CN103695849B - A kind of zinc gallium aluminium ternary oxide rotary ceramic target and preparation method thereof - Google Patents
A kind of zinc gallium aluminium ternary oxide rotary ceramic target and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of zinc gallium aluminium ternary oxide（Hollow tubular）Rotary ceramic target and preparation method thereof.It is characterized in, raw material composition is by percentage to the quality：Oxidation gallium content is that 0.5 3.5%, alumina content is that 0.5 2.5%, tungsten oxide content is 0.002 0.05%, balance of zinc oxide.The present invention, using dry mixed, roasting, wet ball grinding decentralized processing technique, makes each component be evenly distributed in matrix with zinc oxide, gallium oxide, aluminum oxide and micro-oxidation tungsten powder as raw material, and ternary oxide mixed powder has good dispersion and sintering activity.With high compactness, high finished product rate, process equipment is simple, and cost is relatively low, it is easy to industrialize.Target has high density, low poisoning rate, visible ray（400‑700nm）Transmitance >=90%, near infrared region（700‑1400nm）Transmitance >=85%, it is adaptable to DC magnetron sputtering large area film photovoltaic cell plated films.
Description
Technical field
The present invention relates to a kind of zinc gallium aluminium ternary oxide（Hollow tubular）Rotary ceramic target and its system
Preparation Method.
Background technology
ZnO is a kind of energy gap multifunctional semiconductor material wide, with gas sensing property, pressure-sensitive, piezoelectricity,
Transparent conductivity, photo electric and it is easy to various semi-conducting materials and realizes the excellent property such as integrated.
In display device, nonlinear optics device, luminescent device, surface acoustic wave device, solar cell, heat
There is important application in the field such as the ultraviolet light detectors such as radiating mirror and integrated optics.Zno-based film
With its performance it is various, be widely used with the prominent advantage such as cheap, and preparation method it is various,
Technique is relatively easy, be easy to doping vario-property turns into preparation TCO（Transparent conductive oxide）Film is important
Material.It is AZO that it represents material（Aluminium adulterates）、GZO（Gallium adulterates）、BZO（Boron adulterates）Deng.
The performance of the TCO thin film that the zinc oxide adulterated by single-element is constituted and application, because of its contained unit
Element itself intrinsic property and be restricted.In order to optimize the optics of TCO thin film, electricity and chemically
Matter, the new multicomponent compound transparent conductive oxide film being made up of many oxide can be by adjusting
Whole group is into obtaining optimum performance with elemental constituent.
It is to use magnetron sputtering technique that transparent conductive film prepares main technique.Coating performance and target
Can be closely related.In coating process, it is so-called target " poisoning " phenomenon often to go wrong, i.e., abnormal to put
Electricity and target material surface granulating（It is redeposited）, cause sputter procedure continuous, film performance deterioration,
Production efficiency reduction.Generally, it is considered that low compactness target is because its porosity is high and poorly conductive, it is to lead
Causing the one of the main reasons of above-mentioned phenomenon, high density has turned into the important indicator for weighing target performance.Together
When, it is suitably trace doped to be also beneficial to improve target " poisoning " phenomenon.Secondly, with filming equipment
Technological progress, the target with particular cross-section structure just replacing traditional planar targets obtain largely should
With, such as hollow tubular rotary target material, compared to planar targets, 360 ° of target surfaces of rotary target material can be equal
Even etching, utilization rate is up to 80%, and without redeposition area, coating quality and plated film time correlation
It is low, sputter rate higher can be accomplished.TCO is prepared as large area, Large-power High-Speed sputtering
Film developing direction.In addition, in TCO thin film aspect of performance, especially using silicon substrate or other materials
The thin film solar cell of material, it should with more preferable visible ray and near infrared light transmitance, to ensure to obtain
The photoelectric transformation efficiency of get Geng Gao.
The content of the invention
An object of the present invention be to provide a kind of high usage, high density, low poisoning rate, raising can
See the zinc gallium aluminium ternary oxide rotary ceramic target of light and near infrared region transmitance；
The second object of the present invention is to provide a kind of preparation method of above-mentioned target, the method process equipment
Simply, cost is relatively low, it is easy to industrialized production.
A kind of zinc gallium aluminium ternary oxide rotary ceramic target, it is particular in that, raw material composition with
Mass percent is calculated as：Oxidation gallium content is 0.5-3.5%, alumina content is 0.5-2.5%, oxidation
W content is 0.002-0.05%, balance of zinc oxide.
Wherein target density >=5.56g/cm3, body resistivity≤3m Ω .cm, crystal phase structure is single-phase six
Square buergerite ZnO.
