CN100500339C - Device and method for producing low melting point metals and oxide nitride powder - Google Patents
Device and method for producing low melting point metals and oxide nitride powder Download PDFInfo
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- CN100500339C CN100500339C CNB2005101130643A CN200510113064A CN100500339C CN 100500339 C CN100500339 C CN 100500339C CN B2005101130643 A CNB2005101130643 A CN B2005101130643A CN 200510113064 A CN200510113064 A CN 200510113064A CN 100500339 C CN100500339 C CN 100500339C
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 47
- 239000002184 metal Substances 0.000 title claims abstract description 47
- 239000000843 powder Substances 0.000 title claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- 150000004767 nitrides Chemical class 0.000 title claims abstract description 15
- 230000008018 melting Effects 0.000 title claims abstract description 14
- 238000002844 melting Methods 0.000 title claims abstract description 14
- 150000002739 metals Chemical class 0.000 title claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 27
- 230000008016 vaporization Effects 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 19
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 4
- 239000000956 alloy Substances 0.000 claims abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 29
- 239000010439 graphite Substances 0.000 claims description 29
- 229910002804 graphite Inorganic materials 0.000 claims description 29
- 238000009834 vaporization Methods 0.000 claims description 23
- 229910001369 Brass Inorganic materials 0.000 claims description 19
- 239000010951 brass Substances 0.000 claims description 19
- 238000010891 electric arc Methods 0.000 claims description 19
- 239000001301 oxygen Substances 0.000 claims description 17
- 229910052760 oxygen Inorganic materials 0.000 claims description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 16
- 150000001875 compounds Chemical class 0.000 claims description 16
- 239000007789 gas Substances 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 15
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 14
- 229910052802 copper Inorganic materials 0.000 claims description 12
- 239000010949 copper Substances 0.000 claims description 12
- 238000002309 gasification Methods 0.000 claims description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 229910000831 Steel Inorganic materials 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 239000010959 steel Substances 0.000 claims description 8
- 230000001681 protective effect Effects 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 3
- 239000010425 asbestos Substances 0.000 claims description 3
- 230000004888 barrier function Effects 0.000 claims description 3
- 239000001110 calcium chloride Substances 0.000 claims description 3
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 claims description 3
- 239000000428 dust Substances 0.000 claims description 3
- 230000008676 import Effects 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- 229910044991 metal oxide Inorganic materials 0.000 claims description 3
- 150000004706 metal oxides Chemical class 0.000 claims description 3
- 239000002808 molecular sieve Substances 0.000 claims description 3
- 229910052895 riebeckite Inorganic materials 0.000 claims description 3
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 3
- 238000010521 absorption reaction Methods 0.000 claims description 2
- 230000008859 change Effects 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims description 2
- 239000011856 silicon-based particle Substances 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 9
- 230000008901 benefit Effects 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000004663 powder metallurgy Methods 0.000 abstract description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 15
- 239000011701 zinc Substances 0.000 description 10
- 229910052725 zinc Inorganic materials 0.000 description 10
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 239000004411 aluminium Substances 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- 239000002131 composite material Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 239000004482 other powder Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 150000002926 oxygen Chemical class 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000009700 powder processing Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
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Abstract
The present invention is apparatus and method for producing medium and low melting point metals and their oxide or nitride powder, and belongs to the field of interdisciplinary powder metallurgy and machine building technology. The present invention produces metal or alloy powder of melting point in 185-899 deg C in a triphase AC arc vaporizing apparatus, and the triphase AC arc vaporizing process after opening the conic valve is one process including the steps of forming reciprocating liquid flow bridge of molten metal among three electrodes, neck reducing, arcing, breaking liquid flow bridge to vaporize metal and re-forming liquid flow bridge. The present invention has the advantages of high production speed, high product quality, fine powder granularity, low power consumption, etc.
Description
Technical field:
The present invention relates to the apparatus and method of melting point metals and oxygen or nitride powder in a kind of produce, belong to the technical field of powder metallurgy and machine-building cross discipline.
