CN103193475A - Study of preparation technology of AZO composite target material with high performance and low cost - Google Patents
Study of preparation technology of AZO composite target material with high performance and low cost Download PDFInfo
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- CN103193475A CN103193475A CN 201310110996 CN201310110996A CN103193475A CN 103193475 A CN103193475 A CN 103193475A CN 201310110996 CN201310110996 CN 201310110996 CN 201310110996 A CN201310110996 A CN 201310110996A CN 103193475 A CN103193475 A CN 103193475A
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- sintering
- powder
- zinc oxide
- azo
- target material
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- 239000002131 composite material Substances 0.000 title abstract description 15
- 239000013077 target material Substances 0.000 title abstract description 12
- 238000002360 preparation method Methods 0.000 title description 5
- 238000005516 engineering process Methods 0.000 title description 3
- 238000005245 sintering Methods 0.000 claims abstract description 31
- 239000000843 powder Substances 0.000 claims abstract description 25
- JYMITAMFTJDTAE-UHFFFAOYSA-N aluminum zinc oxygen(2-) Chemical compound [O-2].[Al+3].[Zn+2] JYMITAMFTJDTAE-UHFFFAOYSA-N 0.000 claims description 7
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 claims description 6
- 238000000280 densification Methods 0.000 claims description 5
- 229910000611 Zinc aluminium Inorganic materials 0.000 claims description 3
- HXFVOUUOTHJFPX-UHFFFAOYSA-N alumane;zinc Chemical compound [AlH3].[Zn] HXFVOUUOTHJFPX-UHFFFAOYSA-N 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 abstract description 17
- 239000011787 zinc oxide Substances 0.000 abstract description 8
- 239000011521 glass Substances 0.000 abstract description 7
- 229910052782 aluminium Inorganic materials 0.000 abstract description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 5
- 239000004411 aluminium Substances 0.000 abstract description 5
- 150000001875 compounds Chemical class 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 abstract 1
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 abstract 1
- 238000000034 method Methods 0.000 description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
- 239000003795 chemical substances by application Substances 0.000 description 7
- 238000001238 wet grinding Methods 0.000 description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 5
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- -1 polyoxyethylene Polymers 0.000 description 4
- 238000004544 sputter deposition Methods 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- 229910001195 gallium oxide Inorganic materials 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- 238000000498 ball milling Methods 0.000 description 2
- 238000000748 compression moulding Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 229910001449 indium ion Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000004482 other powder Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
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Abstract
The invention discloses a sintering composite zinc oxide aluminium material with high purity, high density and low cost, which belongs to inorganic chemistry metallic elements and compounds thereof. The novel and compact zinc oxide aluminium material disclosed by the invention is characterized in that Ga2O3 powder is added to powder, and no sintering aids are added, so that zinc oxide aluminium is densified in sintering. The sintering AZO has purity of higher than 99.9% and relative density of higher than or equal to 99.4%. The compact composite zinc oxide aluminium can be used as a target material for coating and is widely used in the fields of panel display, photoelectric conversion and electronic glass.
Description
Technical field:
This patent belongs to the inorganic chemistry metallic element; Its compound.
Background technology:
Combined oxidation zinc-aluminium film is a kind of functional materials that is widely studied, and belongs to transparent conductive oxide TCO (Transparent Conductive Oxide).The TCO film is because having the excellent properties of visible light transmissivity height and electric conductivity height (being that resistivity is low), in field widespread uses such as solar film battery, plane demonstration, electronic glasses.It is international main flow operational path that magnetron sputtering prepares the TCO film, and required target has ITO (indium-doped tin oxide) and AZO (doped zinc oxide aluminium).Required indium is rare element in the ITO target, production cost height and poisonous, and indium ion is reduced easily in the processing procedure simultaneously, can reduce electric conductivity and light transmission rate greatly.And AZO target raw material is easy to get, and is with low cost, nontoxic, be easy to realize to mix, and in plasma body good stability, over-all properties is outstanding, is the TCO film target of following main flow.
The AZO target at high temperature all very easily decomposes and volatilizees, and therefore will seriously hinder sintering and densification under its high temperature, makes its sintering difficult unusually.Industry is understood the problems of crack that occurs because the target density is low when sputter AZO target at present.
