CN101246759B - Nano homogeneous phase composite metal oxide conductive powder for transparent conducting material and its preparation method - Google Patents
Nano homogeneous phase composite metal oxide conductive powder for transparent conducting material and its preparation method Download PDFInfo
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- CN101246759B CN101246759B CN2007100540122A CN200710054012A CN101246759B CN 101246759 B CN101246759 B CN 101246759B CN 2007100540122 A CN2007100540122 A CN 2007100540122A CN 200710054012 A CN200710054012 A CN 200710054012A CN 101246759 B CN101246759 B CN 101246759B
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Abstract
The invention is a nanometer homogeneous composite metal oxide conductive powder for transparent conductive material, comprising: In2O3, SnO2, ZnO and Sb2O3 primary crystallization phase, and doping phase having 0.1-20% primary crystallization phase composed of one or more oxides selected from indium, tin, lead, zinc, bismuth, stibium, gallium, germanium, aluminum, copper, titanium, nickel, ferrum, molybdenum, vanadium, vanadium, cerium, zirconium, hafnium, niobium, ruthenium and rhodium. The powder is made by the following steps of: mixing the metals into an alloy in required proportion; melting the alloy; pressing the alloy to a reflector; applying a pressure ranging from 50V to 1000V to the reflector and a current ranging from 50A to 1000A to the reflector; filling the reflector with oxidizing gas mixture; reflecting of the gaseous metal atom with the oxygen atom; atomizing, gasifying and oxidizing the melting metals under intense magnetic field and resistance heat; and cold processing, so that a homogeneous system having two or more mutual melting nanometer oxides is formed. The powder has conductivity, high crystallinity, high dispersivity and strong fluidity.
Description
Technical field
The present invention relates to a kind of nano homogeneous phase composite metal oxide conductive powder that is used for transparent conductive material, particularly a kind of In that comprises
2O
3, SnO
2, ZnO, Sb
2O
3The primary crystallization phase, and primary crystallization mutually 0.1～20% the doping of forming by any two kinds and two or more oxide in the metals such as indium, tin, lead, zinc, bismuth, antimony, gallium, germanium, aluminium, copper, titanium, nickel, iron, molybdenum, vanadium, cerium, zirconium, hafnium, niobium, tantalum, ruthenium, rhodium have the nano homogeneous phase composite metal oxide conductive powder of the transparent conductive material of single homogeneous phase institutional framework mutually.
Background technology
The transparent conductive material that metal oxide constitutes is called for short TCO, but the low emissivity glass (Low-E Window) etc. that is used for the printing opacity conductive electrode reflected infrared ray of various flat-panel screens, become the critical material of transparent conductivity material, had huge market prospects.Make the ITO target with oxides such as indium tin, obtain transparent conductive film, can be used for submarine, tank, aviation and stealth material on the national defence through magnetron sputtering technique; The display that is used for panel TV, LCD, mobile phone on civilian, and at aspects such as solar cell and various functional glass, its potential application also constantly is found.
The TCO material of broad research and application is essentially the n type semiconductor oxide at present, mainly contains In
2O
3, SnO
2, ZnO, Sb
2O
3Form etc. oxide-doped, tin-doped indium oxide (ITO) target has about 1.4 * 10
-4The volume resistivity of Ω cm is the leading role of various transparent conductive materials, mix zinc indium oxide (IZO), antimony doped tin oxide (ATO), mix aluminium zinc oxide (AZO), mix the SnO of niobium indium oxide (INO) and doped with fluorine or aluminium
2Research also deepen continuously, be to have the transparent conductive material of development potentiality or light-colored antistatic to add material most.
