CN1775428A - Method and apparatus for preparing rapid-solidified hydrogen-storage alloy powder material - Google Patents
Method and apparatus for preparing rapid-solidified hydrogen-storage alloy powder material Download PDFInfo
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- CN1775428A CN1775428A CNA2005101147199A CN200510114719A CN1775428A CN 1775428 A CN1775428 A CN 1775428A CN A2005101147199 A CNA2005101147199 A CN A2005101147199A CN 200510114719 A CN200510114719 A CN 200510114719A CN 1775428 A CN1775428 A CN 1775428A
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- 239000000843 powder Substances 0.000 title claims abstract description 178
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 112
- 239000000956 alloy Substances 0.000 title claims abstract description 112
- 238000003860 storage Methods 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 44
- 239000000463 material Substances 0.000 title claims description 34
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 157
- 229910052786 argon Inorganic materials 0.000 claims abstract description 82
- 238000002360 preparation method Methods 0.000 claims abstract description 43
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000001257 hydrogen Substances 0.000 claims abstract description 40
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 40
- 239000002994 raw material Substances 0.000 claims abstract description 25
- 230000006698 induction Effects 0.000 claims abstract description 23
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 50
- 238000001816 cooling Methods 0.000 claims description 41
- 239000011261 inert gas Substances 0.000 claims description 37
- 238000002844 melting Methods 0.000 claims description 34
- 230000008018 melting Effects 0.000 claims description 34
- 238000000889 atomisation Methods 0.000 claims description 28
- 238000000703 high-speed centrifugation Methods 0.000 claims description 26
- 229910052757 nitrogen Inorganic materials 0.000 claims description 25
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 20
- 229910052802 copper Inorganic materials 0.000 claims description 20
- 239000010949 copper Substances 0.000 claims description 20
- 230000004927 fusion Effects 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 238000007712 rapid solidification Methods 0.000 claims description 17
- 238000007711 solidification Methods 0.000 claims description 17
- 230000008023 solidification Effects 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 15
- 238000010298 pulverizing process Methods 0.000 claims description 11
- 238000009833 condensation Methods 0.000 claims description 9
- 230000005494 condensation Effects 0.000 claims description 9
- 238000007599 discharging Methods 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 8
- 235000019580 granularity Nutrition 0.000 claims description 8
- 150000001485 argon Chemical class 0.000 claims description 6
- 238000009690 centrifugal atomisation Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- 230000003534 oscillatory effect Effects 0.000 claims description 5
- 239000007921 spray Substances 0.000 claims description 5
- 238000012216 screening Methods 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 239000004482 other powder Substances 0.000 claims description 3
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 3
- 150000002910 rare earth metals Chemical class 0.000 claims description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 3
- 229910052721 tungsten Inorganic materials 0.000 claims description 3
- 239000010937 tungsten Substances 0.000 claims description 3
- 239000002699 waste material Substances 0.000 claims description 3
- 238000003801 milling Methods 0.000 claims description 2
- 238000003723 Smelting Methods 0.000 abstract description 2
- 235000013312 flour Nutrition 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 230000007812 deficiency Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 238000009825 accumulation Methods 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
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- 206010037211 Psychomotor hyperactivity Diseases 0.000 description 1
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- 238000007667 floating Methods 0.000 description 1
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- 230000005764 inhibitory process Effects 0.000 description 1
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- 229910001338 liquidmetal Inorganic materials 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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Abstract
The present invention provides a preparation method of quickly-coagulable hydrogen storage alloy powder and its equipment. Said preparation method includes four procedures of raw material preparation, smelting, making powder and hydrogenation treatment. Said invention also provides the concrete steps of the above-mentioned every procedure. Said equipment includes induction furnace or argon plasma arc furnace, atomized powder-making device and hydrogenation device, etc.
Description
Technical field:
The present invention relates to a kind of preparation method and device thereof of quickly solidifing hydrogen-stored alloy powder material, specifically, that the present invention relates to is AB
5System and AB
2The preparation method of series hydrogen storage alloy powder and device thereof.
Background technology:
Chinese patent 952212560; No. 133870, U.S. Pat P6174345.B1 and Taiwan patent; a kind of preparation method of hydrogen-storage alloy powder material is disclosed; adopt vacuum (Ar) melting-high pressure; the high pure nitrogen atomizing; high speed rotating plate centrifugal atomizing rapid condensation powder-making technique; can produce 200～350 orders in a large number; the spherical alloy powder and the crystallite dimension of the even segregation-free of composition reach the fine of 0.05～5.0um order of magnitude; ultra-fine high purity alloys powder material; in stove, use argon gas melting and two kinds of gases of nitrogen atomization; but when using nitrogen atomization, can form one deck nitride film on the metal particle top layer, hydrogen-absorbing ability is reduced; must be again through alkali treatment and hydrogenation treatment; remove surfaces nitrided film, the powder recovery rate is reduced, and increase production cost; above-mentioned invention disclosed is semi-continuous process production simultaneously; after every stove production finished, it was reinforced to need to destroy vacuum unlatching furnace shell, not only consumes a large amount of protective gas; and operating rate is low; the energy consumption height, and make the oxygen content and the energy consumption height of product.