Solved the problem in the industry target as sputter process; And the film light transmittance of sputter preparation is＞80% in the visible region, resistivity≤5 * 10-4 Ω cm.
Summary of the invention:
This patent discloses a kind of novel high-purity degree, high-density, sintered combined zinc oxide aluminum material preparation cheaply.It is characterized in that in powder, adding gallium oxide (Ga2O3) powder and do not add any sintering aid and make the zinc oxide aluminum sintering densification.The described sintering AZO of this patent purity is higher than 99.9%, relative density 〉=99.4%.
This patent is started with from the essence of compound AZO target sintering, analyzes target in the sintering process and decomposes influence to intercrystalline cohesive process and bonding force, provides in the game process of sintering and volatilization to be conducive to the condition that its crystal grain is combined most.Study in great detail and grasped:
(1) powder composition proportion and purity: the composite powder composition is that aluminum oxide (Al2O3) 1～5%, gallium oxide (Ga2O3) 0.5～2%, all the other powder are zinc oxide (ZnO) powder, and powder mean particle sizes is 5～30 microns, and raw material powder purity is more than or equal to 4N
(2) ball milling: powder is more thin, and specific surface area is more big, the sintering motivating force is more big, more is conducive to sintering densification; But powder is meticulous, and the decomposition volatilization is just too violent, can hinder crystal grain combination in the sintering process on the contrary.Therefore adopt wet milling process to obtain best size range and size-grade distribution; Ratio of grinding media to material is 3/1～5/1, and wet grinding media is that deionized water, liquid-solid ratio are 1/1～1.5/1, and forming agent is polyoxyethylene glycol (PEG), 6～24 hours ball milling time
(3) moulding: adopt isostatic cool pressing, forming pressure is 0.5～3 ton/square centimeter
(4) sintering: under the high temperature between powder particle faint mechanical level in conjunction with being transformed into the firm metallurgical grade combination of intercrystalline; Can aggravation decompose volatilization but temperature is too high.Therefore sintering temperature is between 800～1400 degree, soaking time 1～4 hour.For obtaining more high performance target, can be at sintering under the atmosphere
By above critical process, prepare high-bond (hardness), high-density, high performance compound AZO target with lower cost.
Description of drawings:
Below in conjunction with accompanying drawing this patent is further explained:
Accompanying drawing: high-performance and low-cost AZO composite target material preparation technology schema.
Below in conjunction with accompanying drawing this patent is described further:
As shown in drawings, the technical process of this patent is: earlier ZnO, Al2O3, Ga2O3 powder and forming agent PEG (polyoxyethylene glycol) are added wet-milling mixing in the ball mill, liquid medium is water, after fully wet-milling mixes, drying is sieved to granulate and is obtained compound, and moulding then (dry-pressing, isostatic cool pressing etc.) obtains green compact, after taking off forming agent, can in air, carry out normal pressure-sintered or gas pressure sintering, obtain high purity, highdensity sintered combined zinc oxide aluminum.
The advantage of this patent is to be applicable to the powder stock (granularity 5-20 micron) of common granularity and ultra-fine powder stock (less than 5 microns), do not add any sintering aid, just can prepare the sintered combined zinc oxide aluminum of high purity, high-density, low cost, various complicated shapes.
Embodiment:
Example 1: high purity, high-compactness AZO composite target material
Mix 2.5% mass percent Al2O3 powder (1.2 microns of mean particle sizes) in the ZnO powder (17 microns of mean particle sizes), 1% Ga2O3 powder (2.0 microns of mean particle sizes), add 1-5% (weight) polyoxyethylene glycol (PEG) again as forming agent, add distilled water in ball mill wet-milling 20-90 hour, compression moulding under 100-200MPa pressure after the drying and screening, take off behind the forming agent in the High Temperature Furnaces Heating Apparatus medium-Si, Mo rod stove, under 1100 ℃-1400 ℃ in air normal pressure-sintered 60-180 minute, the sintering AZO composite target material of furnace cooling system, purity is higher than 99.9%, relative density 〉=99.4%.