Background technology:
The powder-making technique of middle melting point metals or alloy, methods such as electrolytic powder processing, powder reducing process and powder by spraying are arranged at present, and the above two can not produce the composite powder of metal and carbonitride composition, though the latter can produce composite powder, but usually remaining oxygen is lower for the powder that spraying is made, and granularity is thin inadequately, need add mechanical lapping, it is low not only to consume energy, and powder is flakey after grinding, and is unfavorable for the spraying blanking of powder, and above-mentioned three kinds of milling methods all can not be made the powder of nanometer grade simultaneously.The production fine oxide, the nitride attritive powder, common solvent evaporation-cohesion at present and gas chemistry reaction method, these methods not only production efficiency are low, and cost is low, and production scale is little, yields poorly, and powder quality is difficult to control.
Summary of the invention:
The objective of the invention is to overcome the deficiency of prior art, and the apparatus and method of melting point metals and oxygen or nitride powder in a kind of produce are provided.
Principle of the present invention is: molten metal is put into the conical graphite container (6) of apparatus of the present invention, metal bath penetrates from the hollow graphite electrode that connects the alternating current center line, impact on another combination graphite electrode that is connecting low tension live wire (perhaps direct current positive pole), form conduction liquid stream bridge and the electric current of two interpolars is connected, produce corresponding magnetic field around the electric current, liquid stream bridge is compressed in this magnetic field unevenly, make liquid stream bridge form local necking down, bottleneck resistance increases, temperature raises and causes producing electric arc, liquid stream bridge moment is blown up, and the ultralow temperature of electric arc makes the evaporation of vaporizing fast of liquid stream bridge metal.Yet because metal bath is to flow out continuously, the liquid stream bridge of therefore blowing up in short-term is switched on again subsequently, forms second not good liquor stream bridge and secondary necking down, the starting the arc, blow up the vaporization with metal, and process is carried out circularly.
Of the present invention theing contents are as follows:
1. the three-phase alternating current electric arc vapourizing unit of melting point metals and oxygen or nitride powder in producing
Three-phase alternating current electric arc vapourizing unit of the present invention, suitable fusing point is vaporized at 400-899 ℃ middle melting point metals or alloy.
Three-phase alternating current electric arc vapourizing unit is by setscrew nut (1); Supporting angle steel (2); Connect center line conduction red copper board (3); Asbestos board insulating barrier (4); Place stainless steel horn-break switch (5) conical graphite container (6) centerline and threaded shank; Be positioned on the arc vaporization stove center line and metal bath that the bottom has is emitted total runner (19) and three and is the conical graphite container (6) that 120 ° of uniform metal baths are emitted horizontal run (20); Be positioned at metal vapors outlet (7) on the alumina firebrick body of heater (12), insulation ceramic tile layer (8), red copper conducting copper (9), graphite brass compound electrode (10), brass square nut (11), protective gas import (13), gas valve (14), stop valve (17), evaporated metal liquid discharge port (18) not; The not evaporated metal that is positioned at arc vaporization stove middle and lower part is collected pot (15); The steel furnace shell (16) that fixedly is alumina firebrick body of heater (12) outer surface is formed; Three be brass section (22), the square brass nut (11) that cooperates with the brass section (22) of compound electrode of the compound electrode that 120 ° of uniform graphite brass compound electrodes (10) are threaded by the graphite section (21) of compound electrode, with the graphite section (21) of compound electrode, the conducting copper (9) that is welded on the square brass nut (11) constitutes.
