CN1442258A - Hydrogen blasting furnace for breaking rare earth permanent magnetic material and hydrogen blasting technology - Google Patents
Hydrogen blasting furnace for breaking rare earth permanent magnetic material and hydrogen blasting technology Download PDFInfo
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- CN1442258A CN1442258A CN 02104353 CN02104353A CN1442258A CN 1442258 A CN1442258 A CN 1442258A CN 02104353 CN02104353 CN 02104353 CN 02104353 A CN02104353 A CN 02104353A CN 1442258 A CN1442258 A CN 1442258A
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Abstract
A hydrogen explosion furnace and process for breaking the permaneng-magnet RE material (Sm-Co or Nd-Fe-B material) is disclosed. The said furnace is characterized by its additional hydrogen explosion reaction containing a stirrer controlled by external motor for increasing the probability of the permanent-magnet RE particles in contact with hydrogen, vacuum and argon during absorbing and releasing hydrogen and cooling, so shortening its period. In addition, the said hydrogen explosion and powder conveying are performed in sealed state, so preventing the high-temp powder from being oxidized.
Description
The present invention relates to hydrogen breaker---the hydrogen blasting furnace of rare earth permanent-magnetic material, and rare earth permanent-magnetic material is carried out the hydrogen fragmentation with this device, and with a kind of special-purpose milling method of the quick-fried powdered of they hydrogen.
When adopting common powder metallurgical technique to prepare sintered nd-fe-b magnet, at first Nd-Fe-B alloy cast ingot that distinct methods will be obtained or the coarse crushing of casting sheet, broken alloying pellet into about 200-400 μ m size then is after ball milling or airflow milling are worn into the alloy powder of about 3-5 μ m size.At present, in the technological process of the high performance sintered Nd-Fe-B magnet of preparation, the middle fragmentation before the airflow milling is substituted by the quick-fried technology of hydrogen basically.Particularly for the fast quenching casting sheet that obtains with quench, the quick-fried method of hydrogen is the effective method that broken this class fast quenching casting sheet becomes alloy powder.
For producing above-mentioned high performance sintered Nd-Fe-B magnet, (patent No. was embodiment: two patents of CN1249972A and CN1267065A) adopt the form that is similar to vacuum heat treatment furnace to carry out hydrogen and pulverize in the past.Because material is loaded in the box of sealing, be present in the same box when inhaling hydrogen, it is comparatively complete that the top sub-material is inhaled hydrogen, and the latter half is relatively poor, promptly inhales the hydrogen imperfection, influences the fragmentation of material, in further pulverizing, can bring particle size distribution inhomogeneous, the problem of degrade performance.
During dehydrogenation, based on above-mentioned same problem, the top dehydrogenation that can exist close magazine is easier, and the magazine bottom is then difficult, the time of this dehydrogenation that certainly will extend, influence efficient, and when serious, add at double for a long time, even dehydrogenation is perfect inadequately, influences the final performance of material.
Because the dehydrogenation of material needs to carry out (450 ℃～600 ℃) under higher temperature, and because material is fragmented into than fine particle because of inhaling hydrogen-dehydrogenation, thereby very easily oxidation even burning, this just requires powder must be cooled to lower temperature (for example: below 60 ℃) in stove, the container that can move to other further cools off, but because usual way is all contained powder among magazine and carried out, the transmission that this will hinder heat reduces cooling effectiveness.
The objective of the invention is in order to overcome the above three problem.The invention provides a kind of hydrogen breaker---hydrogen blasting furnace, it has advantages such as the simple and easy operation of equipment when shortening the quick-fried process cycle of hydrogen.Utilize hydrogen breaker of the present invention---hydrogen blasting furnace, can be effectively and carry out the hydrogen break process operation of Nd-Fe-B alloy safely, obtain high-quality Nd-Fe-B alloyed powder.
Hydrogen blasting furnace of the present invention has following feature: in body of heater, be provided with a quick-fried still of hydrogen specially, and in the quick-fried still of hydrogen, installed one additional can be by the blender of extraneous motor control.In addition, the quick-fried still of this hydrogen links to each other with discharge nozzle with feeding pipe to be opened/closed, discharge nozzle upper end with join by controllable bar in the external world and still bottom plug.Provide safely in addition in addition and inhale the feed system that one of hydrogen and cooling usefulness is overlapped hydrogen and argon gas in the stove.
