CN104226944B

CN104226944B - The manufacture method of two roller cooling vacuum melting rapid hardening equipment and permanent-magnet alloy, permanent magnet

Info

Publication number: CN104226944B
Application number: CN201410461636.6A
Authority: CN
Inventors: 孙宝玉; 陈晓东
Original assignee: SHENYANG ZHONGBEI VACUUM TECHNOLOGY Co Ltd
Current assignee: SHENYANG ZHONGBEI VACUUM TECHNOLOGY Co Ltd
Priority date: 2014-09-12
Filing date: 2014-09-12
Publication date: 2016-06-15
Anticipated expiration: 2034-09-12
Also published as: CN104226944A

Abstract

The invention discloses kind of two cooling vacuum melting rapid hardening equipment and the production methods of roller, equipment comprises melting kettle, tundish, the first rotating roller, the second rotating roller, described melting kettle is arranged on rotating mechanism, by neodymium iron boron raw material heat fused be refined into molten alloy under vacuum or protective condition, by rotation melting kettle, by the molten alloy liquid quiet pouring in crucible in tundish, molten alloy liquid in tundish flows to the outer rim of the first rotating roller by the gap contacting with the first rotating roller, along with rotating roller rotation, molten alloy liquid forms alloy sheet, alloy sheet leaves the first rotating roller and falls in the outer rim of the second rotating roller along with the second rotating roller rotation subsequently, alloy sheet leaves the second rotating roller whereabouts afterwards, form two-sided cooling alloy sheet.

Description

The manufacture method of two roller cooling vacuum melting rapid hardening equipment and permanent-magnet alloy, permanent magnet

Technical field

The invention belongs to rare earth permanent magnet field, particularly relate to a kind of pair of vacuum melting rapid hardening equipment and the production method that roller is cooling; Equipment of the present invention can also be used for rare earth hydrogen storage alloy, vacuum rapid hardening alloy production.

Background technology

Nd-Fe-B rare earth permanent magnetic material, is more and more applied with its good magnetic property, is widely used in medical Magnetic resonance imaging, computer hard disc driver, sound equipment, mobile phone etc.; Along with energy-conservation and requirement low-carbon economy, Nd-Fe-B rare earth permanent magnetic material starts again at auto parts and components, household electrical appliance, energy-conservation and control motor, hybrid vehicle, field of wind power generation application.

Nineteen eighty-three, Japan Patent 1,622, first 492 and 2,137,496 disclose Nd-Fe-B rare earth permanent magnetic material, announced characteristic, composition and the manufacture method of Nd-Fe-B rare earth permanent magnetic material, US Patent No. 6,461,565; US6,491,765; US6,537,385; US6,527,874; US5,645,651 also disclose the manufacture method of Nd-Fe-B rare-earth permanent magnet.

US Patent No. 7,585, the manufacture method of 378 disclosed Nd-Fe-B rare-earth permanent magnet vacuum rapid hardening alloys, this method as shown in Figure 1, neodymium iron boron raw material is cast to tundish 2 after crucible 1 fusing, the aluminium alloy overflowing from tundish forms alloy sheet 4 by the cooling rapid hardening of chill roll 3, and alloy sheet is thrown to the rotating cylinder 5 with heater, and in rotating cylinder, alloy sheet temperature remains on 700-900 DEG C; Afterwards that alloy sheet is cooling; This characteristic feature of an invention is first alloy to be cooled fast to 700-900 DEG C, and then alloy sheet is 700-900 DEG C of insulation, temperature retention time from more than 15 seconds to below 600 seconds; Compare with two roller rapid hardening technology with single roller rapid hardening technology before, this invention is diffused in principal phase heavy rare earth element Dy by insulation, improve the coercivity of magnet, because rapid hardening temperature is higher than 700 DEG C, Grain-Boundary Phase is liquid phase, the variation of Grain-Boundary Phase, can produce the abnormal growth of crystal grain, be difficult to form uniform crystal grain, change from small to big to scope of freedom crystal grain from the roll surface that connects contacting with chill roll, uncontrollable consistent.

Chinese patent CN97,217,372.2 disclose the cooling vacuum rapid hardening equipment of two rods, and as shown in Figure 2, the aluminium alloy of this equipment is cast to by funnel 6 in the gap of chill roll 7 and chill roll 8 and forms alloy sheet 9; This technology belongs to two rod rolling techniques, and because the time of contact of aluminium alloy and chill roll is too short, the temperature of the alloy sheet after two rod rollings is higher than 800 DEG C, although two rod rollings have solved two-sided cooling problem, but do not reach crystal grain thinning, improve crystal grain uniformity, thereby improve coercitive requirement; In order to improve the shortcoming of aforementioned patent, Chinese patent CN01,241,237.6 disclose on the basis of two rod rollings, increase the technology of a chill roll below two rods again, although this invention has improved the performance of aforementioned patent, the thickness of producing alloy sheet is improved, still or two rod rollings, can not solve alloy sheet and leave chill-roll temperature lower than the problem of 700 DEG C, can not reach the object that reduces heavy rare earth consumption.

Summary of the invention

In order to have reduced the consumption of heavy rare earth, reduce the price of Nd-Fe-B rare-earth permanent magnet, need to reduce neodymium iron boron main phase grain size, improve the uniformity of crystallite dimension, improve the distribution of Grain-Boundary Phase; The present invention, by exploring, has found the method for dealing with problems, and has researched and developed new rare earth permanent magnet vacuum melting rapid hardening equipment, and has produced high performance Fe-B rare-earth permanent magnet.

The present invention is achieved through the following technical solutions:

Pair cooling vacuum melting rapid hardening equipment of roller, described vacuum melting rapid hardening equipment comprises vaccum case, melting kettle, tundish, the first rotating roller, the second rotating roller; Described melting kettle is arranged on rotating mechanism, by rotation melting kettle, by the molten alloy liquid quiet pouring in crucible in tundish, molten alloy liquid in tundish flows to the outer rim of the first rotating roller by the gap contacting with the first rotating roller, along with rotating roller rotation, molten alloy liquid forms alloy sheet, alloy sheet leaves the first rotating roller and falls in the outer rim of the second rotating roller along with the second rotating roller rotation subsequently, alloy sheet leaves the second rotating roller whereabouts afterwards, forms two-sided cooling alloy sheet.

Described tundish is in a side of the first rotating roller, and the second rotating roller is at the opposite side of the first rotating roller, and the first described rotating roller is provided with hollow rotating shaft, rotating shaft horizontal positioned; The second described rotating roller is provided with hollow rotating shaft, the shaft parallel of the hollow rotating shaft of the second rotating roller and the first rotating roller, and the rotating shaft of the second rotating roller is lower than the first rotating roller. The first described rotating roller and the second rotating roller are all that both-end supports, there is hollow rotating shaft at the two ends of rotating roller, bearing is installed on hollow rotating shaft, bearings is on bearing spider, the end of hollow rotating shaft is provided with the sealing device of sealing cooling medium, and cooling medium passes in and out rotating roller by sealing device. Described the first rotating roller and the second rotating roller are provided with interlayer, pass into cooling medium in interlayer, and cooling medium is introduced by the endoporus of hollow rotating shaft, the first described rotating roller rotating speed 1-5m/s, the second rotating roller rotating speed 1-5m/s; The diameter range 500-900mm of the first described rotating roller, the second rotating roller diameter 500-900mm.

Below the second described rotating roller, be provided with rotary machine breaker, the below of Mechanical Crushing device is provided with rewinding tank, on rewinding tank, is provided with cooling device, and cooling medium is more than one in water, refrigerant, argon gas, nitrogen.

Described melting kettle, tundish, the first rotating roller, the second rotating roller are arranged in vaccum case, below the second rotating roller, be provided with rotary machine breaker, the below of Mechanical Crushing device is provided with valve, one end of valve is connected with vaccum case, the other end is connected with rewinding tank, rewinding tank can move, and on rewinding tank, is provided with cooling device, and cooling medium is more than one in water, refrigerant, argon gas, nitrogen.

The side blow-on door that described vaccum case comprises horizontal body of heater and two alternation switches, side blow-on door is connected with body of heater by hinge respectively, in side blow-on door inner side, crucible and crucible rotating device are installed, crucible is outside equipped with load coil, load coil is connected with cable, and the other end of cable is connected with vacuum melting heating power supply through fire door; The temperature of described melting kettle is at 1100-1590 DEG C.

