CN100467384C - Process for producing transparent conductive oxide powder by air jet method - Google Patents
Process for producing transparent conductive oxide powder by air jet method Download PDFInfo
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- CN100467384C CN100467384C CNB011346779A CN01134677A CN100467384C CN 100467384 C CN100467384 C CN 100467384C CN B011346779 A CNB011346779 A CN B011346779A CN 01134677 A CN01134677 A CN 01134677A CN 100467384 C CN100467384 C CN 100467384C
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- powder
- indium
- transparent conductive
- metal
- tin
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Abstract
An air jetting process is suitable for producing various transparent conductive oxide powder (ITO, ZnO, In2O3 and SnO2). The process may have the implementation steps of: melting corresponding metal raw material to obtain melt, producing metal powder by using air jetting process, heating to oxidize the metal powder, and controlling the heat treatment making process parameters to obtain transparent conductive oxide powder with required oxidation degree. The said process is simple and low in cost, and produces no pollutant.
Description
Invention field
The present invention relates to method with gas blowout legal system producing transparent conductive oxide powder, especially refer to a kind of raw material powder of making transparent conductive oxide (TransparentConducting Oxide) with the gas blowout method according to the alloying constituent proportioning, again this powdered alloy is sieved, obtain suitable powder diameter, carry out necessary high temperature oxidation to form the oxide powder of abundant oxidation with this powder at last.
Background technology
At traditional optical plated film (Optical coating) and in than advanced display industry industries such as (LCD liquid-crystal displays), must use so-called transparent conducting glass in a large number, that is must on specific glass, plate the material that layer of transparent is conducted electricity, the transparent conductive material that the most normal present quilt uses in a large number is tin indium oxide (Indium-Tin-Oxide, the preparation method of the most normal ITO), and use forms nesa coating with tin indium oxide (ITO) sputter target in the mode of physically splash plating.Just must make the tin indium oxide powder earlier and will make the tin indium oxide sputter target, form sputter target through the High Temperature High Pressure sintering again.Each big producer making tin indium oxide or other transparent conductive oxide powder all are to use chemical reduction method or chemical pyrolysated mode to make in the past, and its making processes is loaded down with trivial details and expensive.
(Japanese Nikko Materials company all) is described to see also the United States Patent (USP) word No. 5417816, and its step of making tin indium oxide (ITO) powder is: (1) with indium-tin raw material melting to form indium-Xi ingot casting; (2) with indium-Xi ingot casting in NH
4NO
3Carry out electrolysis in the solution, to generate indium hydroxide (Indium Hydroxide) and stannic hydroxide (Tin Hydroxide); (3) indium hydroxide and stannic hydroxide are carried out solid-liquid separation (Filtering); (4) use a large amount of pure water to wash (Rinsing) solid indium hydroxide and stannic hydroxide, to make indium hydroxide and stannic hydroxide mud; (5) with indium hydroxide and stannic hydroxide mud drying and pulverizing; (6) carry out calcination (Calcination) after indium hydroxide after will pulverizing and stannic hydroxide sieve again to obtain tin indium oxide (ITO) powder.
Clearly, use the method for known manufacturing transparent conductive oxide powder, it is numerous and diverse that it produces required step, causes to make degree of difficulty and increase, and required cost is also higher naturally, thereby influences its competitive power; And in above-mentioned making processes, can produce a large amount of trade effluents, the problem that pollutes; It must use a large amount of pure water again, also can increase to make required cost.Above variety of problems all is in the industrial application, the problem that each institute of big producer utmost point desire solves.
Therefore the manufacturing industry of domestic LCD flat-panel screens has accounted for global critical role, and the usage quantity at the sputtered target material of transparent conductive film also significantly increases, relative raw material-transparent conductive oxide powder for sputter target, for example: ITO, ZnO, In
2O
3, SnO
2Deng the powder demand also significantly increase.
