CN1059369C - Method for preparing quickly solidifing hydrogen-stored alloy powder material - Google Patents
Method for preparing quickly solidifing hydrogen-stored alloy powder material Download PDFInfo
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- 239000000956 alloy Substances 0.000 title claims abstract description 148
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 139
- 239000000843 powder Substances 0.000 title claims abstract description 89
- 239000000463 material Substances 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title abstract description 35
- 238000003860 storage Methods 0.000 claims abstract description 85
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 52
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 27
- 238000002844 melting Methods 0.000 claims abstract description 24
- 230000008018 melting Effects 0.000 claims abstract description 24
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- 238000009833 condensation Methods 0.000 claims abstract description 11
- 230000005494 condensation Effects 0.000 claims abstract description 11
- 238000005516 engineering process Methods 0.000 claims abstract description 11
- 230000006698 induction Effects 0.000 claims description 19
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- 238000004519 manufacturing process Methods 0.000 abstract description 20
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 17
- 239000001257 hydrogen Substances 0.000 abstract description 17
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 15
- 229910052751 metal Inorganic materials 0.000 abstract description 8
- 239000002184 metal Substances 0.000 abstract description 8
- 238000003723 Smelting Methods 0.000 abstract description 5
- 238000010438 heat treatment Methods 0.000 abstract description 4
- 238000005204 segregation Methods 0.000 abstract description 4
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- 230000002349 favourable effect Effects 0.000 abstract description 2
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- 229910052802 copper Inorganic materials 0.000 description 9
- 239000010949 copper Substances 0.000 description 9
- 238000012387 aerosolization Methods 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 229910001338 liquidmetal Inorganic materials 0.000 description 7
- YZCKVEUIGOORGS-IGMARMGPSA-N Protium Chemical compound [1H] YZCKVEUIGOORGS-IGMARMGPSA-N 0.000 description 6
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- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000004781 supercooling Methods 0.000 description 1
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- 229910052725 zinc Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
The present invention relates to a preparation method for a hydrogen storage alloy powder material. Concretely, an atomizing milling technology using vacuum (Ar) for smelting high pressure and high purity nitrogen and a milling technology using a high speed rotary disc for centrifugal atomization and rapid condensation are used by the present invention for the mass production of uniform globular alloy powder without segregation of 200-350 meshes and a micro-fine and ultra-fine high-purity alloy powder material, the grain size of which reaches 0.05 to 5.0 mu m. Protective atmosphere, such as Ar, N2, etc., are filled in a furnace, which not only can accelerate a smelting process and reduce the oxidation of furnace atmosphere to molten metal, but also can guarantee the heating of a smelting pool to be uniform. Thus, the protective atmosphere is favorable for preparing the hydrogen storage alloy powder of a microcrystalline structure with low inclusion and segregation degree, and continuous feeding, continuous melting and continuous milling can be realized.
Description
What the present invention relates to is a kind of manufacture method of rapid-solidified hydrogen-storage alloy material, and concretely, that the present invention relates to is AB
5The industrial production manufacturing technology of type MmNiCoMnAl series hydrogen storage alloy dusty material.
As everyone knows, hydrogen is a kind of high-energy-density and the clean desirable energy, and the industrialization of storage alloy material for hydrogen is to be concerned about one of major project that scientific and technical boundary, branch of industry and the government decision department of using energy source and clean energy resource are concerned about very much.The industrialization of storage alloy material for hydrogen relates to the each side such as improved and complete of storage alloy material for hydrogen Application and Development and industrial production manufacturing technology and equipment.
In the prior art, the manufacturing technology of storage alloy material for hydrogen open source literature is as follows:
AB
5The type hydrogen-storage alloy---nearly all disclosed about AB
5The patent of type storage alloy material for hydrogen and the AB that enters the practical stage
5The chemical analysis of type storage alloy material for hydrogen all is roughly the same basically, promptly at the Dutch LaNi that invents of nineteen sixty-eight
5Hydrogen-storage alloy is retrofited on the basis, inhales protium and replaces high pure metal La with more cheap mishmetal Mm, or add the hydrogen absorption capacity of a small amount of Ti, Zr, Ca, Mg suction protium raising hydrogen-storage alloy again; With Co, Mn, Al replacing section Ni or add again oligo-element Ml--2 kind (M represents V, Cr, Fe, W, Mo, Nb, B, Si, Sn, Zn, N or the like) improve hydrogen-storage alloy corrosion resistance, discharge and recharge combination property such as life-span and guarantee that hydrogen-storage alloy is used for the characteristic of big capacity, long-life, highly reliable, Ni-MH battery and the low cost of raw material to enhance competitiveness.