At present, above-mentioned metal nano oxide adopts chemical coprecipitation to make mostly.Application number is the method that the Chinese invention patent prospectus " the indium tin oxide target is preparation method's table " of CN03118371.9 has been stated chemical coprecipitation, be that high pure metal indium (4N-5N) is dissolved in 60% salpeter solution, with aqueous slkali titration such as ammoniacal liquor, the sediment ageing, with unwanted other ions of the pure water flush away overwhelming majority, elimination moisture under vacuum, and use pure water drip washing, use ethanol drip washing at last, oven dry makes sediment remain decentralization particle preferably, the particulate that particle mean size is 0.2～0.3 μ m can be obtained,, the nanometer grade powder of 10-40nm can be prepared by the secondary pulverization process of powder.This is a kind of ito powder with the wet processing preparation.The shortcoming of this method is, product is the mechanical impurity of indium oxide and tin oxide, and conductivity is very poor, must just can be transformed into the ITO conducting powder through high-temperature calcination, and under high-temperature solid the diffusion difficulty, be difficult to form single-phase ito powder fully, Cl is arranged in the final products
-, SO
4 -Anion exists.
Another kind of common method is to adopt two kinds of single metal oxide powders, mixes powder in proportion, high-temperature calcination, pulverizes, sieves, and finally obtains conductive powder, also has diffusion difficulty high-temperature solid under, is difficult to form the problem of complete single-phase ito powder.The shortcoming of the method is that production process is very long, and particle size is big, and impurity content is difficult to control.
Summary of the invention
The object of the invention provides a kind of nano homogeneous phase composite metal oxide conductive powder that is used for transparent conductive material.
Further aim of the present invention provides a kind of manufacture method that is used for the nano homogeneous phase composite metal oxide conductive powder of transparent conductive material.
This nano homogeneous phase composite metal oxide conductive powder that is used for transparent conductive material comprises In
2O
3, SnO
2, ZnO, Sb
2O
3The primary crystallization phase, and primary crystallization 0.1～20% the doping phase of forming by any two kinds and two or more oxide in the metals such as indium, tin, lead, zinc, bismuth, antimony, gallium, germanium, aluminium, copper, titanium, nickel, iron, molybdenum, vanadium, cerium, zirconium, hafnium, niobium, tantalum, ruthenium, rhodium mutually, this composite oxide power has single homogeneous phase institutional framework.
The nano homogeneous phase composite metal oxide conductive powder that is used for transparent conductive material of the present invention is to use this method to make: powder is by with indium, tin, plumbous, zinc, bismuth, antimony, gallium, germanium, aluminium, copper, titanium, nickel, iron, molybdenum, vanadium, cerium, zirconium, hafnium, niobium, tantalum, ruthenium, two or more metal component ratio on demand is made into alloy melting in the metals such as rhodium, the alloy of fusing is pressed into reactor, add voltage 50～1000V to reactor, electric current 50～1000A, feed the oxidizability gaseous mixture in the reactor, the metallic atom of gaseous state and oxygen atom reaction, under resistance heat and strong magnetic field action, motlten metal is atomized, gasification, oxidation, handle the homogeneous system that the two or more nano-oxides of formation merge mutually through quenching.
Wherein, the common nano homogeneous phase composite metal oxide conductive powder that is mainly used in transparent conductive material can make manufacturing with the following method:
Nanometer homogeneous phase ITO conductive powder manufacture method is as follows: In on demand
2O
3, SnO
2Proportioning, its composition range is SnO normally
2Mass percent is 0.1-20%, is converted to the mass ratio of indium and tin.Select the indium and the tin of enough purity for use, the indium tin that will meet ratio is mixed with alloy, alloy is joined in the melter, be heated to about 220 ℃, the indium stannum alloy of fusing is pressed into reactor, adds voltage 50～1000V to reactor, electric current 50～1000A, feed nitrogen oxygen atmosphere in the reactor, the indium of gaseous state, tin atom and oxygen atom reaction.Nanometer homogeneous phase ITO conductive powder shows to have single In through X-ray diffraction analysis
2O
3The powder of body-centered cubic crystal structure.And conventional ITO conductive powder is the In that contains body-centered cubic crystal structure
2O
3SnO with cubic rutile structure
2Two-phase structure.The resistivity of homogeneous phase ITO conductive powder of the present invention is 4.9 * 10
-1Ω cm, purity is 99.99%, average diameter is less than 100nm, specific area 1-40m
2/ g, polymolecularity.Nano-ITO conductive powder transmission electron microscope photo also proves these characteristics.