Example 2: high purity, high-compactness AZO composite target material
Mix 2.0% mass percent Al2O3 powder (1.5 microns of mean particle sizes) in the ZnO powder (10 microns of mean particle sizes), 1% Ga2O3 powder (1.0 microns of mean particle sizes), add 3-5% (weight) polyoxyethylene glycol (PEG) again as forming agent, add distilled water in ball mill wet-milling 20-80 hour, compression moulding under 100-200MPa pressure after the drying and screening, take off behind the forming agent in the High Temperature Furnaces Heating Apparatus medium-Si, Mo rod stove, under 1100 ℃-1200 ℃ in air normal pressure-sintered 60-180 minute, the sintering AZO composite target material of furnace cooling system, purity is higher than 99.92%, relative density 〉=99.7%.
Example 3: the AZO composite target material application example of sintering of the present invention
Use: the photovoltaic glass plated film
Target: sintering AZO composite target material relative density 〉=99.4%
The sputter coating condition: intermediate frequency sputtering current 2.0A, substrate temperature are 200 ℃, and target is 7.5cm apart from substrate distance, Ar Pressure 0.8Pa, base vacuum 2.3x10-3Pa
The light transmittance is 83% in the visible region behind the photovoltaic glass plated film, and resistivity is 5 * 10-4 Ω cm.
Example 4: the AZO composite target material application example of sintering of the present invention
Use: the photovoltaic glass plated film
Target: sintering AZO composite target material relative density 〉=99.7%
The sputter coating condition: intermediate frequency sputtering current 2.0A, substrate temperature are 150 ℃, and target is 7.5cm apart from substrate distance, Ar Pressure 0.8Pa, base vacuum 2.3x10-3Pa
The light transmittance is 87% in the visible region behind the photovoltaic glass plated film, and resistivity is 4 * 10-4 Ω cm.
Example 3 and 4 shows: behind the photovoltaic glass sputter plating AZO composite membrane, can obviously increase transmitance, the reduction resistivity of visible region.
Claims (3)
1. the combined oxidation zinc-aluminium of a novel densification, it is characterized in that in powder, adding gallium oxide (Ga2O3) powder and do not add any sintering aid and make the zinc oxide aluminum sintering densification, described sintering AZO purity is higher than 99.9%, relative density 〉=99.4%.
2. fine and close combined oxidation zinc-aluminium according to claim 1 mainly is to make by ball milling-drying-sieve-operations such as moulding-sintering.
3. sintered combined zinc oxide aluminum according to claim 1, be applicable to the powder stock (granularity 5-20 micron) of common granularity and ultra-fine powder stock (less than 5 microns), do not add any sintering aid, just can prepare the sintered combined zinc oxide aluminum of high purity, high-density, low cost, various complicated shapes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201310110996 CN103193475A (en) | 2013-03-28 | 2013-03-28 | Study of preparation technology of AZO composite target material with high performance and low cost |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201310110996 CN103193475A (en) | 2013-03-28 | 2013-03-28 | Study of preparation technology of AZO composite target material with high performance and low cost |
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| CN103193475A true CN103193475A (en) | 2013-07-10 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103693954A (en) * | 2013-12-09 | 2014-04-02 | 中国科学院福建物质结构研究所 | High conductivity zinc oxide ceramic and preparation method thereof |
| CN106278287A (en) * | 2015-06-08 | 2017-01-04 | 深圳大学 | A kind of preparation and sintering method of WO3 coated AZO powder |
| CN116751048A (en) * | 2023-06-05 | 2023-09-15 | 洛阳晶联光电材料有限责任公司 | A gallium aluminum doped zinc oxide target material and its preparation method and application |
-
2013
- 2013-03-28 CN CN 201310110996 patent/CN103193475A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103693954A (en) * | 2013-12-09 | 2014-04-02 | 中国科学院福建物质结构研究所 | High conductivity zinc oxide ceramic and preparation method thereof |
| CN106278287A (en) * | 2015-06-08 | 2017-01-04 | 深圳大学 | A kind of preparation and sintering method of WO3 coated AZO powder |
| CN106278287B (en) * | 2015-06-08 | 2019-04-26 | 深圳大学 | A kind of preparation of WO3 coated AZO powder and its sintering method |
| CN116751048A (en) * | 2023-06-05 | 2023-09-15 | 洛阳晶联光电材料有限责任公司 | A gallium aluminum doped zinc oxide target material and its preparation method and application |
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Application publication date: 20130710 |