vacuum chamber base vacuum degree and is higher than 2.0 * 10
-4Pa is a substrate with the silica glass, and underlayer temperature remains on 400 ℃, in vacuum chamber, feed 100sccm argon gas (sccm represents standard milliliter per minute), the adjusting pressure in vacuum tank is 0.15Pa, and regulating radio-frequency power supply power is 100W, the earlier pre-sputter 10min of target before formal deposit film.Prepare the indium adulterated zinc oxide transparent conductive film that thickness is about 300nm according to above-mentioned processing condition.The crystalline structure that shows this nesa coating after tested is the hexagonal wurtzite phase structure along (002) orientation, and resistivity is 8 * 10
-4Ω cm, (400～800nm) high permeabilities can reach 92% to visible-range, and average transmittances is 85%.
Claims (6)
1. indium doping zinc-oxide target, it is characterized in that: this target is formed through sintering by zinc, indium oxide powder; Wherein the mass content of Indium sesquioxide is 0.5-10%; The purity of target is not less than 99.9%; The relative density of target is not less than 95%, reaches as high as 99.5%.
2. the preparation method of the described indium doping zinc-oxide of claim 1 target, it is characterized in that: the preparation process of this target may further comprise the steps:
(1). the zinc for preparing, indium oxide powder are at first pressed pre-molding at stainless steel mould through 1～50Mpa single shaft, again through 100～300MPa cold isostatic compaction, the block after the moulding is dried down at 70-150 ℃ remove forming agent then.
(2). the block after the oven dry is sintering under vacuum state, and sintering temperature is 900-1500 ℃.
(3). the target germule behind the sintering placed carry out anneal under the purity oxygen atmosphere, annealing temperature is 800-1200 ℃.
(4). the target germule cutting after the anneal, polishing and installation backboard.
3. the preparation method of the described indium doping zinc-oxide of claim 2 target, it is characterized in that: the employed zinc of this target of sintering, indium oxide powder are by coprecipitation method, sol-gel method, hydrolysis method, hydrothermal method, microemulsion method or solid phase Prepared by Ball Milling; Having added mass content in the process of preparation zinc, indium oxide powder is the dispersion agent of 0-5%, and dispersion agent comprises polyvinyl alcohol, polyoxyethylene glycol, polyvinyl butyral acetal, dioctyl sodium sulfosuccinate, Sodium dodecylbenzene sulfonate, Sodium glycocholate and tween etc.; Under air atmosphere or oxygen atmosphere, through 400-800 ℃ of presintering, carry out granulation then, sieving has promptly obtained zinc, indium oxide powder after zinc, the indium oxide presoma drying.
4. indium adulterated zinc oxide transparent conductive film is characterized in that: this nesa coating is to adopt the described indium doping zinc-oxide of claim 1 target to prepare through sputtering method.
5. the described indium adulterated zinc oxide transparent conductive film of claim 4, it is characterized in that: this nesa coating is the hexagonal wurtzite phase structure, and resistivity reaches 10
-4Ω cm, lowest resistivity 7 * 10
-4Ω cm, at the high permeability 92% of visible-range 400～800nm, average transmittances is not less than 84%.
6. the preparation method of the described indium adulterated zinc oxide transparent conductive film of claim 4 is characterized in that: in the sputter coating process, working gas pure argon mixing 0-20% oxygen is formed, and pressure is 0.1～2.0Pa, and underlayer temperature is room temperature～700 ℃.
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Cited By (11)
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| CN102586736A (en) * | 2012-02-23 | 2012-07-18 | 西北稀有金属材料研究院 | Doped ZnO-based sputtering target material and preparation method thereof |
| CN102691037A (en) * | 2011-03-21 | 2012-09-26 | 海洋王照明科技股份有限公司 | Gallium-doped zinc oxide film, and preparation method and application thereof |
| CN102747334A (en) * | 2012-07-30 | 2012-10-24 | 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 |
| CN103203912A (en) * | 2012-01-12 | 2013-07-17 | 上海北玻玻璃技术工业有限公司 | Novel AZO coated glass and preparation technology thereof |
| CN103232234A (en) * | 2013-04-28 | 2013-08-07 | 西南交通大学 | Microwave doped sintering method of high-density and low-resistance ITO (Indium Tin Oxide) target |
| CN103896578A (en) * | 2014-03-19 | 2014-07-02 | 桂林电子科技大学 | Method for preparing high-density and low-resistivity zinc oxide ceramic target |
| CN105777107A (en) * | 2016-03-17 | 2016-07-20 | 江苏新浦电子科技有限公司 | Ceramic target for preparing conducting glass by aid of magnetron sputtering method |
| CN107267936A (en) * | 2016-03-31 | 2017-10-20 | 捷客斯金属株式会社 | Indium oxide is Zinc-oxide-based（IZO）Sputtering target and its manufacture method |
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| CN103232234A (en) * | 2013-04-28 | 2013-08-07 | 西南交通大学 | Microwave doped sintering method of high-density and low-resistance ITO (Indium Tin Oxide) target |
| CN103896578A (en) * | 2014-03-19 | 2014-07-02 | 桂林电子科技大学 | Method for preparing high-density and low-resistivity zinc oxide ceramic target |
| CN114892129A (en) * | 2015-05-08 | 2022-08-12 | 应用材料公司 | Method for manufacturing a layer for display manufacturing using water vapor and apparatus of said method |
| CN105777107A (en) * | 2016-03-17 | 2016-07-20 | 江苏新浦电子科技有限公司 | Ceramic target for preparing conducting glass by aid of magnetron sputtering method |
| CN107267936A (en) * | 2016-03-31 | 2017-10-20 | 捷客斯金属株式会社 | Indium oxide is Zinc-oxide-based（IZO）Sputtering target and its manufacture method |
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Application publication date: 20110921 |