Below the second described rotating roller, be provided with rotary machine breaker, breaker below is provided with guide cylinder, there is rewinding case guide cylinder below, and it is indoor that rewinding case is arranged on the rewinding being connected with vaccum case, and the two ends of rewinding chamber are connected with two preparation rooms respectively by valve; Alloy sheet through breaker fragmentation imports the indoor rewinding case of rewinding by the guide cylinder of breaker below; In rewinding case, there is alloy sheet cooling body, when alloy sheet casting, rewinding case moves back and forth, after rewinding completes, the rewinding case that alloy sheet is housed is sent into preparation room by valve and is carried out cooling or heating, and another rewinding case is sent into rewinding chamber from another preparation room again by valve.

A kind of manufacture method of rare earth permanent magnet rapid hardening alloy, first by neodymium iron boron rapid hardening alloy raw material heat fused be refined into molten alloy under vacuum or protective condition, afterwards the aluminium alloy of melting is formed to alloy sheet by trough casting to being with in water-cooled the first rotating roller, alloy sheet is along with rotating roller is rotated, leaving afterwards rotating roller drops to and is with in water-cooled the second rotating roller, leave subsequently rotating roller, form two-sided cooling alloy sheet; First described rotating roller contacts with the one side of alloy sheet, and second rotating roller contacts with the another side of alloy sheet; The thickness 0.1-0.6mm of described alloy sheet; The rotating speed 0.5-5m/s of the first described rotating roller; Described alloy sheet leaves the temperature of the second rotating roller lower than 690 DEG C.

First neodymium iron boron rapid hardening alloy raw material is heated to more than 500 DEG C under vacuum condition, being filled with afterwards argon gas continuation heating is fused into neodymium iron boron raw material alloy and carries out refining, refining temperature is at 1400-1470 DEG C, after refining by the aluminium alloy of melting by trough casting to being with water-cooled first to revolve and form alloy sheet in rotating roller, alloy sheet fall immediately in the second rotating roller, continue cooling, alloy sheet leaves the temperature of the second rotating roller 640-460 DEG C of scope, the first described rotating roller rotating speed 1-3m/s, the second rotating roller rotating speed 1-5m/s.

Described alloy sheet carries out Mechanical Crushing after leaving the second rotating roller, is broken into the alloy sheet that the length of side is less than 15mm, and alloy sheet falls into rewinding case by the guide cylinder with cooling again; Described alloy sheet leaves the temperature of guide cylinder lower than 350 DEG C; Described alloy sheet is cooled to the time of 350 DEG C to be less than 9 seconds.

Described alloy sheet falls into rewinding tank after leaving the second rotating roller, on rewinding tank, is provided with cooling device, and cooling medium is more than one in water, refrigerant, argon gas, nitrogen, and alloy sheet is time of staying 0.5-9 hour in rewinding tank.

Described alloy sheet falls into rewinding tank after leaving the second rotating roller, on rewinding tank, is provided with heater, the heating-up temperature 300-900 DEG C of alloy sheet.

Described alloy sheet falls into rotating cylinder after leaving the second rotating roller, is provided with heater on rotating cylinder, the heating-up temperature 300-900 DEG C of alloy sheet.

A kind of manufacture method of Fe-B rare-earth permanent magnet, first by neodymium iron boron raw material heat fused be refined into molten alloy under vacuum or protective condition, afterwards the aluminium alloy of melting is formed to alloy sheet by trough casting on the outer rim with water-cooled the first rotating roller, alloy sheet is along with rotating roller is rotated, leaving afterwards rotating roller drops in the outer rim with water-cooled the second rotating roller, leave subsequently rotating roller, form two-sided cooling alloy sheet; Then cooled alloy sheet is carried out to hydrogen fragmentation, airflow milling, pressing under magnetic field, sintering, timeliness and make Fe-B rare-earth permanent magnet; Permanent magnet is made Nd-Fe-B rare-earth permanent magnet device through machining, surface treatment again.

The one side of described two-sided cooling alloy sheet contacts with first rotating roller, and another side contacts with second rotating roller; The thickness 0.1-0.6mm of described alloy sheet; The rotating speed 0.5-5m/s of the first described rotating roller, the second rotating roller rotating speed 1-15m/s; Described alloy sheet leaves the temperature of the second rotating roller lower than 700 DEG C.

Before described airflow milling powder, also add Dy₂O₃、Al₂O₃More than one in micro mist.

After described pressing under magnetic field, also have the static pressure operation of grade, wait and magnetic patch is sent into vacuum sintering furnace under protective atmosphere after static pressure and carried out sintering.

A kind of manufacture method of pairing gold Fe-B rare-earth permanent magnet, first by Nd Fe B alloys raw material heat fused be refined into molten alloy under vacuum or protective condition, afterwards the aluminium alloy of melting is formed to alloy sheet by trough casting on the outer rim with water-cooled the first rotating roller, alloy sheet is along with rotating roller is rotated, leaving afterwards rotating roller drops in the outer rim with water-cooled the second rotating roller, leave subsequently rotating roller, form two-sided cooling alloy sheet as the first alloy, the alloy sheet thickness 0.1-0.5mm of the first alloy; Then adopt vacuum melting strip casting to prepare the second alloy, the alloy sheet thickness 0.1-0.4mm of the second alloy; Afterwards the alloy sheet of the first alloy and the second alloy is mixed, after mixing, carry out hydrogen fragmentation, carry out afterwards airflow milling, pressing under magnetic field, sintering and timeliness and make Fe-B rare-earth permanent magnet; Permanent magnet is made Nd-Fe-B rare-earth permanent magnet device through machining, surface treatment again.

The alloy sheet thickness 0.2-0.5mm of the first described alloy, average grain size 2-3.5 μ m, contains Nd, Co, Cu, Al element in alloy sheet; The alloy sheet thickness 0.1-0.3mm of the second described alloy, average grain size 1-2.5 μ m, contains Dy, Co, Cu, Al, Ga, Zr, Mn element in alloy sheet, contain Nd, Dy, Co, Cu, Al, Ga, Zr, Mn element in described permanent magnet.

The alloy sheet thickness 0.1-0.3mm of the first described alloy, average grain size 1-2.5 μ m, contains Dy, Co, Cu, Al, Ga, Zr, Mn element in alloy sheet; The alloy sheet thickness 0.2-0.4mm of the second described alloy, average grain size 2-3.5 μ m, contains Nd, Co, Cu, Al element in alloy sheet, contain Nd, Dy, Co, Cu, Al, Ga, Zr, Mn element in described permanent magnet.

Described Fe-B rare-earth permanent magnet is made up of principal phase and Grain-Boundary Phase, and principal phase has R₂（Fe,Co,Al,Mn）₁₄B structure, wherein principal phase from the heavy rare earth Dy content in inside 1/3 scope of outer rim the heavy rare earth Dy content higher than principal phase center, in Grain-Boundary Phase, there is small Nd₂O₃Particulate; Wherein R represents more than one in the rare earth element that comprises Nd.

Beneficial effect of the present invention:

1. the two rollers of vacuum melting rapid hardening equipment continue two-sided coolingly, leave tundish contact with the first rotating roller to alloy sheet and leave the second rotating roller from aluminium alloy, and the anglec of rotation of being detained in rotating roller is greater than 135 °, and cool time is long, cooling even.

2. while manufacturing rapid hardening alloy, alloy sheet holdup time in rotating roller is long, and carries out two-sided coolingly, and temperature when alloy sheet leaves the second rotating roller is lower than 700 DEG C, crystal grain high conformity, and Grain-Boundary Phase is careful, is evenly distributed.

3, the Fe-B rare-earth permanent magnet that adopts the technology of the present invention to manufacture, the consumption of heavy rare earth Dy is low, and magnetic energy product is high, saves rare heavy rare earth resource, and product cost is low.

Brief description of the drawings

Fig. 1 is existing vacuum melting rapid hardening equipment schematic diagram;

Fig. 2 is the equipment schematic diagram of another kind of prior art;

Fig. 3 is vacuum melting rapid hardening equipment schematic diagram of the present invention;

Fig. 4 is the vacuum melting rapid hardening equipment schematic diagram of another kind of Nd-Fe-B rare-earth permanent magnet rapid hardening alloy of the present invention;

Fig. 5 is another double door vacuum rapid hardening equipment schematic diagram;

Fig. 6 is the rewinding case schematic diagram of another kind of vacuum melting rapid hardening equipment.