Summary of the invention:
The objective of the invention is to overcome the deficiencies in the prior art, a kind of preparation method and device thereof of improved quickly solidifing hydrogen-stored alloy powder material is provided, realize full serialization production.
For achieving the above object, the present invention adopts the basic design of technical scheme to be: a kind of preparation method of quickly solidifing hydrogen-stored alloy powder material is characterized in that this method may further comprise the steps:
(a) raw-material preliminary treatment; to adjust as the composition of raw-material intermediate alloy or foundry alloy; utilize fully continuous type vacuum argon induction melting high-pressure inert gas powder by atomization device; by its continuous charging jar, control valve, feeding screw, raw material are sent into continuously preheating in the batch can in the middle of the heat-conducting of its vacuum one argon protection.
(b) raw material of the preheating vibration charging plate by batch can bottom in the middle of the heat-conducting is directly added melting in the vacuum one argon induction furnace, or by with heat-conducting in the middle of the self-conveyor feed that is connected of batch can send into melting in crucible in the argon plasma stove vacuum chamber of high speed centrifugation quick solidification apparatus or the water jacketed copper crucible, make intermediate alloy or foundry alloy form the alloy of fusion.
(c) with the alloy powder process of fusion, the alloy of the crucible of vacuum argon induction furnace or argon plasma stove or the fusion of water jacketed copper crucible institute utilizes high pressure and the two kinds of inert gas atomizers of low pressure that make up atomizer, centrifugal atomization and the rapid condensation formation crystallite hydrogen-storage alloy powder that cools off or utilize the high speed centrifugation quick solidification apparatus respectively, the former is spherical for its shape, and the latter is flat sheet.
(d) the crystallite hydrogen-storage alloy powder that rapid condensation is formed carries out hydrogenation treatment in spiral hydrogen treating device.
Described vacuum one argon induction furnace vacuum chamber and the maximum pressure of argon plasma stove vacuum chamber after vacuumizing are 5 * 10
-4Holder.
The method of described utilization combination atomizer powder process comprises, the alloy of described vacuum one argon induction furnace fusion injects tundish, adjust temperature, regulate the viscosity and the flow velocity of molten alloy, introduce the combination atomizer through control valve and feed trumpet, open the argon pressure control valve again, make the high-pressure inert gas argon enter the ring-type atomizer of combination atomizer, the winding-up atomized molten alloy and form powder, the pressure of this inert gas argon is that 40-60 crust purity is 99.999%, in the time of with atomizing, opens the nitrogen pressure control valve, make low-pressure inert gas nitrogen enter the ring-type cooling jet of combination atomizer, the powder that nozzle atomization forms makes powder cooling and rapid solidification, and the pressure of this inert gas nitrogen is the 1-5 crust, purity is 99.999%, and cooling velocity is 1000-5000 ℃/second.
The formed hydrogen-storage alloy powder of described utilization combination atomizer also cools off in spray chamber and cooling cone, through the magnetic suspension device powder is suspended, on ebullated bed, further cool off then with nitrogen, its superfine alloy powder less than 10 μ is collected by the superfines gatherer, all the other powder fully are cooled to below 35 ℃ through conveyance conduit, middle batch can, vibration coldplate again, through discharge gate, vibratory sieve enters storage powder bucket again.
Described raw-material preliminary treatment also is included in and adds rare earth metal and hydrogen-storage alloy waste material step in the raw material.
Described raw-material preheat temperature is 650 ℃.
The described centrifugal atomization milling method that utilizes the high speed centrifugation quick solidification apparatus, be after sending into the raw material melting of passing through preliminary treatment and preheating in crucible or the water jacketed copper crucible, the alloy of fusion is injected the high speed rotating disc of high speed centrifugation quick solidification apparatus by the pouring opening of automatic tilting device and crucible or water jacketed copper crucible, by centrifugal force or high speed rotating plate centrifugal atomizing method, the alloy atomization of fusion is become droplet and is fallen out to fly on the cooling reflecting plate, by the cooling reflecting plate droplet that the high speed rotating disc falls out is cooled off and rapid solidification, form hydrogen-storage alloy powder and fall into powder catcher, send in the storage powder bucket from discharging opening again.
The granularity of the spherical hydrogen-storage alloy powder of described utilization combination atomizer preparation is the 120-350 order.