AB
5The type hydrogen-storage alloy has now developed into similar MmNiCoMnAl alloy series.AB
5The suction protium of type hydrogen-storage alloy and the proportioning of non-suction protium were generally 1: 5 by atomic molar ratio.Different patents and manufacturer also suitably align by the situation of oneself.The content of inhaling protium is improved some or reduce.The total amount of non-suction protium generally is controlled at 4.8-5.2.The component of each element is generally: Ni1.5-3.5, Co1.5-3.5, Mn0.1-1, Al0.05-0.5, add the content 0.05-0.2 of metal M on a small quantity.
Norium Mm has rich lanthanum, rich cerium two major types, and its main rare-earth elements La, Ce, Nd, Pr content differ different because of the place of production.For guaranteeing the hydrogen absorption capacity of hydrogen-storage alloy, generally control La+Ce＞70%.
The patent of the hydrogen-storage alloy manufacture method of having published, the overwhelming majority stress hydrogen-storage alloy be used to make nickel-hydrogen battery negative pole for the corresponding levelling alloy composition of combination property that improves negative pole, improve institutional framework of alloy material or the like, and to the industrial production of hydrogen-storage alloy manufacture method, on patent, seldom relate to.The AB that on partial monopoly, mentions
5The manufacture method of type hydrogen-storage alloy can be summarized as follows:
(1) vacuum arc melting ingot casting Mechanical Crushing powder process method
Adopt suitable norium and the raw metal of purity higher granularity,, mix, put into water jacketed copper crucible, vacuumize, logical Ar melting by the weighing of alloying component proportioning.In order to obtain the ingot casting of uniform ingredients unanimity, often need repeatedly melting, use Mechanical Crushing powder process again.The flat 3-289644 peace of Japan Patent 4-52242, flat 4-168240 promptly prepares the hydrogen-storage alloy sample with the method.
(2) vacuum induction melting, the water cooled copper mould ingot casting, Mechanical Crushing powder process method,
Adopt vacuum induction furnace (Ar protection) melting,, produce ingot casting, Mechanical Crushing powder process again with column crystal through liquid metal fast cold cast in tabular water cooled copper mould of melting.Under vacuum or Ar protection, 900-1200 ℃ of high temperature homogeneous handled.On hydrogen-storage alloy microcrystalline powder surface and crystal boundary, form fine and close complex oxide film.The flat 3-188234 of Japan Patent now has been useful for the commodity production of MmNiCoMnAl series hydrogen storage alloy dusty material.And the bigger manufacturer of production scale is because big capacity electric induction furnace is difficult to control the tabular ingot quality of steady production less than 10 μ m microstructures, so also in the manufacture method of seeking other.
(3) liquid metal single roller rapid quenching system band, Mechanical Crushing powder process method, Japan Patent flat-301531 proposes AB
5Type AB
2Type and AB type hydrogen-storage alloy are made 5-15MM earlier; the fritter foundry alloy is placed on after the coarse crushing in the quartz ampoule, is liquid metal with the remelting of 2KV high-frequency induction heating; with the Ar protection down; rotation (2000RPM) water-cooled copper roller at a high speed (on the ∮ 300 * 40mn), fast quenching system band, Mechanical Crushing powder process again; the fast quenching sample is compared with method in the past; can improve thermal conductivity, control the micronizing of hydrogen-storage alloy, improve the cycle lie that discharges and recharges of alloy powder.
(4) aerosolization legal system is got the hydrogen-storage alloy powder material, and Japan Patent discloses flat 3-22408, proposes AB
5Type hydrogen-storage alloy liquid metal adopts the atomizing of flow at high speed inert gas to produce the nonequilibrium condition hydrogen-storage alloy powder, can improve the self discharge of capacity and inhibition Ni-MH battery, prolongs to charge and discharge cycle lie.
