CN101851739A - AZO sputtering target for high-stability transparent conductive film and manufacturing method - Google Patents
AZO sputtering target for high-stability transparent conductive film and manufacturing method Download PDFInfo
- Publication number
- CN101851739A CN101851739A CN200910133329A CN200910133329A CN101851739A CN 101851739 A CN101851739 A CN 101851739A CN 200910133329 A CN200910133329 A CN 200910133329A CN 200910133329 A CN200910133329 A CN 200910133329A CN 101851739 A CN101851739 A CN 101851739A
- Authority
- CN
- China
- Prior art keywords
- powder
- transparent conductive
- conductive film
- sputtering target
- micron
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
The invention discloses an AZO sputtering target for a high-stability transparent conductive film and a manufacturing method. The raw material powder used by an IZGO sputtering target comprises 2 to 3wt% of Al2O3, 0.1 to 3wt% of B2O3 and the balance of ZnO powder; the average grain diameter of the powder is 0.05 to 50 microns, and the purity of the raw material powder is larger than or equal to 4N. The material of the invention is easier to control when used in the production process of the transparent conductive film through magnetron sputtering, a serious poisoning phenomenon similar to an ITO does not exist, and the sputtering process does not need heating, which has more advantages in the production of flexible conductive films such as plastics, and the stability and the weatherability of the film are much superior to that of the ITO and traditional zinc aluminum oxide conductive films. The resistivity of the produced transparent conductive film is smaller than 5*10 to 4Omega.cm, the visible light transmittance of 400 to 700nm is larger than 85%, and the requirements of various transparent conductive films can be satisfied.
Description
Technical field
The present invention relates to a kind of photoelectric material, specifically, the present invention is a kind of AZO sputtering target for high-stability transparent conductive film and manufacture method.
Background technology
With the transparent conductive film that magnetron sputtering is made, be liquid-crystal display, flat pannel display, electrostatic shielding, the essential functional materials of solar cell.At present, direct current magnetron sputtering process is the leading preparation technology of the high-grade display device in the current world with nesa coating.Traditional technology is with ITO semiconductive ceramic (90%In
2O
3-10%SnO
2) as sputtering source, generally in argon gas or argon oxygen gas mixture atmosphere, preparing the ITO transparent conductive film with direct current magnetron sputtering process under substrate 100-550 degree centigrade, prepared transparent conductive film is best in quality, visible light transmissivity＞85%, and resistivity is less than 10 * 10
-4Ω .cm.But since ITO material with high costs, the rare indium metal of main constitutive material wherein, and storage is limited in the earth's crust, and the ITO conducting film is unstable under reducing atmosphere and relative damp atmosphere environment, can't satisfy the service requirements in these fields.
Summary of the invention
Goal of the invention of the present invention provides a kind of AZO sputtering target for high-stability transparent conductive film.
Another object of the present invention provides a kind of manufacture method of AZO sputtering target for high-stability transparent conductive film.
In order to realize above-mentioned goal of the invention, the present invention by the following technical solutions:
A kind of AZO sputtering target for high-stability transparent conductive film, in the used material powder, Al
2O
3Content be 2～3wt%, and B
2O
3Content 0.1-3wt%, surplus is the ZnO powder; The powder median size is the 0.05-50 micron, and the purity of material powder is more than or equal to 4N.
Described material powder is ZnO/Al
2O
3/ B
2O
3Thorough mixing powder or chemical coprecipitation amyloplast.
The manufacture method of above-mentioned AZO sputtering target for high-stability transparent conductive film, the concrete step that adopts following order:
A. with purity more than or equal to the ZnO powder of 4N, median size 0.05-50 micron as the target main raw material, mix up weight ratio 2～3wt% median size 0.05-50 micron Al
2O
3With 0.1-3wt% median size 0.05-50 micron B
2O
3High-purity powder;
B. the deionization pure water of above powder and 20-50% weight is mixed, the trolamine that adds 0.1-0.5wt% mixes more than 16 hours as organic additive with the ball mill ball milling;
C. the slurry of step B gained adds the 0.8-1.5% polyvinyl alcohol as organic adhesive, ball milling 2-3 hour then;
D. the product to step C carries out the spray drying granulation processing, promptly gets the target raw material of averaged particles footpath 10-100 micron;
E. adopt one of following three kinds of processing modes to process step D gained raw material, obtain relative density greater than 50% base substrate:
E1. use metal pattern 1-3 ton/CM
2Pressure forming;
E2. cold isostatic compaction;
E3. gel casting forming;
F. the 400-600 degree centigrade of insulation in air furnace of this base substrate removed organic additive in 2-5 hour, be warmed up to 1250-1600 degree centigrade of densified sintering product, obtain relative density greater than 98% ceramic semiconductors, promptly.