A kind of preparation method of zinc gallium aluminium ternary oxide rotary ceramic target, it is particular in that,
Comprise the following steps：
（1）According to the raw material proportioning described in claim 1, by gallium oxide, aluminum oxide, oxidation
After zinc and tungsten oxide powder dry mixed, it is calcined, powders calcined is with deionized water or absolute ethyl alcohol
Wet ball grinding disperses, slurry atomization granulation；
（2）The prilling powder for obtaining loads mould, and cold isostatic compaction is made hollow tubular biscuit,
Biscuit is sintered in oxygen atmosphere, that is, obtains zinc gallium aluminium ternary oxide tubular body, cleaved,
Hollow tubular sputtering target material is obtained after grinding, polishing.
Step（1）Middle Zinc oxide powder specific surface area 4-10m2/ g, alumina powder is γ-Al2O3,
Specific surface area 10-25m2/g；Gallium oxide powder is β-Ga2O3, specific surface area 3-10m2/g；Oxidation
Tungsten powder is WO3, specific surface area 1-6m2/g。
Step（1）The sintering temperature of middle dry mixed powder is 600-1000 DEG C, and the time is 2-10hr.
Further, sintering temperature is 800-950 DEG C, and the time is 4-6hr.
Step（1）The powders calcined of middle raw material zinc oxide, aluminum oxide, gallium oxide and tungsten oxide is through wet
Method ball milling disperses, and Specific Surface Area Measurement is 3-10m2/g。
Further, Specific Surface Area Measurement is 6-8m2/g。
Step（2）Middle PO2It is 0.1-0.3MPa, oxygen flow 20-200L/min.
Step（2）Middle use rubber mold.
Compared with prior art, the invention has the advantages that：
1st, the present invention is adopted with zinc oxide, gallium oxide, aluminum oxide and micro-oxidation tungsten powder as raw material
With dry mixed, roasting, wet ball grinding decentralized processing technique, each component is set to be evenly distributed in matrix,
Ternary oxide mixed powder has good dispersion and sintering activity.Hollow tubular oxidate sintered body has
There are high compactness, high finished product rate, process equipment is simple, and cost is relatively low, it is easy to industrialized production.
2nd, it is present approach provides a kind of material composition：Zinc oxide（94-99%, mass%）、
Gallium oxide（0.5-3.5%, mass%）, aluminum oxide（0.5-2.5%, mass%）, tungsten oxide content be
The preparation method of the ternary oxide hollow tubular target of 0.002-0.05%.Target density >=
5.56g/cm3, body resistivity≤3m Ω .cm, crystalline phase be single-phase hexagonal wurtzite ZnO structures.The target
Material has high density, low poisoning rate, visible ray（400-700nm）Transmitance >=90%, near infrared region
（700-1400nm）Transmitance >=85%, it is adaptable to DC- magnetron sputtering large area film photovoltaic cells
Plated film requirement.
Specific embodiment
Preparation method of the invention is completed as follows：
1. according to composition, by the gallium oxide of purity >=99.95% and appropriate specific surface area, aluminum oxide,
Zinc oxide, tungsten oxide powder after dry mixed, 2-10hr are calcined in 600-1000 DEG C in proportion.Roasting
Powder is disperseed with deionized water or absolute ethyl alcohol wet ball grinding, to Specific Surface Area Measurement 3-10m2/ g, material
Slurry atomization granulation.
2. cold isostatic compaction：The atomization granulation powder of above-mentioned steps 1 is loaded into rubber mold,
Pressurize 5-20min is made hollow tubular biscuit under 240-320MPa, and wherein molding biscuit relative density is
65-75%。
3. it is the characteristics such as control target sintered body crystal phase structure, compactness, body resistivity, degree of deformation,
Using following sintering process：- 900 DEG C of room temperature, 2-8 DEG C of heating rate/min；900-1200 DEG C, heat up
1-3 DEG C of speed/min；1200-1500 DEG C, 0.5-1 DEG C of heating rate/min is incubated 2-10hr；Oxygen
Sintering atmosphere,It is 0.1-0.3MPa, oxygen flow 20-200L/min.
4. zinc gallium aluminium ternary oxide tubular body is obtained, it is hollow after cleaved, grinding, polishing
Tubular rotary ceramic target,
5., by above-mentioned steps, target density >=5.56g/cm is obtained3, body resistivity≤3m Ω .cm, crystalline substance
Phase structure is single-phase hexagonal wurtzite ZnO.With high density, low poisoning rate, visible ray and near-infrared
The high usage tubular rotary target of area's high transmittance.
Embodiment 1：
From purity >=99.95% oxide powder.Weigh specific surface area 6.8m2/ g Zinc oxide powders
9600g；Specific surface area 13.5m2/gγ-Al2O3Powder 150g；Specific surface area 5.6m2/gβ-Ga2O3
Powder 250g；Specific surface area 3m2/g WO3Powder 5g.Dry mixed 4hr is after 800 DEG C of roastings
4hr.Powders calcined is disperseed with deionized water or absolute ethyl alcohol as abrasive media wet ball grinding, to powder
Specific surface area 6-7m2/ g, slurry atomization granulation.Atomization granulation powder is loaded into rubber mold, 280MPa
Lower pressurize 10min cold isostatic compactions are made hollow tubular biscuit, and molding biscuit relative density is 67%.
