CN104229872A - Process for continuously producing micron-sized gallium oxide powder - Google Patents
Process for continuously producing micron-sized gallium oxide powder Download PDFInfo
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- CN104229872A CN104229872A CN201410478701.6A CN201410478701A CN104229872A CN 104229872 A CN104229872 A CN 104229872A CN 201410478701 A CN201410478701 A CN 201410478701A CN 104229872 A CN104229872 A CN 104229872A
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- gallium oxide
- oxide powder
- gallium
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a process for continuously producing micron-sized gallium oxide powder. According to the process, micron-sized gallium oxide powder is prepared by a full-automatic gallium oxide producing device; the full-automatic gallium oxide producing device comprises a reactor, cyclone separators, collectors and automatic packing machines; when micron-sized gallium oxide powder is continuously produced by metal gallium, the metal gallium flows out of a molten metal hole after heated and melted by an electric arc furnace; preheated air is sprayed out from four air flow holes simultaneously, liquid metal gallium is impacted and sheared in the air flow intersection position, an oxidation reaction is performed simultaneously, and the micron-sized gallium oxide powder is formed; and the micron-sized gallium oxide powder sequentially enters a cyclone separator I and a cyclone separator II for classification with air flow and then is collected in the collectors, and continuous production of the micron-sized gallium oxide powder prepared by the metal gallium is completed. The process completely realizes full-automatic continuous production of micron-sized gallium oxide, the purity of the prepared gallium oxide is high, the grain diameter is small, the distribution range is small, gallium oxide with different grain diameters is obtained through classification and meet different use demands, and the process is environment-friendly and low in cost.
Description
Technical field
The present invention relates to a kind of technique of continuous seepage micron order gallium oxide powder, belong to the technical field of gallium oxide powder preparation.
Background technology
One, the purposes of gallium oxide: gallium oxide is a kind of transparent conductive oxide semiconductor material, has broad application prospects in opto-electronic device, mainly for the production of luminescent material, crystalline material, catalyzer and other goods.
The abbreviation that IGZO (Indium Gallium Zinc Oxide) is Indium sesquioxide gallium zinc, it is a kind of membrane transistor technology, refers on TFT-LCD active layers, stamps layer of metal oxide compound.IGZO material is for the channel layer materials in thin-film transistor technologies of new generation, is the one of metal oxide (Oxied) panel technology.
The energy gap of IGZO, at about 3.5eV, is a kind of N-type semiconductor material.In
2o
3in In can form 5S electronic orbit, be conducive to the high-speed transfer of current carrier, the mobility of electronics is at 35cm
2/ VS; Ga
2o
3there is very strong ionic linkage, the generation in O room can be suppressed; Zn in ZnO
2+stable tetrahedral structure can be formed, metal oxide IGZO can be made to form stable non-crystal structure.Therefore, metal oxide IGZO is applicable to make high mobility thin film transistor.
Two, existing major technique:
1, chemical method: normally adopt gallium and nitric acid or sulfuric acid reaction, generates gallium salt, then adopts and calcine in hydrothermal reaction kettle, generate ultra-fine gallium oxide product; Or make gallium sulfate and ammonium sulfate in aqueous polymerizable crystallizable separate out ammonium gallium sulfate crystal, by ammonium gallium sulfate crystal through repeatedly recrystallization process, obtained high-purity sulphuric acid gallium ammonium crystal, eventually passes ovens dry, roasting, acquisition high-purity gallium oxide.Owing to employing strong acid (sulfuric acid or nitric acid) in production process, therefore produce dangerous large, big for environment pollution, chemical method complicated operation, yields poorly, and the superfine bismuth oxide that chemical method is produced easily is reunited.
2, electrochemical process: using gallium in the electrolyzer adding alkali lye as electrolytic anode, carry out electrolytic preparation sodium solution gallate; Be intermediate material by sodium solution gallate again, carry out neutralizing, wash, dry, roasting, obtained high-purity gallium oxide.Owing to employing alkali lye in production process, inevitably brought basic metal or alkaline-earth metal ions into, affected the purity of gallium oxide, and the production cycle is long.
3, sol-gel method: be dissolved into by gallium nitrate in concentrated nitric acid, drips strong aqua adjust ph; Solution heated and adds citric acid, after stirring cooling, becoming clear gel; Be placed in retort furnace, at high temperature dry, obtain gallium oxide; Second step: utilize tube type vacuum stove to prepare gan superfine crystal, load in vitrified pipe by gallium oxide/agraphitic carbon mixture, exhausted air is filled with ammonia; 1 hour is incubated at temperature 850 ~ 950 DEG C; Obtained gan superfine crystal after passing into argon gas cooling again.Sol-gel method also needs to use nitric acid, and the danger in operation is large, big for environment pollution, and complicated operation, yield poorly.