Sintered compact processing is ground to desired size, promptly can be used for magnetron sputtering and make transparent conductive film.
AZO material advantage relative and the ITO material is being:
1. used main raw material zinc oxide is base oxide, and reserves are abundant in the earth's crust, and manufacturing cost is an ITO material 1/10.
2. be used for magnetron sputtering produce nesa coating the sputter rate height, do not exist similar ITO owing to the decomposition of principal constituent indium trioxide in sputter procedure cause target surface poison phenomenon, the production efficiency height.
3. production process is more easy to control, does not need to adjust oxygen partial pressure, substrate not to need heating in the sputter procedure, is more having superiority in the production of flexible conductive films such as plastics.
4. the nesa coating resistivity that AZO target of the present invention is produced is less than 2.1 * 10
-4Ω .cm, visible light transmissivity (400-700nm) are greater than 85%, and conducting film stability under reducing atmosphere and relative high humidity environment is good, satisfies various nesa coating requirements.
The present invention has following advantage:
Material of the present invention is used for magnetron sputtering, and to produce the production process of nesa coating more easy to control, do not have that similar ITO's seriously poison phenomenon, sputter procedure does not need heating, this more has superiority in the production of flexible conductive films such as plastics, and the stability of film and weathering resistance are better than ITO and traditional zinc oxide aluminum conducting film greatly.The nesa coating resistivity of producing is less than 5 * 10
-4Ω .cm, 400-700nm visible light transmissivity can satisfy various nesa coating requirements greater than 85%.
Embodiment
Embodiment 1
Weighing purity is ZnO powder 600 grams of 0.5 micron of 4N, median size, adds 10 microns Al of weight ratio 2% median size
2O
3B with 7 microns of 0.3% median sizes
2O
3Powder.Adding the deionization pure water of 35% weight and 0.5% trolamine organic additive mixes, mix more than 16 hours with the ball mill ball milling, the polyvinyl alcohol organic adhesive that adds gross weight 1%, ball milling is 2 hours again, the slip spray drying granulation is handled, obtain the target raw material in 50 microns in averaged particles footpath, with 1 ton/CM of metal pattern
2Pressure forming obtain the base substrate of relative density greater than 10 millimeters of 150 millimeters thickness of diameter of 54%, the 500 degrees centigrade of insulations in air furnace of this base substrate were removed organic additive in 45 hours, be warmed up to 1500 degrees centigrade of densified sintering products, the ceramic semiconductors that obtains relative density 99% is ground to sintered compact processing the target of 6 millimeters of 76 millimeters thickness of diameter.
Direct magnetic control plated film in SIM560 magnetron sputtering machine, power 120W, Ar
2Pressure 0.6Pa, glass substrate temperature room temperature, it is stable to continue sputter sputter in 3 hours, sputter rate was up to 260nm/ minute, record colorless film thickness 450 nanometers with the measurement of XP-1 step instrument, the CARY-100 spectrophotometer records the visible light transmissivity 91% of 400-700 nanometer, records resistivity 2.1 * 10 with SZ-82 four point probe tester
-4Ω .cm.The bright and clean no plethora of AZO target material surface after the sputter produces.
Under same sputtering condition, use the relative density 99%ITO (90%In of 6 millimeters of 76 millimeters thickness of diameter
2O
3+ 10%SnO
2) the target as sputter plated film, sputter is sputter aura instability after 1.8 hours, and sputter rate descends and continues to add the high-power 138W of arriving, sputter 1 hour, the CARY-100 spectrophotometer records film thickness 410 nanometers, and it is golden yellow that film is, and records resistivity 4.9 * 10 with SZ-82 four point probe tester
-4Ω cm, transmitance 80% in the visible-range of 400-700 nanometer.ITO target material surface after the sputter has obvious plethora to distribute.