Molding biscuit with oxygen as sintering atmosphere,It is 0.2MPa, oxygen flow 100L/min conditions
Under.Sintering process is -900 DEG C of room temperature, 5 DEG C/min of heating rate；900-1200 DEG C, heating rate 2
℃/min；1200-1400 DEG C, heating rate 0.8 DEG C/min, 1400 DEG C of insulation 8hr.
Zinc gallium aluminium ternary oxide tubular body is obtained, after cleaved, grinding, polishing, in obtaining
Blank pipe shape rotary target material.
Archimedes method detection target density 5.58g/cm3, four probe method monitored body resistance rate 1.8m
Ω .cm, XRD detection crystal phase structures are single-phase hexagonal wurtzite ZnO.With special glass as substrate,
DC magnetron sputtering platings, nesa coating in wavelength 400-700nm, film average transmittance 91%,
Wavelength 700-1400nm, film average transmittance 85%.
Embodiment 2：
From purity >=99.95% oxide powder.Weigh specific surface area 5.3m2/ g Zinc oxide powders
9540g；Specific surface area 12m2/gγ-Al2O3Powder 200g；Specific surface area 6.6m2/gβ-Ga2O3
Powder 260g；Specific surface area 2m2/g WO3Powder 3g.Dry mixed 5hr is after 950 DEG C of roastings
4hr.Powders calcined is disperseed with deionized water or absolute ethyl alcohol as abrasive media wet ball grinding, to powder
Specific surface area 7-8m2/ g, slurry atomization granulation.Atomization granulation powder is loaded into rubber mold, 320MPa
Lower pressurize 10min cold isostatic compactions are made hollow tubular biscuit, and molding biscuit relative density is 72%.
Molding biscuit with oxygen as sintering atmosphere,It is 0.1MPa, oxygen flow 30L/min conditions
Under.Sintering process is -900 DEG C of room temperature, 7 DEG C/min of heating rate；900-1250 DEG C, heating rate 3
℃/min；1250 DEG C of insulation 3hr, 1250-1450 DEG C, 1 DEG C/min of heating rate, 1450 DEG C of insulations
5hr。
Zinc gallium aluminium ternary oxide tubular body is obtained, after cleaved, grinding, polishing, in obtaining
Blank pipe shape rotary target material.
Archimedes method detection target density 5.591g/cm3, four probe method monitored body resistance rate 1.6m
Ω .cm, XRD detection crystal phase structures are single-phase hexagonal wurtzite ZnO.With special glass as substrate,
DC magnetron sputtering platings, nesa coating in wavelength 400-700nm, film average transmittance 90%,
Wavelength 700-1400nm, film average transmittance 87%.
Comparative example 1：
From purity >=99.95% oxide powder.Weigh specific surface area 6.8m2/ g Zinc oxide powders
9800g；Specific surface area 13.5m2/gγ-Al2O3Powder 200g；Undope micro-oxidation tungsten powder.
Dry mixed 3hr is calcined 4hr after 800 DEG C.Powders calcined with deionized water or absolute ethyl alcohol be grinding
Medium wet ball grinding disperses, to Specific Surface Area Measurement 6-7m2/ g, slurry atomization granulation.Atomization is made
Grain powder loads rubber mold, and pressurize 10min cold isostatic compactions are made hollow tubular under 280MPa
Biscuit, molding biscuit relative density is 69%.
Molding biscuit with oxygen as sintering atmosphere,It is 0.2MPa, oxygen flow 100L/min conditions
Under.Sintering process is -900 DEG C of room temperature, 5 DEG C/min of heating rate；900-1200 DEG C, heating rate 2
℃/min；1200-1400 DEG C, heating rate 0.7 DEG C/min, 1400 DEG C of insulation 8hr.
Zinc-aluminum binary oxide tubular body is obtained, after cleaved, grinding, polishing, obtains hollow
Tubular rotary target.
Archimedes method detection target density 5.54g/cm3, four probe method monitored body resistance rate 4.2m
Ω .cm, XRD detection crystal phase structures are single-phase hexagonal wurtzite ZnO.With special glass as substrate,
DC magnetron sputtering platings, nesa coating in wavelength 400-700nm, film average transmittance 87%,
Wavelength 700-1400nm, film average transmittance 75%.
