CN103801703B - Rare earth permanent magnetic alloy continuous hydrogen decrepitation process method - Google Patents
Rare earth permanent magnetic alloy continuous hydrogen decrepitation process method Download PDFInfo
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- CN103801703B CN103801703B CN201210444480.1A CN201210444480A CN103801703B CN 103801703 B CN103801703 B CN 103801703B CN 201210444480 A CN201210444480 A CN 201210444480A CN 103801703 B CN103801703 B CN 103801703B
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 73
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 73
- 238000000034 method Methods 0.000 title claims abstract description 22
- 229910001004 magnetic alloy Inorganic materials 0.000 title claims abstract description 15
- 230000008569 process Effects 0.000 title claims abstract description 15
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 10
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 10
- 125000004435 hydrogen atom Chemical class [H]* 0.000 title 1
- 238000010438 heat treatment Methods 0.000 claims abstract description 66
- 238000001816 cooling Methods 0.000 claims abstract description 52
- 238000006356 dehydrogenation reaction Methods 0.000 claims abstract description 52
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 150000002431 hydrogen Chemical class 0.000 claims abstract description 37
- 239000011261 inert gas Substances 0.000 claims abstract description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000001301 oxygen Substances 0.000 claims abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 4
- 239000007789 gas Substances 0.000 claims description 15
- 239000000956 alloy Substances 0.000 claims description 10
- 229910045601 alloy Inorganic materials 0.000 claims description 9
- 238000009423 ventilation Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000000926 separation method Methods 0.000 claims description 5
- 239000000112 cooling gas Substances 0.000 claims description 3
- 230000007717 exclusion Effects 0.000 claims 1
- 239000000843 powder Substances 0.000 abstract description 16
- 239000002245 particle Substances 0.000 abstract description 4
- 238000011282 treatment Methods 0.000 abstract description 4
- 238000010924 continuous production Methods 0.000 abstract description 2
- 238000010521 absorption reaction Methods 0.000 abstract 2
- 239000013078 crystal Substances 0.000 abstract 1
- 238000003754 machining Methods 0.000 abstract 1
- 238000004382 potting Methods 0.000 abstract 1
- 238000009413 insulation Methods 0.000 description 19
- 229910052756 noble gas Inorganic materials 0.000 description 17
- 150000002835 noble gases Chemical class 0.000 description 17
- 238000007789 sealing Methods 0.000 description 11
- 239000000498 cooling water Substances 0.000 description 9
- 230000007704 transition Effects 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000005086 pumping Methods 0.000 description 5
- 230000007306 turnover Effects 0.000 description 5
- 238000013467 fragmentation Methods 0.000 description 4
- 238000006062 fragmentation reaction Methods 0.000 description 4
- 239000006247 magnetic powder Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
- 229920001971 elastomer Polymers 0.000 description 3
- 229910001172 neodymium magnet Inorganic materials 0.000 description 3
- 239000005060 rubber Substances 0.000 description 3
- 238000007599 discharging Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 241000167880 Hirundinidae Species 0.000 description 1
- 241001347978 Major minor Species 0.000 description 1
- 229910018095 Ni-MH Inorganic materials 0.000 description 1
- 229910018477 Ni—MH Inorganic materials 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- FMGSKLZLMKYGDP-USOAJAOKSA-N dehydroepiandrosterone Chemical class C1[C@@H](O)CC[C@]2(C)[C@H]3CC[C@](C)(C(CC4)=O)[C@@H]4[C@@H]3CC=C21 FMGSKLZLMKYGDP-USOAJAOKSA-N 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000010079 rubber tapping Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/023—Hydrogen absorption
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0573—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes obtained by reduction or by hydrogen decrepitation or embrittlement
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C2202/00—Physical properties
- C22C2202/02—Magnetic
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
Landscapes
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Furnace Details (AREA)
- Sorption Type Refrigeration Machines (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention provides a rare earth permanent magnetic alloy continuous hydrogen decrepitation process method. A hydrogen absorption chamber, a heating dehydrogenation chamber and a cooling chamber are serially connected by valves between the chambers, a rare earth permanent magnetic alloy is subjected to the treatments of hydrogen absorption, heating dehydrogenation and cooling in equipment disclosed by the invention at one step, and collecting and potting treatments under the protection atmosphere of inert gas can be expanded based on the equipment. The machining process is continuous production performed under vacuum and the protection atmosphere of the inert gas, broken powder contains less oxygen, and single crystal particles in the powder are large in proportion.
Description
Technical field
The present invention relates to a kind of continuous hydrogen of permanent-magnet rare-earth NdFeB alloy breaks process.
Background technology
Nd-Fe-B rare-earth permanent magnet rapidly quenched magnetic powder and resin etc. mix, and can make bonded permanent magnet.It is widely used in electronics, electricity
Device, motor etc., have more and more extensive use.Rare earth hydrogen storage alloy is also the negative material of Ni-MH battery, is widely used in
Electric tool, hybrid vehicle etc., have more and more extensive use.
