CN103801703A - Rare earth permanent magnetic alloy continuous hydrogen decrepitation process method - Google Patents

Rare earth permanent magnetic alloy continuous hydrogen decrepitation process method Download PDF

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Publication number
CN103801703A
CN103801703A CN201210444480.1A CN201210444480A CN103801703A CN 103801703 A CN103801703 A CN 103801703A CN 201210444480 A CN201210444480 A CN 201210444480A CN 103801703 A CN103801703 A CN 103801703A
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chamber
hydrogen
valve
heating
cooling
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CN201210444480.1A
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CN103801703B (en
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陈晓东
孙宝玉
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SHENYANG ZHONGBEI TONGCI TECHNOLOGY Co Ltd
Shenyang General Magnetic Co Ltd
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SHENYANG ZHONGBEI TONGCI TECHNOLOGY Co Ltd
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Priority to CN201210444480.1A priority Critical patent/CN103801703B/en
Priority to PCT/CN2013/071354 priority patent/WO2014071707A1/en
Priority to US14/075,801 priority patent/US9543063B2/en
Publication of CN103801703A publication Critical patent/CN103801703A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/023Hydrogen absorption
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets 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
    • H01F1/04Magnets 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
    • H01F1/047Alloys characterised by their composition
    • H01F1/053Alloys characterised by their composition containing rare earth metals
    • H01F1/055Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571Alloys 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
    • H01F1/0573Alloys 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
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C2202/00Physical properties
    • C22C2202/02Magnetic
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C33/00Making ferrous alloys
    • C22C33/02Making ferrous alloys by powder metallurgy

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  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Sorption Type Refrigeration Machines (AREA)
  • Furnace Details (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

The continuous hydrogen of RE permanent magnetic alloy breaks process
Technical field
The present invention relates to the broken process of the continuous hydrogen of a kind of permanent-magnet rare-earth NdFeB alloy.
Background technology
Nd-Fe-B rare-earth permanent magnet rapidly quenched magnetic powder mixes with resin etc., can make bonded permanent magnet.Be widely used in electronics, electrical equipment, motor etc., have use more and more widely.Rare earth hydrogen storage alloy is also the negative material of Ni-MH battery, is widely used in electric tool, hybrid vehicle etc., has use more and more widely.
The broken equipment of existing permanent-magnet rare-earth NdFeB alloy hydrogen is a kind of rotation liner hydrogen broken furnace, rotatable flue is supported on two end supports part, electric furnace is made up of left and right body of heater that can opening and closing, be wrapped in flue skin, one end of flue is charging and discharging mouth, and the other end communicates with vacuum extractor and air distributing device sealing.
It is very difficult that existing rotary hydrogen broken furnace takes out magnetic under inert gas shielding; Cooling rate is low, and the processing time is long, from tens to 30 hours; Be the Muffle furnace of external-heat, energy resource consumption is large.
summary of the invention
In order to solve the technical problem of above-mentioned existence, the invention provides the broken process of the continuous hydrogen of a kind of RE permanent magnetic alloy.
Process of the present invention, comprises the steps:
1) charging basket that RE permanent magnetic alloy is housed is sent into and is inhaled hydrogen chamber, after closing valve, vacuumize inhaling hydrogen chamber, when vacuum is higher than 50Pa or oxygen content≤0.1%(volume) after, fill hydrogen to-0.05~+ 0.5MPa, keep, after 10 minutes~120 minutes, hydrogen being got rid of; In the time inhaling hydrogen chamber and Heating Dehydrogenation chamber pressure balance, open the separation valve door of inhaling between hydrogen chamber and Heating Dehydrogenation chamber, charging basket is sent to heating clamber, close separation valve door;
2) in the time of Heating Dehydrogenation chamber pressure≤0.1Pa, start heating, the maximum temperature of heating is 500~900 ℃, heat time is 4~20 hours, opens between Heating Dehydrogenation chamber and cooling chamber closing valve after charging basket is sent to cooling chamber by separation valve door in the time of Heating Dehydrogenation chamber and cooling chamber pressure balance;
3) after cooling chamber filling with inert gas, when gas pressure reaches after-0.05~+ 0.5MPa, start blower fan and alloy in charging basket and charging basket is carried out cooling, behind temperature≤120 ℃, equalizing pressure, to atmospheric pressure, is opened discharge door, and charging basket is spread out of.