Claims (7)
1. a kind of zinc gallium aluminium ternary oxide rotary ceramic target, it is characterised in that raw material composition with
Mass percent is calculated as：Oxidation gallium content is 0.5-3.5%, alumina content is 0.5-2.5%, oxidation
W content is 0.002-0.05%, balance of zinc oxide；
Wherein target density >=5.56g/cm3, body resistivity≤3m Ω .cm, crystal phase structure is single-phase six
Square buergerite ZnO.
2. a kind of preparation method of zinc gallium aluminium ternary oxide rotary ceramic target, it is characterised in that
Comprise the following steps：
(1) according to the raw material proportioning described in claim 1, by gallium oxide, aluminum oxide, oxidation
After zinc and tungsten oxide powder dry mixed, it is calcined, powders calcined is with deionized water or absolute ethyl alcohol
Wet ball grinding disperses, slurry atomization granulation；
(2) prilling powder for obtaining loads mould, and cold isostatic compaction is made hollow tubular biscuit,
Biscuit is sintered in oxygen atmosphere, that is, obtains zinc gallium aluminium ternary oxide tubular body, cleaved,
Hollow tubular sputtering target material is obtained after grinding, polishing；
Zinc oxide powder specific surface area 4-10m in step (1)2/ g, alumina powder is γ-Al2O3,
Specific surface area 10-25m2/g；Gallium oxide powder is β-Ga2O3, specific surface area 3-10m2/g；Oxidation
Tungsten powder is WO3, specific surface area 1-6m2/g；
The sintering temperature of dry mixed powder is 600-1000 DEG C in step (1), and the time is 2-10 hours.
3. a kind of preparation of zinc gallium aluminium ternary oxide rotary ceramic target as claimed in claim 2
Method, it is characterised in that：Sintering temperature is 800-950 DEG C, and the time is 4-6 hours.
4. a kind of preparation of zinc gallium aluminium ternary oxide rotary ceramic target as claimed in claim 2
Method, it is characterised in that：Raw material zinc oxide, aluminum oxide, gallium oxide and tungsten oxide in step (1)
Powders calcined through wet ball grinding disperse, Specific Surface Area Measurement is 3-10m2/g。
5. a kind of preparation of zinc gallium aluminium ternary oxide rotary ceramic target as claimed in claim 4
Method, it is characterised in that：Specific Surface Area Measurement is 6-8m2/g。
6. a kind of preparation of zinc gallium aluminium ternary oxide rotary ceramic target as claimed in claim 2
Method, it is characterised in that：Oxygen pressure is 0.1-0.3MPa, oxygen flow in step (2)
20-200L/min。
7. a kind of preparation of zinc gallium aluminium ternary oxide rotary ceramic target as claimed in claim 2
Method, it is characterised in that：Step uses rubber mold in (2).
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| CN106278287B (en) * | 2015-06-08 | 2019-04-26 | 深圳大学 | A kind of WO3Coat preparation and its sintering method of AZO powder |
| CN107523794A (en) * | 2017-09-07 | 2017-12-29 | 于盟盟 | A kind of target for being used to sputter transparent conductive film |
| CN112341168A (en) * | 2020-09-23 | 2021-02-09 | 先导薄膜材料（广东）有限公司 | Rare earth doped zinc-gallium-aluminum oxide powder and preparation method thereof |
| CN113215545A (en) * | 2021-05-12 | 2021-08-06 | 杭州盛宣新材料科技有限公司 | Method for preparing Ni-doped zinc-aluminum oxide conductive film material by adopting magnetron sputtering technology |
| CN114524664B (en) * | 2022-02-25 | 2023-07-18 | 洛阳晶联光电材料有限责任公司 | Ceramic target for solar cell and preparation method thereof |
| CN115141012A (en) * | 2022-07-25 | 2022-10-04 | 宁波江丰电子材料股份有限公司 | Ternary metal oxide ceramic target material and preparation method thereof |
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| CN101661808A (en) * | 2009-09-15 | 2010-03-03 | 中国科学院上海硅酸盐研究所 | Multi-doping zinc-oxide-base wide-bandgap conducting material and preparation method thereof |
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| JP5358891B2 (en) * | 2006-08-11 | 2013-12-04 | 日立金属株式会社 | Method for producing sintered zinc oxide |
| JPWO2009078329A1 (en) * | 2007-12-19 | 2011-04-28 | 日立金属株式会社 | Zinc oxide sintered body and manufacturing method thereof, sputtering target, electrode |
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| CN101661808A (en) * | 2009-09-15 | 2010-03-03 | 中国科学院上海硅酸盐研究所 | Multi-doping zinc-oxide-base wide-bandgap conducting material and preparation method thereof |
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| Title |
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| W掺杂ZnO透明导电薄膜的理论及实验研究;王延峰等;《物理学报》;20120731;第61卷(第13期);第2页右栏第1段，第3页左栏第1段，第4页右栏第2段 * |
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