Detailed description of the invention

By reference to the accompanying drawings, several vacuum melting rapid hardening equipment and the melting rapid hardening method that in the present invention, relate to are described.

Fig. 1 is existing vacuum melting rapid hardening equipment schematic diagram, as shown in Figure 1, neodymium iron boron raw material is cast to tundish 2 after melting in crucible 1, and the aluminium alloy overflowing from tundish 2 forms alloy sheet 4 by the cooling rapid hardening of chill roll 3, and alloy sheet 4 is thrown to the rotating cylinder 5 with heater.

Fig. 2 is the equipment schematic diagram of another kind of prior art, and as shown in Figure 2, the aluminium alloy of melting is cast to by the aperture of funnel 6 bottoms in the gap of chill roll 7 and chill roll 8 and forms alloy sheet 9, and alloy sheet 9 is collected in the rewinding case of vacuum quick quenching furnace bottom.

Fig. 3 is vacuum melting rapid hardening equipment schematic diagram of the present invention, as shown in Figure 3, neodymium iron boron raw material is fused into molten alloy in vacuum induction heating crucible 10, constant current control is cast in tundish 11, by the gap nozzle on tundish 11 again constant current be cast in the outer rim of the first rotating roller 12 of rotation, the alloy strip 13 of the first rotating roller outer fringe surface is close in formation, alloy strip 13 is along with the first rotating roller 12 is rotated, under the effect of gravity and centrifugal force, depart from the first rotating roller 12, fall in the outer rim of the second rotating roller 14 along with the second rotating roller 14 is rotated, the scope of freedom of alloy strip 13 contacts with the outer fringe surface of the second rotating roller 14, form two-sided cooling alloy sheet, under the effect of gravity and centrifugal force, depart from the second rotating roller 14, fall the crushing mechanism 15 of the second rotating roller 14 belows, alloy sheet is broken into the alloy sheet 16 that maximal side is less than 15mm, alloy sheet 16 is collected afterwards.

Fig. 4 is the vacuum melting rapid hardening equipment schematic diagram of another kind of Nd-Fe-B rare-earth permanent magnet rapid hardening alloy of the present invention, and as shown in Figure 4, equipment comprises vaccum case 19, vacuum unit 29, vacuum induction heating power supply 17; In vaccum case 19, be provided with melting kettle 21, tundish 22, the first rotating roller 23, the second rotating roller 25; Described melting kettle 21 is arranged on rotating mechanism, there is induction coil 20 in melting kettle 21 outsides, form rotating inductor by melting kettle 21, induction coil 20 and fixed part, on inductor, there are axle and support component 30, be supported on vaccum case 19, induction coil 20 is by being connected through the cable 18 of vaccum case 19 and the vacuum induction heating power supply 17 of outside, tundish 22 is in a side of the first rotating roller 23, the second rotating roller 25 is at the opposite side of the first rotating roller 23, the first rotating roller 23 is provided with hollow rotating shaft 52, rotating shaft 52 horizontal positioned; The second rotating roller 25 is provided with the hollow rotating shaft 53 of hollow rotating shaft 53, the second rotating rollers 25 and the rotating shaft 53 of the first rotating roller 23 is parallel, and the rotating shaft 53 of the second rotating roller 25 is lower than the first rotating roller 23; Below the second rotating roller 25, be provided with rotary machine breaker 26, the below of Mechanical Crushing device 26 is provided with valve 28, one end of valve 28 is connected with vaccum case 19, the other end is connected with rewinding tank 27, rewinding tank 27 can move, on rewinding tank 27, be provided with cooling device, cooling medium is more than one in water, refrigerant, argon gas, nitrogen.

Fig. 5 is another double door vacuum rapid hardening equipment schematic diagram, as shown in Figure 5, double door vacuum rapid hardening equipment comprises bedroom vacuum furnace body 38, side blow-on door 31, hinge 32, induction heater 34, support component 33, tundish 35, the first rotating roller 36, the second rotating roller 37, crushing mechanism 39, vacuum valve 40, rewinding case 41; Two side blow-on doors are connected with horizontal vacuum body of heater 38 by hinge respectively, alternation switch; Induction heater 34 comprises crucible, induction coil, insulation material, permeability magnetic material, insulating materials, fixed part, rotating shaft, in the crucible of neodymium iron boron raw material in induction heater 34, melt, induction heater 34 can rotate around the axis, realize the steady constant current of aluminium alloy casting, inductor by supporting units support on side blow-on door 31; Tundish 35 is arranged between induction heater 34 and the first rotating roller 36, approaches the outer rim of the first rotating roller 36 on tundish 35 with the nozzle in gap, and the distance of nozzle and the first rotating roller 36 outer rims is less than 5mm; Be provided with the second rotating roller 37 at the other end of the first rotating roller 36 with respect to tundish 35, the shaft parallel of the rotating shaft of the second rotating roller 37 and the first rotating roller 36, the rotating shaft of the second rotating roller 37 is below the rotating shaft of the first rotating roller 36, distance between the first rotating roller 36 and the second rotating roller 37 is greater than 0.3mm, the first rotating roller 36 and the relative rotation of the second rotating roller 37; Below the second rotating roller 37, be provided with crushing mechanism 39, alloy sheet drops to the rewinding case 41 of crushing mechanism 39 belows after crushing mechanism 39 fragmentations; Rewinding case 41 is connected with vacuum furnace body 38 by valve 40.

Fig. 6 is the rewinding case schematic diagram of another kind of vacuum melting rapid hardening equipment, as shown in Figure 6, alloy sheet through crushing mechanism fragmentation imports the rewinding case 47 in rewinding chamber 46 by the guide cylinder 42 of crushing mechanism 50 belows, in rewinding case 47, there is alloy sheet cooling body, when alloy sheet casting, rewinding case 47 moves back and forth, after rewinding completes, the rewinding case 47 that alloy sheet is housed is sent into the first preparation room 49 by valve 48 and is carried out cooling or heating, another rewinding case 44 is sent into rewinding chamber 46 from the second preparation room 43 again by valve 45, valve-off carries out next furnace operating, loop, described rewinding chamber 46 is connected with vaccum case 51, and the first preparation room 49 is connected with rewinding chamber 46 by valve 48, and the second preparation room 43 is also connected with the other end of rewinding chamber 46 by another valve 45.

Further illustrate remarkable result of the present invention below by the contrast of embodiment.

Embodiment 1

Adopt the manufacture method of a kind of Nd-Fe-B rare-earth permanent magnet rapid hardening alloy of Fig. 4 equipment, first neodymium iron boron raw material 600Kg is added to melting kettle, the heating-up temperature of melting kettle at 1430 DEG C, after refining, be cast to tundish, by the gap of tundish, aluminium alloy quiet pouring is to the first rotating roller, the first rotating roller rotating speed 1.2m/s, the diameter 610mm of the first rotating roller, alloy sheet is along with rotating roller is rotated, 140 ° of the anglec of rotation of alloy sheet in the first rotating roller, fall immediately in the second rotating roller, the scope of freedom contacts with the second rotating roller, form alloy sheet, the second rotating roller rotating speed 1.6m/s, the second rotating roller diameter 610mm, 58 ° of the anglec of rotation of alloy sheet in the second rotating roller, alloy sheet leaves 590 DEG C of the temperature of the second rotating roller, alloy sheet drops on crushing mechanism afterwards, alloy sheet is fractured into the alloy sheet that the length of side is less than 9mm, alloy sheet falls into rewinding tank by the valve of opening afterwards, after charging by rewinding cover upper cover valve-off, afterwards the rewinding tank that alloy sheet is housed is removed, move into again empty rewinding tank and carry out next furnace operating, the rewinding tank temperature of charging is opened rewinding cover during lower than 90 DEG C and is checked alloy sheet, through measuring, alloy sheet is two-sided the vestige contacting with rotating roller, the thickness 0.2-0.23mm of alloy sheet, crystallite dimension 0.24-0.28 μ m, aforesaid rotating roller, rewinding tank are all provided with cooling device, by water quench, and cooling water intake pressure 0.3MPa, the overcoat of aforesaid rotating roller is manufactured by copper alloy, and the direction of rotation of two rotating rollers is contrary, lists the magnetic property of different Dy content of the present invention in table 1 embodiment, and comparative example is the performance that adopts the Nd-Fe-B permanent magnet of conventional single alloy strip casting manufacture.