When described heat de-airing chamber arranges more than 2 or 2, step 2) heat time all assigns to each heat de-airing chamber.
When described cooling chamber arranges more than 2 or 2, all assign to each cooling chamber the cool time of step 3).
beneficial effect of the present invention:
The present invention is compared with existing rotary hydrogen broken furnace; be that suction hydrogen chamber, Heating Dehydrogenation chamber and cooling chamber are connected in series by valve between chamber, RE permanent magnetic alloy once completed in present device and inhale hydrogen processing, Heating Dehydrogenation processing, cooling processing and the rewinding tinning processing under inert gas shielding atmosphere.Avoid existing rotary hydrogen broken furnace under inert gas shielding, to take out magnetic very difficult, cooling rate is low, and the processing time is long, the large problem of Muffle furnace energy consumption of external-heat.Processing technology is the continuous production of carrying out in vacuum and inert gas shielding atmosphere; reducing under the prerequisite of energy consumption; high and the good product consistency of production capacity; broken powder oxygen content is few; in powder, monocrystal particle accounts for very large proportion; performance is high, improves service life of equipment simultaneously, has shortened the equipment maintenance time.
Accompanying drawing explanation
Fig. 1 is the broken device structure schematic diagram of the RE permanent magnetic alloy hydrogen of invention.
Fig. 2 inhales hydrogen cell structure schematic diagram 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 cutaway view in Fig. 8.
Figure 10 is B-B cutaway 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 connect structural representation of partial structurtes of rewinding chamber of the present invention.
In figure: 1, the first motor; 2, magazine; 3, inlet side transition frame; 4,1# vacuum plant; 5, sliding vane rotary pump; 6, lobe pump; 7, flapper valve; 8,1# valve; 9, inert gas imports pipeline; 10,2# vacuum plant; 11, the main valve of taking out; 12, filter; 13, by-passing valve; 14, inhale hydrogen chamber; 15, hydrogen ingress pipe road; 16, passive security valve; 17, active safety valve; 18, electro connecting pressure gauge; 19, vacuum gauge; 20, pressure sensor; 21, the first thermocouple; 22,2# valve; 23, Heating Dehydrogenation chamber; 24,3# vacuum plant; 25,3# valve; 26,4# vacuum plant; 27, cooling chamber; 28, the second motor; 29, blower fan; 30, heat exchanger; 31,4# valve; 32, go out to hold transition frame; 33, optoelectronic switch; 34, inert gas imports pipeline flange; 35, hydrogen ingress pipe road flange; 36, safety valve pipeline flange; 37, roller; 38, the second sprocket wheel; 39, gear pair; 40, bearing block; 41, cooling water nozzle; 42, vacuum-pumping pipeline flange; 43, thermocouple; 44, latch plate; 45, chain; 46, the 3rd motor; 47, bin; 48, track; 49, safety valve pipeline flange; 50, inflation flange; 51, thermal insulation board; 52, the flange of finding time; 53, upper thermal insulation board; 54, the first cylinder; 55, the second thermocouple; 56, water cooled electrode; 57, side thermal insulation board; 58, heater; 59, lower thermal insulation board; 60, mozzle; 61, deflector; 62, end turnover door; 63, charging basket; 64, support; 65. ventilation ducts, 66. hinges, 67, the second cylinder; 68, the first limit switch; 69, front blind flange; 70, exhaust flange; 71, inflation flange; 72, valve body; 73, the second limit switch; 74, cylinder or oil cylinder; 75, cushion rubber; 76, thermal insulation layer; 77, the first valve plate; 77 ', the second valve plate; 78. rear blind flanges, 79, pulley; 80, guide rail; 81, pulley connecting plate; 82, get on the right track; 83, cooling water tubular axis; 84, flexible pipe; 85,5# separation valve door; 86, loading line; 87, Pressure gauge; 88, vent valve; 89,6# valve; 90, recovering hopper; 91, Hand-operated butterfly valve; 92, glove box; 93, batch can; 94, discharge chamber; 95, aspirating hole; 96, dovetail groove; 97, the first sprocket wheel; 98, Chain plate.