The described thickness of the flat sheet hydrogen-storage alloy powder of high speed centrifugation quick solidification apparatus preparation that utilizes is 10-100 μ m, and radial dimension is 0.5-3.0mm.
The rotating speed of the high speed rotating disc of described high speed centrifugation quick solidification apparatus is 2000-6000r/min.
The described hydrogen-storage alloy powder that rapid condensation is formed carries out hydrogenation treatment and may further comprise the steps in spiral hydrogen treating device: being 99.999% hydrogen with purity adds the hydrogen heat process chamber of hydrogenation apparatus by hydrogen charging port, to produce atmosphere of hydrogen; Utilize feed appliance that hydrogen-storage alloy powder is sent into the hydrogen heat process chamber; Utilization is positioned at the spiral vibrating grinder of bottom variable frequency and amplitude, and powder is pulverized; The powder of pulverizing is sent into spiral conveying groove from bottom to top along helix and the powder on the helicla flute is heated to assigned temperature through the internal heat type heater, thereby heating powder is also carried out hydrogenation treatment, the powder of heating enters oscillatory type cooling chamber, middle accumulator by discharge gate, again with the powder inputted vibration sieve screening powder that stores, powder is separated into different granularities herein, the granularity different according to powder put into one or more storage powder buckets with the powder that separates.
Be 5-20 minute powder heat time heating time of described pulverizing, and maximum heating temperature is 850 ℃.
It is that vibration is pulverized under screw that described powder is pulverized, and pulverizing is carried out under 1-10bar pressure.
A kind of combination atomizer of implementing the described quickly solidifing hydrogen-stored alloy powder material preparation method of claim 1, it is characterized in that: described combination atomizer be located at feed trumpet in the described fully continuous type vacuum one argon melting high-pressure inert gas powder by atomization device below, the argon pressure control valve that comprises porous type ring-type atomizer and control connection argon gas thereof is socketed in the circular seam type ring-type cooling jet of porous type ring-type atomizer outside and the nitrogen pressure control valve that nitrogen is connected in control thereof.
A kind of high speed centrifugation quick solidification apparatus of implementing the described quickly solidifing hydrogen-stored alloy powder material preparation method of claim 1, it is characterized in that: described high speed centrifugation quick solidification apparatus is located at a side of described fully continuous type vacuum one argon melting high-pressure inert gas powder by atomization device, comprise argon plasma stove vacuum chamber, this argon plasma stove vacuum chamber is connected by batch can in the middle of the heat-conducting of self-conveyor feed and fully continuous type vacuum one argon melting high-pressure inert gas powder by atomization device, be provided with the crucible or water jacketed copper crucible and the automatic tilting device thereof that adapt with self-conveyor feed in this argon plasma stove vacuum chamber, the top of crucible or water jacketed copper crucible is provided with tungsten electrode, the below of the pouring opening of crucible or water jacketed copper crucible is provided with the high speed rotating disc, one inboard of argon plasma stove vacuum chamber is provided with the relative cooling reflecting plate of droplet direction that falls out with the high speed rotating disc, be provided with powder catcher and the discharging opening that is connected with argon plasma stove vacuum chamber below the cooling reflecting plate, the storage powder bucket of this discharging opening and fully continuous type vacuum one argon melting high-pressure inert gas powder by atomization device is connected.
After adopting such scheme, the present invention with compare with technology is arranged, have following beneficial effect:
The present invention has utilized fully continuous type vacuum one argon melting high-pressure inert gas powder by atomization device and spiral hydrogen treating device, a kind of preparation method of quickly solidifing hydrogen-stored alloy powder is provided, collection is reinforced, preheating, melting, powder process and hydrogenation treatment are one, realized that full inhibition and generation operation continuously replaces semicontinuous, isolated fully in process of production contact atmosphere, continuous charging, powder process continuously, it is even to be suitable for composition, the large-scale industrialized production of the hydrogen-storage alloy powder that the segregation degree is low.In making service cycle, do not open by stove the body of heater vacuum chamber all the time, induction furnace, crucible and residual metal be ingress of air not, oxygen content and nitrogenize are mingled with to be reduced more than 40%, productivity ratio doubles, overcome in the semicontinuous operation, after every stove melting finishes, needed to open reinforced the vacuumizing again of body of heater vacuum chamber and cause oxidation and the low disadvantage of operating rate.
The present invention because adopted the high pressure of the combination atomizer of forming by atomizer and cooling jet and two kinds of inert gas nozzle of low pressure respectively with the alloy atomization and the cooling of vacuum argon induction furnace fusion, replaced and integrated the single injector that atomizing is cooled off, the atomizer of this combination atomizer atomizes with 40-60 crust argon, cooling jet cools off with 1-5 crust nitrogen, liquid metal does not contact nitrogen when making atomizing, solved molten molten metal nitrogenize problem, make hydrogen-storage alloy oxygen absorbed and activation capacity improve 30%, the powder oxygen content is reduced to below 0.01% from 005%.