2., the method for melting point metals and oxygen or nitride powder in the production
This method is molten metal to be put into the conical graphite container (6) of the said device of claim 1, and the liquid stream bridge → necking down → starting the arc → liquid stream bridge that just forms reciprocation cycle is blown up and the vaporization of metal → form the again vaporization pulverizing process of liquid stream bridge; Wherein:
When producing metal dust, need in gasification burner, to feed argon gas and make protection gas; Form metal for non-nitride, also can protect toward feeding nitrogen in the gasification burner; For the cheap nitrogen or the argon gas of purity less than 99.99%, need to remove moisture content through silicon particle bottle and granular calcium chloride bottle, and with the residual oxygen in the 5A type molecular sieve absorption protective gas;
When producing metal oxide powder, need in gasification burner, to feed industrial oxygen, make the metallic vapour of arc vaporization at high temperature be oxidized to oxide; Produce nitride powder, when in stove, feeding nitrogen, can make the close nitrogen element steam of vaporization under the high temperature change into nitride;
The spacing of each the phase electrode pair in the control three-phase electric arc gasification burner is that the starting the arc voltage across poles between 10-14mm, each phase electrode pair is 110 ± 5 volts, and the automatic fluctuation range of voltage is the 100-130 volt; When forming liquid stream bridge and electric arc, the automatic fluctuation range of each phase current is the 350-370 peace.
The present invention has following advantage:
(1) product speed is fast, the production capacity height of unit equipment;
(2) product quality is excellent, and the remaining oxygen of metal dust is lower than other powder production methods, and product purity is lower than input
The purity of raw material, illustrating still has the effect of removing impurity in the arc vaporization process;
(3) powder size is thin, and about 40% reach nanoscale, more than 70% less than 10 μ m;
(4) equipment investment is little, and floor space is few, and energy consumption of unit product is low.
Description of drawings:
Fig. 1 always schemes for three-phase alternating current electric arc gasification burner device.
Each sequence number among the figure is: (1) setscrew nut; (2) supporting angle steel (18-8 steel); (3) connect alternating current center line conduction red copper board; (4) asbestos board insulating barrier; (5) stainless steel horn-break switch; (6) conical graphite container; (7) metal vapors outlet; (8) insulation ceramic tile layer; (9) red copper conducting copper; (10) graphite brass compound electrode; (11) brass square nut; (12) alumina firebrick layer (thick 70mm); (13) protective gas import; (14) gas valve; (15); Evaporated metal is not collected pot (18-8 steel); (16) A
3The steel furnace shell; (17) stop valve; (18) evaporated metal liquid discharge port not.
Fig. 2 is a three-phase alternating current electric arc gasification burner device II-II cutaway view.
Fig. 3 is a three-phase alternating current electric arc gasification burner device partial enlarged drawing.
Fig. 4 is the bottom amplification assumption diagram of conical graphite container (6).
Each sequence number among the figure is: (6) conical graphite container, (19) metal bath are emitted total runner, (20) metal bath is emitted the horizontal thin runner.
Fig. 5 is graphite brass compound electrode (10) structure chart and 120 ° of equal Bututs.
Each sequence number among the figure is: the graphite section of (21) compound electrode, the brass section of (22) compound electrode, (11) square brass nut, (9) conducting copper.
The zinc powder that Fig. 6 produces for the vaporization of three-phase alternating current electric arc amplifies 1000 times displaing micro picture.
The specific embodiment:
Implement 1: super-fine zinc dust is produced in the vaporization of three-phase alternating current electric arc
The operating process of producing super-fine zinc dust with device shown in Figure 1 is as follows: No. 4 zinc (about 60 kilograms) of packing in the stainless steel crucible, the heating crucible makes the zinc fusing in well formula resistance furnace, the zinc melt temperature is superheated to about 510 ℃, hold the zinc crucible with the crane lifting then, the zinc melt is changed in the conical graphite container of three-phase electric arc vapourizing unit (6), and adjust the zinc liquid temperature that conical graphite holds in the zinc device and be not less than 460 ℃ (being lower than the U-shaped electric heating tube that this temperature can be reinstated 5KW).Start three-phase transformer, make the voltage of three-phase firewire center line reach 120 volts, and then activated cone control valve, the just ejection from three horizontal thin runners (20) of zinc liquid, impact on three the 120 ° combinatory graphite electrodes uniform and with voltage (10), form three 120 ° uniform horizontal liquid stream bridges, three-phase alternating current is connected, and produce 360~430 the peace monophase currents, after this, because the effect in magnetic field forms liquid stream bridge and produces necking down, the starting the arc, moment is blown up the quick vaporization of liquid stream bridge and metallic zinc, and then forming liquid stream bridge and electric arc, process is carried out circularly.The internal diameter in the horizontal graphite thread road (20) that the metal bath of this device is emitted is φ 1.4mm.