In desirable embodiment, the blender in the quick-fried still of hydrogen should make during forward rotation that Nd-Fe-B alloy powder moves up and down in the kettle, so that in inhaling hydrogen, dehydrogenation and cooling procedure, plays the limit and stirs, and the effect of hydrogen, limit dehydrogenation and limit cooling is inhaled on the limit; The quick-fried powder of hydrogen outside in moves in the kettle and should make during backward rotation.
In desirable embodiment, when being rotated by the blender of extraneous motor control, the dynamic seal of rotating shaft of stirrer can keep the hydrogen blasting furnace seal.
In desirable embodiment, when the quick-fried powder of hydrogen has been cooled near room temperature, by mentioning the still bottom plug by the bar of external world's control, the backward rotation blender, the quick-fried powder of hydrogen moves to the upper port of discharge nozzle, enter the upper port of discharge nozzle, and can be transported in the quick-fried powder storage tank of the external hydrogen of hydrogen blasting furnace, so that further cool to room temperature in tank or under the spray by discharge nozzle.
In desirable embodiment, after the quick-fried powder of hydrogen all shifts out the quick-fried still of hydrogen,,, can put down the still bottom plug by bar by external world's control as in nitrogen or argon gas at oxygen-free atmosphere or inert gas.Then, open the pan feeding pipe valve, the hydrogen for the treatment of in the storage tank is pulverized material and is transported in the kettle of the quick-fried still of hydrogen by feeding pipe, carry out the quick-fried technology of hydrogen of next cycle.
Hydrogen breaking method of the present invention is to use above-mentioned hydrogen blasting furnace to come broken bulk or flaky rare earth permanent magnet alloy, makes the quick-fried one-tenth alloyed powder of its hydrogen.
Be the embodiment sketch of hydrogen blasting furnace below:
Fig. 1 is the profile according to hydrogen blasting furnace main body embodiment of the present invention.
Fig. 2 is the top view according to hydrogen blasting furnace embodiment of the present invention.
Its symbol description is as follows:
1---storage tank; 2---exhaust pipe; 3---isolating valve; 4---feed pipe; 5---the stopper rod driving head; 6---beater motor; 7---multiple vacuum sealed box; 8---blender; 9---vacuum chamber; 10---heat shield; 11---heater; 12---the quick-fried still of hydrogen; 13---pumped vacuum systems; 14---the still bottom plug; 15---discharge nozzle; 16---the discharging isolating valve; 17---cooling system; 18---the still bracing frame; 19---heating electrode; 20---air inlet pipe; 21---muffler; 22---discharge tank; 23---the quick-fried kettle cover of hydrogen; 24---the body of heater bracing frame.
Embodiment is described as follows:
Fig. 1 is the profile according to hydrogen blasting furnace main body embodiment of the present invention.Fig. 2 is the top view according to hydrogen blasting furnace embodiment of the present invention.This hydrogen blasting furnace is except that the setting with conventional vacuum heat treatment air-quenching furnace---and vacuum system 13, calandria 11, gas quenching are but system 17,20,21 and the automatic control system, principal character is to be provided with specially a quick-fried still 12 of hydrogen in body of heater, and in the quick-fried still of hydrogen, installed one additional can be by the blender 8 of extraneous motor control.In addition, the quick-fried still of this hydrogen links to each other with discharge nozzle 15 with feed pipe 4 to be opened/closed, the discharge nozzle upper port with join by the controllable still bottom plug 14 in the external world.Provide in addition in addition and inhale the feed system that one of hydrogen and cooling usefulness is overlapped hydrogen and argon gas in the stove safely.