The present invention is owing to make furnace charge pre-alloyed to composition of raw material adjustment, and implemented the preheating furnace charge in the batch can in the middle of heat-conducting, but and the non-oxidation attitude reinforced, thereby reduced smelting time.Increase cool time owing to adopted the magnetic suspension device that powder is fully stirred in the magnetcisuspension floating region, reduced the refrigerating gas consumption.
The present invention with the alloy atomization of argon plasma stove fusion, replaces the scanning electron rifle owing to also adopted high speed rotating plate centrifugal atomizing method, has improved the productivity ratio and the efficiency of heating surface, and reduces the element volatilization.
The present invention carries out hydrogenation treatment with the crystallite hydrogen-storage alloy powder that rapid condensation forms, and also is significant owing to adopted improved spiral hydrogen treating device, its effect, mainly is:
The spiral vibrating grinder of variable frequency and amplitude can be adjusted feeding speed, has overcome the deficiency of former fixing a kind of speed;
Increase the oscillatory type cooling chamber, accelerate to be made crystal grain be easy to fragmentation by the quick cooling of heat treatment material than former cooling naturally;
Heater has overcome former open-type ribbon heater with heat pipe in the totally enclosed type, the deficiency of easy short circuit behind the accumulation dust;
Under certain amplitude and frequency, reverse from bottom to top conveying can fully be heated and hydrogenation powder through helicla flute for back runing type feeding, powder, and having overcome former powder from top to bottom has accumulation phenomenon;
The swing crushing device makes the intercrystalline cracking and unlikely efflorescence, and recovery rate reaches 95% than former Mechanical Method hammer crushing powder recovery rate 60% raising 35%.
Below in conjunction with accompanying drawing the specific embodiment of the present invention is described in further detail.
Description of drawings
Fig. 1 is fully continuous type vacuum one an argon induction melting high-pressure inert gas atomising device schematic diagram of the present invention;
Fig. 2 is the high speed centrifugation rapid solidification flour device schematic diagram that is communicated with batch can 2 in the middle of Fig. 1 heat-conducting;
Fig. 3 is the spiral hydrogen treating device schematic diagram of the present invention;
Fig. 4 is the structural representation of combination atomizer 22 among Fig. 1.
The specific embodiment
The invention provides a kind of preparation method and device thereof of quickly solidifing hydrogen-stored alloy powder material.This method may further comprise the steps:
(a) raw-material preliminary treatment will be adjusted as the composition of raw-material intermediate alloy or alloy, and add rare earth metal and hydrogen-storage alloy waste material step in raw-material.Utilize fully continuous type vacuum argon induction furnace high-pressure inert gas powder by atomization device as shown in Figure 1; by its continuous charging jar 5, control valve 4, feeding screw 3; raw material are sent into continuously in the middle of the heat-conducting of its vacuum one argon protection and carried out preheating in the batch can 2, described raw-material preheat temperature is 650 ℃.
(b) raw material of the preheating vibration charging plate 1 by batch can 2 bottoms in the middle of the heat-conducting is directly added melting in the vacuum one argon induction furnace 8, or by with heat-conducting in the middle of the self-conveyor feed 017 that is connected of batch can 2 send into melting in crucible in the argon plasma stove vacuum chamber 04 of high speed centrifugation rapid solidification flour device as shown in Figure 2 or the water jacketed copper crucible 010, make intermediate alloy or foundry alloy form the alloy of fusion.
(C) with the alloy powder process of fusion, the crucible of vacuum one argon induction furnace 8 or argon plasma stove or the alloy of 010 fusion of water jacketed copper crucible utilize high pressure and the two kinds of inert gas atomizers of low pressure that make up atomizer 22, centrifugal atomization and the rapid solidification formation crystallite hydrogen-storage alloy powder that cools off or utilize high speed centrifugation rapid solidification flour device respectively, the former is spherical for its shape, and the latter is flat sheet.
(D) the crystallite hydrogen-storage alloy powder that rapid condensation is formed carries out hydrogenation treatment in spiral hydrogen treating device as shown in Figure 3.
Among a kind of preparation method of quickly solidifing hydrogen-stored alloy powder material, described vacuum one argon induction furnace vacuum chamber 6 and the maximum pressure of argon plasma stove vacuum 04 after vacuumizing are 5*10
-4Holder.