With the AZO that as above makes and ITO nesa coating in the air oven of relative humidity 80% after the 250 degree insulations cooling in 2 hours, survey the performance variation of film, AZO film of the present invention transmitance 93% in the visible-range of 400-700 nanometer records resistivity 2.2 * 10
-4Ω cm; Transmitance drops to 79% in the visible-range of ITO nesa coating 400-700 nanometer, and it is 3.7 * 10 that resistivity raises
-3Ω cm, above embodiment prove that the nesa coating of AZO material of the present invention manufacturing has excellent stability.
Embodiment 2
Weighing purity is ZnO powder 950 grams of 0.5 micron of 5N, median size, adds 10 microns Al of 20 gram median sizes
2O
3B with 7 microns of 30 gram median sizes
2O
3Powder.The deionization pure water and the 5 gram trolamines that add 200 grams are mixed, mix more than 16 hours with the ball mill ball milling, add the polyvinyl alcohol organic adhesive of gross weight 1%, ball milling is 2 hours again, the slip spray drying granulation is handled, and obtains the target raw material in 50 microns in averaged particles footpath, with 2 tons/CM of metal pattern
2Pressure forming obtain the base substrate of relative density greater than 10 millimeters of 150 millimeters thickness of diameter of 54%, the 500 degrees centigrade of insulations in air furnace of this base substrate were removed organic additive in 45 hours, be warmed up to 1500 degrees centigrade of densified sintering products, the ceramic semiconductors that obtains relative density 99% is ground to sintered compact processing the target of 6 millimeters of 76 millimeters thickness of diameter.
Embodiment 3
Weighing purity is ZnO powder 969 grams of 0.5 micron of 6N, median size, adds 10 microns Al of 30 gram median sizes
2O
3B with 7 microns of 1 gram median sizes
2O
3Powder.Adding the deionization pure water of 350 grams and the trolamine organic additive of 5 grams mixes, mix more than 16 hours with the ball mill ball milling, the polyvinyl alcohol organic adhesive that adds 10 grams, ball milling is 2 hours again, the slip spray drying granulation is handled, obtain the target raw material in 50 microns in averaged particles footpath, with 3 tons/CM of metal pattern
2Pressure forming obtain the base substrate of relative density greater than 10 millimeters of 150 millimeters thickness of diameter of 54%, the 500 degrees centigrade of insulations in air furnace of this base substrate were removed organic additive in 45 hours, be warmed up to 1500 degrees centigrade of densified sintering products, the ceramic semiconductors that obtains relative density 99% is ground to sintered compact processing the target of 6 millimeters of 76 millimeters thickness of diameter.
Embodiment 4
Weighing purity is ZnO powder 940 grams of 0.5 micron of 4N, median size, adds 10 microns Al of 30 gram median sizes
2O
3B with 7 microns of 30 gram median sizes
2O
3Powder.Adding the deionization pure water of 350 gram weight and the trolamine organic additive of 5 grams mixes, mix more than 16 hours with the ball mill ball milling, the polyvinyl alcohol organic adhesive that adds 10 grams, ball milling is 2 hours again, the slip spray drying granulation is handled, obtain the target raw material in 50 microns in averaged particles footpath, with 2 tons/CM of metal pattern
2Pressure forming obtain the base substrate of relative density greater than 10 millimeters of 150 millimeters thickness of diameter of 54%, the 500 degrees centigrade of insulations in air furnace of this base substrate were removed organic additive in 45 hours, be warmed up to 1600 degrees centigrade of densified sintering products, the ceramic semiconductors that obtains relative density 99% is ground to sintered compact processing the target of 6 millimeters of 76 millimeters thickness of diameter.
More than indium zinc gallium oxide (IZGO) sputtering target for transparent conductive film provided by the present invention and manufacture method are described in detail, used specific case herein principle of the present invention and embodiment are set forth, the explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof; Simultaneously, for one of ordinary skill in the art, according to thought of the present invention, the part that all can change in specific embodiments and applications, in sum, this description should not be construed as limitation of the present invention.
Claims (4)
1. AZO sputtering target for high-stability transparent conductive film is characterized in that: in the used material powder, and Al
2O
3Content be 2～3wt%, and B
2O
3Content 0.1-3wt%, surplus is the ZnO powder; The powder median size is the 0.05-50 micron, and the purity of material powder is more than or equal to 4N.