Nanometer IZO conductive powder manufacture method is as follows: In on demand
2O
3, ZnO proportioning, its composition range normally Zn mass percent is 0.1-20%.Select the indium and the zinc of enough purity for use, the indium and the zinc that will meet ratio are mixed with alloy, alloy is joined in the melter, be heated to about 620 ℃, the indium kirsite that melts is pressed into reactor, add voltage 50～1000V to reactor, electric current 50～1000A, feed nitrogen oxygen atmosphere in the reactor, the indium of gaseous state and zinc atom and oxygen atom reaction, generation has In
2O
3Crystal structure mix zinc IZO powder.This powder has the In of body-centered cubic crystal structure
2O
3Homogeneous structure, have good electric conductivity.This powder purity can reach 99.99%, average diameter is less than 100nm, specific area 1-40m
2The nano-oxide powder of/g, polymolecularity.
Nano ATO conductive powder manufacture method is as follows: SnO on demand
2: Sb
2O
3Proportioning, its composition range is Sb normally
2O
3Mass percent is 1-18%, is converted to the mass ratio of tin antimony.Select the tin and the antimony of enough purity for use, the tin and the antimony that will meet ratio are mixed with alloy, alloy is joined in the melter, melter is heated to about 520 ℃, and the tin pewter that melts is pressed into reactor, adds voltage 50～1000V to reactor, electric current 50～1000A, feed nitrogen oxygen atmosphere in the reactor, the tin of vaporization attitude, antimony atoms and oxygen atom reaction, generation has SnO
2The Sb-doped nano ATO conductive powder of crystal structure.The SnO of this powder four directions rutile structure
2Homogeneous structure, have good electric conductivity.This powder purity can reach 99.99%, average diameter is less than 100nm, specific area 1-60m
2The nano-oxide powder of/g, polymolecularity.
Other composite oxide of metal manufacture method is as follows: form alloy by a certain percentage, motlten metal is fed reactor, add voltage 50～1000V to reactor, electric current 50～1000A, feed nitrogen oxygen atmosphere in the reactor, under resistance heat and strong magnetic field action, atomizing, gasification, oxidation, handle through quenching, form the composite nano oxide powder.This composite oxide of metal comprises by in the metals such as indium, tin, lead, zinc, bismuth, antimony, gallium, germanium, aluminium, copper, titanium, nickel, iron, molybdenum, vanadium, cerium, zirconium, hafnium, niobium, tantalum, ruthenium, rhodium any two kinds and two or more.
This nano composite oxide powder, need not sintering and postprocessing working procedures promptly have conductivity, high product purity, high crystalline, polymolecularity, mobile strong do not contain acid radical anion in the powder, healthy very useful for environment and workman.The present invention can make composite oxides conductive powder manufacturing process shorten greatly, and production capacity increases substantially.
Description of drawings
Fig. 1 is the nano-ITO powder X-ray diffractogram, shows that nano-ITO powder has single In
2O
3Body-centered cubic crystal structure.
Fig. 2 is conventional ITO conductive powder X-ray diffraction facies analysis figure.
Fig. 3 contains SnO
2It is 10% nano-ITO conductive powder transmission electron microscope photo.
Embodiment 1:
Nano-ITO prepares the preparation method
1, the oxide of indium tin is pressed In
2O
3: SnO
2=9: 1 proportioning is converted to the weight of indium and tin by weight.
2, the fusing of indium tin is mixed with alloy.
3, alloy is joined in the melter, energising is heated to about 220 ℃.
4, the indium kirsite with fusing is pressed into reactor.
5, add voltage to reactor, voltage 50～1000V, electric current 50～1000A.Feed nitrogen oxygen atmosphere in the reactor.
6, open the receipts powder system.
Produce product index and see Table 1.
Table 1 nano-ITO technical target of the product
| The name of an article | In 2O 3∶SnO 2 | Average grain diameter nm | Specific area m 2/g | Purity | Dispersed | Powder resistance rate Ω cm |
| ITO | 9∶1 | 30～70 | 12 | ＞99.99％ | Hard aggregation-free | 4.9×10 -1 |
Nano-ITO powder has single In through the X-ray diffraction facies analysis
2O
3Body-centered cubic crystal structure.