Among a kind of preparation method of quickly solidifing hydrogen-stored alloy powder material, the method of described utilization combination atomizer powder process comprises, the alloy of described vacuum one argon induction furnace 8 fusions injects tundish 25, adjust temperature and insulation, adjust the viscosity and the flow velocity of molten alloy, make up atomizer 22 as shown in Figure 4 through control valve 24 and feed trumpet 23 introducings, open argon pressure control valve 4 ' again, make the high-pressure inert gas argon enter the ring-type atomizer 2 ' of combination atomizer along G arrow direction, the winding-up atomized molten alloy 3 ' and form fine and fine peritectic alloy powder, the pressure of this inert gas argon is the 40-60 crust, purity is 99.999%, in the time of with atomizing, opens nitrogen pressure control valve 5 ', make low-pressure inert gas nitrogen enter the ring-type cooling jet 1 ' of combination atomizer along D arrow direction, the powder that the winding-up atomizing forms makes powder cooling and rapid solidification, and the pressure of this inert gas nitrogen is the 1-5 crust, purity is 99.999%, and cooling velocity is 1000-5000 ℃/second.The also cooling in spray chamber 18 and cooling cone 16 of above-mentioned utilization combination atomizer 22 formed hydrogen-storage alloy powders, make powder suspension through magnetic suspension device 17, on ebullated bed 15, further cool off then with nitrogen, its superfine alloy powder 20 less than 10 μ is collected by superfines gatherer 19, all the other powder are again through conveyance conduit 14, middle batch can 9, vibration coldplate 10 fully is cooled to below 35 ℃, enters storage powder bucket 13 through discharge gate 11, vibratory sieve 12.The described granularity of the spherical hydrogen-storage alloy powder of this combination atomizer preparation of utilizing is the 120-350 order.
Among a kind of preparation method of quickly solidifing hydrogen-stored alloy powder material, the described method of utilizing the centrifugal atomization powder process of high speed centrifugation rapid solidification flour device, be to send into the raw material that pass through preliminary treatment and preheating in crucible or the water jacketed copper crucible 010, after plasma-arc 02 by tungsten electrode 01 carries out vacuum or the melting of vacuum argon gas, consult Fig. 2, the alloy 011 of fusion is injected the high speed rotating disc 09 of high speed centrifugation quick solidification apparatus with certain flow velocity by the pouring opening 03 of automatic tilting device 012 and crucible or water jacketed copper crucible, its rotating speed is 2000-6000r/min, is preferably 4000r/min.By centrifugal force or high speed rotating plate centrifugal atomizing method, the alloy 011 of fusion is atomized into droplet and fallen out fly on cooling reflecting plate 05, by cooling reflecting plate 05 droplet that high speed rotating disc 09 falls out is cooled off and rapid solidification, form hydrogen-storage alloy powder 06 and fall into powder catcher 07, send in the storage powder bucket 13 from discharging opening 08 again.The described thickness of the flat sheet hydrogen-storage alloy powder of high speed centrifugation rapid solidification flour device preparation that utilizes is 10-100 μ m, and optimum value is 50 μ m, and radial dimension is 0.5-3.0mm, and optimum value is 0.75-1.0mm.This powder has the micro crystal structure, and its crystal grain is between 0.05-5 μ.
Among a kind of preparation method of quickly solidifing hydrogen-stored alloy powder material, the described hydrogen-storage alloy powder that rapid solidification is formed carries out hydrogenation treatment and may further comprise the steps in spiral hydrogenation treatment apparatus: as shown in Figure 3, with purity is that 99.999% nitrogen adds hydrogen heat process chambers 100 by inflation inlet 110, to produce atmosphere of hydrogen; Utilize feed appliance 900 that hydrogen-storage alloy powder is sent into hydrogen heat process chamber 100, utilization is positioned at the spiral vibrating grinder 400 of bottom variable frequency and amplitude, dusty material is pulverized, it is that vibration is pulverized under screw that described powder is pulverized, pulverizing is carried out under 1-10bar pressure, the powder of pulverizing is sent into spiral conveying groove 300 from bottom to top along helix, the powder on the helicla flute is heated to the temperature of appointment through internal heat type heater 200, thereby heating powder, be 5-20 minute powder heat time heating time of described pulverizing, and maximum heating temperature is 850 ℃; The powder of heating enters oscillatory type cooling chamber 500, middle accumulator 600 by discharge gate 101; With the powder inputted vibration sieve 700 screening powder of storage, powder is separated into different granularities herein, and the powder that separates is put into one or more storage powder buckets 800 again.
At last, Vacuum Package hydrogen-storage alloy powder.
The spiral hydrogen treating device that the present invention is used, can be used for continuous homogeneous processing and hydrogen heat handles, also can with the supporting use of other production equipment, promptly use with fully continuous type vacuum argon induction melting high-pressure inert gas powder by atomization matched with devices, so just, can form a whole set of continuous production equipment of preparation hydrogen-storage alloy powder, powder-making technique, hydrogen activation processing and screening operation.Thereby realize efficient, high-quality, economic, the stable large-scale industrialized production of hydrogen-storage alloy powder.