It is a kind of rotation liner hydrogen broken furnace that existing permanent-magnet rare-earth NdFeB alloy hydrogen breaks equipment, and rotatable flue supports
On the support member of two ends, electric furnace, by can the left and right body of heater of opening and closing constitute, is wrapped in flue outer layer, one end of flue is
Into and out of material mouth, the other end is communicated with vacuum extractor and air distributing device sealing.
It is highly difficult that existing rotary hydrogen broken furnace takes out magnetic powder under inert gas shielding；Cooling rate is low, and process time is long, from
More than ten to three ten hours；It is the Muffle furnace of external-heat, energy resource consumption is big.
Content of the invention
In order to solve above-mentioned technical problem, the present invention provides a kind of continuous hydrogen of RE permanent magnetic alloy to break technique side
Method.
The process of the present invention, comprises the steps:
1) charging basket that will be equipped with RE permanent magnetic alloy sends into suction hydrogen room, to inhaling hydrogen room evacuation after closing valve, works as vacuum
After 50pa or oxygen volume content≤0.1%, it is flushed with hydrogen gas to -0.05～+0.5mpa, after keeping 10 minutes～120 minutes, will
Hydrogen is excluded；When inhaling hydrogen room and Heating Dehydrogenation chamber pressure dynamic balance, open the separation valve door inhaled between hydrogen room and Heating Dehydrogenation room, will
Charging basket is sent to Heating Dehydrogenation room, closes separation valve door；
2) begin to warm up as Heating Dehydrogenation chamber pressure≤0.1pa, the maximum temperature of heating is 500～900 DEG C, during heating
Between be 4～20 hours, open when Heating Dehydrogenation room and cooling chamber pressure balance Heating Dehydrogenation room and cooling interventricular septum from valve
Charging basket is sent to closing valve after cooling chamber；
3) after cooling chamber filling with inert gas, after gas pressure reaches -0.05～+0.5mpa, start blower fan to charging basket and
In charging basket, alloy is cooled down, and behind temperature≤120 DEG C, balance pressure, to atmospheric pressure, is opened discharge door, charging basket is spread out of.
When described heat de-airing room arranges more than 2, step 2) all assign to each Heating Dehydrogenation room heat time heating time.
When described cooling chamber arranges more than 2, step 3) cool time all assign to each cooling chamber.
Beneficial effects of the present invention:
The present invention, compared with existing rotary hydrogen broken furnace, is to pass through valve between room by inhaling hydrogen room, Heating Dehydrogenation room and cooling chamber
Door is connected in series, and RE permanent magnetic alloy is once completed in present device inhale hydrogen process, Heating Dehydrogenation process, cooling treatment
Process with the rewinding tinning under inert gas shielding atmosphere.Existing rotary hydrogen broken furnace is avoided to take out under inert gas shielding
Magnetic powder is highly difficult, and cooling rate is low, and process time is long, the big problem of the Muffle furnace energy consumption of external-heat.Processing technique is in vacuum and lazy
Property gas atmosphere in the continuous production that carries out, on the premise of reducing energy consumption, production capacity is high and good product consistency, broken
Powder body oxygen content is few, and in powder body, monocrystal particle accounts for very big proportion, and performance is high, improves service life of equipment simultaneously, shortens equipment
The maintaining time.
Brief description
Fig. 1 is that the RE permanent magnetic alloy hydrogen of invention breaks device structure schematic diagram.
Fig. 2 is suction hydrogen room structural representation in Fig. 1.
Fig. 3 is the left view of Fig. 2.
Fig. 4 is the i portion enlarged diagram of Fig. 3.
Fig. 5 is Heating Dehydrogenation cell structure schematic diagram in Fig. 1.
Fig. 6 is magazine structural representation in Fig. 1.
Fig. 7 is the left view of Fig. 6.
Fig. 8 is one-way sealing schematic diagram in the present invention.
Fig. 9 is a-a sectional view in Fig. 8.
Figure 10 is b-b sectional view in Fig. 8.
Figure 11 is two-way seal insert plate valve schematic diagram in the present invention.
Figure 12 is cooling chamber structural representation in Fig. 1.
Figure 13 is the structural representation of the partial structurtes of present invention series connection rewinding room.