The Dy content of device fabrication magnet and the relation of magnetic property shown in table 1. comparative example and Fig. 4 of the present invention

Embodiment 2

A kind of method of the pairing gold rare earth permanent magnet rapid hardening alloy that adopts the double door vacuum rapid hardening equipment shown in Fig. 5, first will contain Pr, the neodymium iron boron rapid hardening alloy raw material of Nd packs in the crucible of the induction heater that first side opens the door, close upside blow-on door, after vacuumizing, start heating, be heated to 800 DEG C, being filled with afterwards argon gas continuation heating is fused into neodymium iron boron raw material alloy and carries out refining, refining temperature is at 1440 DEG C, after refining by the aluminium alloy of melting by trough casting to being with water-cooled first to revolve and form alloy sheet in rotating roller, alloy sheet is fallen immediately and in the second rotating roller, is continued cooling formation alloy sheet, alloy sheet leaves the temperature of the first rotating roller 820 DEG C of scopes, the first described rotating roller rotating speed 1m/s, the diameter 810mm of the first rotating roller, 130 ° of the anglec of rotation of alloy sheet in the first rotating roller, fall immediately in the second rotating roller, the scope of freedom contacts with the second rotating roller, form alloy sheet, the second rotating roller rotating speed 1.3m/s, the second rotating roller diameter 810mm, 46 ° of the anglec of rotation of alloy sheet in the second rotating roller, alloy sheet leaves the temperature 640 of the second rotating roller and spends, distance 16mm between the first rotating roller and the second rotating roller, alloy sheet drops on crushing mechanism afterwards, alloy sheet is fractured into the alloy sheet that the length of side is less than 6mm, be called the first alloy, alloy sheet falls into rewinding tank A1 by the valve of opening afterwards, after charging, rewinding tank A1 is closed the lid and valve-off, afterwards the rewinding tank A1 that the first alloy is housed is removed, move into again empty rewinding tank B1, then the neodymium iron boron rapid hardening alloy raw material that contains Dy is packed in the crucible of the induction heater that second side open the door, vacuum furnace body is inflated, after reaching furnace pressure balance, open first side blow-on door, shut second side blow-on door that raw material is housed, repeat last time alloy sheet manufacture method operation, after vacuumizing, start heating, be heated to 900 DEG C, being filled with afterwards argon gas continuation heating is fused into neodymium iron boron raw material alloy and carries out refining, refining temperature is at 1470 DEG C, after refining by the aluminium alloy of melting by trough casting to being with water-cooled first to revolve and form alloy sheet in rotating roller, alloy sheet is fallen immediately and in the second rotating roller, is continued cooling formation alloy sheet, alloy sheet leaves the temperature of the first rotating roller 720 DEG C of scopes, the first described rotating roller rotating speed 2m/s, 120 ° of the anglec of rotation of alloy sheet in the first rotating roller, fall immediately in the second rotating roller, the scope of freedom contacts with the second rotating roller, form alloy sheet, the second rotating roller rotating speed 2.3m/s, 40 ° of the anglec of rotation of alloy sheet in the second rotating roller, alloy sheet leaves the temperature 560 of the second rotating roller and spends, distance 30mm between the first rotating roller and the second rotating roller, alloy sheet drops on crushing mechanism afterwards, alloy sheet is fractured into the alloy sheet that the length of side is less than 4mm, be referred to as the second alloy, the second alloy falls into rewinding tank B1 by the valve of opening afterwards, the rewinding tank temperature of charging is opened rewinding cover during lower than 70 DEG C and is checked alloy sheet, through measuring, the first alloy is two-sided the vestige contacting with rotating roller, the thickness 0.26-0.28mm of alloy sheet, crystallite dimension 2.6-2.9 μ m, the second alloy is two-sided the vestige contacting with rotating roller, the thickness 0.12-0.1.5mm of alloy sheet, crystallite dimension 1.6-1.9 μ m, aforesaid rotating roller, rewinding tank are all provided with cooling device, by water quench, and cooling water intake pressure 0.4MPa, the overcoat of aforesaid rotating roller is manufactured by copper alloy, the direction of rotation of two rotating rollers is contrary, select the first alloy and second alloy of different proportion, the different neodymium iron boron rapid hardening alloys containing Dy amount of configuration, make Fe-B rare-earth permanent magnet through hydrogen fragmentation, airflow milling powder, pressing under magnetic field, sintering and timeliness, the relation of Dy content of the present invention and magnetic property is listed table 2 in, and in table 2, comparative example is the magnet performance that adopts conventional pairing gold process to manufacture.

The Dy content of two alloy magnets of device fabrication and the relation of magnetic property shown in table 2. comparative example and Fig. 5 of the present invention

Embodiment 3

First the raw material that contains table 3 composition is prepared burden respectively by sequence number, raw material is selected in the praseodymium neodymium alloy of market sale, lanthanoid metal, metallic cerium, neodymium metal, terbium metal, gadolinium iron, holmium iron, dysprosium iron, pure iron, ferro-boron, ferro-niobium, gallium, metal zirconium, metallic cobalt, metallic aluminium, metallic copper, pure iron in neodymium iron boron raw material, ferro-boron, metallic cobalt, metallic copper are heated to temperature 300-1500 DEG C scope under vacuum condition, control vacuum 5 × 10³Pa to 5 × 10^-2Pa scope, after time 10-240 minute, is filled with argon gas and adds remaining neodymium iron boron raw material, is heated to afterwards raw material and is melted into molten alloy, under molten condition, becomes two-sided cooling rapid hardening alloy sheet by trough casting, pack alloy sheet into hydrogen crushing furnace, pass into hydrogen and inhale hydrogen by alloy sheet, heat afterwards and vacuumize dehydrogenation, after dehydrogenation, involutory gold plaque is cooling, pack alloy sheet into batch mixer afterwards, before batch mixing, also add containing carbon solvent and air, addition containing carbon solvent is 0.05-0.3wt%, the addition of air is 0.01-0.7wt%, carry out afterwards batch mixing, mixing time is greater than 15 minutes, the laggard row airflow milling powder of batch mixing, carry out afterwards moulding and sintering and make 9 kinds of corrosion-resistant high-performance permanents of table 1 composition, after testing, the O of 9 kinds of corrosion-resistant high-performance permanents, C, N, H, Mn, the content of Si, magnetic property and decay resistance are listed table 4 in. can find out that by table 3 and table 3 Composition Control of the present invention and manufacture method can produce corrosion-resistant high-performance Ne-Fe-B rare-earth permanent magnet.

The constituent content of table 3. Fe-B rare-earth permanent magnet

Content, magnetic property and the decay resistance of O, C in table 4. embodiment 3 Fe-B rare-earth permanent magnets, N, H, Mn, Si