The specific embodiment
Below in conjunction with drawings and Examples, the present invention will be further described
Embodiment: as shown in Figure 1, equipment of the present invention is to comprise the inlet side transition frame 3 that sets gradually, 1# valve 8, inhale hydrogen chamber 14,2# valve 22, Heating Dehydrogenation chamber 23,3# valve 25, cooling chamber 27,4# valve 31, go out to hold transition frame 32, loop line frame, and electrical control cabinet and vacuum extractor; Inhale between hydrogen chamber 14, Heating Dehydrogenation chamber 23 and cooling chamber 27 and be connected from valve by interventricular septum respectively, described transmission device is arranged on the top of inhaling hydrogen chamber 14, Heating Dehydrogenation chamber 23 and cooling chamber 27, magazine 2 is suspended on transmission device, carries successively along transmission device through inhaling hydrogen chamber 14, Heating Dehydrogenation chamber 23 and cooling chamber 27 rollings.The transmission device of loop line frame and each chamber forms annular conveyor track, forms the annular load mode moving in circles.Magazine 2 is suspended on transmission device, slides along conveyor track.
Described inlet side transition frame 3 is that transitional region is prepared in the logistics circulation of production process, can be the Working gantry under atmospheric condition, can be also a seal case, on this casing top feeding pipe, has valve, has charge can on valve.Magazine 2 vertical hangings are carried at transmission device upper roller track sprocket wheel chain, frequency control.
As shown in Figure 2 and Figure 3, described suction hydrogen chamber 14 is vertical cabinets, cabinet exterior is with water cooling tube or chuck, be provided with vacuum suction pipeline, hydrogen ingress pipe road 15, inert gas importing pipeline 9, electric-controlled type active safety valve 17, fragmentation formula passive security valve 16, electro connecting pressure gauge 18, vacuum gauge 19, pressure sensor 20 and the first thermocouple 21 at suction 14 tops, hydrogen chamber, vacuum-pumping pipeline is connected with vacuum extractor.Inhale hydrogen chamber 14 and stop importing hydrogen when leak rate exceedes predetermined value, stop importing hydrogen when temperature exceeds setting; As shown in Figure 4, inhaling hydrogen chamber 14 flanges is all to adopt two annular dovetail slots 96 that two cushion rubbers are housed respectively to form dual vacuum seal, has aspirating hole 95 between two dovetail grooves 96, can be filled with inert gas; Magazine 2 is suspended on transmission device, and the optoelectronic switch that the symmetrical side plate in casing top is provided with shows controls magazine 2 positions, frequency control; RE permanent magnetic alloy completes and is broken into powder in suction hydrogen chamber.
As shown in Figure 5, described Heating Dehydrogenation chamber 23 is vertical cabinets, at least one, when multiple, series connection arranges, this example adopts 1, cabinet exterior, with water cooling tube or chuck, is provided with vacuum-pumping pipeline, inert gas importing pipeline, electric-controlled type active safety valve 17, fragmentation formula passive security valve 16, electro connecting pressure gauge, vacuum gauge and loading line at top, Heating Dehydrogenation chamber, vacuum-pumping pipeline is connected with vacuum extractor; Heating Dehydrogenation chamber interior has vertical rectangle heating furnace, inside heating furnace has the thermal insulation layer being made up of upper thermal insulation board 53, side thermal insulation board 57 and lower thermal insulation board 59, there are many group heaters 58 thermal insulation layer inside, every group of interior thermocouple 43 of all establishing of heater 58, and heter temperature grouping is controlled; Transmission device is outside heating furnace, and heating furnace top is provided with the thermal insulation board 51 of opening and closing left and right, and thermal insulation board 51 both sides connect respectively cylinder 54, and in the time that bin is walked about, thermal insulation board 51 is opened, and forbids in heating furnace when bin, and thermal insulation board 51 is closed; Heating furnace sidewall has water cooled electrode 56 and thermocouple 55; Safety valve exit and vacuum-pumping pipeline blast pipe place are connected with inert gas piping, play anti-explosion safety effect; Heating Dehydrogenation chamber 23 flanges are all to adopt two annular dovetail slots 96 that two cushion rubbers are housed respectively to form dual vacuum seal, between two dovetail grooves 96, have aspirating hole 95, can protect by filling with inert gas, identical with the dual vacuum seal structure of flange of inhaling hydrogen chamber 14, as shown in Figure 4; Pressure sensor is equipped with on 23 tops, Heating Dehydrogenation chamber, and the hydrogen of emitting when Heating Dehydrogenation chamber 23 exceeds authorized pressure, stops heating; Magazine 2 is suspended on transmission device, and symmetrical side plate top, Heating Dehydrogenation chamber heating furnace is provided with correlation optoelectronic switch outward, shows and controls magazine 2 positions, frequency control; The broken powder of hydrogen in magazine 2 carries out dehydrogenation processing in Heating Dehydrogenation chamber 23.