Embodiment 2
Nanometer IZO powder preparation method
1, indium zinc is pressed In
2O
3: ZnO=93: 7 proportioning, be converted to the quality of corresponding indium and zinc by mass ratio, join in the melting furnace.
2, the melter energising is heated to about 620 ℃, makes the fusing of indium kirsite.
3, the indium kirsite with fusing is pressed into reactor.
4, add voltage to reactor, voltage 50～1000V, electric current 50～1000A feeds pure oxygen in the reactor.
5, open the receipts powder system.
Product index sees Table 2
Table 2 nanometer IZO technical target of the product
| The name of an article | In 2O 3∶ZnO | Granularity nm | Specific area m 2/g | Purity | Dispersed |
| IZO | 93∶7 | 30～70 | 22 | ＞99.99％ | Hard aggregation-free |
Nanometer IZO powder has single In through the X-ray diffraction facies analysis
2O
3Body-centered cubic crystal structure.
Embodiment 3
The nano ATO powder preparation method
1, tin antimony is pressed SnO
2: Sb
2O
3=98: 2 proportioning, the quality of converting out corresponding tin antimony in proportion adds in the melting furnace.
2, the melter energising is heated to about 520 ℃, makes the tin pewter fusing.
3, the tin pewter with fusing is pressed into reactor.
4, add voltage to reactor, voltage 5～1000V, electric current 50～1000A.Bubbling air in the reactor.
5, open the receipts powder system.
The ATO technical indicator sees Table 3.
Table 3 nano ATO technical indicator
| The name of an article: | SnO 2∶Sb 2O 3 | Granularity nm | Specific area m 2/g | Purity | Dispersed | Powder resistance rate Ω cm |
| ATO | 98∶2 | 20～50 | 20 | ＞99.99％ | Hard aggregation-free | 4.4×10 -1 |
The nano ATO powder has single S nO through the X-ray diffraction facies analysis
2Body-centered cubic crystal structure.
Claims (8)
1. a nano homogeneous phase composite metal oxide conductive powder that is used for transparent conductive material comprises In
2O
3, SnO
2, ZnO, Sb
2O
3The primary crystallization phase, and mass content is mutually 0.1～20% the doping phase of being made up of any one or more than one oxide in indium, tin, lead, zinc, bismuth, antimony, gallium, germanium, aluminium, copper, titanium, nickel, iron, molybdenum, vanadium, cerium, zirconium, hafnium, niobium, tantalum, ruthenium, the rhodium metal of primary crystallization, and it is characterized in that: this composite metal oxide conductive powder has single homogeneous phase institutional framework.
2. according to the described nano homogeneous phase composite metal oxide conductive powder that is used for transparent conductive material of claim 1, it is characterized in that: the primary crystallization of this composite metal oxide conductive powder is In mutually
2O
3, mixing is SnO mutually
2, described doping phase SnO
2Quality be In
2O
3The 0.1-20% of quality, this composite metal oxide conductive powder has single In
2O
3Body-centered cubic crystal structure.
3. according to the described nano homogeneous phase composite metal oxide conductive powder that is used for transparent conductive material of claim 2, it is characterized in that: powder purity is more than 99.99%, and average diameter is less than 100nm, specific area 1-40m
2/ g has polymolecularity.
4. according to the described nano homogeneous phase composite metal oxide conductive powder that is used for transparent conductive material of claim 1, it is characterized in that: the primary crystallization of this composite metal oxide conductive powder is In mutually
2O
3, mixing is ZnO mutually, the quality of described doping phase ZnO is In
2O
3The 0.1-20% of quality, this composite metal oxide conductive powder has single In
2O
3Body-centered cubic crystal structure.
5. according to the described nano homogeneous phase composite metal oxide conductive powder that is used for transparent conductive material of claim 4, it is characterized in that: powder purity is more than 99.99%, and average diameter is less than 100nm, specific area 1-40m
2/ g has polymolecularity.