The open 5-222474 of Japan Patent proposes AB
5The liquid metal four special electrode methods of type hydrogen-storage alloy LmNiCoMnAl+Zr, cooled and solidified speed) 500 ℃/second, it is few, fine to obtain the composition segregation with 600-900 ℃ of homogeneous heat treatment in 2-5 hour of Ar protection again, homogeneous structure.Improve the corrosion resistance of alloy material, prolong and discharge and recharge cycle lie, can be used to produce big capacity (the initial capacity 300mah/g long-life charges and discharge cycle lie) 300 times) nickel-hydrogen battery negative pole, and can save alloy cast ingot Mechanical Crushing engineering, shorten the hydrogen-storage alloy powder material technological process of production.
(5) rare earth oxide is produced hydrogen-storage alloy powder material high temperature reduction diffusion method, and Japan Patent discloses flat 3-170601, adopts high purity rare earth oxides La
2O
3(purity 99.99%) and granularity 5.0-8.8 μ m high pure metal Ni (99.7%), (purity 99% mixes, in reaction vessel to add the high-purity Ca of reducing agent, with 970 ℃, 1.5-4 hour, reduction diffusion reaction, through cooling, washing filtering is removed reaction product CaO, the LaNi that makes
5Hydrogen-storage alloy powder, its composition are La 31.4%, Ca 0.43-0.61%, O
20.06-0.12%, (0.01-0.02%, alloy initial capacity 295-297mah/g).
Japan Patent discloses flat 3-281710 and adopts mixed rare-earth oxide (La
2O
350.63/27.61, CeO
22.81/50.1 Pr
6O 11/4.32, Sm
2O
30.2/0.01Ni powder, CoMmCuAl metal oxide powder, the chemical theory equivalent proportioning of pressing the hydrogen-storage alloy composition is added one of a small amount of Ca, Mg, Li again, mix, produce the MmNiCoMnAl alloy with the high temperature reduction diffusion method, reaction temperature 1000-1200 ℃, reaction time 4-6 hour.Rare earth oxide is reduced, alloying, powder process is combined in the procedure and implements.Can save alloy cast ingot Mechanical Crushing engineering, improve heat conductivity, electric conductivity, prevent alloy powder micronizing and the danger that reduces the broken powder process of hydrogenation, but complex process, and can not produce continuously, can not satisfy hydrogen-storage alloy industrialization large-scale production needs.
The object of the invention is to overcome the deficiency that exists in the above-mentioned preparation hydrogen-storage alloy powder material method, a kind of high efficiency, the method for large-scale continuous production hydrogen-storage alloy powder material in high quality are provided, simple, the easy row of this method is applicable to the industrialization large-scale production of hydrogen-storage alloy powder material.
The preparation method of hydrogen-storage alloy powder material provided by the invention:
One, vacuum (Ar) melting---high pressure nitrogen atomizing preparation hydrogen-storage alloy powder material:
1. raw material is handled
(1) Main Ingredients and Appearance of the norium of the different lot numbers of the different places of production of market supply, different vendor even same manufacturer, constituent contents such as La, Ce, Nd, Pr differ.In order to guarantee that producing the MmNiCoMnAl series hydrogen storage alloy in a large number has stabilized quality, must stablize the raw material quality.The norium strictness of coming into operation is closed batch by specification requirement or again with the Main Ingredients and Appearance proportioning of vacuum induction furnace remelting levelling alloy, and be processed into certain particle size usefulness Vacuum Package with anti-oxidation.
(2) effective addition of volatile alloy additive when controlling the vacuum melting hydrogen-storage alloy can prepare intermediate alloy in advance, NiMg alloy for example, NiB alloy, BaAl alloy or the like.
(3) preparation of MmNiCoMl foundry alloy.
2. vacuum (Ar) melting---high pressure nitrogen atomizing preparation hydrogen-storage alloy powder material:
Will be through giving the furnace charge of processing, promptly close again batch or with the Main Ingredients and Appearance proportioning of vacuum induction furnace remelting levelling and alloy and be processed into certain particle size by specification requirement, with the norium of Vacuum Package and the intermediate alloy of corresponding proportioning, or hydrogen-storage alloy foundry alloy, with vacuum (Ar) induction melting, the liquid alloy of fusion with high pure nitrogen with 1000-5000 ℃ of/second cooling velocity atomize fast cooling, solidify, can produce spherical crystallite hydrogen-storage alloy powder.Described vacuum melting is that the liquid alloy of fusion atomizes with 40-60 atmospheric pressure 99.999% high pure nitrogen with the logical Ar melting hydrogen-storage alloy furnace charge of vacuum induction furnace, and cooled and solidified becomes the spherical crystallite AB of 150-350 order fast
5The type hydrogen-storage alloy powder.