As shown in figure 12, cooling chamber 27 is vertical cabinets, at least arranges one, and this example arranges 1; Cabinet exterior has water cooling tube or chuck, sidewall is provided with the second motor 28, inside is provided with bellows, bellows one sidewall is provided with multiple mozzles 60, corresponding opposite side is provided with the high-performance heat exchanger 30 that high density fin is wound around, heat exchanger 30 air outlets are facing to blower fan 29, and blower fan 29 is connected with the second motor 28 axles, and cooling chamber 27 inner peripheral wall are provided with arc deflector 61; Be externally connected to the pipeline of finding time, inert gas importing pipeline and safety valve pipeline; Vacuum-pumping pipeline is connected with vacuum extractor.Magazine 2 is suspended on transmission device, and roller track sprocket wheel chain is carried, and the symmetrical side plate of cooling chamber 27 top is provided with correlation optoelectronic switch and shows control magazine 2 positions, frequency control; The broken powder of hydrogen carries out cooling processing at cooling chamber 27 to be filled with inert gas mode, refrigerating gas can move in circles carry out cooling; When powder material reaches after tapping temperature, stop cooling blower, magazine 2 enters discharge chamber 94.
The present invention is also serially connected with discharge chamber 94 at cooling chamber 27 ends, as shown in figure 13, described discharge chamber 94 belows are provided with recovering hopper 90, and recovering hopper 90 connects batch can 93 by glove box 92, and discharge chamber 94 is provided with inert gas loading line 86, Pressure gauge 87 and vent valve 88.Wherein glove box 92 is the gloves casings with observation window, and glove box 92 passes in and out and on pipeline, is respectively equipped with manually-operated gate 91.In the time of discharging, the interior magazine of discharge chamber 94 2 end turnover door is opened, and material enters into recovering hopper 90; Discharge chamber 94 is provided with exhaust pipe, inert gas imports pipeline, discharging pipeline and glove box 92; Magazine 2 is suspended on transmission device, and 94 liang of symmetrical side plate tops of discharge chamber are provided with correlation optoelectronic switch, shows and controls magazine 2 positions, frequency control; The broken powder of hydrogen is divided in multiple batch cans 93 at discharge chamber 94.
Between this routine Heating Dehydrogenation chamber 23 and suction hydrogen chamber 14 and suction hydrogen chamber 14 and atmosphere, two-way seal insert plate valve is set, other each chambers arrange one-way sealing push-pull valve.
As Figure 8-Figure 10, described one-way sealing push-pull valve comprises valve body 72, the second cylinder 67, multiple cylinder or oil cylinder 74, the first valve plate 77, valve plate running gear, rigidity cooling water inlet/outlet pipe assembly and forward and backward blind flange 69,78, wherein, the corresponding both sides of valve body 72 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 assembly, in valve body 72, be provided with first valve plate 77 parallel with the other both sides of valve body 72, the first valve plate 77 is hung in valve body 72 internal upper parts by valve plate running gear, the cylinder rod cylinder head part of valve plate running gear and outside the second cylinder 67 is rigidly connected, the first valve plate 77 bottoms are provided with pulley 79, coordinate with the guide rail 80 in valve body 72, on the first valve plate 77, be welded with water cooling tube or chuck, water cooling tube 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 tubular axis 83 is connected with the cylinder rod of the second cylinder 67, realize interlock, the first valve plate 77 is relative with cooling water tubular axis 83 static while displacement, multiple cylinders or oil cylinder 74 are placed in outside valve body 72, be connected respectively locking the first valve plate 77 with the two ends of the first valve plate 77, realize sealing.First, second limit switch 68,73 is separately positioned on the second cylinder 67 and a row cylinder or oil cylinder 74, control the position of the first valve plate 77, on the first valve plate 77, corresponding valve port place is provided with O-ring seal 75, the first valve plate 77 is promoted by multiple cylinders or oil cylinder 74, guarantee that the first valve plate 77 is stressed evenly, the first valve plate 77 is provided with O-ring seal 75, and the decrement of O-ring seal 75 is large, guarantees large scale valve port valve plate sealing property.The forward and backward blind flange 69,78 of valve body 72 first valve plate 72 in the time of maintenance can shift out from valve body 72 sides.On the first valve plate 77, thermal insulation board can also be installed.On valve body 72, be also provided with inflation flange 71, exhaust flange 70 and Pressure gauge, valve valve in the time of closed condition has inflation flange 71 to the interior filling with inert gas of valve body 72, has exhaust flange 70 to be connected with vacuum plant, carries out pressure detecting simultaneously.