In hydrogen blasting furnace of the present invention, be to implement like this to the hydrogen fragmentation of Nd-Fe-B alloy cast ingot or casting sheet:
At first, in nitrogen or inert gas, utilize Mechanical Method that the coarse crushing of Nd-Fe-B alloy cast ingot is become the block raw material of centimetre magnitude, and these Nd-Fe-B alloy raw materials are put into be full of in nitrogen or the inert gas raw material storage tank 1.Subsequently, raw material storage tank 1 is docked with feed pipe 4, utilize vacuum system 13 to vacuumize by 2 pairs of storage tanks 1 of exhaust pipe, after waiting to reach the certain vacuum degree, stop to vacuumize, open valve 3 after charging into inert gas, make the Nd-Fe-B alloy raw material for the treatment of the hydrogen fragmentation enter the quick-fried kettle 12 of hydrogen by way of feed pipe 4.After the raw material in the storage tank all is delivered into the quick-fried still of hydrogen, should close valve separately.Then, the quick-fried technology of beginning hydrogen.At first vacuumize, the vacuum degree in the furnace chamber is reached about 0.01Pa by opening 13 pairs of hydrogen blasting furnace chambers of vacuum system.Stop then finding time, carry hydrogen to the hydrogen blasting furnace chamber, the hydrogen pressure during beginning in the furnace chamber should be between 0.2-0.6MPa.Start blender 8 simultaneously, its rotation period is controlled at about per minute 2-6 circle.Through the suction hydrogen incubation period of a few minutes, the Nd-Fe-B alloy begins to inhale in a large number hydrogen and explosion.Should provide sufficient hydrogen this moment to the hydrogen blasting furnace chamber, and the hydrogen pressure in the furnace chamber is maintained more than the 0.2MPa.Because inhaling hydrogen is exothermic reaction, with the carrying out that inhales the hydrogen process, the temperature of furnace chamber increases.This suction hydrogen process approximately continues 0.5-1 hour.Inhale hydrogen-explosion process through this section, block raw material Nd-Fe-B alloy hydrogen fully is quick-fried into about the fine particle that is 200-400 μ m size.Inhale hydrogen-explosion process this moment and finish, then need the quick-fried powder of hydrogen is carried out dehydrogenation.Because of being preferably under the temperature between 450-600 ℃, this process carries out, so, at first furnace temperature must be elevated to above-mentioned temperature, and vacuumize simultaneously.In order to accelerate the carrying out of certain embodiments, at this moment, blender 8 keeps stirring.Along with the increase of dehydrogenation time, the hydrogen pressure in the furnace chamber descends constantly.After 4-5 hour lasting dehydrogenation of process, hydrogen pressure in the furnace chamber has dropped to 1-10Pa, can finish the dehydrogenation operation, promptly cut off the stove heating power supply, and then carry argon gas to the hydrogen blasting furnace chamber, pressure in the furnace chamber is risen to more than the 0.01Mpa, and start the blower fan of cooling system 17 immediately, the quick-fried powder of hydrogen in the quick-fried still of hydrogen is cooled off fast.At this moment, blender 8 keeps stirring.Along with the increase of cooling time, the temperature of the quick-fried powder of hydrogen in the quick-fried still of hydrogen descends constantly.After 4-5 hour lasting cooling of process, the temperature of the quick-fried powder of hydrogen can drop to 50-60 ℃, just can finish refrigerating work procedure, i.e. the blower fan of stop cooling system 17 running.
At last, by mentioning the still bottom plug by the bar of external world's control, the backward rotation blender, the quick-fried powder of hydrogen moves to the upper port of discharge nozzle, enter the upper port of discharge nozzle, and can being transported to by the discharge nozzle 15 of having opened valve in the outer storage tank 22 of body of heater, so that further cool to room temperature in tank or under the spray.After the quick-fried powder of hydrogen all entered discharge nozzle, the stop blender rotated, and can put down the still bottom plug by the bar by external world's control.At this moment, should close the valve 16 of the quick-fried powder storage tank of discharge nozzle and hydrogen.So far, the quick-fried technology of hydrogen is all over.
Utilize hydrogen breaker of the present invention---hydrogen blasting furnace, 200kg Nd-Fe-B alloy cast ingot is carried out the hydrogen fragmentation according to the foregoing description, only need be with 10-12 hour.The present invention has advantages such as the simple and easy operation of equipment when shortening the quick-fried process cycle of hydrogen.Utilize hydrogen blasting furnace of the present invention, can be efficiently and carry out the hydrogen break process operation of Nd-Fe-B alloy safely, prevent the oxidation of Nd-Fe-B alloyed powder, thereby can obtain high-quality Nd-Fe-B alloyed powder, help improving the magnetic property of sintered nd-fe-b magnet.