The present invention has utilized improved fully continuous type vacuum argon induction melting high-pressure inert gas powder by atomization device and spiral hydrogen treating device when implementing described quickly solidifing hydrogen-stored alloy powder material preparation method.
As shown in Figure 1, the structure of the fully continuous type vacuum argon induction melting high-pressure inert gas powder by atomization device that the present invention utilized is as follows, and this device comprises continuous charging jar 5 and the control valve 4 that is connected successively with its underpart, feeding screw 3, batch can 2 in the middle of the heat-conducting, vibration charging plate 1, vacuum furnace shell 6 and vacuum chamber 7 thereof, vacuum valve 21, vacuum one argon induction furnace 8 in the vacuum chamber 7, tundish 25, control valve 24, feed trumpet 23, combination atomizer 22, the bottom of vacuum furnace shell 6 is connected with spray chamber 18 and sidepiece is collected the superfines gatherer 19 of superfines 20, spray chamber 18 bottoms are provided with magnetic suspension device 17, cooling cone 16, ebullated bed 15, the bottom of cooling cone 16 is connected with conveyance conduit 14 in turn, middle batch can 9, vibration coldplate 10, discharge gate 11, vibratory sieve 12, storage powder bucket 13.
In Fig. 1 fuel pulverizing plant, one of device of realizing the used key of described quickly solidifing hydrogen-stored alloy powder material preparation method is a combination atomizer 22, consult Fig. 4, described combination atomizer 22 be located at feed trumpet 23 in the described fully continuous type vacuum one argon melting high-pressure inert gas powder by atomization device below, the argon pressure control valve 4 ' that comprises porous type ring-type atomizer 2 ' and control connection argon gas thereof is socketed in the circular seam type ring-type cooling jet 1 ' of porous type ring-type atomizer 2 ' outside and the nitrogen pressure control valve 5 ' that nitrogen 0 is connected in control thereof.
In Fig. 1 fuel pulverizing plant, the another kind of key device of realizing described quickly solidifing hydrogen-stored alloy powder material preparation method is a high speed centrifugation rapid solidification flour device, but do not draw among Fig. 1 as space is limited, in fact, described high speed centrifugation rapid solidification flour device is located at a side of described fully continuous type vacuum argon melting high-pressure inert gas powder by atomization device, consult Fig. 2, the structure of this device comprises: argon plasma vacuum chamber 04, this argon plasma vacuum chamber is connected by the middle batch can 2 of the self-conveyor feed 017 and the heat-conducting of fully continuous type vacuum one argon melting high-pressure inert gas powder by atomization device, be provided with heater 015 in the batch can 2 in the middle of the heat-conducting, the part of batch can more than 2 is same as shown in Figure 1 in the middle of the heat-conducting described in Fig. 2, as continuous charging jar 5.Be provided with the crucible or water jacketed copper crucible 010 and the automatic tilting device 012 thereof that adapt with self-conveyor feed 017 in this argon plasma stove vacuum chamber 04, the below of the pouring opening 03 of crucible or water jacketed copper crucible is provided with high speed rotating disc 09, one inboard of argon plasma stove vacuum chamber 04 is provided with the relative cooling reflecting plate 05 of droplet direction that falls out with high speed rotating disc 09, be provided with powder catcher 07 and the discharging opening 08 that is connected with argon plasma stove vacuum chamber 04 below the cooling reflecting plate, this discharging opening 08 is connected with the storage powder bucket 13 of fully continuous type vacuum one argon melting high-pressure inert gas powder by atomization device.
Powder by above-mentioned used combination atomizer and two kinds of method preparations of high speed centrifugation rapid solidification flour device powder process can carry out hydrogenation treatment in the spiral hydrogen treating device of the present invention.
As shown in Figure 3, the structure of the spiral hydrogen treating device of the present invention comprises: the feed appliance 900 of hydrogen heat process chamber 100 is sent into hydrogen-storage alloy powder at hydrogen heat process chamber 100 and top thereof, the sidewall of hydrogen heat process chamber 100 is provided with hydrogen charging port 110, so that with purity is that 99.999% hydrogen charges in the hydrogen heat process chamber 100, the intracavity bottom of hydrogen heat process chamber 100 is provided with the vibration grinder 400 of spiral variable frequency and amplitude, the upper inside wall of hydrogen heat process chamber 100 is provided with spiral conveying groove 300 and interior internal heat type heater 200 thereof, and the sidewall of hydrogen heat process chamber 100 is provided with discharge gate 101 and reaches and its oscillatory type cooling chamber 500 that links successively, middle accumulator 600, vibratory sieve 700, one or more storage powder buckets 800.