In figure: 1, the first motor；2nd, magazine；3rd, inlet side transition frame；4th, 1# vacuum equipment；5th, sliding vane rotary pump；6th, lobe pump；7、
Flapper valve；8th, 1# valve；9th, noble gases incoming line；10th, 2# vacuum equipment；11st, master takes out valve；12nd, filter；13rd, bypass
Valve；14th, inhale hydrogen room；15th, hydrogen ingress pipe road；16th, passive security valve；17th, active safety valve；18th, electro connecting pressure gauge；19、
Vacuum gauge；20th, pressure transducer；21st, the first thermocouple；22nd, 2# valve；23rd, Heating Dehydrogenation room；24th, 3# vacuum equipment；25、
3# valve；26th, 4# vacuum equipment；27th, cooling chamber；28th, the second motor；29th, blower fan；30th, heat exchanger；31st, 4# valve；32nd, go out
End transition frame；33rd, photoswitch；34th, noble gases incoming line flange；35th, hydrogen ingress pipe road flange；36th, relief valve pipe
Road flange；37th, roller；38th, the second sprocket wheel；39th, gear pair；40th, bearing block；41st, cooling water nozzle；42nd, vacuum-pumping pipeline flange；
43rd, thermocouple；44th, latch plate；45th, chain；46th, the 3rd motor；47th, bin；48th, track；49th, relief valve pipeline flange；50、
Inflation flange；51st, thermal insulation board；52nd, evacuate flange；53rd, upper thermal insulation board；54th, the first cylinder；55th, the second thermocouple；56th, water-cooled
Electrode；57th, side thermal insulation board；58th, heater；59th, lower thermal insulation board；60th, mozzle；61st, deflector；62nd, bottom turnover door；63rd, expect
Basket；64th, support；65. ventilation ducts, 66. hinges, the 67, second cylinder；68th, the first limit switch；69th, front blind flange；70th, it is evacuated
Flange；71st, inflate flange；72nd, valve body；73rd, the second limit switch；74th, cylinder or oil cylinder；75th, cushion rubber；76th, thermal insulation layer；77、
First valve plate；77 ', second valve plate；Blind flange after 78., 79, pulley；80th, guide rail；81st, pulley connecting plate；82nd, get on the right track；83rd, cold
But water pipe axle；84th, flexible pipe；85th, 5# separation valve door；86th, loading line；87th, pressure gauge；88th, vent valve；89th, 6# valve；90、
Recovering hopper；91st, Hand-operated butterfly valve；92nd, glove box；93rd, batch can；94th, discharge chamber；95th, aspirating hole；96th, dovetail groove；97th, the first chain
Wheel；98th, Chain plate.
Specific embodiment
The present invention will be further described with reference to the accompanying drawings and examples
Embodiment: as shown in figure 1, the equipment of the present invention is including the inlet side transition frame 3 setting gradually, 1# valve 8, inhales hydrogen
Room 14,2# valve 22, Heating Dehydrogenation room 23,3# valve 25, cooling chamber 27,4# valve 31, go out to hold transition frame 32, loop line frame, with
And electrical control cabinet and vacuum extractor；Inhale and pass through interventricular septum between hydrogen room 14, Heating Dehydrogenation room 23 and cooling chamber 27 respectively from valve
Door connects, and described actuating device is arranged on the top inhaling hydrogen room 14, Heating Dehydrogenation room 23 and cooling chamber 27, and magazine 2 is suspended on biography
On dynamic device, roll conveying through inhaling hydrogen room 14, Heating Dehydrogenation room 23 and cooling chamber 27 successively along actuating device.Loop line frame and each room
Actuating device composition endless drive track, form the annular load mode that moves in circles.Magazine 2 is suspended on actuating device,
Slide along conveyor track.
Described inlet side transition frame 3 is that the logistics circulation of production process prepares transitional region, can be under atmospheric condition
Working gantry or a seal case, this casing top feeding pipe has valve, valve has charge can.Material
Box 2 vertical hanging conveys in actuating device upper roller track sprocket wheel chain, frequency control.
As shown in Figure 2 and Figure 3, described suction hydrogen room 14 is vertical cabinet, and cabinet exterior carries water cooling tube or chuck, is inhaling hydrogen
Room 14 top be provided with vacuum suction pipeline, hydrogen ingress pipe road 15, noble gases incoming line 9, electric-controlled type active safety valve 17,
Fragmentation formula passive security valve 16, electro connecting pressure gauge 18, vacuum gauge 19, pressure transducer 20 and the first thermocouple 21, evacuation
Pipeline is connected with vacuum extractor.Inhale hydrogen room 14 to stop importing hydrogen when leak rate exceedes predetermined value, when temperature is stopped beyond setting
Only import hydrogen；As shown in figure 4, inhaling hydrogen room 14 flange is all to be respectively provided with two cushion rubbers using two annular dovetail slots 96
Composition double manifold vacuum sealing, has aspirating hole 95 between two dovetail grooves 96, can be filled with noble gases；Magazine 2 is suspended on biography
On dynamic device, photoswitch display control magazine 2 position that the symmetrical side plate in casing top is provided with, frequency control；Rare earth permanent magnet
Alloy completes to be broken into powder in suction hydrogen room.