Maximum defect is, above 3 kinds of methods all cannot realize full-automation.
Summary of the invention
For the defect preparing gallium oxide existence in prior art, the object of the invention is to be to provide a kind of simple to operate, cost is low, the work method of energy continuous prodution micron level gallium oxide, obtained gallium oxide purity is high, particle diameter is little, and narrow diameter distribution, meet application particle diameter being had to particular requirement.
The invention provides a kind of technique of continuous seepage micron order gallium oxide powder, this technique adopts gallium oxide fully-automatic production device to prepare micron order gallium oxide powder, described gallium oxide fully-automatic production device comprises reactor, cyclonic separator I and cyclonic separator II, collector and automatic packing machine, described reactor is connected with cyclonic separator II with cyclonic separator I successively, cyclonic separator I is provided with a collector, cyclonic separator II top and bottom are respectively provided with a collector, and each collector is respectively furnished with an automatic packing machine; Described reactor forms by being oxidized nozzle, air compressor and electric arc furnace; Described oxidation nozzle central authorities are provided with metal fluid apertures, metal fluid apertures is connected with electric arc furnace, described metal fluid apertures surrounding is evenly distributed with 4 airflow holes, and described airflow hole 20 ~ 40 ° along metal fluid apertures axle center angle directions are arranged, and described airflow hole is connected with air compressor; When carrying out gallium quantity-produced micron order gallium oxide powder, gallium, after electric arc furnace is heated to 200 ~ 300 DEG C, flows out from metal fluid apertures; Now, open the preheated air of air compressor conveying 200 ~ 300 DEG C, described preheated air sprays with the pressure of 5 ~ 10MPa from 4 airflow holes simultaneously, liquid metal gallium in air-flow intersection by gas shock, shearing, carry out oxidizing reaction simultaneously, form median size at 2.5 ~ 3 μm, size distribution is 0.1 ~ 10 μm of gallium oxide powder accounting for more than 99.5%; Gained gallium oxide powder enters cyclonic separator I successively with air-flow and cyclonic separator II carries out classification, particle diameter is obtained at the gallium oxide powder being greater than 6.5 μm in the collector of cyclonic separator I, the gallium oxide powder that particle diameter is less than 0.8 μm is obtained in the collector that cyclonic separator II top is connected, and in the collector that the gallium oxide powder collection of other particle diameter is connected bottom cyclonic separator II; Gallium oxide powder in each collector is packed by automatic packing machine, completes the continuous seepage that gallium prepares micron order gallium oxide powder.
The technique of continuous seepage micron order gallium oxide powder of the present invention also comprises following preferred version:
In preferred scheme, gallium is after electric arc furnace is heated to 240 ~ 260 DEG C, flows out from metal fluid apertures.
In preferred scheme, the temperature of preheated air is 240 ~ 260 DEG C.
In preferred scheme, along metal fluid apertures axle center, 25 ~ 35 ° of angle directions are arranged airflow hole; Most preferably be 30 °.
In preferred scheme, preheated air sprays with the pressure of 6 ~ 8MPa from 4 airflow holes simultaneously, most preferably is 7MPa.
Beneficial effect of the present invention: the continuous seepage 1, realizing micron level gallium oxide powder completely, and the gallium oxide powder that simultaneously can obtain three kinds of different-grain diameter distribution ranges further, to adapt to different application gallium oxide particle diameter being had to particular requirement; 2, little, the narrowly distributing of the gallium oxide powder diameter prepared of the method, and purity is high; 3, omnidistance without soda acid use, environmental protection, and labour intensity is low, realize full-automatic continuous prodution, production cost reduces greatly.
Accompanying drawing explanation
[Fig. 1] is gallium oxide fully-automatic production device schematic diagram of the present invention;
[Fig. 2] is for being oxidized nozzle section figure in fully-automatic production device;
The gallium oxide grain size distribution that [Fig. 3] obtains for embodiment 1;
1 is air compressor, and 2 is arc electric furnace, and 3 is oxidation nozzle, and 4 is reactor, and 5-1 is cyclonic separator I, and 5-2 is cyclonic separator II, 6-1,6-2,6-3 be collector, 7-1,7-2,7-3 are automatic packing machine, and 8 is airflow hole, and 9 is metal fluid apertures.
Embodiment
Following examples are intended to further illustrate content of the present invention, instead of limit the scope of the invention.