In a word; the present invention has utilized fully continuous type vacuum argon melting high-pressure inert gas powder by atomization device and spiral hydrogen treating device; adopted the twin-jet nozzle of forming by atomizer and cooling jet to make up two kinds of methods of atomizer and the powder process of high speed centrifugation rapid solidification flour device; realize reinforced; preheating; melting; the full serialization production of powder process; and can guarantee to be in all the time in the stove under the protection gaseity; make melting reach high purification; the molten bath homogeneous heating helps making and low is mingled with segregation degree and nitrogen content very lowly, and the microstructure with overactivity ability is store hydrogen and closed powder.
Claims (15)
1. the preparation method of a quickly solidifing hydrogen-stored alloy powder material is characterized in that this method may further comprise the steps:
(a) raw-material preliminary treatment; to adjust as the composition of raw-material intermediate alloy or foundry alloy; utilize fully continuous type vacuum argon induction melting high-pressure inert gas powder by atomization device; by its continuous charging jar, control valve, feeding screw, raw material are sent into continuously preheating in the batch can in the middle of the heat-conducting of its vacuum one argon protection.
(b) raw material of the preheating vibration charging plate by batch can bottom in the middle of the heat-conducting is directly added melting in the vacuum one argon induction furnace, or by with heat-conducting in the middle of the self-conveyor feed that is connected of batch can send into melting in crucible in the argon plasma stove vacuum chamber of high speed centrifugation quick solidification apparatus or the water jacketed copper crucible, make intermediate alloy or foundry alloy form the alloy of fusion.
(c) with the alloy powder process of fusion, the alloy of the crucible of vacuum argon induction furnace or argon plasma stove or the fusion of water jacketed copper crucible institute utilizes high pressure and the two kinds of inert gas atomizers of low pressure that make up atomizer, centrifugal atomization and the rapid condensation formation crystallite hydrogen-storage alloy powder that cools off or utilize the high speed centrifugation quick solidification apparatus respectively, the former is spherical for its shape, and the latter is flat sheet.
(d) the crystallite hydrogen-storage alloy powder that rapid condensation is formed carries out hydrogenation treatment in spiral hydrogen treating device.
2. the preparation method of a kind of quickly solidifing hydrogen-stored alloy powder material according to claim 1, it is characterized in that: described vacuum-argon induction furnace vacuum chamber and the maximum pressure of argon plasma stove vacuum chamber after vacuumizing are 5 * 10
-4Holder.
3. the preparation method of a kind of quickly solidifing hydrogen-stored alloy powder material according to claim 1, it is characterized in that: the method for described utilization combination atomizer powder process comprises, the alloy of described vacuum one argon induction furnace fusion injects tundish, adjust temperature, regulate the viscosity and the flow velocity of molten alloy, introduce the combination atomizer through control valve and feed trumpet, open the argon pressure control valve again, make the high-pressure inert gas argon enter the ring-type atomizer of combination atomizer, the winding-up atomized molten alloy and form powder, the pressure of this inert gas argon is that 40-60 crust purity is 99.999%, in the time of with atomizing, open the nitrogen pressure control valve, make low-pressure inert gas nitrogen enter the ring-type cooling jet that makes up atomizer, the powder that nozzle atomization forms, make powder cooling and rapid solidification, the pressure of this inert gas nitrogen is the 1-5 crust, and purity is 99.999%, and cooling velocity is 1000-5000 ℃/second.
4. the preparation method of a kind of quickly solidifing hydrogen-stored alloy powder material according to claim 1, it is characterized in that: the formed hydrogen-storage alloy powder of described utilization combination atomizer also cools off in spray chamber and cooling cone, through the magnetic suspension device powder is suspended, on ebullated bed, further cool off then with nitrogen, its superfine alloy powder less than 10 μ is collected by the superfines gatherer, all the other powder fully are cooled to below 35 ℃ through conveyance conduit, middle batch can, vibration coldplate again, through discharge gate, vibratory sieve enters storage powder bucket again.
5. the preparation method of a kind of quickly solidifing hydrogen-stored alloy powder material according to claim 1 is characterized in that: described raw-material preliminary treatment also is included in and adds rare earth metal and hydrogen-storage alloy waste material step in the raw material.
6. the preparation method of a kind of quickly solidifing hydrogen-stored alloy powder material according to claim 1, it is characterized in that: described raw-material preheat temperature is 650 ℃.