Embodiment 4

First the raw material that contains table 3 composition is prepared burden respectively by sequence number, raw material is selected in praseodymium neodymium alloy, lanthanoid metal, metallic cerium, neodymium metal, terbium metal, metal dysprosium, gadolinium iron, holmium iron, dysprosium iron, pure iron, ferro-boron, ferro-niobium, gallium, metal zirconium, metallic cobalt, metallic aluminium, metallic copper, pack pure iron as raw material, ferro-boron, metallic cobalt, metallic copper into vacuum smelting fast solidification stove afterwards, vacuumize rear beginning eddy-current heating, be heated to temperature 300-1500 DEG C scope, control vacuum 5 × 10³Pa to 5 × 10^-2Pa scope, after time 10-240 minute, be filled with argon gas and add remaining neodymium iron boron raw material, be heated to afterwards raw material and be melted into molten alloy, continuing to be heated to 1450 DEG C of refinings cast after 30 minutes, evenly be cast on water-cooled copper roller and formed alloy sheet by tundish, alloy sheet is cooled to 80 DEG C to come out of the stove below, alloy sheet is sent into vacuum hydrogen crushing furnace and carry out hydrogen fragmentation, after vacuumizing, be filled with hydrogen, after suction hydrogen is saturated, vacuumize and Heating Dehydrogenation, desorption temperature 600-800 DEG C, dehydrogenation stops dehydrogenation to vacuum after higher than 5Pa, is filled with argon gas and carries out argon gas circulation rapid cooling, is cooled to 300 DEG C and is filled with hydrogen, the hydrogen amount of being filled with 0.01-0.1wt%, continues to be cooled to below 80 DEG C afterwards, pack alloy sheet into batch mixer afterwards, then add containing the solvent of C and add oxygen, the addition that contains the solvent of C is 0.05-0.3wt%, the addition of oxygen is 0.01-0.7wt%, mixing time is more than 60 minutes, the laggard row airflow milling powder of batch mixing, the particle mean size 2.0-2.9 μ m of powder process, afterwards powder is sent into the moulding of protective atmosphere Magnetic field press, compact dimensions is that 50 × 40 × 30mm differently-oriented directivity is 30 dimensional directions, after moulding, in press, use thin plastics package, after packaging, send into isostatic pressing machine from press taking-up and wait static pressure, hydrostatic pressure 150MPa, send into afterwards the glove box being connected with vacuum sintering furnace, at the nitrogen protection dress that goes down to substitute, pack magnetic patch into sintering magazine, open valve magazine is sent into vacuum sintering furnace, after being evacuated to 5Pa, start heating, 300 DEG C of insulations 90 minutes, continue to be heated to 800 DEG C of insulations 120 minutes, be heated to again 1020 DEG C of insulations 120 minutes, be heated to again 60 minutes applying argon gas of 1060 DEG C of insulations cooling, carry out high-temperature aging and low temperature aging at 890 DEG C and 460 DEG C afterwards, low temperature aging insulation finishes the rear argon gas rapid cooling of using, come out of the stove below for 80 DEG C, make 9 kinds of corrosion-resistant high-performance permanents of table 1 composition, after testing, 9 kinds of corrosion-resistant high-performance permanents (sequence number 10-18) O, C, N, H, Mn, the content of Si, magnetic property and decay resistance are listed table 3 in. can find out that by table 3 and table 5 Composition Control of the present invention and manufacture method can produce corrosion-resistant high-performance Ne-Fe-B rare-earth permanent magnet.

Content, magnetic property and the decay resistance of O, C in table 5. embodiment 4 Fe-B rare-earth permanent magnets, N, H, Mn, Si

Embodiment 5

First the raw material that contains table 3 composition is prepared burden respectively by sequence number, raw material is selected in the praseodymium neodymium alloy of market sale, lanthanoid metal, metallic cerium, neodymium metal, terbium metal, gadolinium iron, holmium iron, dysprosium iron, pure iron, ferro-boron, ferro-niobium, gallium, metal zirconium, metallic cobalt, metallic aluminium, metallic copper, pure iron in neodymium iron boron raw material, ferro-boron, metallic cobalt, metallic copper are heated to temperature 300-1500 DEG C scope under vacuum condition, control vacuum 5 × 10³Pa to 5 × 10^-2Pa scope, after time 10-240 minute, is filled with argon gas and adds remaining neodymium iron boron raw material, is heated to afterwards raw material and is melted into molten alloy, under molten condition, becomes two-sided cooling rapid hardening alloy sheet by trough casting, pack alloy sheet into hydrogen crushing furnace, pass into hydrogen and inhale hydrogen by alloy sheet, heat afterwards and vacuumize dehydrogenation, after dehydrogenation, involutory gold plaque is cooling, control alloy sheet ingress of air, allow alloy sheet suck quantitative oxygen, pack alloy sheet into batch mixer afterwards, then add dysprosia micro mist, alumina powder, addition is respectively 0.02-0.08wt%, 0.1-0.5wt%, also add the solvent containing C, the addition that contains the solvent of C is 0.05-0.3wt%, carry out afterwards batch mixing, mixing time is more than 60 minutes, the laggard row airflow milling powder of batch mixing, the particle mean size 2.2-2.9 μ m of powder process, afterwards powder is sent into the moulding of protective atmosphere Magnetic field press, compact dimensions is that 50 × 40 × 30mm differently-oriented directivity is 30 dimensional directions, after moulding, in press, use thin plastics package, after packaging, send into isostatic pressing machine from press taking-up and wait static pressure, hydrostatic pressure 150MPa, send into afterwards the glove box being connected with vacuum sintering furnace, at the nitrogen protection dress that goes down to substitute, pack magnetic patch into sintering magazine, open valve magazine is sent into vacuum sintering furnace, after being evacuated to 5Pa, start heating, 300 DEG C of insulations 90 minutes, continue to be heated to 800 DEG C of insulations 120 minutes, be heated to again 1020 DEG C of insulations 120 minutes, be heated to again 60 minutes applying argon gas of 1060 DEG C of insulations cooling, carry out high-temperature aging and low temperature aging at 890 DEG C and 460 DEG C afterwards, low temperature aging insulation finishes the rear argon gas rapid cooling of using, come out of the stove below for 80 DEG C, make 9 kinds of corrosion-resistant high-performance permanents of table 1 composition, after testing, 9 kinds of corrosion-resistant high-performance permanents (sequence number 19-27) O, C, N, H, Mn, the content of Si, magnetic property and decay resistance are listed table 6 in. can find out that by table 3 and table 6 Composition Control of the present invention and manufacture method can produce corrosion-resistant high-performance Ne-Fe-B rare-earth permanent magnet.

Content, magnetic property and the decay resistance of O, C in table 6. embodiment 5 Fe-B rare-earth permanent magnets, N, H, Mn, Si

Embodiment 6

The raw material that contains Nd, Co, Cu, Al composition is prepared burden respectively by 1-9 sequence number, afterwards raw material is packed into two cooling vacuum melting rapid hardening equipment of roller and prepare two-sided cooling rapid hardening alloy sheet as the first alloy; The alloy sheet average grain size of the first alloy is greater than 1.6 μ m, is less than 3.3 μ m; Again the raw material that contains Dy, Co, Cu, Al, Ga, Zr, Mn composition is prepared burden respectively by 1-9 sequence number, afterwards raw material is packed into two cooling vacuum melting rapid hardening equipment of roller and prepare two-sided cooling rapid hardening alloy sheet as the second alloy; The alloy sheet average grain size of the second alloy is greater than 1.1 μ m, is less than 2.9 μ m; First, second described alloy melting all carries out the de-Mn process of vacuum, and de-300-1500 DEG C of scope of Mn process control heating-up temperature, controls vacuum 5 × 10²Pa to 5 × 10^-1Pa scope, temperature retention time 10-180 minute, continue to be afterwards heated to 1430-1470 DEG C of refining, after refining, be cast in the outer rim of water-cooled the first rotating roller and form alloy sheet by the gap of tundish, alloy sheet is along with the first rotating roller is rotated, leaving afterwards rotating roller drops in the outer rim with water-cooled the second rotating roller again along with the second rotating roller rotation, leave afterwards the second rotating roller and fall, form two-sided cooling alloy sheet, described alloy sheet carries out Mechanical Crushing after leaving the second rotating roller, and the alloy sheet after fragmentation imports material collecting device along the guide cylinder with cooling, and alloy sheet leaves the temperature of guide cylinder lower than 390 DEG C, and the maximal side of alloy sheet is less than 13mm, be greater than 0.5 second the cool time of described alloy sheet, is less than 230 seconds, the first alloy and the second alloy are pressed to different ratio proportionings, the composition of the permanent magnet after proportioning meets the composition of table 3, alloy sheet after proportioning is sent into vacuum hydrogen crushing furnace, pass into hydrogen and inhale hydrogen by alloy sheet, heat afterwards and vacuumize dehydrogenation, after dehydrogenation, involutory gold plaque is cooling, controls alloy sheet ingress of air, allows alloy sheet suck quantitative oxygen, pack alloy sheet into batch mixer afterwards, then add dysprosia micro mist, the content 0.1-0.3wt% of dysprosia, also add the solvent containing C, the addition that contains the solvent of C is 0.05-0.3wt%, carry out afterwards batch mixing, mixing time is more than 60 minutes, the laggard row airflow milling powder of batch mixing, the particle mean size 2.2-2.9 μ m of powder process, afterwards powder is sent into the moulding of protective atmosphere Magnetic field press, compact dimensions is that 50 × 40 × 30mm differently-oriented directivity is 30 dimensional directions, after moulding, in press, use thin plastics package, after packaging, send into isostatic pressing machine from press taking-up and wait static pressure, hydrostatic pressure 150MPa, send into afterwards the glove box being connected with vacuum sintering furnace, at the nitrogen protection dress that goes down to substitute, pack magnetic patch into sintering magazine, opening valve sends magazine into vacuum sintering furnace and carries out vacuum-sintering and timeliness, its process has vacuum to take off C, O, N process, de-C temperature 300-650 DEG C, de-C time 120-480 minute, de-O, N temperature 700-950 DEG C, de-O, N time 90-540 minute, carry out afterwards presintering, sintering and timeliness, pre-sintering temperature is lower than sintering temperature 50-90 DEG C, and sintering temperature 1020-1085 DEG C, carries out timeliness after sintering, aging temp 450-950 DEG C, and timeliness is carried out at twice, make 9 kinds of corrosion-resistant high-performance permanents of table 1 composition, after testing, content, magnetic property and the decay resistance of 9 kinds of corrosion-resistant high-performance Ne-Fe-B rare-earth permanent magnets (sequence number 28-36) O, C, N, H, Mn, Si are listed table 7 in. can find out that by table 3 and table 7 Composition Control of the present invention and manufacture method can produce corrosion-resistant high-performance Ne-Fe-B rare-earth permanent magnet, the average grain size 8-14 μ m of described permanent magnet principal phase.