6. according to the described nano homogeneous phase composite metal oxide conductive powder that is used for transparent conductive material of claim 1, it is characterized in that: the primary crystallization of this composite metal oxide conductive powder is SnO mutually
2, mixing is Sb mutually
2O
3, described doping phase Sb
2O
3Quality be SnO
2The 1-18% of quality has single SnO
2Four directions rutile crystal structure.
7. according to the described nano homogeneous phase composite metal oxide conductive powder that is used for transparent conductive material of claim 6, it is characterized in that: powder purity is more than 99.99%, and average diameter is less than 100nm, specific area 1-60m
2/ g has polymolecularity.
8. make claim 1 for one kind, 2,4 or the 6 described methods that are used for the nano homogeneous phase composite metal oxide conductive powder of transparent conductive material, it is characterized in that: with indium, tin, plumbous, zinc, bismuth, antimony, gallium, germanium, aluminium, copper, titanium, nickel, iron, molybdenum, vanadium, cerium, zirconium, hafnium, niobium, tantalum, ruthenium, two or more metal component ratio on demand is made into alloy melting in the rhodium metal, the alloy of fusing is pressed into reactor, add voltage 50～1000V to reactor, electric current 50～1000A, feed the oxidizability gaseous mixture in the reactor, the metallic atom of gaseous state and oxygen atom reaction, under resistance heat and strong magnetic field action, motlten metal is atomized, gasification, oxidation, handle the homogeneous system that two or more nano-oxide of formation merges mutually through quenching.
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| CN102332325B (en) * | 2011-10-13 | 2012-11-14 | 扬州大学 | In (indium)-Sn (stannum)-Mo (molybdenum)-Nb (niobium)-codoped transparent conductive film and manufacturing method thereof |
| CN104229873B (en) * | 2014-08-14 | 2015-09-23 | 宁波今心新材料科技有限公司 | A kind of preparation method being applicable to the dusty blue pigment of spray ink Printing ceramic ink |
| CN106663493A (en) | 2014-08-28 | 2017-05-10 | E.I.内穆尔杜邦公司 | Copper-containing conductive pastes and electrodes made therefrom |
| JP6564024B2 (en) | 2014-08-28 | 2019-08-21 | イー・アイ・デュポン・ドウ・ヌムール・アンド・カンパニーＥ．Ｉ．Ｄｕ Ｐｏｎｔ Ｄｅ Ｎｅｍｏｕｒｓ Ａｎｄ Ｃｏｍｐａｎｙ | Method for manufacturing a solar cell having a copper electrode |
| DE112014006910T5 (en) | 2014-08-28 | 2017-05-18 | E.I. Du Pont De Nemours And Company | Copper-containing conductive pastes and electrodes made therefrom |
| CN104152670B (en) * | 2014-08-29 | 2016-05-25 | 云南天浩稀贵金属股份有限公司 | The pre-treating technology that a kind of indium germanium refines |
| CN111847594B (en) * | 2019-04-30 | 2022-10-21 | 中关村至臻环保股份有限公司 | Nano electrochemical electrode, electrode assembly and preparation method thereof |
| CN113716953B (en) * | 2021-09-14 | 2022-10-28 | 基迈克材料科技（苏州）有限公司 | Cerium oxide doped IZO powder, target material and preparation method |
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| CN1351961A (en) * | 2001-11-09 | 2002-06-05 | 财团法人工业技术研究院 | Process for producing transparent conductive oxide powder by air jet method |
| CN1529766A (en) * | 2001-07-17 | 2004-09-15 | ������������ʽ���� | Sputtering target and transparent conductive film |
| CN1281544C (en) * | 1998-08-31 | 2006-10-25 | 出光兴产株式会社 | Target for transparent conductive film, transparent conductive material, transparent conductive glass, and transparent conductive film |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1281544C (en) * | 1998-08-31 | 2006-10-25 | 出光兴产株式会社 | Target for transparent conductive film, transparent conductive material, transparent conductive glass, and transparent conductive film |
| CN1529766A (en) * | 2001-07-17 | 2004-09-15 | ������������ʽ���� | Sputtering target and transparent conductive film |
| CN1351961A (en) * | 2001-11-09 | 2002-06-05 | 财团法人工业技术研究院 | Process for producing transparent conductive oxide powder by air jet method |
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