Described valve plate running gear comprise be arranged at valve body 2 interior upper ends get on the right track 82, assembly pulley and pulley connecting plate 81, described assembly pulley is placed in and gets on the right track in 82, assembly pulley is hung in valve plate to get on the right track on 82 by pulley connecting plate 81.
As shown in figure 11, described two-way seal insert plate valve is in described one-way sealing push-pull valve, to be also provided with and two row cylinder or the oil cylinders that are connected with the second valve plate 77 ' two ends outside the second valve plate 77 ' of the first valve plate 77 symmetries and valve body 72; Each valve plate is connected with described valve plate running gear respectively.
As Fig. 2, shown in Fig. 3, transmission device described in the present invention comprises the 3rd motor 46, chain 45, gear pair 39, diaxon bearing 40, two parallel orbits 48, two groups of rollers 37, two first sprocket wheels 97, the second sprocket wheel 38 and Chain plate 98, described two first sprocket wheels 97 are arranged on through each chamber housing and stretch out on the hinge axis outside housing, between the 3rd motor 46 output shafts and the first sprocket wheel 97, be connected by chain 45, diaxon bearing 40 one end are arranged on respectively on the sprocket shaft in housing, between the other end, be connected with the axle parallel with hinge axis, on this axle and hinge axis, be separately installed with the gear pair 39 cooperatively interacting, the second sprocket wheel 38 is arranged on the sprocket shaft in housing, two groups of rollers 37 that are placed in two parallel orbits 48 connect by its roller shaft, the Chain plate 98 coordinating with the second sprocket wheel 38 is installed on roller shaft, described Chain plate 98 other ends connect bin 2 connecting rods.On bearing block 40, be connected with latch plate 44, latch plate 44 other ends connect the housing of each chamber, and when work, stressed second sprocket wheel 38 that makes is closely connected with Chain plate 98.
As shown in Figure 6, Figure 7, magazine 2 described in the present invention, its charging basket 63 two opposite sides plates are welded with the oblate special-shaped ventilation duct 65 that many rows are run through magazine 2 inner chambers, have multiple passages and communicate with charging basket 63 inner chambers on special-shaped ventilation duct 65, and magazine 2 base plates 62 are the door-plates with the outside upset of hinge 66; On charging basket 63, be welded with support 64.
Each vacuum plant adopts lobe pump 6 and sliding vane rotary pump 5 units, wherein inhale hydrogen chamber 14 and Heating Dehydrogenation chamber 23 and be connected with main take out valve 11 pipelines and by-passing valve 13 pipelines, wherein master takes out valve 11 pipelines and by-passing valve 13 pipeline parallel connections, sliding vane rotary pump and filter connecting line have inert gas to import pipeline, vavuum pump quits work, and is filled with inert gas (vacuum breaker).2#, 3#, the 4 # vacuum plant 10,14,26 of inhaling hydrogen chamber 14, Heating Dehydrogenation chamber 23 and cooling chamber 27 have dust filter unit 12.1#, 2#, 3# valve 8,22,25 are by the public 1 cover 1# evacuator 4 of flapper valve 7.
use procedure of the present invention:
Be illustrated below with reference to Fig. 1, check power electric, power gas source, circulating water for cooling and medium source of the gas.Check that all major-minor Plant in good condition are harmless, in running order.Adopt scatter operation pattern, making equipment meet production technology state is that vacuum system starts and in interlocking state, regulation flow is opened and adjusted to inert gas dilution valve; Inhaling hydrogen chamber 14 and Heating Dehydrogenation chamber 23 automatic leak detection results does not leak; Between chamber, 2#, 3# valve 22,25 are closed; Heating Dehydrogenation chamber 23 interior heaters 58 are intact; Dielectric gas is set to predetermined value through flowmeter, all the sensors---electro connecting pressure gauge 18, vacuum gauge 19, pressure sensor 20, the first thermocouple 21, the stable state of the second thermocouple 55 in work.