As shown in figure 5, described Heating Dehydrogenation room 23 is vertical cabinet, at least one, it is arranged in series when multiple, this example adopts
1, cabinet exterior carry water cooling tube or chuck, Heating Dehydrogenation ceiling portion be provided with vacuum-pumping pipeline, noble gases incoming line,
Electric-controlled type active safety valve 17, fragmentation formula passive security valve 16, electro connecting pressure gauge, vacuum gauge and loading line, vacuum-pumping tube
Road is connected with vacuum extractor；Heating Dehydrogenation chamber interior has vertical rectangle heating furnace, and inside heating furnace has by upper thermal insulation board 53, side
Thermal insulation board 57 and the thermal insulation layer of lower thermal insulation board 59 composition, have multigroup heater 58, are all provided with every group of heater 58 inside thermal insulation layer
Thermocouple 43, heter temperature packet controls；Outside heating furnace, heating furnace top is provided with the thermal insulation board of opening and closing left and right to actuating device
51, thermal insulation board 51 both sides connect cylinder 54 respectively, and when bin is walked about, thermal insulation board 51 is opened, when bin is forbidden in heating furnace,
Thermal insulation board 51 is closed；Heating furnace sidewall has water cooled electrode 56 and thermocouple 55；Relief valve exit and vacuum-pumping pipeline exhaustor
Place is connected with inert gas piping, plays anti-explosion safety effect；Heating Dehydrogenation room 23 flange is all using two annular swallows
Stern notch 96 is respectively provided with two cushion rubber composition double manifold vacuum sealings, has aspirating hole 95, Ke Yichong between two dovetail grooves 96
Inert gas shielding, identical with the flange double manifold vacuum sealing structure inhaling hydrogen room 14, as shown in Figure 4；Heating Dehydrogenation room 23
Top, equipped with pressure transducer, when the hydrogen that Heating Dehydrogenation room 23 releases exceeds authorized pressure, stops heating；Magazine 2 is suspended on
On actuating device, Heating Dehydrogenation room symmetrical side plate top heating furnace is externally provided with correlation photoswitch, display control magazine 2
Put, frequency control；Hydrogen in magazine 2 breaks powder and carries out Dehydroepiandrosterone derivative in Heating Dehydrogenation room 23.
As shown in figure 12, cooling chamber 27 is vertical cabinet, and at least provided with one, this example arranges 1；Cabinet exterior has water-cooled
Pipe or chuck, side wall is provided with the second motor 28, and inside is provided with bellows, and bellows side wall is provided with multiple mozzles 60, corresponding another
Side is provided with the high-performance heat exchanger 30 of high density fin winding, and heat exchanger 30 air outlet is against blower fan 29, blower fan 29 and the second electricity
Machine 28 axle connects, and cooling chamber 27 inner peripheral wall is provided with arc deflector 61；It is externally connected to evacuation pipeline, noble gases ingress pipe
Road and relief valve pipeline；Vacuum-pumping pipeline is connected with vacuum extractor.Magazine 2 is suspended on actuating device, roller track sprocket wheel
Chain conveys, and the symmetrical side plate top of cooling chamber 27 is provided with correlation photoswitch display control magazine 2 position, frequency control；Hydrogen
Broken powder carries out cooling treatment in cooling chamber 27 to be filled with noble gases mode, and cooling gas can move in circles and be cooled down；When
After powder material reaches tapping temperature, stop cooling blower, magazine 2 enters discharge chamber 94.
The present invention is also serially connected with discharge chamber 94 in cooling chamber 27 end, as shown in figure 13, is provided with below described discharge chamber 94
Recovering hopper 90, recovering hopper 90 connects batch can 93 by glove box 92, and discharge chamber 94 is provided with inert gas plenum pipeline 86, pressure
Table 87 and vent valve 88.Wherein glove box 92 is the glove casing with observation window, and glove box 92 turnover pipeline is respectively equipped with
Manually-operated gate 91.In discharging, in discharge chamber 94, magazine 2 bottom turnover door is opened, and material enters into recovering hopper 90；Discharge chamber 94 sets
There are exhaust pipe, noble gases incoming line, discharging pipeline and glove box 92；Magazine 2 is suspended on actuating device, discharge chamber 94
Two symmetrical side plate tops are provided with correlation photoswitch, display control magazine 2 position, frequency control；Hydrogen breaks powder in discharge chamber 94
It is divided in multiple batch cans 93.
Between this example Heating Dehydrogenation room 23 and suction hydrogen room 14 and suction hydrogen room 14 and air, two-way seal insert plate valve is set, other are each
Room arranges one-way sealing push-pull valve.