2. AZO sputtering target for high-stability transparent conductive film according to claim 1 is characterized in that: described material powder is ZnO/Al
2O
3/ B
2O
3Thorough mixing powder or chemical coprecipitation amyloplast.
3. the manufacture method of the described AZO sputtering target for high-stability transparent conductive film of claim 1 is characterized in that, adopts following steps:
A. with purity more than or equal to the ZnO powder of 4N, median size 0.05-50 micron as the target main raw material, mix up weight ratio 2～3wt% median size 0.05-50 micron Al
2O
3With 0.1-3wt% median size 0.05-50 micron B
2O
3High-purity powder;
B. the deionization pure water of above powder and 20-50% weight is mixed, the trolamine that adds 0.1-0.5wt% mixes more than 16 hours as organic additive with the ball mill ball milling;
C. the slurry of step B gained adds the 0.8-1.5% polyvinyl alcohol as organic adhesive, ball milling 2-3 hour then;
D. the product to step C carries out the spray drying granulation processing, promptly gets the target raw material of averaged particles footpath 10-100 micron;
E. adopt one of following three kinds of processing modes to process step D gained raw material, obtain relative density greater than 50% base substrate:
E1. use metal pattern 1-3 ton/CM
2Pressure forming;
E2. cold isostatic compaction;
E3. gel casting forming;
F. the 400-600 degree centigrade of insulation in air furnace of this base substrate removed organic additive in 2-5 hour, be warmed up to 1250-1600 degree centigrade of densified sintering product, obtain relative density greater than 98% ceramic semiconductors, promptly.
4. the manufacture method of AZO sputtering target for high-stability transparent conductive film according to claim 3, it is characterized in that: material powder is ZnO/Al
2O
3/ B
2O
3Thorough mixing powder or chemical coprecipitation amyloplast.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910133329A CN101851739A (en) | 2009-04-02 | 2009-04-02 | AZO sputtering target for high-stability transparent conductive film and manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910133329A CN101851739A (en) | 2009-04-02 | 2009-04-02 | AZO sputtering target for high-stability transparent conductive film and manufacturing method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101851739A true CN101851739A (en) | 2010-10-06 |
Family
ID=42803414
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910133329A Pending CN101851739A (en) | 2009-04-02 | 2009-04-02 | AZO sputtering target for high-stability transparent conductive film and manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101851739A (en) |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102134702A (en) * | 2010-10-22 | 2011-07-27 | 迟伟光 | Method for preparing AZO powder and flat and rotary targets by spray drying process |
| 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 |
| CN102432274A (en) * | 2011-09-18 | 2012-05-02 | 陈海军 | Production process for alumina ceramic target |
| 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 |
| CN102965620A (en) * | 2011-08-29 | 2013-03-13 | 三菱综合材料株式会社 | Sputtering target and manufacturing method thereof, film obtained by utilizing the target, film sheet and laminating sheet |
| CN103643207A (en) * | 2013-12-26 | 2014-03-19 | 河北东同光电科技有限公司 | Preparation method of high-performance ZAO (Zinc Aluminum Oxide) rotating target material |
| 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 |
| CN104136654A (en) * | 2012-03-30 | 2014-11-05 | 吉坤日矿日石金属株式会社 | Sputtering target and process for manufacturing same |
| CN105374901A (en) * | 2015-11-18 | 2016-03-02 | 南京迪纳科光电材料有限公司 | Preparation method for IWO material used for thin film solar cell transparent electrode |
| CN109207947A (en) * | 2018-09-28 | 2019-01-15 | 上海大学 | A kind of preparation method of target |
| CN111439997A (en) * | 2020-05-25 | 2020-07-24 | 先导薄膜材料（广东）有限公司 | Zinc-aluminum oxide target material and preparation method thereof |
-
2009
- 2009-04-02 CN CN200910133329A patent/CN101851739A/en active Pending
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102134702A (en) * | 2010-10-22 | 2011-07-27 | 迟伟光 | Method for preparing AZO powder and flat and rotary targets by spray drying process |
| 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 |
| CN102351526B (en) * | 2011-06-11 | 2013-05-15 | 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 |