Inhale hydrogen chamber 14 and 1# valve 8 in atmospheric pressure, open 1# valve 8, start the first motor 1 and the 3rd motor 46, the bin 47 of waiting in inlet side transition frame 3 carries magazine 2 and enters suction hydrogen chamber 14, closes 1# valve 8.
1# vacuum plant 4 imports pipeline by lobe pump 6, sliding vane rotary pump 5, flapper valve 7, bellows, pipeline and inert gas and forms, and by Pneumatic baffle valve 7,1# valve 8 is vacuumized; In the time of 1# valve 8 pressure≤0.1Pa, inert gas imports pipeline 9 and recharges inert gas.
2# vacuum plant 10 by lobe pump, sliding vane rotary pump, slightly take out valve, by-passing valve 13, bellows, pipeline and filter 12 and form, vacuumize inhaling hydrogen chamber 14 through vacuum-pumping pipeline flange 42; In the time of pressure≤0.1Pa, automatic vacuum leak detection result is not leaked, and by inert gas purge, then vacuumizes, fills Hydrogen Vapor Pressure reach 0.096MPa by hydrogen ingress pipe road 15, and the valve on hydrogen ingress pipe road 15 is closed automatically.It is complete that RE permanent magnetic alloy material hydrogen abstraction reaction in magazine 2 is broken into powder, vacuumizes and recharge inert gas, and tail gas pipeline washes away from discharge room, roof through inert gas.Electro connecting pressure gauge 18, vacuum gauge 19, pressure sensor 20 and the first thermocouple 21 complete pressure and temperature control.Safety valve pipeline has electric-controlled type active safety valve 17 and fragmentation formula passive security valve 18.Inhale hydrogen chamber 14 outer walls and want water-cooled, have turnover cooling water nozzle 41.
Wherein the conveying of magazine 2 is to drive chain 45 by the sprocket wheel on transmission device the 3rd motor 46 axles, power is incorporated in vacuum chamber by seal transmission shaft, by the stressed gear pair 39 of latch plate 44, moment of torsion 40 is delivered on the second sprocket wheel 38 by the bearing seat of winning in succession, the second sprocket wheel 38 is stirred bin pulling axis, roller 37 on bin is walked on track 48, and optoelectronic switch 33 is limit switches, frequency control.
Inhale hydrogen chamber 14, Heating Dehydrogenation chamber 23 and 2# valve 22 and be all under inert gas atmosphere or vacuum state and pressure balance, 2# valve 22 is opened, and magazine 2 enters Heating Dehydrogenation chamber 23, closes 2# valve 22.
3# vacuum plant 24 by lobe pump, sliding vane rotary pump, slightly take out valve, bypath valve, bellows, filter and pipeline and form, through finding time, flange 52 vacuumizes Heating Dehydrogenation chamber 23, in the time of pressure≤0.1Pa, automatic vacuum leak detection result is not leaked, and inert gas cleans Heating Dehydrogenation chamber 23 through inflation flange 50.Again vacuumize; In the time of pressure≤0.1Pa, start heating, 500~900 ℃ of desorption temperatures, magnetic dehydrogenation reaction is complete, vacuumizes and recharges inert gas, and tail gas pipeline washes away from discharge room, roof through inert gas.Pressure gauge, vacuum gauge, pressure sensor and thermocouple complete pressure and temperature control.Safety valve pipeline flange 49 is connected to electric-controlled type active safety valve 17 and fragmentation formula passive security valve 18.Thermal insulation board 51 that can opening and closing left and right by the first cylinder 54 is arranged at the heating furnace top in Heating Dehydrogenation chamber 23; There are upper thermal insulation board 53, side thermal insulation board 57 and lower thermal insulation board 59; There are three sections of heaters 58 of upper, middle and lower, are connected with power cabinet by water cooled electrode 56, the second thermocouple 55 subregion temperature controls.
When Heating Dehydrogenation chamber 23, cooling chamber 27 and 3# valve 25 are all under inert gas atmosphere or vacuum state and pressure balance, open 3# valve 25, magazine 2 enters cooling chamber 27, closes 3# valve 25.