Above-mentioned vacuum (Ar) melting--high pressure nitrogen atomizing prepare the method for hydrogen-storage alloy powder material can be in vacuum as shown in Figure 1 (Ar) melting that the applicant develops--is finished in the high pressure nitrogen powder by atomization device, realize continuous charging, quicken the continuous flow procedure of powder process.This device is a vacuum (Ar) sealing and inert gas N
2The alloy fuel pulverizing plant of gas shiled is made up of vacuum chamber 1, electric induction furnace 2, tundish and feed trumpet 3, high pressure nitrogen atomizer 4, aerosolization chamber 5, cooling cone 6, ebullated bed 7, superfine powder gatherer 8, conveyance conduit 9, middle batch can 10, vibratory sieve 11 and storage powder bucket 12 etc.
Hydrogen-storage alloy furnace charge through giving processing is filled melting in the Ar induction furnace 2 in vacuum; The liquid metal of fusion injects tundish and feed trumpet 3 after the control temperature, enter high pressure nitrogen atomizer 4 with temperature and the flow velocity of stipulating.The atmospheric high pressure nitrogen of 40-60 enters the circumferential weld nozzle by control valve, and the broken atomizing of metal liquid stream is become 150-350 purpose alloy liquid droplet, makes hydrogen-storage alloy powder through supercooling.The cooling velocity of liquid alloy is generally 1000-5000 ℃/sec, can produce alloy composition height uniformity, the spherical alloy powder of segregation-free fine crystal.Alloy powder is through the cooling of aerosolization chamber 5 and cooling cone 6, and in ebullated bed 7, further cool off by nitrogen, by nitrogen alloy powder is sent into middle batch can 10 by conveyance conduit 9, again through continuous shaking sieve 11, divide and to sift out the varigrained alloy powder product material storage barrel of packing into, the vacuum packing promptly makes hydrogen-storage alloy powder.
A small amount of＜10 μ m fine alloy the powder that produce in the aerosolization process are by superfine powder gatherer 8 centralized collection that are connected with 5 tops, aerosolization chamber.The nitrogen that nitrogen ebullated bed and conveyance conduit are used all is that the used nitrogen of high-pressure aerial fog chemical combination bronze fully utilizes.
Adopt the present invention, can realize efficient, economical, stably produce the high-quality hydrogen-storage alloy powder material in a large number.
Two, the centrifugal atomizing rapid condensation prepares hydrogen-storage alloy microcrystalline powder technology.
1. raw material gives and handles that to give processing identical with the raw material described in " ".
2. centrifugal atomizing rapid condensation preparation:
Will be through giving the furnace charge of processing, promptly close again and criticize or aligned the main proportioning of alloy and be processed into certain particle size with the vacuum induction furnace remelting by specification requirement, with the norium of Vacuum Package and the intermediate alloy or the melting of hydrogen-storage alloy foundry alloy of corresponding proportioning, the liquid alloy of fusion is produced the sheet-like crystallite hydrogen-storage alloy powder with high speed rotating plate centrifugal atomizing rapid condensation, after promptly furnace charge through giving processing or hydrogen-storage alloy foundry alloy are liquid alloy with vacuum (Ar) electric arc melting, inject on the centrifugal pan that rotates at a high speed with 2000-5000RPM centrifugal continuously, be atomized into droplet, be to cool off on the collection rotating disk of 2000-5000RPM at rotating speed, make 0.5-3mm sheet hydrogen-storage alloy powder, its crystal grain has the micro crystal structure between 0.05-5.0 μ m.
This method can be finished in the high speed rotating plate decentralization rapid condensation fuel pulverizing plant as shown in Figure 2 of the applicant's development continuously.This device comprises vacuum chamber 21, feeder 22, water-cooled copper crucible 23, scanning electron rifle 24, vavuum pump 25, centrifugal turntable 26, catch tray 27, scraping blade 28, gatherer 29 parts such as grade.Two automatic feeders 22 that structure is identical, two feeders alternately open and close by valve during running, and continuous charging injects the copper crucible 23 of water-cooled that is arranged in vacuum chamber 21 with furnace charge or hydrogen-storage alloy foundry alloy, can change the inclination angle of crucible 23 by automatic tilting device, and regulate its position.The final vacuum of vavuum pump 25 is 5 * 10 negative 4 power Torr.The powder by atomization system is made of a high speed centrifugation atomizing disk 26 and another powder collection rotating disk vertical with the high speed centrifugation atomizing disk.The rotating speed of the two is 2000-5000rpm; The liquid alloy of fusion is injected on the high speed centrifugation atomizing disk 26 with certain flow in the crucible 23, be atomized into droplet, fly on the powder collection rotating disk 27 vertical by centrifugal force with atomizing disk 26, be set in rotation and collect alloy powder on the rotating disk and scrape by scraping blade 28 and enter gatherer 29, scanning electron rifle 24 is decided program scan round on crucible by giving.