Composition graphs 1 and Fig. 2 gallium oxide fully-automatic production device to the employing of the invention process 1 and embodiment 2 is made an explanation: gallium oxide fully-automatic production device comprises reactor 4, cyclonic separator I5-1 and cyclonic separator II5-2, collector 6-1, 6-2, 6-3, with automatic packing machine 7-1, 7-2, 7-3, described reactor 4 is connected with cyclonic separator II5-2 with cyclonic separator I5-1 successively, cyclonic separator I5-1 is provided with a collector 6-1, is furnished with automatic packing machine 7-1, cyclonic separator II5-2 top is provided with collector 6-3, and be furnished with automatic packing machine 7-3 and bottom is provided with collector 6-2, and be furnished with an automatic packing machine 7-2, described reactor 4 is made up of oxidation nozzle 3, air compressor 1 and electric arc furnace 2, described oxidation nozzle 3 central authorities are provided with metal fluid apertures 9, metal fluid apertures 9 is connected with electric arc furnace 2, described metal fluid apertures 9 surrounding is evenly distributed with 4 airflow holes 8, and described airflow hole 20 ~ 40 ° along metal fluid apertures axle center angle directions are arranged, and described airflow hole 8 is connected with air compressor 1.
Embodiment 1
When carrying out gallium quantity-produced micron order gallium oxide powder, gallium is after electric arc furnace is heated to 240 DEG C, and molten metal gallium flows out from metal fluid apertures; Now, open the preheated air that air compressor carries 250 DEG C, described preheated air sprays with the pressure of 7MPa from 4 airflow holes simultaneously, jet angle is along direction, 30 °, metal fluid apertures axle center, liquid metal gallium by gas shock, shearing, carries out oxidizing reaction in air-flow intersection simultaneously, forms median size at 2.673 μm, size distribution accounts for 99.70% for being less than 10 μm, is less than the gallium oxide powder that 5 μm account for 85.88%; Gained gallium oxide powder enters cyclonic separator I successively with air-flow and cyclonic separator II carries out classification, particle diameter is obtained at the gallium oxide powder being greater than 6.5 μm in the collector of cyclonic separator I, the gallium oxide powder that particle diameter is less than 0.8 μm is obtained in the collector that cyclonic separator II top is connected, and in the collector that the gallium oxide powder collection of other particle diameter is connected bottom cyclonic separator II; Gallium oxide powder in each collector is packed by automatic packing machine, and packing pack is delivered to the material storage area of specifying automatically respectively, and complete the continuous seepage that gallium prepares micron order gallium oxide powder, the gallium oxide powder purity obtained is 99.9%.
Embodiment 2
When carrying out gallium quantity-produced micron order gallium oxide powder, gallium is after electric arc furnace is heated to 250 DEG C, and molten metal gallium flows out from metal fluid apertures; Now, open the preheated air that air compressor carries 260 DEG C, described preheated air sprays with the pressure of 6MPa from 4 airflow holes simultaneously, jet angle is along direction, 30 °, metal fluid apertures axle center, liquid metal gallium by gas shock, shearing, carries out oxidizing reaction in air-flow intersection simultaneously, forms median size at 2.875 μm, size distribution accounts for 99.52% for being less than 10 μm, is less than the gallium oxide powder that 5 μm account for 84.62%; Gained gallium oxide powder enters cyclonic separator I successively with air-flow and cyclonic separator II carries out classification, particle diameter is obtained at the gallium oxide powder being greater than 6.5 μm in the collector of cyclonic separator I, the gallium oxide powder that particle diameter is less than 0.8 μm is obtained in the collector that cyclonic separator II top is connected, and in the collector that the gallium oxide powder collection of other particle diameter is connected bottom cyclonic separator II; Gallium oxide powder in each collector is packed by automatic packing machine, and packing pack is delivered to the material storage area of specifying automatically respectively, and complete the continuous seepage that gallium prepares micron order gallium oxide powder, the gallium oxide powder purity obtained is 99.9%.