Content, magnetic property and the decay resistance of O, C in table 7. embodiment 6 Fe-B rare-earth permanent magnets, N, H, Mn, Si

Embodiment 7

The raw material that contains Nd, Co, Cu, Al composition is prepared burden respectively by 1-9 sequence number, afterwards raw material is packed into two cooling vacuum melting rapid hardening equipment of roller and prepare two-sided cooling rapid hardening alloy sheet as the first alloy; The alloy sheet average grain size of the first alloy is greater than 2.1 μ m, is less than 3.0 μ m; Again the raw material that contains Dy, Co, Cu, Al, Ga, Zr, Mn composition is prepared burden respectively by 1-9 sequence number, afterwards raw material is packed into two cooling vacuum melting rapid hardening equipment of roller and prepare two-sided cooling rapid hardening alloy sheet as the second alloy; The alloy sheet average grain size of the second alloy is greater than 1.5 μ m, is less than 2.7 μ m; First, second described alloy melting all carries out heating in vacuum, and heating-up temperature, to 400-900 DEG C of scope, is controlled vacuum 5 × 10²Pa to 5 × 10^-1Pa scope, continue to be afterwards heated to 1440-1460 DEG C of refining, after refining, be cast in the outer rim of water-cooled the first rotating roller and form alloy sheet by the gap of tundish, alloy sheet is along with the first rotating roller is rotated, leaving afterwards rotating roller drops in the outer rim with water-cooled the second rotating roller again along with the second rotating roller rotation, leave afterwards the second rotating roller and fall, form two-sided cooling alloy sheet; Described alloy sheet carries out Mechanical Crushing after leaving the second rotating roller, and the alloy sheet after fragmentation imports material collecting device along the guide cylinder with cooling, and alloy sheet leaves the temperature of guide cylinder lower than 340 DEG C, and the maximal side of alloy sheet is less than 10mm; Be greater than 0.5 second the cool time of described alloy sheet, is less than 300 seconds; The first alloy and the second alloy are pressed to different ratio proportionings, the composition of the permanent magnet after proportioning meets the composition of table 1, alloy sheet after proportioning is sent into vacuum hydrogen crushing furnace, pass into hydrogen and inhale hydrogen by alloy sheet, heat afterwards and vacuumize dehydrogenation, after dehydrogenation, involutory gold plaque is cooling, controls alloy sheet ingress of air, allows alloy sheet suck quantitative oxygen; Pack alloy sheet into batch mixer afterwards, then add dysprosia micro mist, the content 0.1-0.3wt% of dysprosia; Also adding the solvent containing C, is 0.05-0.3wt% containing the addition of the solvent of C, carries out afterwards batch mixing, and mixing time is more than 50 minutes, the laggard row airflow milling powder of batch mixing, the particle mean size 2.2-2.9 μ m of powder process; After airflow milling powder, also mix powder, when mixed powder, vacuumize vacuum 500Pa-5 × 10^-2Pa, after vacuumizing, be filled with argon gas, after mixed powder, carry out again after pressing under magnetic field vacuumizes being filled with argon gas, then under argon shield, mix powder, afterwards powder is sent into the moulding of protective atmosphere Magnetic field press, compact dimensions is that 50 × 40 × 30mm differently-oriented directivity is 30 dimensional directions, after moulding, in press, use thin plastics package, after packaging, send into isostatic pressing machine from press taking-up and wait static pressure, hydrostatic pressure 150MPa, send into afterwards the glove box being connected with vacuum sintering furnace, at the nitrogen protection dress that goes down to substitute, pack magnetic patch into sintering magazine, open valve magazine is sent into vacuum sintering furnace, after being evacuated to 5Pa, start heating, 300 DEG C of insulations 90 minutes, continue to be heated to 800 DEG C of insulations 120 minutes, be heated to again 1020 DEG C of insulations 120 minutes, be heated to again 60 minutes applying argon gas of 1060 DEG C of insulations cooling, carry out high-temperature aging and low temperature aging at 890 DEG C and 460 DEG C afterwards, low temperature aging insulation finishes the rear argon gas rapid cooling of using, come out of the stove below for 80 DEG C, after timeliness, carry out machining, after machining, carry out vacuum heat, when heat treatment, add respectively Dy, Tb, Ho, Gd, Y element more than one, vacuum heat temperature 400-940 DEG C, make 9 kinds of corrosion-resistant high-performance permanents of table 3 composition, after testing, content, magnetic property and the decay resistance of 9 kinds of corrosion-resistant high-performance permanents (sequence number 37-45) O, C, N, H, Mn, Si are listed table 8 in. can find out that by table 3 and table 8 Composition Control of the present invention and manufacture method can produce corrosion-resistant high-performance Ne-Fe-B rare-earth permanent magnet, the average grain size 9-14 μ m of described permanent magnet principal phase.

Content, magnetic property and the decay resistance of O, C in table 8. embodiment 7 Fe-B rare-earth permanent magnets, N, H, Mn, Si

Embodiment 8

The raw material that contains Nd, Co, Cu, Al composition is prepared burden respectively by 1-9 sequence number, afterwards raw material is packed into two cooling vacuum melting rapid hardening equipment of roller and prepare two-sided cooling rapid hardening alloy sheet as the first alloy; The alloy sheet average grain size of the first alloy is greater than 1.6 μ m, is less than 3.3 μ m; Again the raw material that contains Dy, Co, Cu, Al, Ga, Zr, Mn composition is prepared burden respectively by 1-9 sequence number, afterwards raw material is packed into two cooling vacuum melting rapid hardening equipment of roller and prepare two-sided cooling rapid hardening alloy sheet as the second alloy; The alloy sheet average grain size of the second alloy is greater than 1.5 μ m, is less than 2.9 μ m; First, second described alloy melting all carries out heating in vacuum, and heating-up temperature 500-850 DEG C of scope controlled vacuum 5 × 10³Pa to 5 × 10^-2Pa scope, continue to be afterwards heated to 1430-1470 DEG C of refining, after refining, be cast in the outer rim of water-cooled the first rotating roller and form alloy sheet by the gap of tundish, alloy sheet is along with the first rotating roller is rotated, leaving afterwards rotating roller drops in the outer rim with water-cooled the second rotating roller again along with the second rotating roller rotation, leave afterwards the second rotating roller and fall, form two-sided cooling alloy sheet, described alloy sheet carries out Mechanical Crushing after leaving the second rotating roller, and the alloy sheet after fragmentation imports material collecting device along the guide cylinder with cooling, and alloy sheet leaves the temperature of guide cylinder lower than 330 DEG C, and the maximal side of alloy sheet is less than 15mm, be greater than 0.5 second the cool time of described alloy sheet, is less than 100 seconds, the first alloy and the second alloy are pressed to different ratio proportionings, the composition of the permanent magnet after proportioning meets the composition of table 1, alloy sheet after proportioning is sent into vacuum hydrogen crushing furnace, pass into hydrogen and inhale hydrogen by alloy sheet, heat afterwards and vacuumize dehydrogenation, after dehydrogenation, involutory gold plaque is cooling, controls alloy sheet ingress of air, allows alloy sheet suck quantitative oxygen, pack alloy sheet into batch mixer afterwards, then add dysprosia micro mist, the content 0.1-0.3wt% of dysprosia, also adding the solvent containing C, is 0.05-0.3wt% containing the addition of the solvent of C, carries out afterwards batch mixing, and mixing time is more than 60 minutes, the laggard row airflow milling powder of batch mixing, the particle mean size 2.2-2.9 μ m of powder process, the mist that the gas that airflow milling powder uses is nitrogen, argon gas and helium, the content of helium in mist is lower than 45%, after airflow milling, mix powder, afterwards powder is sent into the moulding of protective atmosphere Magnetic field press, compact dimensions is that 50 × 40 × 30mm differently-oriented directivity is 30 dimensional directions, after moulding, in press, use thin plastics package, after packaging, send into isostatic pressing machine from press taking-up and wait static pressure, hydrostatic pressure 150MPa, send into afterwards the glove box being connected with vacuum sintering furnace, at the nitrogen protection dress that goes down to substitute, pack magnetic patch into sintering magazine, open valve magazine is sent into vacuum sintering furnace, after being evacuated to 5Pa, start heating, 300 DEG C of insulations 90 minutes, continue to be heated to 800 DEG C of insulations 120 minutes, be heated to again 1020 DEG C of insulations 120 minutes, be heated to again 60 minutes applying argon gas of 1060 DEG C of insulations cooling, carry out high-temperature aging and low temperature aging at 890 DEG C and 460 DEG C afterwards, low temperature aging insulation finishes the rear argon gas rapid cooling of using, come out of the stove below for 80 DEG C, after timeliness, carry out machining, after machining, carry out vacuum passivation, vacuum passivation comprises vacuum and vacuumizes rear heating and thermal insulation process, and holding temperature 100-200 DEG C, is incubated and is filled with air after 5-120 minute, controls vacuum at 10-1000Pa, keeps stopping being filled with air after 5-180 minute, continue afterwards heating and insulation, holding temperature 400-600 DEG C, 9 kinds of corrosion-resistant high-performance Ne-Fe-B rare-earth permanent magnet devices making table 3 composition, after testing, content, magnetic property and the decay resistance of 9 kinds of corrosion-resistant high-performance permanents (sequence number 46-54) O, C, N, H, Mn, Si are listed table 9 in. can find out that by table 3 and table 9 Composition Control of the present invention and manufacture method can produce corrosion-resistant high-performance Ne-Fe-B rare-earth permanent magnet, the average grain size 11-14 μ m of described permanent magnet principal phase, described permanent magnet has corrosion resistant oxide-film.