As Figure 8-Figure 10, described one-way sealing push-pull valve includes valve body 72, the second cylinder 67, multiple cylinder or oil cylinder
74th, the first valve plate 77, valve plate running gear, rigid cooling water turnover tube assembly and forward and backward blind flange 69,78, wherein, valve body 72
Corresponding both sides are respectively arranged with forward and backward blind flange 69,78, and the outer top of front blind flange 69 is provided with the second cylinder 67 and cooling water pipe group
Part；It is provided with first valve plate 77 parallel with the other both sides of valve body 72, the first valve plate 77 passes through valve plate running gear in valve body 72
It is hung in valve body 72 internal upper part, valve plate running gear is rigidly connected with the cylinder rod cylinder head part of outside second cylinder 67, the first valve
Plate 77 bottom is provided with pulley 79, coordinates with the guide rail 80 in valve body 72, and the first valve plate 77 is welded with water cooling tube or chuck, water-cooled
Pipe or chuck are connected on two sealing rigidity cooling water pipe axles 83 by the flexible pipe 84 of cooling water pipe assembly, cooling water pipe axle 83
It is connected with the cylinder rod of the second cylinder 67, realize linkage, with cooling water pipe axle 83 geo-stationary during the first valve plate 77 displacement, multiple
Cylinder or oil cylinder 74 are placed in outside valve body 72, are connected locking the first valve plate 77 respectively with the two ends of the first valve plate 77, realize sealing.The
First, the second limit switch 68,73 is separately positioned on the second cylinder 67 and string cylinder or oil cylinder 74, controls the first valve plate 77
Position, is provided with O-ring seal 75 at corresponding valve port, the first valve plate 77 is pushed away by multiple cylinders or oil cylinder 74 on the first valve plate 77
Dynamic it is ensured that the first valve plate 77 uniform force, the first valve plate 77 is provided with O-ring seal 75, and the decrement of O-ring seal 75 is big, protects
Card large scale valve port valve plate sealing property.First valve plate 72 can be from valve body in maintenance for the forward and backward blind flange 69,78 of valve body 72
72 side removals.First valve plate 77 is also equipped with thermal insulation board.Inflation flange 71, exhaust flange are additionally provided with valve body 72
70 and pressure gauge, when valve is closed, valve has inflation flange 71 to filling with inert gas in valve body 72, has exhaust flange
70 are connected with vacuum equipment, carry out pressure detecting simultaneously.
Described valve plate running gear includes upper rail 82, assembly pulley and the pulley connecting plate 81 being arranged at upper end in valve body 2,
Described assembly pulley is placed in upper rail 82, and assembly pulley by pulley connecting plate 81, valve plate is hung on upper rail 82.
As shown in figure 11, described two-way seal insert plate valve is to be additionally provided with described one-way sealing push-pull valve and first
The second symmetrical valve plate 77 ' of valve plate 77 and the outer two row cylinders being connected with the second valve plate 77 ' two ends of valve body 72 or oil cylinder；Each valve
Plate is respectively connected with described valve plate running gear.
As shown in Figure 2 and Figure 3, heretofore described actuating device includes the 3rd motor 46, chain 45, gear pair 39, two
Bearing block 40,48, two groups of rollers 37 of two parallel orbits, two first sprocket wheels 97, the second sprocket wheel 38 and Chain plate 98, described two first
Sprocket wheel 97 is arranged on the hinge axis stretching out outside housing through each room housing, logical between the 3rd motor 46 output shaft and the first sprocket wheel 97
Cross chain 45 to connect, two bearings seat 40 one end is separately mounted on the sprocket shaft in housing, is connected with and hinge axis between the other end
Parallel axle, this axle and hinge axis are separately installed with the gear pair 39 cooperating, and the second sprocket wheel 38 is arranged in housing
On sprocket shaft, two groups of rollers 37 being placed in two parallel orbits 48 are connected by its roller shaft, are provided with and the on roller shaft
The Chain plate 98 of two sprocket wheel 38 cooperation, described Chain plate 98 other end connects bin 2 connecting rod.Bearing block 40 is connected with spring
Plate 44, latch plate 44 other end connects the housing of each room, and during work, stress makes the second sprocket wheel 38 and Chain plate 98 closely connect.
As shown in Figure 6, Figure 7, heretofore described magazine 2, its charging basket 63 two opposite sides plate is welded with and multiple rows of runs through magazine 2
The oblate abnormal shape ventilation duct 65 of inner chamber, special-shaped ventilation duct 65 is had multiple passages and is communicated with charging basket 63 inner chamber, magazine 2 base plate
62 is the door-plate of the outside upset with hinge 66；Support 64 is welded with charging basket 63.
Each vacuum equipment adopts lobe pump 6 and sliding vane rotary pump 5 unit, wherein inhales hydrogen room 14 and Heating Dehydrogenation room 23 is connected with master
Take out valve 11 pipeline and bypass valve 13 pipeline, wherein master takes out valve 11 pipeline and bypass valve 13 pipeline is in parallel, sliding vane rotary pump and filter are even
There is noble gases incoming line on adapter road, and vacuum pump quits work, and is filled with noble gases (vacuum breaker).Inhale hydrogen room 14, heating takes off
2#, 3#, 4# vacuum equipment 10,14,26 of hydrogen room 23 and cooling chamber 27 has dust filter unit 12.1#, 2#, 3# valve 8,22,25
By the public 1 set of 1# evacuator 4 of flapper valve 7.