The powder that adopts high speed rotating plate centrifugal atomizing technology to make, generally in the form of sheets, the thickness of flake powder is between 10-100 μ m, and radial dimension is 0.5-3mm, and this powder has the micro crystal structure, and its crystallite dimension is between 0.05-5.0 μ m.Adopt high speed rotating plate centrifugal atomizing fuel pulverizing plant, can realize continuous charging, continuous smelting, powder process continuously, not only can reduce production costs but also can improve to produce and render a service.Adopt the copper crucible of water-cooled can eliminate the contamination of alloy melt, reduce nonmetal inclusion.The scanning electron rifle is decided program cycle scanning by giving; charge into protective atmospheres such as Ar, N2 in the stove, both can quicken fusion process, reduce the oxidation of furnace atmosphere motlten metal; can protect the molten bath homogeneous heating again, favourable making is mingled with the microstructure hydrogen-storage alloy powder very low with the segregation degree.
Embodiment describes the present invention in detail below in conjunction with accompanying drawing:
Accompanying drawing 1 is vacuum (Ar) melting---high pressure nitrogen powder by atomization apparatus structure schematic diagram;
Accompanying drawing 2 is the structural representation of centrifugal atomizing rapid condensation high speed rotating plate centrifugal atomizing rapid condensation fuel pulverizing plant;
Wherein, 1--vacuum chamber, 2--electric induction furnace, 3--tundish and feed trumpet, 4--high pressure nitrogen atomizer, 5--aerosolization chamber, 6--cooling cone, 7--ebullated bed, 8--superfine powder gatherer, batch can in the middle of the 9--conveyance conduit, 10--, 11--vibratory sieve, the 12--material storage barrel, 21--vacuum chamber, 22--feeder, 23--water-cooled copper crucible, 24--scanning electron rifle, 25--vavuum pump, 26--centrifugal turntable, the 27--catch tray, 28 scraping blades, 29--gatherer.
Embodiment 1:
High pressure nitrogen prepares the technology of hydrogen-storage alloy powder material to use vacuum (Ar) melting--high pressure nitrogen powder by atomization device and vacuum provided by the invention (Ar) melting--shown in the accompanying drawing 1, produces AB
5Hydrogen-storage alloy powder.
1. raw material gives processing
(1) Main Ingredients and Appearance of the norium of the different lot numbers of the different places of production of market supply, different vendor even same manufacturer, constituent contents such as La, Ce, Nd, Pr differ, and it is as shown in the table.In order to guarantee that producing the MmNiCoMnAl series hydrogen storage alloy in a large number has stabilized quality, must stablize the raw material quality.The norium strictness of coming into operation is closed batch by specification requirement or again with the Main Ingredients and Appearance proportioning of vacuum induction furnace remelting levelling alloy, and be processed into certain particle size, the usefulness Vacuum Package is with anti-oxidation.
(2) effective addition of volatile alloy additive when controlling the vacuum melting hydrogen-storage alloy can prepare intermediate alloy in advance, NiMg alloy for example, NiB alloy, BaAl alloy or the like.
(3) for preventing that harmful element, impurity from entering smelting furnace and staiing hydrogen-storage alloy, the raw material chemical analysis that all put into production use, surface quality, lumpiness size etc. must have into factory's chemical analysis list, or the quality certificate of manufacturer, strict specification requirement according to alloy cast ingot feeds intake, with the control stabilised quality.
(4) preparation of MmNiCoMl foundry alloy.