Content, magnetic property and the decay resistance of O, C in table 9. embodiment 8 Fe-B rare-earth permanent magnets, N, H, Mn, Si

Comparative example

First the raw material that contains table 1 composition is prepared burden respectively by sequence number, raw material is at the praseodymium neodymium alloy of market sale, lanthanoid metal, metallic cerium, neodymium metal, terbium metal, gadolinium iron, holmium iron, dysprosium iron, pure iron, ferro-boron, ferro-niobium, gallium, metal zirconium, metallic cobalt, metallic aluminium, in metallic copper, select, first adopt conventional vacuum melting strip casting to make alloy sheet, pack alloy sheet into hydrogen crushing furnace afterwards, pass into hydrogen and inhale hydrogen by alloy sheet, heat afterwards and vacuumize dehydrogenation, after dehydrogenation, involutory gold plaque is cooling, carry out afterwards airflow milling powder, pressing under magnetic field, vacuum-sintering and timeliness are made 9 kinds of Fe-B rare-earth permanent magnets (sequence number 55-63) of table 1 composition, after testing, the O of 9 kinds of Fe-B rare-earth permanent magnets, C, N, H, Mn, the content of Si, magnetic property and decay resistance are listed table 10 in.

The O of Fe-B rare-earth permanent magnet, C, N, H, Mn, Si content, magnetic property and decay resistance in table 10. comparative example

The result of embodiment 1-8 and comparative example further illustrates of the present invention pair of cooling vacuum rapid hardening equipment and the production method of roller and is applicable to manufacturing rare earth permanent magnet rapid hardening alloy sheet and Fe-B rare-earth permanent magnet, there is obvious advantage to controlling O, C, N, H, Mn, Si content in neodymium iron boron, equipment of the present invention and production method are conducive to produce corrosion-resistant, high-performance Ne-Fe-B permanent magnet, can be used for producing in batches Nd-Fe-B permanent magnet.

Claims

1. the two cooling vacuum melting rapid hardening equipment of roller, is characterized in that: described vacuum melting rapid hardening equipment comprises vaccum case, melting kettle, tundish, the first rotating roller, the second rotating roller; The first rotating roller and the second rotating roller are all provided with hollow rotating shaft, and the hollow rotating shaft of the second rotating roller is below the hollow rotating shaft of the first rotating roller; Described melting kettle is arranged on rotating mechanism, by rotation melting kettle, by the molten alloy liquid quiet pouring in crucible in tundish, molten alloy liquid in tundish flows to the outer rim of the first rotating roller by the gap contacting with the first rotating roller, along with the first rotating roller rotation, molten alloy liquid forms alloy sheet, alloy sheet leaves the first rotating roller and falls in the outer rim of the second rotating roller along with the second rotating roller rotation subsequently, alloy sheet leaves the second rotating roller whereabouts afterwards, forms two-sided cooling alloy sheet;

The rotating speed of the first rotating roller and the second rotating roller is 1-5m/s.

2. the cooling vacuum melting rapid hardening equipment of a kind of pair of roller according to claim 1, it is characterized in that: described tundish is in a side of the first rotating roller, the second rotating roller is at the opposite side of the first rotating roller, and the first described rotating roller is provided with hollow rotating shaft, rotating shaft horizontal positioned; The second described rotating roller is provided with hollow rotating shaft, the shaft parallel of the hollow rotating shaft of the second rotating roller and the first rotating roller, and the rotating shaft of the second rotating roller is lower than the first rotating roller; The first described rotating roller and the second rotating roller are all that both-end supports, there is hollow rotating shaft at the two ends of the first rotating roller and the second rotating roller, the end of hollow rotating shaft is provided with the sealing device of sealing cooling medium, and cooling medium passes in and out the first rotating roller and the second rotating roller by sealing device; Described the first rotating roller and the second rotating roller are provided with interlayer, pass into cooling medium in interlayer, and cooling medium is introduced by the endoporus of hollow rotating shaft, the first described rotating roller rotating speed 1-5m/s, the second rotating roller rotating speed 1-5m/s; The diameter range 500-900mm of the first described rotating roller, the second rotating roller diameter 500-900mm.

3. the cooling vacuum melting rapid hardening equipment of a kind of pair of roller according to claim 1, it is characterized in that: below the second described rotating roller, be provided with rotary machine breaker, the below of Mechanical Crushing device is provided with rewinding tank, on rewinding tank, be provided with cooling device, cooling medium is more than one in water, refrigerant, argon gas, nitrogen.

4. the cooling vacuum melting rapid hardening equipment of a kind of pair of roller according to claim 1, it is characterized in that: described melting kettle, tundish, the first rotating roller, the second rotating roller are arranged in vaccum case, below the second rotating roller, be provided with rotary machine breaker, the below of Mechanical Crushing device is provided with valve, one end of valve is connected with vaccum case, the other end is connected with rewinding tank, rewinding tank can move, on rewinding tank, be provided with cooling device, cooling medium is more than one in water, refrigerant, argon gas, nitrogen.

5. the cooling vacuum melting rapid hardening equipment of a kind of pair of roller according to claim 1, it is characterized in that: the side blow-on door that described vaccum case comprises horizontal body of heater and two alternation switches, side blow-on door is connected with body of heater by hinge respectively, in side blow-on door inner side, crucible and crucible rotating device are installed, crucible is outside equipped with load coil, load coil is connected with cable, and the other end of cable is connected with vacuum melting heating power supply through fire door; The temperature of described melting kettle is at 1100-1590 DEG C.

6. the cooling vacuum melting rapid hardening equipment of a kind of pair of roller according to claim 1, it is characterized in that: below the second described rotating roller, be provided with rotary machine breaker, breaker below is provided with guide cylinder, there is rewinding case guide cylinder below, it is indoor that rewinding case is arranged on the rewinding being connected with vaccum case, and the two ends of rewinding chamber are connected with two preparation rooms respectively by valve; Alloy sheet through breaker fragmentation imports the indoor rewinding case of rewinding by the guide cylinder of breaker below; In rewinding case, there is alloy sheet cooling body, when alloy sheet casting, rewinding case moves back and forth, after rewinding completes, the rewinding case that alloy sheet is housed is sent into preparation room by valve and is carried out cooling or heating, and another rewinding case is sent into rewinding chamber from another preparation room again by valve.