| CN102965620A (en) * | 2011-08-29 | 2013-03-13 | 三菱综合材料株式会社 | Sputtering target and manufacturing method thereof, film obtained by utilizing the target, film sheet and laminating sheet |
| CN102432274A (en) * | 2011-09-18 | 2012-05-02 | 陈海军 | Production process for alumina ceramic target |
| CN102432274B (en) * | 2011-09-18 | 2013-01-30 | 陈海军 | Production process for alumina ceramic target |
| CN104136654A (en) * | 2012-03-30 | 2014-11-05 | 吉坤日矿日石金属株式会社 | Sputtering target and process for manufacturing same |
| CN104136654B (en) * | 2012-03-30 | 2016-11-09 | 吉坤日矿日石金属株式会社 | Sputtering target and manufacture method 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 |
| 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 |
| CN103643207A (en) * | 2013-12-26 | 2014-03-19 | 河北东同光电科技有限公司 | Preparation method of high-performance ZAO (Zinc Aluminum Oxide) rotating target material |
| CN103896578B (en) * | 2014-03-19 | 2016-09-14 | 桂林电子科技大学 | A kind of preparation method of high density low resistivity zinc oxide ceramic 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 |
| CN105374901A (en) * | 2015-11-18 | 2016-03-02 | 南京迪纳科光电材料有限公司 | Preparation method for IWO material used for thin film solar cell transparent electrode |
| CN109207947A (en) * | 2018-09-28 | 2019-01-15 | 上海大学 | A kind of preparation method of target |
| CN111439997A (en) * | 2020-05-25 | 2020-07-24 | 先导薄膜材料（广东）有限公司 | Zinc-aluminum oxide target material and preparation method thereof |
| CN111439997B (en) * | 2020-05-25 | 2022-01-18 | 先导薄膜材料（广东）有限公司 | Zinc-aluminum oxide target material and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101851739A (en) | AZO sputtering target for high-stability transparent conductive film and manufacturing method | |
| CN101851745B (en) | Indium zinc gallium oxide (IZGO) sputtering target for transparent conductive film and manufacturing method | |
| CN102212781B (en) | Method for manufacturing high-density and low-cost zinc oxide aluminum sputtering target | |
| CN101851740A (en) | Conductive Nb2O5-x target material for magnetron sputtering coating and production method thereof | |
| JP3746094B2 (en) | Target and manufacturing method thereof | |
| CN101580384B (en) | Yttrium-doped AZO target and preparation method thereof | |
| CN102731067B (en) | Preparation method of high-density ITO (indium tin oxide) evaporation target | |
| CN104416160B (en) | High-density zinc oxide based target and preparation method thereof | |
| CN105374901A (en) | Preparation method for IWO material used for thin film solar cell transparent electrode | |
| CN101660120A (en) | Multi-element doping n-type zinc-oxide-base transparent conducting film and preparation method thereof | |
| CN101985735A (en) | Alumina target material and transparent conductive film prepared thereby | |
| JP2011006725A (en) | Indium-oxide-based sputtering target and method for manufacturing the same | |
| CN102320838A (en) | Flexible transparent conducting film is with metal oxide semiconductor material and preparation method thereof | |
| CN103695849B (en) | A kind of zinc gallium aluminium ternary oxide rotary ceramic target and preparation method thereof | |
| CN101575207A (en) | Ge-doped AZO target and preparation method thereof | |
| CN109879667B (en) | Preparation method of dense oxygen-loss zinc oxide ceramic body | |
| CN102180653A (en) | Preparation method for high-density indium tin oxide target material | |
| CN103332929A (en) | Forming process of high density large size AZO target material blank body | |
| CN108914064B (en) | Multi-element conductive oxide material for RPD and preparation method thereof | |
| CN102181826B (en) | Gallium-molybdenum-codoped indium tin oxide ceramic target, gallium-molybdenum-codoped indium tin oxide transparent conductive film and preparation method | |
| KR100948557B1 (en) | ???2 sputtering target and process for producing same | |
| CN101870580A (en) | ZD(H)O material for transparent conductive film and preparation method thereof | |
| CN106245007B (en) | A kind of preparation method being orientated ito thin film | |
| CN102650044B (en) | A kind of preparation method of SGZO-Au-SGZO nesa coating | |
| CN105274486A (en) | Preparing method for amorphous AlGaZnO transparent electrode material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| AD01 | Patent right deemed abandoned |
Effective date of abandoning: 20101006 |
|
| C20 | Patent right or utility model deemed to be abandoned or is abandoned |