The norium composition of the different places of production, manufacturer-supplied is listed as representing: table one
| The place of production | No | La | Ce | Nd | Pr | Sm and other element |
| Shanghai | (1) | 54.8 | 1.9 | 33.70 | 9.7 | |
| (2) | 75.1 | 5.28 | 0.57 | 19.71 | ||
| (3) | 75 | 5.0 | ＜0.1 | 20.0 | ||
| Zhejiang | (4) | 41-51 | 3-53 | 35-41 | 9-11 | Sm0.5 Y＜0.5 |
| A | (5) | 26 | 47 | 18 | 9 | |
| (6) | 57 | 16 | 18 | 9 | ||
| (7) | 85 | 2 | 13 | |||
| (8) | 99 | |||||
| B | (9) | 30.4 | 49.9 | 14.9 | 4.7 | |
| (10) | 25-35 | 40-50 | 5-15 | 2-10 | ||
| C | (11) | 28.1 | 49.97 | 15.37 | 4.71 | 0.12 |
| D | (12) | 41-51 | 3-5 | 35-41 | 20 |
2. vacuum (Ar) melting--high pressure nitrogen atomizing preparation AB
5Hydrogen-storage alloy powder material: furnace charge melting in vacuum (filling Ar) induction furnace 2 that will be through giving processing, the liquid metal of fusion is after the control temperature, inject tundish and feed trumpet 3, temperature and flow velocity with regulation enter high pressure nitrogen atomizer 4, the atmospheric high pressure nitrogen of 40-60 enters the circumferential weld nozzle by control valve, the broken atomizing of metal liquid stream becomes 150-350 order alloy powder, alloy powder is through the cooling of aerosolization chamber 5 and cooling cone 6, enter ebullated bed 7, in ebullated bed 7, further cool off by nitrogen, by nitrogen alloy powder is sent into middle batch can 10 by conveyance conduit 9, pass through vibratory sieve continuous shaking again, sieve out pack into material storage barrel 12 and use vacuum seal of varigrained alloy powder product.In the aerosolization process＜and 10 μ m fine alloy powder, by superfine powder gatherer collection management.
Embodiment 2:
The technology of using high speed rotating plate centrifugal atomizing rapid condensation fuel pulverizing plant shown in the accompanying drawing 2 and centrifugal atomizing rapid condensation provided by the invention to prepare hydrogen-storage alloy powder material prepares AB
5, AB, AB
2The type hydrogen-storage alloy powder material.
1. raw material gives processing and gives processing with the raw material of embodiment 1.
2. the centrifugal atomizing rapid condensation prepares the alloy powder.
High speed rotating plate centrifugal atomizing powder process stove, two automatic feeders 22 that structure is identical are arranged, two feeders alternately open and close by valve during running, continuously will furnace charge add in the cold-crucible 23 in the vacuum chamber 21 through giving processing, carry out melting, the liquid alloy of fusion melts from copper crucible 23 changes, be injected on the high-speed and continuous centrifugal atomizing dish 26 with certain flow, be atomized into droplet, fly to powder collection rotating disk 27 by centrifugal force, scrape by scraping blade 28 again and enter storage vat 29, high speed centrifugation atomizing disk 26 and collection rotating disk 28 rotating speeds are 2000-5000rpm, the alloy powder that makes in the form of sheets, the thickness of flake powder is between 10-100 μ m, radial dimension is between the 0.5-5.0 μ m.
Claims (6)
1. the preparation method of a quickly solidifing hydrogen-stored alloy powder material, it is characterized in that adopting vacuum (Ar) melting--high pressure nitrogen atomizing preparation hydrogen-storage alloy powder technology: will be through giving furnace charge vacuum (Ar) induction melting of processing, the liquid alloy of fusion atomizes fast, cools off, solidifies with 1000-5000 ℃ of/second cooling velocity with high pure nitrogen, can make spherical crystallite hydrogen-storage alloy powder material.
2. press the preparation method of the described hydrogen-storage alloy powder material of claim 1, it is characterized in that described vacuum (Ar) induction melting, can in vacuum (Ar) electric induction furnace, carry out, the nitrogen pressure of described high pure nitrogen atomizing is the 40-60 atmospheric pressure, purity is 99.999%, and the powder size of atomizing is at the 150-350 order.
3. press the preparation method of the described hydrogen-storage alloy powder material of claim 1, it is characterized in that described furnace charge through giving processing is meant by specification requirement the Main Ingredients and Appearance of various noriums again in batches or with the Main Ingredients and Appearance proportioning of the positive alloy of vacuum induction furnace remelting adjustment, and be processed into the norium of certain particle size and the intermediate alloy of corresponding proportioning, or hydrogen-storage alloy foundry alloy.