Summary of the invention
An object of the present invention is to allocate the making transparent conductive oxide powder in proportion according to required alloying constituent for a kind of method with gas blowout legal system producing transparent conductive oxide powder is provided.
A further object of the present invention is for a kind of method with gas blowout legal system producing transparent conductive oxide powder being provided, can adjusting the degree of oxidation of powder by the process parameter of powder oxidizing thermal treatment.
A further object of the present invention is for a kind of method with gas blowout legal system producing transparent conductive oxide powder is provided, to simplify processing procedure, to reduce cost.
A further object of the present invention is for a kind of method with gas blowout legal system producing transparent conductive oxide powder being provided, can avoiding producing any trade effluent, and the byproduct of other pollution.
The present invention is for reaching above-mentioned purpose, so propose a kind of method with gas blowout legal system producing transparent conductive oxide powder, it comprises will provide the raw metal of making transparent conductive oxide powder to be melt into molten metal; With the gas blowout method this molten metal is made metal-powder; This metal-powder of oxidation of heating, and control process of thermal treatment parameter are to obtain the transparent conductive oxide powder of required degree of oxidation.
The gas blowout method as the term suggests promptly be to utilize gas when the spraying media, be dispersed as small droplets with the melt metal liquation or utilize centrifugal force that it is fallen and loose into small droplets, becomes the method for metal-powder again through cooled and solidified.Its gas commonly used has air and rare gas element, and as nitrogen, argon gas etc., and required gas atomization device can be divided into horizontal and rectilinear two kinds.
The size of the particle diameter of made powder and spray condition concern that empirical formula is as follows:
Wherein, D: powder diameter
C: nozzle geometric constant
V: the speed of spray gas
U
m: the viscosity of metal melting body
ρ
m: the density of metal melting body
γ: the surface tension of metal melting body
By following formula as can be known, the size of made powder particle and the inversely proportional relation of the speed of spray gas, that is the speed of spray gas is faster, made powder diameter is littler, also can use different controlled variable, controls the powder diameter size.
The preferably, promptly a kind of method with gas blowout legal system producing transparent conductive oxide indium (In) tin powder comprises indium metal (In) and tin (Sn) are heated between 600 ℃-800 ℃ simultaneously, makes it be melt into indium-Xi mixed molten liquid; With the gas blowout method this indium-Xi mixed molten liquid is made indium-Xi mixed powder; Be heated to 850 ℃ and continue 2 hours, make this indium-Xi mixed powder complete oxidation, to make tin indium oxide (Indium-Tin-Oxide; ITO) powder.
Method with gas blowout legal system producing transparent conductive oxide powder of the present invention is for various transparent conductive oxide powder (ITO, ZnO, In
2O
3, SnO
2) all can use.
Not only processing procedure is simple for method with gas blowout legal system producing transparent conductive oxide powder of the present invention, and its need heated oxide in air, by control process of thermal treatment parameter, can obtain required degree of oxidation, so can reduce cost, and it more can avoid producing any trade effluent, and the byproduct of other pollution, thereby has thoroughly improved all shortcomings of known technology.
Further the present invention is done more deep explanation below in conjunction with embodiment.
Description of drawings
Wherein, accompanying drawing 1 is the schema of the present invention with gas blowout legal system producing transparent conductive oxide powder.
Accompanying drawing 2 is the employed gas atomization device of a gas blowout method of the present invention synoptic diagram.
Accompanying drawing 3 is made the schema of tin indium oxide (ITO) powder with the gas blowout legal system for the present invention.
Accompanying drawing 4 is made indium trioxide (In for the present invention with the gas blowout legal system
2O
3) schema of powder.
Accompanying drawing 5 is made tindioxide (SnO for the present invention with the gas blowout legal system
2) schema of powder.
Accompanying drawing 6 is made the schema of zinc oxide (ZnO) powder with the gas blowout legal system for the present invention.