The use process of the present invention:
It is illustrated referring to Fig. 1, check power current, power gas source, circulating water for cooling and medium source of the gas.Check institute
There is major-minor Plant in good condition lossless, in running order.Using scatter operation pattern, making equipment meet production technology state is vacuum
System start-up is simultaneously in interlocking state, and noble gases dilution valves are opened and are adjusted to regulation flow；Inhale hydrogen room 14 and Heating Dehydrogenation
Room 23 automatic leak detection result is not leaked；Between room, 2#, 3# valve 22,25 is closed；Heating Dehydrogenation room 23 interior heater 58 is intact；
Dielectric gas is through flow meter settings to predetermined value, all the sensors electro connecting pressure gauge 18, vacuum gauge 19, pressure transducer
20th, the first thermocouple 21, the second thermocouple 55 are in the steady statue of work.
Inhale hydrogen room 14 and 1# valve 8 be in atmospheric pressure, open 1# valve 8, start the first motor 1 and the 3rd motor 46,
The bin 47 waiting in inlet side transition frame 3 carries magazine 2 and enters inhales hydrogen room 14, closes 1# valve 8.
1# vacuum equipment 4 is by lobe pump 6, sliding vane rotary pump 5, flapper valve 7, corrugated tube, pipeline and noble gases incoming line group
Become, by Pneumatic baffle valve 7 to 1# valve 8 evacuation；As 1# valve 8 pressure≤0.1pa, noble gases incoming line 9 times
Filling with inert gas.
2# vacuum equipment 10 is by lobe pump, sliding vane rotary pump, roughing valve door, bypass valve 13, corrugated tube, pipeline and 12 groups of filter
Become, evacuated pipeline flange 42 is to suction hydrogen room 14 evacuation；As pressure≤0.1pa, automatic vacuum leak detection result is not leaked, and uses
Inert gas purge, then evacuation, be flushed with hydrogen atmospheric pressure by hydrogen ingress pipe road 15 and reach 0.096mpa, hydrogen ingress pipe road 15
On valve be automatically switched off.RE permanent magnetic alloy material hydrogen abstraction reaction in magazine 2 is broken into powder and finishes, and evacuation recharges indifferent gas
Body, tail gas pipeline washes away from roof discharge room through noble gases.Electro connecting pressure gauge 18, vacuum gauge 19, pressure transducer 20
Complete pressure and temperature control with the first thermocouple 21.Relief valve pipeline has electric-controlled type active safety valve 17 and fragmentation formula passively to pacify
Full valve 18.Inhale hydrogen room 14 outer wall and want water-cooled, have turnover cooling water nozzle 41.
The conveying of wherein magazine 2 is to drive chain 45 by the sprocket wheel on actuating device the 3rd motor 46 axle, and power is led to
Cross seal transmission shaft to be incorporated in vacuum chamber, by the gear pair 39 of latch plate 44 stress, moment of torsion is won in succession seat by bearing
40 are delivered on the second sprocket wheel 38, and bin pulling axis stirred by the second sprocket wheel 38, and roller 37 in rail 48 on bin is walked, photoelectricity
Switch 33 is limit switch, frequency control.
Suction hydrogen room 14, Heating Dehydrogenation room 23 and 2# valve 22 are under inert gas atmosphere or vacuum state and pressure is put down
Weighing apparatus, 2# valve 22 is opened, and magazine 2 enters Heating Dehydrogenation room 23, closes 2# valve 22.
3# vacuum equipment 24 is by lobe pump, sliding vane rotary pump, roughing valve door, bypath valve, corrugated tube, filter and pipeline group
Become, through evacuating flange 52 to Heating Dehydrogenation room 23 evacuation, as pressure≤0.1pa, automatic vacuum leak detection result is not leaked, inertia
Gas cleans to Heating Dehydrogenation room 23 through inflation flange 50.Evacuation again；Begin to warm up as pressure≤0.1pa, dehydrogenation temperature
500～900 DEG C of degree, magnetic powder dehydrogenation reaction finishes, and evacuation recharges noble gases, and tail gas pipeline washes away from roof through noble gases
Discharge outside room.Pressure gauge, vacuum gauge, pressure transducer and thermocouple complete pressure and temperature control.Relief valve pipeline flange 49 connects
There are electric-controlled type active safety valve 17 and fragmentation formula passive security valve 18.Heating furnace top in Heating Dehydrogenation room 23 has by first
Cylinder 54 can be with the thermal insulation board 51 of opening and closing left and right；There are upper thermal insulation board 53, side thermal insulation board 57 and lower thermal insulation board 59；There is three sections of upper, middle and lower
Heater 58, is connected with power cabinet by water cooled electrode 56, the second thermocouple 55 subregion temperature control.
When Heating Dehydrogenation room 23, cooling chamber 27 and 3# valve 25 are under inert gas atmosphere or vacuum state and pressure
Balance, opens 3# valve 25, and magazine 2 enters cooling chamber 27, closes 3# valve 25.