Technological parameter in the production process is: the spacing between each electrode pair is 12mm, in the production process, single-phase voltage across poles during the starting the arc is 115 ± 5 volts, and each single-phase phase voltage fluctuation range (process self fluctuation) is: 100-130 volts, monophase current fluctuation range are the 360-440 peace.The zinc powder of being produced reaches nanoscale more than 40%, 70% below 10 μ m, and powder contains oxygen<0.03%.Feed the nitrogen protection of 99.9% purity in the production process, through silica gel and calcium chloride dehydration, deoxydization by molecular sieve.
Implement 2: ultra-fine Al is produced in the vaporization of three-phase alternating current electric arc
2O
3Powder
Produce Al with device shown in Figure 1
2O
3Powder, make raw material with No. 4 aluminium, its equipment is all identical with embodiment 1 with operating procedure, and different only have 3 points: the aluminium liquid that (1) is transferred to from resistance melting furnace in the conical graphite container (6) should remain on more than 700 ℃, is lower than 700 ℃ and should starts the U-shaped electric heater and be warmed up to this more than temperature; (2) protective gas that feeds in the gasification burner no longer is nitrogen or argon, but purity is 99.5% industrial oxygen.This oxygen will make the aluminium steam oxidation that forms in the arc vaporization process become Al
2O
3Powder particle; When (3) producing metal oxide, the seal approach of receiving powder system does not need strictness, and the suitable air that bleeds also helps and makes unoxidized aluminum vapor further be oxidized to Al
2O
3The diameter that three graphite metal baths are emitted horizontal run (20) in the production process is φ 1.0mm, the spacing 10mm between each phase electrode pair.The starting voltage of every phase and voltage between phases and current fluctuation scope are with embodiment 1 in the production process.
Table 1 arc vaporization is produced zinc and is divided and Al
2O
3The technical-economic index of powder
Sequence number | Product | Production method | Average power consumption (degree/kilogram) | 0.2m 3The productivity ratio of gasification burner (kilogram/hour) | Powder-product purity | Remaining oxygen | Granularity |
1 | Zinc powder | The three-phase alternating current vaporization | 33.5 | 76.4 | >99.9 | <0.05 % | 40%<0.01μm, 70%<10μm |
3 | Al 2O 3Powder | The three-phase alternating current vaporization | 38.9 | 87.7 | >99.9 | — | The same |
Claims (2)
1, the device of melting point metals and oxygen or nitride powder in a kind of produce is characterized in that to fusing point being that three-phase alternating current electric arc vapourizing unit is adopted in 400-899 ℃ middle melting point metals or alloy vaporization; Wherein:
1.1 three-phase alternating current electric arc vapourizing unit is by setscrew nut (1); Supporting angle steel (2); Connect center line conduction red copper board (3); Asbestos board insulating barrier (4); Place stainless steel horn-break switch (5) conical graphite container (6) centerline and threaded shank; Be positioned on the arc vaporization stove center line and the bottom has metal bath and emits total runner (19) and three and be the conical graphite container (6) that 120 ° of uniform metal baths are emitted horizontal run (20); Be positioned at metal vapors outlet (7) on the alumina firebrick body of heater (12), insulation ceramic tile layer (8), red copper conducting copper (9), graphite brass compound electrode (10), brass square nut (11), protective gas import (13), gas valve (14), stop valve (17), evaporated metal liquid discharge port (18) not; The not evaporated metal that is positioned at arc vaporization stove middle and lower part is collected pot (15); The steel furnace shell (16) that is fixed on alumina firebrick body of heater (12) outer surface is formed; Three be brass section (22), the square brass nut (11) that cooperates with the brass section (22) of compound electrode of the compound electrode that 120 ° of uniform graphite brass compound electrodes (10) are threaded by the graphite section (21) of compound electrode, with the graphite section (21) of compound electrode, the conducting copper (9) that is welded on the square brass nut (11) constitutes.