4# vacuum plant 26 vacuumizes cooling chamber 27.Filling with inert gas, pressure reaches 0.19~0.29Mpa, starts the second motor 28, and blower fan 29 starts the powder in magazine 2 and magazine 2 cooling, has a lot of ventilation ducts 63 in magazine 2, and refrigerating gas is taken away the heat of powder by ventilation duct.Heated gas is cooling by high-performance heat exchanger 30 under the driving of blower fan 29, then blows to magazine 2 by blower fan 29 again through deflector 64.
The interior numerous special-shaped mozzles 60 that run through charging basket 63 cavitys of magazine 2 improve powder contact area, and special-shaped mozzle 60 has passage to communicate with in cavity, make material inhale hydrogen speed, Heating Dehydrogenation speed and cooling velocity and accelerate, and improve the broken efficiency of hydrogen.Magazine 2 is suspended on transmission device.
In the time that cooling chamber 27 pressure are 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 for.
Equipment can also be expanded discharge chamber, and 4# vacuum plant 26 vacuumizes and recharge inert gas to discharge chamber.Between cooling chamber 27, discharge chamber 94 and chamber, valve is all under inert gas atmosphere and pressure balance, opens valve between chamber, and magazine 2 enters discharge chamber, valve-off.Under inert gas atmosphere, start shedding mechanism, powder in magazine 2 is collected in the batch can of circulation by valve pipeline.
Aborning, control system can continuously scan status of equipment, and automatically moves according to predefined program.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; The running status of vavuum pump, vacuum valve and vacuum line vacuum; Drive and the conveying of demonstration bin and running status; Valve running status between driving and display room; Show each independent vacuum chamber, the family of power and influence's vacuum, pressure and heating-up temperature; Dielectric gas running status, safety valve state; Actual cooling water, power atmospheric pressure, dielectric gas are reported to the police; Alarming and managing; Show all relevant technological parameters (setting value and actual value); Parameter input; Historical technological parameter/data show and store; The all main components of equipment can the operation of transmission display screen.
Can find out by above-described embodiment, rare earth alloy by hydrogen break, Heating Dehydrogenation and process for cooling, improved powder size and distributed and powder particle shape, raising magnet performance is had to significant impact, the automaticity of production improves greatly.
This professional those of ordinary skill should be able to be understood essence of the present invention, and recognizes that specific embodiment of the invention details can make various variations such as for example expanding multiple Heating Dehydrogenations chamber and cooling chamber in claim protection domain. ?

Claims (3)

1. the broken process of RE permanent magnetic alloy hydrogen, is characterized in that: comprise the steps:
1) charging basket that RE permanent magnetic alloy is housed is sent into and is inhaled hydrogen chamber, after closing valve, vacuumize inhaling hydrogen chamber, when vacuum is higher than 50Pa or oxygen content≤0.1%(volume) after, fill hydrogen to-0.05~+ 0.5MPa, keep, after 10 minutes~120 minutes, hydrogen being got rid of; In the time inhaling hydrogen chamber and Heating Dehydrogenation chamber pressure balance, open the separation valve door of inhaling between hydrogen chamber and Heating Dehydrogenation chamber, charging basket is sent to heating clamber, close separation valve door;
2) in the time of Heating Dehydrogenation chamber pressure≤0.1Pa, start heating, the maximum temperature of heating is 500~900 ℃, heat time is 4~20 hours, opens between Heating Dehydrogenation chamber and cooling chamber closing valve after charging basket is sent to cooling chamber by separation valve door in the time of Heating Dehydrogenation chamber and cooling chamber pressure balance;
3) after cooling chamber filling with inert gas, when gas pressure reaches after-0.05~+ 0.5MPa, start blower fan and alloy in charging basket and charging basket is carried out cooling, behind temperature≤120 ℃, equalizing pressure, to atmospheric pressure, is opened discharge door, and charging basket is spread out of.
2. the broken process of the continuous hydrogen of a kind of RE permanent magnetic alloy according to claim 1, is characterized in that: when described heat de-airing chamber arranges more than 2 or 2, step 2) heat time all assigns to each heat de-airing chamber.
3. the broken process of the continuous hydrogen of a kind of RE permanent magnetic alloy according to claim 1, is characterized in that: when described cooling chamber arranges more than 2 or 2, all assign to each cooling chamber the cool time of step 3).
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