Claims (16)
1. hydrogen blasting furnace, its main application is to carry out rare earth permanent-magnetic material (SmCo Sm-Co, neodymium iron boron Nd-Fe-B) hydrogen pulverization process operation.It is except that the feature that possesses general vacuum heat air-quenching furnace, main feature is to be provided with a quick-fried still of hydrogen in body of heater specially, and in the quick-fried still of hydrogen, installed one additional can be by the blender of extraneous motor control.The quick-fried still of hydrogen links to each other with discharge nozzle with feeding pipe to be opened/closed, discharge nozzle upper end with join by the controllable still bottom plug in the external world.Provide safely in addition in addition and inhale the feed system that one of hydrogen and cooling usefulness is overlapped hydrogen and argon gas in the stove.
2. hydrogen blasting furnace according to claim 1 has a quick-fried still of hydrogen of depositing hydrogen pulverization process material in the body of heater.The quick-fried still of this hydrogen is made of three parts such as kettle, kettle cover and still bottom plugs.
3. according to claim 1 and 2 described hydrogen blasting furnaces, the kettle of the quick-fried still of hydrogen and still bottom plug are to be made by the copper or the stainless steel material of high heat conduction.Kettle cover is to be made by the stainless steel material of low heat conduction.
4. hydrogen blasting furnace according to claim 1, have in the quick-fried still of hydrogen one can be by the blender of external control rotating speed and direction.The blade of this blender is to be made by the copper of high heat conduction or stainless steel material.
5. according to claim 1 and 4 described hydrogen blasting furnaces, the rotating shaft of blender is to be made by the stainless steel material of low heat conduction.
6. hydrogen blasting furnace according to claim 1, the kettle cover of the quick-fried still of hydrogen links to each other with feeding pipe to be opened/closed, and feeding pipe is to be made by the stainless steel material of low heat conduction.
7. hydrogen blasting furnace according to claim 1 links to each other with discharge nozzle to be opened/closed at the bottom of the still.Discharge nozzle is to be made by the stainless steel material of low heat conduction.
8. hydrogen blasting furnace according to claim 1 outside the quick-fried body of heater of dehydrogenation, provides in addition and inhales the feed system that one of hydrogen and cooling usefulness is overlapped hydrogen and argon gas in the stove safely.
9. quick-fried technology of hydrogen, it is to use, and the described hydrogen blasting furnace of arbitrary claim carries out the processing method that hydrogen is pulverized in the claim 1 to 7.It is characterized in that rare earth permanent-magnetic material is carried out the processing method that hydrogen is pulverized.
10. rare earth permanent-magnetic material manufacturing method of power is characterized in that with thickness being that the R-T-B alloy of 0.03mm-10mm is inhaled hydrogen, dehydrogenation and refrigerating work procedure in the quick-fried still of hydrogen.
11. according to Claim 8 with 9 described rare earth permanent-magnetic material manufacturing method of power, also comprise in its technology, that collects from body of heater outside supply before hydrogen is quick-fried in the quick-fried still of hydrogen waits to pulverize the coarse grained operation of rare earth permanent-magnetic material, and through the quick-fried powder of cooled hydrogen, the road transfers out the outer operation of body of heater through still bottom plug and discharge nozzle.These operations are all carried out in oxygen-free atmosphere or inert gas atmosphere.
12. with 9 described rare earth permanent-magnetic material manufacturing method of power, it is characterized in that the suction hydrogen of described material and consequential hydrogen are quick-fried according to Claim 8, in the quick-fried still of hydrogen, realizing while stirring under the nitrogen atmosphere.
13., it is characterized in that the dehydrogenation of the quick-fried powder of described material hydrogen realizes while stirring under vacuum atmosphere in the quick-fried still of hydrogen according to Claim 8 with 9 described rare earth permanent-magnetic material manufacturing method of power.