4# vacuum equipment 26 is to cooling chamber 27 evacuation.Filling with inert gas, pressure reaches 0.19～0.29mpa, starts
Second motor 28, blower fan 29 starts, to the powder body cooling in magazine 2 and magazine 2, there is a lot of ventilation ducts 65, cooling gas in magazine 2
The heat of powder body is taken away by body by ventilation duct.It is cold that heated gas passes through high-performance heat exchanger 30 under the driving of blower fan 29
But, then again magazine 2 is blowed to by blower fan 29 through deflector 64.
In magazine 2, numerous special-shaped mozzles 60 running through charging basket 63 cavity improve powder body contact area, special-shaped mozzle 60
There is passage to communicate with cavity, make material inhale hydrogen speed, Heating Dehydrogenation speed and rate of cooling and accelerate, improve hydrogen and break efficiency.
Magazine 2 is suspended on actuating device.
When cooling chamber 27 pressure is atmospheric pressure, open 4# valve 31, magazine 2 enters into out end transition frame 32.
Magazine 2, through loop line frame, enters into inlet side transition frame 3 and waits.
Equipment can also extend discharge chamber, and 4# vacuum equipment 26 to discharge chamber evacuation and recharges noble gases.Cooling
Between room 27, discharge chamber 94 and room, valve is under inert gas atmosphere and pressure balance, opens valve between room, and magazine 2 enters
Discharge chamber, closes valve.Start shedding mechanism under inert gas atmosphere, powder body in magazine 2 is collected by valve pipeline
In the batch can of circulation.
Aborning, control system can continuously be scanned to status of equipment, and according to program set in advance
Carry out automatic running.Whole operation is to complete in the man machine interface of computer.
The display screen of electric control system can provide following information: the purity of hydrogen；Vacuum pump, vacuum valve and vacuum
The running status of pipeline vacuum；Drive and display bin conveying and running status；Drive valve running status and between display room；
Show each independent vacuum chamber, the vacuum of gate valve, pressure and heating-up temperature；Dielectric gas running status, safe valve state；Real
Border cooling water, power atmospheric pressure, dielectric gas are reported to the police；Alarming and managing；Display all related technological parameter (setting value and reality
Value)；Parameter inputs；Historical process parameter/data display and storage；The all main components of equipment can be through display screen behaviour
Make.
By above-described embodiment as can be seen that rare earth alloy pass through hydrogen break, Heating Dehydrogenation and cooling technique, improve powder
Particle size distribution and powder particle shape, have significant impact to improving magnet performance, the automaticity of production greatly improves.
One of ordinary skill in the art should be able to understand the essence of the present invention, and recognizes the specific implementation details of the present invention
Can make in claims and for example extend the various changes such as multiple Heating Dehydrogenation rooms and cooling chamber.
Claims (3)
1. a kind of continuous hydrogen of RE permanent magnetic alloy break process it is characterised in that: comprise the steps:
1) charging basket that will be equipped with RE permanent magnetic alloy sends into suction hydrogen room, to inhaling hydrogen room evacuation after closing valve, when vacuum is higher than
After 50pa or oxygen volume content≤0.1%, it is flushed with hydrogen gas to -0.05～+0.5mpa, after keeping 10 minutes～120 minutes, by hydrogen
Exclusion；When inhaling hydrogen room and Heating Dehydrogenation chamber pressure dynamic balance, open the separation valve door inhaled between hydrogen room and Heating Dehydrogenation room, by charging basket
It is sent to Heating Dehydrogenation room, close separation valve door；
2) begin to warm up as Heating Dehydrogenation chamber pressure≤0.1pa, the maximum temperature of heating is 500～900 DEG C, heat time heating time is
4～20 hours, open Heating Dehydrogenation room when Heating Dehydrogenation room and cooling chamber pressure balance and cooling interventricular septum will be expected from valve
Basket is sent to closing valve after cooling chamber；
3) after cooling chamber filling with inert gas, after gas pressure reaches -0.05～+0.5mpa, start blower fan to charging basket and charging basket
Interior alloy is cooled down, and behind temperature≤120 DEG C, balance pressure, to atmospheric pressure, is opened discharge door, charging basket is spread out of；
Described suction hydrogen room, Heating Dehydrogenation room and cooling chamber are vertical cabinets, inhale the top of hydrogen room, Heating Dehydrogenation room and cooling chamber
It is provided with actuating device；Described cooling chamber outer wall has water collar or chuck, and inwall is provided with arc deflector, is provided with inside cooling chamber
Bellows, the inwall of bellows side is provided with multiple mozzles, and the opposite side inwall of bellows is provided with finned heat exchanger；Described charging basket
For multiple, and it is integrated in a magazine；Magazine is suspended on actuating device, de- through suction hydrogen room, heating successively along actuating device
Hydrogen room and cooling chamber conveying；Two of described charging basket side plate relatively is welded with multiple rows of special-shaped ventilation duct running through magazine inner chamber, special-shaped
Multiple passages are had on ventilation duct communicate with charging basket inner chamber, make being fully contacted of gas and RE permanent magnetic alloy, make rare earth forever
The suction hydrogen of magnetic alloy, Heating Dehydrogenation and cooling procedure are quick and uniform；
In described charging basket and charging basket, when cooling interior is cooled down, cooling gas pass through special-shaped ventilation duct by charging basket to alloy
The heat of alloy is taken away, and heated gas is cooled down by finned heat exchanger under the driving of blower fan, then through deflector again by
Blower fan blows to magazine.