Wherein, label is expressed as respectively in the accompanying drawing:
1 is the raw material preparation;
1a is indium metal (In), metallic tin (Sn);
1b is indium metal (In);
1c is metallic tin (Sn);
1d is metallic zinc (Zn);
2 are the powder process of gas blowout method;
2a is for being indium metal-tin melt with indium metal-Xi fusion, with the powder process of gas blowout method;
2b is for being the indium metal liquation with the indium metal fusion, with the powder process of gas blowout method;
2c is for being the metallic tin liquation with the metallic tin fusion, with the powder process of gas blowout method;
2d is for being the metallic zinc liquation with the metallic zinc fusion, with the powder process of gas blowout method;
3 for powder is collected, screening;
3a is for collecting, sieve indium-tin powder;
3b is for collecting, sieve the indium powder;
3c is for collecting, sieve tin powder;
3d is for collecting, sieve zinc powder;
4 is the high temperature oxidation powder;
4a is high temperature oxidation indium-tin powder;
4b is a high temperature oxidation indium powder;
4c is the high temperature oxidation tin powder;
4d is the high temperature oxidation zinc powder;
5 for finishing transparent conductive oxide powder;
5a is for making tin indium oxide (ITO) powder;
5b is for making indium trioxide (In
2O
3) powder;
5c is for making tindioxide (SnO
2) powder;
5d is for making zinc oxide (ZnO) powder;
6 is rectilinear gas atomization device;
60 is that furnace is melted in induction;
600 is crucible;
601 is well heater;
61 is nozzle;
62 are the spraying storehouse;
63 is the powder collection storehouse;
7 is molten metal;
70 is the hollow form cone;
71 is metal-powder;
8 is high pressure gas.
A kind of method with gas blowout legal system producing transparent conductive oxide powder, its better implementation step be as shown in Figure 1:
(a) raw material prepares 1: according to want to make different transparent conductive oxide powders, for example: ITO, ZnO, In2O
3、SnO
2Deng, prepare required different metal raw material.
(b) gas blowout legal system powder 2: required different metal raw material is inserted the gas atomization device In, make metal dust to carry out the gas blowout legal system, this moment, the metal dust of gained only had the surface slightly Low-level oxidation.
(c) powder is collected, is sieved 3: the prepared metal dust of step (b) is collected After, sieving to stay the powder that meets required particle diameter, it amounts to material output capacity (Yield) More than 85%.
(d) the high-temperature oxydation powder 4: the metal dust that screening in the step (c) is good is according to different Demand imposes the high-temperature oxydation of different time and temperature, and controls the process of thermal treatment parameter, To obtain required degree of oxidation.
(e) finish transparent conductive oxide powder 5: the high-temperature oxydation through step (d) makes Get the metal dust complete oxidation, thereby make the transparent conductive oxide powder of required degree of oxidation The end.
The gas blowout process is described as an example of rectilinear gas atomization device example below.
Embodiment
The employed gas atomization device of gas blowout method of the present invention synoptic diagram as shown in Figure 2.Rectilinear gas atomization device 6, be that raw metal is put into the crucible 600 that furnace 60 is melted in induction, utilize induction to melt well heater 601 heating of furnace 60, make raw metal be melt into molten metal 7, and the high pressure gas 8 of utilization feeding, molten metal 7 is sprayed fast by nozzle 61, because molten metal 7 is subjected to the effect of high pressure gas 8 rapid expansion in nozzle 61 exits, forming hollow form cone 70 in spraying storehouse 62 outwards disperses, if molten metal 7 has sufficient superheating temperature and is subjected to the effect of shearing stress and accelerating force again, at first form tough band shape, then form spheric metal-powder 71 subsequently and concentrate in the powder collection storehouse 63.
The present invention as shown in Figure 3 makes the schema of tin indium oxide (ITO) powder with the gas blowout legal system, and its step is as follows:
(a) indium metal (In), metallic tin (Sn) 1a: the pure indium (In) and the pure tin (Sn) of purity 99.99% are ready to complete according to component proportions.