2., the method for melting point metals and oxygen or nitride powder in a kind of the production, it is characterized in that molten metal puts into the conical graphite container (6) of the said device of claim 1, the liquid stream bridge → necking down → starting the arc → liquid stream bridge that just forms reciprocation cycle is blown up and the vaporization of metal → form the again vaporization pulverizing process of liquid stream bridge; Wherein:
2.1 when producing metal dust, need in gasification burner, to feed argon gas and make protection gas; For the cheap argon gas of purity less than 99.99%, need to remove moisture content through silicon particle bottle and granular calcium chloride bottle, and with the residual oxygen in the 5A type molecular sieve absorption protective gas;
2.2 when producing metal oxide powder, need in gasification burner, to feed industrial oxygen, make the metallic vapour of arc vaporization at high temperature be oxidized to oxide; Produce the metal nitride powder, when in stove, feeding nitrogen, make the close nitrogen element steam of vaporization under the high temperature change into nitride;
2.3 the spacing of each the phase electrode pair in the control three-phase electric arc gasification burner is that the starting the arc voltage across poles between 10-14mm, each phase electrode pair is 110 ± 5 volts, the automatic fluctuation range of voltage is the 100-130 volt; When forming liquid stream bridge and electric arc, the automatic fluctuation range of each phase current is the 350-370 peace.
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CNA03135937XA CN1526497A (en) | 2003-09-25 | 2003-09-25 | Apparatus and method for producing high and medium melting point metal and its oxide or nitride powder |
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CNA03135937XA Division CN1526497A (en) | 2003-09-25 | 2003-09-25 | Apparatus and method for producing high and medium melting point metal and its oxide or nitride powder |
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CN1781629A CN1781629A (en) | 2006-06-07 |
CN100500339C true CN100500339C (en) | 2009-06-17 |
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CNA03135937XA Pending CN1526497A (en) | 2003-09-25 | 2003-09-25 | Apparatus and method for producing high and medium melting point metal and its oxide or nitride powder |
CNB2005101130643A Expired - Fee Related CN100500339C (en) | 2003-09-25 | 2003-09-25 | Device and method for producing low melting point metals and oxide nitride powder |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8671855B2 (en) | 2009-07-06 | 2014-03-18 | Peat International, Inc. | Apparatus for treating waste |
Families Citing this family (5)
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CN108325782B (en) * | 2017-10-25 | 2023-07-04 | 湖北三行科技股份有限公司 | Powder adjusting structure and enamel powder collecting box with same |
CN108580916A (en) * | 2018-08-01 | 2018-09-28 | 重庆国际复合材料股份有限公司 | A kind of electric spark corrode prepares the reaction unit of metal powder |
CN112299385B (en) * | 2020-10-10 | 2021-05-07 | 浙江宇耀新材料有限公司 | Nano aluminum nitride powder synthesis production line |
CN113414398A (en) * | 2021-06-21 | 2021-09-21 | 江苏天楹等离子体科技有限公司 | Equipment and method for preparing metal powder by using plasma |
CN113976900B (en) * | 2021-11-01 | 2022-10-28 | 电子科技大学 | Equipment for preparing ultrafine powder by batch electric spark and ultrafine powder production system |
-
2003
- 2003-09-25 CN CNA03135937XA patent/CN1526497A/en active Pending
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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US8671855B2 (en) | 2009-07-06 | 2014-03-18 | Peat International, Inc. | Apparatus for treating waste |
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CN1526497A (en) | 2004-09-08 |
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