2. a kind of continuous hydrogen of RE permanent magnetic alloy according to claim 1 break process it is characterised in that: described heating
When dehydrogenation room arranges more than 2, step 2) all assign to each Heating Dehydrogenation room heat time heating time.
3. a kind of continuous hydrogen of RE permanent magnetic alloy according to claim 1 break process it is characterised in that: described cooling
Room arrange more than 2 when, step 3) cool time all assign to each cooling chamber.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210444480.1A CN103801703B (en) | 2012-11-08 | 2012-11-08 | Rare earth permanent magnetic alloy continuous hydrogen decrepitation process method |
| PCT/CN2013/071354 WO2014071707A1 (en) | 2012-11-08 | 2013-02-05 | Continuous hydrogen decrepitation processing method for rare earth permanently magnetic alloy and production equipment therefor |
| US14/075,801 US9543063B2 (en) | 2012-11-08 | 2013-11-08 | Continuous hydrogen pulverization method and production device of rare earth permanent magnetic alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210444480.1A CN103801703B (en) | 2012-11-08 | 2012-11-08 | Rare earth permanent magnetic alloy continuous hydrogen decrepitation process method |
Publications (2)
| Publication Number | Publication Date |
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| CN103801703A CN103801703A (en) | 2014-05-21 |
| CN103801703B true CN103801703B (en) | 2017-01-18 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210444480.1A Active CN103801703B (en) | 2012-11-08 | 2012-11-08 | Rare earth permanent magnetic alloy continuous hydrogen decrepitation process method |
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| Country | Link |
|---|---|
| CN (1) | CN103801703B (en) |
| WO (1) | WO2014071707A1 (en) |
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| CN113649580B (en) * | 2021-07-13 | 2023-07-25 | 杭州电子科技大学 | Efficient hydrogen breaking device and rare earth alloy hydrogen breaking method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1249972A (en) * | 1998-10-07 | 2000-04-12 | 住友特殊金属株式会社 | Hydrogen damage technology and box for rare earth metal-base magnetic material |
| CN2555932Y (en) * | 2002-07-26 | 2003-06-18 | 太原市佳世特净化设备有限公司 | Hydrogen grinder for magnetic material |
| CN1442258A (en) * | 2002-03-05 | 2003-09-17 | 赵宇靖 | Hydrogen blasting furnace for breaking rare earth permanent magnetic material and hydrogen blasting technology |
| CN1877755A (en) * | 2006-07-04 | 2006-12-13 | 包头稀土研究院 | Hydrogen-pulverized flexible processing method for Nd-Fe-B |
| CN102211199A (en) * | 2011-06-10 | 2011-10-12 | 北京大学 | Method for crushing rare earth-iron type alloy |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4451632B2 (en) * | 2003-10-14 | 2010-04-14 | 株式会社アルバック | Hydrogen crusher for rare earth magnet materials |
| CN201589006U (en) * | 2009-12-24 | 2010-09-22 | 川北真空科技(北京)有限公司 | Water-cooled vacuum gate valve |
| CN202943253U (en) * | 2012-11-08 | 2013-05-22 | 沈阳中北真空磁电科技有限公司 | Rare-earth permanent magnet alloy hydrogen breaking continuous production equipment |
-
2012
- 2012-11-08 CN CN201210444480.1A patent/CN103801703B/en active Active
-
2013
- 2013-02-05 WO PCT/CN2013/071354 patent/WO2014071707A1/en not_active Ceased
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1249972A (en) * | 1998-10-07 | 2000-04-12 | 住友特殊金属株式会社 | Hydrogen damage technology and box for rare earth metal-base magnetic material |
| CN1442258A (en) * | 2002-03-05 | 2003-09-17 | 赵宇靖 | Hydrogen blasting furnace for breaking rare earth permanent magnetic material and hydrogen blasting technology |
| CN2555932Y (en) * | 2002-07-26 | 2003-06-18 | 太原市佳世特净化设备有限公司 | Hydrogen grinder for magnetic material |
| CN1877755A (en) * | 2006-07-04 | 2006-12-13 | 包头稀土研究院 | Hydrogen-pulverized flexible processing method for Nd-Fe-B |
| CN102211199A (en) * | 2011-06-10 | 2011-10-12 | 北京大学 | Method for crushing rare earth-iron type alloy |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2014071707A1 (en) | 2014-05-15 |
| CN103801703A (en) | 2014-05-21 |
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