Embodiment 3
When carrying out gallium quantity-produced micron order gallium oxide powder, gallium is after electric arc furnace is heated to 200 DEG C, and molten metal gallium flows out from metal fluid apertures; Now, open the preheated air that air compressor carries 220 DEG C, described preheated air sprays with the pressure of 5MPa from 4 airflow holes simultaneously, jet angle is along direction, 40 °, metal fluid apertures axle center, liquid metal gallium by gas shock, shearing, carries out oxidizing reaction in air-flow intersection simultaneously, forms median size at 2.985 μm, size distribution accounts for 99.50% for being less than 10 μm, is less than the gallium oxide powder that 5 μm account for 83.79%; Gained gallium oxide powder enters cyclonic separator I successively with air-flow and cyclonic separator II carries out classification, particle diameter is obtained at the gallium oxide powder being greater than 6.5 μm in the collector of cyclonic separator I, the gallium oxide powder that particle diameter is less than 0.8 μm is obtained in the collector that cyclonic separator II top is connected, and in the collector that the gallium oxide powder collection of other particle diameter is connected bottom cyclonic separator II; Gallium oxide powder in each collector is packed by automatic packing machine, and packing pack is delivered to the material storage area of specifying automatically respectively, and complete the continuous seepage that gallium prepares micron order gallium oxide powder, the gallium oxide powder purity obtained is 99.6%.
Claims (5)
1. the technique of a continuous seepage micron order gallium oxide powder, it is characterized in that, gallium oxide fully-automatic production device is adopted to prepare micron order gallium oxide powder, described gallium oxide fully-automatic production device comprises reactor, cyclonic separator I and cyclonic separator II, collector and automatic packing machine, described reactor is connected with cyclonic separator II with cyclonic separator I successively, cyclonic separator I is provided with a collector, cyclonic separator II top and bottom are respectively provided with a collector, and each collector is respectively furnished with an automatic packing machine; Described reactor forms by being oxidized nozzle, air compressor and electric arc furnace; Described oxidation nozzle central authorities are provided with metal fluid apertures, metal fluid apertures is connected with electric arc furnace, described metal fluid apertures surrounding is evenly distributed with 4 airflow holes, and described airflow hole 20 ~ 40 ° along metal fluid apertures axle center angle directions are arranged, and described airflow hole is connected with air compressor; When carrying out gallium quantity-produced micron order gallium oxide powder, gallium, after electric arc furnace is heated to 200 ~ 300 DEG C, flows out from metal fluid apertures; Now, open the preheated air of air compressor conveying 200 ~ 300 DEG C, described preheated air sprays with the pressure of 5 ~ 10MPa from 4 airflow holes simultaneously, liquid metal gallium in air-flow intersection by gas shock, shearing, carry out oxidizing reaction simultaneously, form median size at 2.5 ~ 3 μm, size distribution is 0.1 ~ 10 μm of gallium oxide powder accounting for more than 99.5%; Gained gallium oxide powder enters cyclonic separator I successively with air-flow and cyclonic separator II carries out classification, particle diameter is obtained at the gallium oxide powder being greater than 6.5 μm in the collector of cyclonic separator I, the gallium oxide powder that particle diameter is less than 0.8 μm is obtained in the collector that cyclonic separator II top is connected, and in the collector that the gallium oxide powder collection of other particle diameter is connected bottom cyclonic separator II; Gallium oxide powder in each collector is packed by automatic packing machine, completes the continuous seepage that gallium prepares micron order gallium oxide powder.
2. technique as claimed in claim 1, it is characterized in that, gallium, after electric arc furnace is heated to 240 ~ 260 DEG C, flows out from metal fluid apertures.
3. technique as claimed in claim 1, it is characterized in that, the temperature of preheated air is 240 ~ 260 DEG C.
4. technique as claimed in claim 1, is characterized in that, airflow hole 25 ~ 35 ° along metal fluid apertures axle center angle directions are arranged.
5. technique as claimed in claim 1, is characterized in that, preheated air sprays with the pressure of 6 ~ 8MPa from 4 airflow holes simultaneously.
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Cited By (3)
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| CN110655104A (en) * | 2019-11-19 | 2020-01-07 | 武汉拓材科技有限公司 | Novel preparation process of high-purity gallium oxide |
| CN110854013A (en) * | 2019-11-11 | 2020-02-28 | 中国科学院金属研究所 | Large-area continuous ultrathin two-dimensional Ga2O3Preparation method and application of amorphous film |
| CN114408954A (en) * | 2022-01-26 | 2022-04-29 | 株洲科能新材料股份有限公司 | Preparation method of single crystal alumina micro powder |
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| CN114408954A (en) * | 2022-01-26 | 2022-04-29 | 株洲科能新材料股份有限公司 | Preparation method of single crystal alumina micro powder |
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Address after: 412000 Jinshan private science and Technology Park, Hetang District, Zhuzhou City, Hunan Province Patentee after: Zhuzhou Keneng New Material Co.,Ltd. Address before: 412000 Jinshan private science and Technology Park, Hetang District, Zhuzhou City, Hunan Province Patentee before: ZHUZHOU KENENG NEW MATERIAL Co.,Ltd. |