7. the preparation method of a kind of quickly solidifing hydrogen-stored alloy powder material according to claim 1, it is characterized in that: the described centrifugal atomization milling method that utilizes the high speed centrifugation quick solidification apparatus, be after sending into the raw material melting of passing through preliminary treatment and preheating in crucible or the water jacketed copper crucible, the alloy of fusion is injected the high speed rotating disc of high speed centrifugation quick solidification apparatus by the pouring opening of automatic tilting device and crucible or water jacketed copper crucible, by centrifugal force or high speed rotating plate centrifugal atomizing method, the alloy atomization of fusion is become droplet and is fallen out to fly on the cooling reflecting plate, by the cooling reflecting plate droplet that the high speed rotating disc falls out is cooled off and rapid solidification, form hydrogen-storage alloy powder and fall into powder catcher, send in the storage powder bucket from discharging opening again.
8. the preparation method of a kind of quickly solidifing hydrogen-stored alloy powder material according to claim 1 is characterized in that: the granularity of the spherical hydrogen-storage alloy powder of described utilization combination atomizer preparation is the 120-350 order.
9. the preparation method of a kind of quickly solidifing hydrogen-stored alloy powder material according to claim 1, it is characterized in that: the described thickness of the flat sheet hydrogen-storage alloy powder of high speed centrifugation quick solidification apparatus preparation that utilizes is 10-100 μ m, and radial dimension is 0.5-3.0mm.
10. according to the preparation method of claim 1 or 7 described a kind of quickly solidifing hydrogen-stored alloy powder materials, it is characterized in that: the rotating speed of the high speed rotating disc of described high speed centrifugation quick solidification apparatus is 2000-6000r/min.
11. the preparation method of a kind of quickly solidifing hydrogen-stored alloy powder material according to claim 1 is characterized in that: the described hydrogen-storage alloy powder that rapid condensation is formed carries out hydrogenation treatment and may further comprise the steps in spiral hydrogen treating device:
Being 99.999% hydrogen with purity adds the hydrogen heat process chamber of hydrogenation apparatus by hydrogen charging port, to produce atmosphere of hydrogen; Utilize feed appliance that hydrogen-storage alloy powder is sent into the hydrogen heat process chamber; Utilization is positioned at the spiral vibrating grinder of bottom variable frequency and amplitude, and powder is pulverized; The powder of pulverizing is sent into spiral conveying groove from bottom to top along helix and the powder on the helicla flute is heated to assigned temperature through the internal heat type heater, thereby heating powder is also carried out hydrogenation treatment, the powder of heating enters oscillatory type cooling chamber, middle accumulator by discharge gate, again with the powder inputted vibration sieve screening powder that stores, powder is separated into different granularities herein, the granularity different according to powder put into one or more storage powder buckets with the powder that separates.
12. the preparation method of a kind of quickly solidifing hydrogen-stored alloy powder material according to claim 11 is characterized in that: be 5-20 minute powder heat time heating time of described pulverizing, and maximum heating temperature is 850 ℃.
13. the preparation method of a kind of quickly solidifing hydrogen-stored alloy powder material according to claim 11 is characterized in that: it is that vibration is pulverized under screw that described powder is pulverized, and pulverizing is carried out under 1-10bar pressure.
14. combination atomizer of implementing the described quickly solidifing hydrogen-stored alloy powder material preparation method of claim 1, it is characterized in that: described combination atomizer be located at feed trumpet in the described fully continuous type vacuum one argon melting high-pressure inert gas powder by atomization device below, the argon pressure control valve (4 ') that comprises porous type ring-type atomizer (2 ') and control connection argon gas thereof is socketed in the circular seam type ring-type cooling jet (1 ') of porous type ring-type atomizer (2 ') outside and the nitrogen pressure control valve (5 ') that nitrogen is connected in control thereof.
15. high speed centrifugation quick solidification apparatus of implementing the described quickly solidifing hydrogen-stored alloy powder material preparation method of claim 1, it is characterized in that: described high speed centrifugation quick solidification apparatus is located at a side of described fully continuous type vacuum one argon melting high-pressure inert gas powder by atomization device, comprise argon plasma stove vacuum chamber (04), this argon plasma stove vacuum chamber (04) is connected by the self-conveyor feed (017) and the middle batch can of heat-conducting (2) of fully continuous type vacuum one argon melting high-pressure inert gas powder by atomization device, be provided with crucible or the water jacketed copper crucible (010) that adapts with self-conveyor feed 017 in this argon plasma stove vacuum chamber (04) and topple over dress (012) automatically, the top of crucible or water jacketed copper crucible (010) is provided with tungsten electrode (01), the below of the pouring opening of crucible or water jacketed copper crucible (03) is provided with high speed rotating disc (09), one inboard of argon plasma stove vacuum chamber (04) is provided with the relative cooling reflecting plate (05) of droplet direction that falls out with high speed rotating disc (09), below at cooling reflecting plate (05) is provided with powder catcher (07) and the discharging opening (08) that is connected with argon plasma stove vacuum chamber (04), and this discharging opening (08) is connected with the storage powder bucket (13) of fully continuous type vacuum one argon melting high-pressure inert gas powder by atomization device.
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