(b) be indium metal-tin melt with indium metal-Xi fusion, with gas blowout legal system powder 2a: the raw material that step (a) is ready to complete, insert and carry out the powder process of gas blowout method in the gas atomization device, the employed nozzle material of this gas atomization device is boron nitride (BN), bore is 2.5-4.0mm, and it is material that crucible then adopts zirconium white.Place crucible to be heated to 600-800 ℃ indium metal-Xi, making indium metal-Xi fusion is indium metal-tin melt, and nozzle cools off so that current are logical, and with pure oxygen (O
2) spray, spray pressure is set at 80-90kg/cm
2, the atomization process of this gas blowout manufactured indium-tin powder lasts about 2-4 minute altogether.
(c) collect, sieve indium-tin powder 3a: indium-tin powder is collected and sieved, amounting to material output capacity (Yield) is 90%, powder diameter is distributed in 40-100 μ m, by the appearance color of indium-tin powder is this indium-tin powder of decidable complete oxidation not as yet, even if using pure oxygen sprays, the process of its powder process is quite quick, so indium-tin powder complete oxidation not.
(d) high temperature oxidation indium-tin powder 4a: step (c) indium-tin powder finished of sieving is inserted in the atmospheric furnace, and bubbling air is heated between 750 ℃-950 ℃, and the required time of heated oxide is 1-3 hour.In the present embodiment, adopting Heating temperature is 850 ℃, thermal treatment 2 hours, makes the oxidation in high temperature of indium-tin powder.
(e) make tin indium oxide (ITO) powder 5a: behind the high temperature oxidation through step (d), this moment, indium-tin powder became the yellow of complete oxidation by original gray iron look, through XRD analysis as can be known, had made tin indium oxide (ITO) powder.
The present invention as shown in Figure 4 makes indium trioxide (In with the gas blowout legal system
2O
3) schema of powder, its step is as follows:
(a) indium metal (In) 1b: the pure indium (In) of purity 99.99% is ready to complete.
(b) be the indium metal liquation with the indium metal fusion, with gas blowout legal system powder 2b: with the raw material that step (a) is ready to complete, insert and carry out the powder process of gas blowout method in the gas atomization device, this gas atomization device also is to adopt rectilinear gas atomization device, then can make the indium powder.
(c) collect, screening indium powder 3b: with the indium powder collection and sieve; Certainly also complete oxidation not as yet of the indium powder of this moment, its oxygen level is 0.35wt%.
(d) high temperature oxidation indium powder 4b: step (c) the indium powder of finishing that sieves is inserted in the atmospheric furnace, bubbling air, carry out oxidation in the high temperature, it selects different condition respectively: 800 ℃ of * 4Hr (hour), 800 ℃ of * 8Hr (hour), 800 ℃ of * 12Hr (hour).
(e) make indium trioxide (In
2O
3) powder 5b: behind the high temperature oxidation through step (d), the prepared indium trioxide powder of different condition is as can be known by analysis again: 800 ℃ of * 4Hr (hour) prepared indium trioxide powder oxygen level be 16.9wt%, 800 ℃ of * 8Hr (hour) prepared indium trioxide powder oxygen level be 18.7wt%, 800 ℃ of * 12Hr (hour) prepared indium trioxide powder oxygen level is 17.2wt%, so, obtain the indium trioxide powder of different demands as can be known by the condition of control high temperature oxidation.
The present invention as shown in Figure 5 makes tindioxide (SnO with the gas blowout legal system
2) schema of powder, the present invention as shown in Figure 6 does with the gas blowout legal system in the schema of zinc oxide (ZnO) powder as can be seen, the flow process that it adopted is all similar with the step of front, it is the raw material difference that adopts, and the powder that desire is made is also different, also express the method for the present invention with gas blowout legal system producing transparent conductive oxide powder, all can use for making various transparent conductive oxide powder, not only processing procedure is simple, and its need heated oxide in air, by control process of thermal treatment parameter, can obtain required degree of oxidation, so can reduce cost, and it more can avoid producing any trade effluent, and the byproduct of other pollution, thereby has thoroughly improved all shortcomings of known technology.