14. according to Claim 8 with 9 described rare earth permanent-magnetic material manufacturing method of power, the cooling that it is characterized in that the quick-fried powder of described material hydrogen is to realize while stirring in the quick-fried still of hydrogen in the inert gas that is cooled.
15. according to claim 1 and 7 described hydrogen blasting furnaces, it is characterized in that the quick-fried powder of described material hydrogen only need be cooled to a proper temperature in the quick-fried still of hydrogen, the quick-fried powder of the hydrogen that is higher than room temperature can be transferred out in the quick-fried powder storage tank of the external hydrogen of hydrogen blasting furnace further cool to room temperature in tank or under the spray subsequently.
16., it is characterized in that block raw material can directly enter the quick-fried still of hydrogen from feeding pipe to be opened/closed and carry out the hydrogen break process under the situation of not opening stove according to claim 1 and 6 described hydrogen blasting furnaces.
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| CN 02104353 CN1442258A (en) | 2002-03-05 | 2002-03-05 | Hydrogen blasting furnace for breaking rare earth permanent magnetic material and hydrogen blasting technology |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100408231C (en) * | 2005-12-23 | 2008-08-06 | 上海大学 | Method for forming anisotropic neodymium iron boron binding magnet and apparatus thereof |
| CN101767200B (en) * | 2010-01-05 | 2012-05-09 | 北京科技大学 | Minute spherical Nd-Fe-B powder preparation method |
| CN102982936A (en) * | 2012-11-09 | 2013-03-20 | 厦门钨业股份有限公司 | Manufacture method for dispense process of sintering Nd-Fe-B serial magnet |
| CN103801703A (en) * | 2012-11-08 | 2014-05-21 | 沈阳中北通磁科技股份有限公司 | Rare earth permanent magnetic alloy continuous hydrogen decrepitation process method |
| CN104001927A (en) * | 2013-08-13 | 2014-08-27 | 中磁科技股份有限公司 | Neodymium-iron-boron-hydrogen tank breaking cooling system |
| CN108417372A (en) * | 2018-01-30 | 2018-08-17 | 宁波铄腾新材料有限公司 | A kind of preparation method of rich cerium magnet for driving motor |
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2002
- 2002-03-05 CN CN 02104353 patent/CN1442258A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100408231C (en) * | 2005-12-23 | 2008-08-06 | 上海大学 | Method for forming anisotropic neodymium iron boron binding magnet and apparatus thereof |
| CN101767200B (en) * | 2010-01-05 | 2012-05-09 | 北京科技大学 | Minute spherical Nd-Fe-B powder preparation method |
| CN103801703A (en) * | 2012-11-08 | 2014-05-21 | 沈阳中北通磁科技股份有限公司 | Rare earth permanent magnetic alloy continuous hydrogen decrepitation process method |
| CN103801703B (en) * | 2012-11-08 | 2017-01-18 | 沈阳中北通磁科技股份有限公司 | Rare earth permanent magnetic alloy continuous hydrogen decrepitation process method |
| CN102982936A (en) * | 2012-11-09 | 2013-03-20 | 厦门钨业股份有限公司 | Manufacture method for dispense process of sintering Nd-Fe-B serial magnet |
| CN102982936B (en) * | 2012-11-09 | 2015-09-23 | 厦门钨业股份有限公司 | The manufacture method saving operation of sintered Nd-Fe-B based magnet |
| US20150279530A1 (en) * | 2012-11-09 | 2015-10-01 | Xiamen Tungsten Co., Ltd. | Manufacturing method of a powder for compacting rare earth magnet and the rare earth magnet omitting jet milling process |
| US10381141B2 (en) * | 2012-11-09 | 2019-08-13 | Xiamen Tungsten Co., Ltd. | Rare earth magnet and a method for manufacturing compactable powder for the rare earth magnet without jet milling |
| CN104001927A (en) * | 2013-08-13 | 2014-08-27 | 中磁科技股份有限公司 | Neodymium-iron-boron-hydrogen tank breaking cooling system |
| CN108417372A (en) * | 2018-01-30 | 2018-08-17 | 宁波铄腾新材料有限公司 | A kind of preparation method of rich cerium magnet for driving motor |
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