7. the manufacture method of a rare earth permanent magnet rapid hardening alloy, it is characterized in that: first by neodymium iron boron rapid hardening alloy raw material heat fused be refined into molten alloy under vacuum or protective condition, afterwards the aluminium alloy of melting is formed to alloy sheet by trough casting to being with in water-cooled the first rotating roller, alloy sheet is along with the first rotating roller is rotated, leaving afterwards the first rotating roller drops to and is with in water-cooled the second rotating roller, leave subsequently the second rotating roller and fall, form two-sided cooling alloy sheet; First described rotating roller contacts with the one side of alloy sheet, and second rotating roller contacts with the another side of alloy sheet; The thickness 0.1-0.6mm of described alloy sheet; The rotating speed 0.5-5m/s of the first described rotating roller; Described alloy sheet leaves the temperature of the second rotating roller lower than 690 DEG C; The first rotating roller and the second rotating roller are all provided with hollow rotating shaft, and the hollow rotating shaft of the second rotating roller is below the hollow rotating shaft of the first rotating roller.

8. the manufacture method of a kind of rare earth permanent magnet rapid hardening alloy according to claim 7, it is characterized in that: first neodymium iron boron rapid hardening alloy raw material is heated to more than 500 DEG C under vacuum condition, being filled with afterwards argon gas continuation heating is fused into neodymium iron boron raw material alloy and carries out refining, refining temperature is at 1400-1470 DEG C, after refining, the aluminium alloy of melting is formed to alloy sheet by trough casting to being with in water-cooled the first rotating roller, alloy sheet fall immediately in the second rotating roller, continue cooling, alloy sheet leaves the temperature of the second rotating roller 640-460 DEG C of scope, the first described rotating roller rotating speed 1-3m/s, the second rotating roller rotating speed 1-5m/s.

9. the manufacture method of a kind of rare earth permanent magnet rapid hardening alloy according to claim 7, it is characterized in that: described alloy sheet carries out Mechanical Crushing after leaving the second rotating roller, be broken into the alloy sheet that the length of side is less than 15mm, alloy sheet falls into rewinding case by the guide cylinder with cooling again; Described alloy sheet leaves the temperature of guide cylinder lower than 350 DEG C; Described alloy sheet is cooled to the time of 350 DEG C to be less than 9 seconds.

10. the manufacture method of a kind of rare earth permanent magnet rapid hardening alloy according to claim 7, it is characterized in that: described alloy sheet falls into rewinding tank after leaving the second rotating roller, on rewinding tank, be provided with cooling device, cooling medium is more than one in water, refrigerant, argon gas, nitrogen, and alloy sheet is time of staying 0.5-9 hour in rewinding tank.

The manufacture method of 11. a kind of rare earth permanent magnet rapid hardening alloys according to claim 7, is characterized in that: described alloy sheet falls into rewinding tank after leaving the second rotating roller, on rewinding tank, is provided with heater, the heating-up temperature 300-900 DEG C of alloy sheet.

The manufacture method of 12. a kind of rare earth permanent magnet rapid hardening alloys according to claim 7, is characterized in that: described alloy sheet falls into rotating cylinder after leaving the second rotating roller, is provided with heater on rotating cylinder, the heating-up temperature 300-900 DEG C of alloy sheet.

The manufacture method of 13. 1 kinds of Fe-B rare-earth permanent magnets, it is characterized in that: first by neodymium iron boron raw material heat fused be refined into molten alloy under vacuum or protective condition, afterwards the aluminium alloy of melting is formed to alloy sheet by trough casting on the outer rim with water-cooled the first rotating roller, alloy sheet is along with the first rotating roller is rotated, leaving afterwards the first rotating roller drops in the outer rim with water-cooled the second rotating roller, leave subsequently the second rotating roller and fall, form two-sided cooling alloy sheet; Then cooled alloy sheet is carried out to hydrogen fragmentation, airflow milling, pressing under magnetic field, sintering, timeliness and make Fe-B rare-earth permanent magnet; Permanent magnet is made Nd-Fe-B rare-earth permanent magnet device through machining, surface treatment again; The first rotating roller and the second rotating roller are all provided with hollow rotating shaft, and the hollow rotating shaft of the second rotating roller is below the hollow rotating shaft of the first rotating roller; The rotating speed of the first rotating roller is 0.5-5m/s.

The manufacture method of 14. a kind of Fe-B rare-earth permanent magnets according to claim 13, is characterized in that: the one side of described two-sided cooling alloy sheet contacts with first rotating roller, and another side contacts with second rotating roller; The thickness 0.1-0.6mm of described alloy sheet; The rotating speed 0.5-5m/s of the first described rotating roller, the second rotating roller rotating speed 1-15m/s; Described alloy sheet leaves the temperature of the second rotating roller lower than 700 DEG C.

The manufacture method of 15. a kind of Fe-B rare-earth permanent magnets according to claim 13, is characterized in that: before described airflow milling powder, also add Dy₂O₃、Al₂O₃More than one in micro mist.

The manufacture method of 16. a kind of Fe-B rare-earth permanent magnets according to claim 13, is characterized in that: after described pressing under magnetic field, also have the static pressure operation of grade, wait and magnetic patch is sent into vacuum sintering furnace under protective atmosphere after static pressure and carried out sintering.

The manufacture method of 17. 1 kinds of pairing gold Fe-B rare-earth permanent magnets, it is characterized in that: first by Nd Fe B alloys raw material heat fused be refined into molten alloy under vacuum or protective condition, afterwards the aluminium alloy of melting is formed to alloy sheet by trough casting on the outer rim with water-cooled the first rotating roller, alloy sheet is along with the first rotating roller is rotated, leaving afterwards the first rotating roller drops in the outer rim with water-cooled the second rotating roller, leaving subsequently the second rotating roller falls, form two-sided cooling alloy sheet as the first alloy, the alloy sheet thickness 0.1-0.5mm of the first alloy, then adopt vacuum melting strip casting to prepare the second alloy, the alloy sheet thickness 0.1-0.4mm of the second alloy, afterwards the alloy sheet of the first alloy and the second alloy is mixed, after mixing, carry out hydrogen fragmentation, carry out afterwards airflow milling, pressing under magnetic field, sintering and timeliness and make Fe-B rare-earth permanent magnet, permanent magnet is made Nd-Fe-B rare-earth permanent magnet device through machining, surface treatment again, the first rotating roller and the second rotating roller are all provided with hollow rotating shaft, and the hollow rotating shaft of the second rotating roller is below the hollow rotating shaft of the first rotating roller, the rotating speed of the first rotating roller is 0.5-5m/s.

The manufacture method of 18. a kind of pairing gold Fe-B rare-earth permanent magnets according to claim 17, it is characterized in that: the alloy sheet thickness 0.2-0.5mm of the first described alloy, average grain size 2-3.5 μ m, contains Nd, Co, Cu, Al element in alloy sheet; The alloy sheet thickness 0.1-0.3mm of the second described alloy, average grain size 1-2.5 μ m, contains Dy, Co, Cu, Al, Ga, Zr, Mn element in alloy sheet, contain Nd, Dy, Co, Cu, Al, Ga, Zr, Mn element in described permanent magnet.

The manufacture method of 19. a kind of pairing gold Fe-B rare-earth permanent magnets according to claim 17, it is characterized in that: the alloy sheet thickness 0.1-0.3mm of the first described alloy, average grain size 1-2.5 μ m, contains Dy, Co, Cu, Al, Ga, Zr, Mn element in alloy sheet; The alloy sheet thickness 0.2-0.4mm of the second described alloy, average grain size 2-3.5 μ m, contains Nd, Co, Cu, Al element in alloy sheet, contain Nd, Dy, Co, Cu, Al, Ga, Zr, Mn element in described permanent magnet.

The manufacture method of 20. a kind of pairing gold Fe-B rare-earth permanent magnets according to claim 17, is characterized in that: described Fe-B rare-earth permanent magnet is made up of principal phase and Grain-Boundary Phase, and principal phase has R₂（Fe,Co,Al,Mn）₁₄B structure, wherein principal phase from the heavy rare earth Dy content in inside 1/3 scope of outer rim the heavy rare earth Dy content higher than principal phase center, in Grain-Boundary Phase, there is small Nd₂O₃Particulate; Wherein R represents more than one in the rare earth element that comprises Nd.