4. the preparation method of a hydrogen-storage alloy powder material, it is characterized in that the centrifugal atomizing rapid condensation prepares hydrogen-storage alloy microcrystalline powder technology: will be through giving the furnace charge melting of processing, the droplet that the liquid alloy of melting becomes with the high speed rotating plate centrifugal atomizing, cool off preparation sheet-like crystallite hydrogen-storage alloy powder material collecting on the rotating disk.
5. press the preparation method of the described hydrogen-storage alloy powder material of claim 4, it is characterized in that the furnace charge melting is vacuum in the water-cooled crucible (Ar) electric arc melting, described furnace charge through giving processing is meant by specification requirement the Main Ingredients and Appearance of various noriums again in batches or with the Main Ingredients and Appearance proportioning of the positive alloy of vacuum induction furnace remelting adjustment, and be processed into the norium of certain particle size and the intermediate alloy of corresponding proportioning, or hydrogen-storage alloy foundry alloy.
6. by the preparation method of the described hydrogen-storage alloy powder material of claim 4, it is characterized in that the rotating speed of high speed rotating plate atomizing is 2000-5000RPM, the collection rotary speed is 2000-5000RPM, and hydrogen-storage alloy powder crystal grain is between 0.05-5.0 μ m.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95109468A CN1059369C (en) | 1995-09-07 | 1995-09-07 | Method for preparing quickly solidifing hydrogen-stored alloy powder material |
| AU69228/96A AU6922896A (en) | 1995-09-07 | 1996-09-09 | A method and an equipment for producing rapid condensation hydrogen storage alloy powder |
| PCT/CN1996/000077 WO1997009144A1 (en) | 1995-09-07 | 1996-09-09 | A method and an equipment for producing rapid condensation hydrogen storage alloy powder |
| US09/029,878 US6174345B1 (en) | 1995-09-07 | 1996-09-09 | Method and an equipment for producing rapid condensation hydrogen storage alloy powder |
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| Application Number | Priority Date | Filing Date | Title |
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| CN95109468A CN1059369C (en) | 1995-09-07 | 1995-09-07 | Method for preparing quickly solidifing hydrogen-stored alloy powder material |
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| Publication Number | Publication Date |
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| CN1130114A CN1130114A (en) | 1996-09-04 |
| CN1059369C true CN1059369C (en) | 2000-12-13 |
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| CN95109468A Expired - Fee Related CN1059369C (en) | 1995-09-07 | 1995-09-07 | Method for preparing quickly solidifing hydrogen-stored alloy powder material |
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| CN101797647B (en) * | 2010-03-10 | 2011-06-08 | 株洲弗拉德科技有限公司 | Vertical multi-channel ultrahigh-temperature induction-heating continuous spheroidizing furnace |
| CN103182513B (en) * | 2013-04-01 | 2015-06-03 | 江苏鹰球集团有限公司 | Device for preparing metal powder by inert gas shielded plasmas |
| CN106216697A (en) * | 2016-09-29 | 2016-12-14 | 柳州增程材料科技有限公司 | The preparation method of 3D printing alloy powder |
| CN107322001A (en) * | 2017-06-19 | 2017-11-07 | 湖南工业大学 | A kind of 3D printing metal dust and its preparation facilities and method |
| CN107971500B (en) * | 2017-12-01 | 2020-09-25 | 北京汽车集团越野车有限公司 | Manufacturing method of magnesium alloy part and magnesium alloy part |
| CN113414397B (en) * | 2021-05-25 | 2023-01-17 | 鞍钢股份有限公司 | A continuous preparation method of iron-based metal powder by vacuum atomization |
| CN114192790B (en) * | 2021-11-29 | 2024-01-23 | 成都先进金属材料产业技术研究院股份有限公司 | Spherical titanium and titanium alloy powder preparation device and method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1051002A (en) * | 1990-12-05 | 1991-05-01 | 中南工业大学 | Make the method and apparatus of refining metallic powder |
| CN1029631C (en) * | 1993-03-08 | 1995-08-30 | 太原工业大学 | Method for preparing magnesium-base alloy hydrogen-storage material |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1051002A (en) * | 1990-12-05 | 1991-05-01 | 中南工业大学 | Make the method and apparatus of refining metallic powder |
| CN1029631C (en) * | 1993-03-08 | 1995-08-30 | 太原工业大学 | Method for preparing magnesium-base alloy hydrogen-storage material |
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