Of the present invention graphic with describe as above with the preferred embodiment explanation, association obtains easily, such as: use other raw material to make transparent conductive oxide powder, or earlier raw materials melt is become liquation, just put into the gas atomization device and carry out gas blowout method powder process or the like, be familiar with this field skill person after comprehension spirit of the present invention, all can expect changing enforcement, so the explanation of preferred embodiment of the present invention only is used for helping to understand the present invention, non-in order to limit spirit of the present invention, in not breaking away from spiritual scope of the present invention, to replace when doing a little change retouching and equal variation, it does not also break away from the spirit and scope of the present invention.
Claims (2)
1, a kind of method with gas blowout legal system producing transparent conductive indium trioxide powder, tindioxide powder, tin indium oxide powder, Zinc oxide powder, it is as follows to it is characterized in that step comprises:
A, will provide raw metal indium, tin, the zinc of making transparent conductive oxide powder or the group that they constituted to be melt into molten metal;
B, this molten metal is made metal-powder with the gas blowout method;
C, this metal-powder of oxidation of heating are to make transparent conductive oxide powder.
2, in accordance with the method for claim 1, it is characterized in that its step includes:
A, with indium metal and tin simultaneously between 600 ℃ of-800 ℃ of temperature ranges heating and melting become indium-Xi mixed molten liquid;
B, this indium-Xi mixed molten liquid is made indium-Xi mixed powder with the gas blowout method;
C, the indium-Xi mixed powder of step b gained was heated 1-3 hour between 750 ℃ of-950 ℃ of temperature ranges, make the tin indium oxide powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011346779A CN100467384C (en) | 2001-11-09 | 2001-11-09 | Process for producing transparent conductive oxide powder by air jet method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011346779A CN100467384C (en) | 2001-11-09 | 2001-11-09 | Process for producing transparent conductive oxide powder by air jet method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1351961A CN1351961A (en) | 2002-06-05 |
| CN100467384C true CN100467384C (en) | 2009-03-11 |
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ID=4672661
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB011346779A Expired - Lifetime CN100467384C (en) | 2001-11-09 | 2001-11-09 | Process for producing transparent conductive oxide powder by air jet method |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101246759B (en) * | 2007-02-15 | 2010-09-08 | 中国船舶重工集团公司第七二五研究所 | Nano homogeneous phase composite metal oxide conductive powder for transparent conducting material and its preparation method |
| CN102701272B (en) * | 2012-05-25 | 2014-04-30 | 中南大学 | Method and device for preparing stannic oxide powder |
| US9922807B2 (en) | 2013-07-08 | 2018-03-20 | Jx Nippon Mining & Metals Corporation | Sputtering target and method for production thereof |
| CN103318952B (en) * | 2013-07-17 | 2015-03-25 | 柳州百韧特先进材料有限公司 | Method for producing nano-sized tin dioxide |
| CN104445398B (en) * | 2014-09-18 | 2016-04-20 | 株洲科能新材料有限责任公司 | The method of superfine bismuth oxide powder is prepared based on fluidized bed airflow pulverizer |
| CN104276597B (en) * | 2014-09-18 | 2016-03-23 | 株洲科能新材料有限责任公司 | The preparation method of the special gallium oxide powder of a kind of IGZO target |
| CN107673402B (en) * | 2017-09-30 | 2019-04-02 | 广东天高科技有限公司 | A kind of glass putty production and processing technology |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5417816A (en) * | 1992-12-09 | 1995-05-23 | Nikko Kyodo, Ltd. | Process for preparation of indium oxide-tin oxide powder |
-
2001
- 2001-11-09 CN CNB011346779A patent/CN100467384C/en not_active Expired - Lifetime
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5417816A (en) * | 1992-12-09 | 1995-05-23 | Nikko Kyodo, Ltd. | Process for preparation of indium oxide-tin oxide powder |
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