CN103996521B - A kind of vacuum presintering method and apparatus of Fe-B rare-earth permanent magnet - Google Patents
A kind of vacuum presintering method and apparatus of Fe-B rare-earth permanent magnet Download PDFInfo
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- CN103996521B CN103996521B CN201410194946.6A CN201410194946A CN103996521B CN 103996521 B CN103996521 B CN 103996521B CN 201410194946 A CN201410194946 A CN 201410194946A CN 103996521 B CN103996521 B CN 103996521B
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Abstract
The invention discloses a kind of presintering method and apparatus of Fe-B rare-earth permanent magnet, described vacuum presintering is to carry out in continous vacuum presintering equipment, sintering bin enters the preparation room of continous vacuum presintering equipment successively, degreasing chamber, the first degas chamber, the second degas chamber, the 3rd degas chamber, the first presintering chamber, the second presintering chamber and cooling chamber carry out preheating degreasing, Heating Dehydrogenation is degassed, presintering and cooling, cooling employing argon gas, cooling rear sintering bin takes out and magazine is installed to timeliness bin again from continous vacuum pre-burning freezing of a furnace, timeliness bin plays and sends into continous vacuum sintering aging furnace and carry out sintering, high-temperature aging, pre-cooled, low temperature aging and air cooling fast.
Description
Technical field
The invention belongs to permanent magnet devices field, particularly relate to a kind of vacuum presintering method and apparatus of Fe-B rare-earth permanent magnet.
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-two, first SUMITOMO CHEMICAL particulate metal company disclosed the Japan Patent 1 of Nd-Fe-B rare earth permanent magnetic material, 622,492 and 2,137,496, apply for immediately United States Patent (USP) and European patent, announce characteristic, composition and the manufacture method of Nd-Fe-B rare earth permanent magnetic material, confirm principal phase: Nd2Fe14B phase, Grain-Boundary Phase: rich Nd phase, rich B phase and rare earth oxide impurity.
On April 1st, 2007, Japanese Hitachi Metals and SUMITOMO CHEMICAL metal merged, and had inherited the right and duty of the patent grant of the Fe-B rare-earth permanent magnet of Sumitomo Metal Industries. On August 17th, 2012, Hitachi Metals, for to US International Trade Commission (ITC) litigate, proposes it and has the US6 at U. S. application, 461,565; US6,491,765; US6,537,385; US6,527,874 patents.
Patent CN1187152C is disclosed is the sinter box for rare earth permanent magnet sintering, and patent CN1240088C is disclosed is the method for preparing rare-earth sintering magnet.
Summary of the invention
Prior art is improving magnetic property and is reducing costs Shortcomings, and for this reason, the present invention finds a kind of new manufacture method and equipment.
Along with the expansion of the application market of Nd-Fe-B rare earth permanent magnetic material, the problem of rare earth resources shortage is more and more serious, especially at electronic devices and components, energy-conservation and control the application of motor, auto parts and components, new-energy automobile, field of wind power generation, need more heavy rare earth to improve coercivity. Therefore, how to reduce the use of rare earth, the especially use of heavy rare earth, is the important topic of pendulum in face of us. Through exploring, we have found a kind of high-performance Ne-Fe-B rare earth permanent magnet device making method.
The present invention is achieved through the following technical solutions:
A kind of vacuum presintering method of Fe-B rare-earth permanent magnet, described vacuum presintering is to carry out at continous vacuum pre-burning freezing of a furnace, the magazine that magnetic patch after moulding is housed is contained on sintering bin, under the drive of transmission device, sintering bin enters the preparation room of continous vacuum pre-burning freezing of a furnace successively, degreasing chamber, the first degas chamber, the second degas chamber, the 3rd degas chamber, the first presintering chamber, the second presintering chamber and cooling chamber carry out preheating degreasing, Heating Dehydrogenation is degassed, presintering and cooling, cooling employing argon gas, cooling rear sintering bin takes out and magazine is installed to timeliness bin again from continous vacuum pre-burning freezing of a furnace, timeliness bin plays and sends into the preheating chamber of continous vacuum sintering aging furnace, heating clamber, agglomerating chamber, high-temperature aging chamber, fore-cooling room, low temperature aging chamber and cooling chamber carry out sintering, high-temperature aging, pre-cooled, low temperature aging and air cooling fast.
Described preheating skimming temp scope is at 200-400 DEG C, the degassed temperature range of Heating Dehydrogenation is at 400-900 DEG C, pre-sintering temperature scope is at 900-1050 DEG C, sintering range is at 1010-1085 DEG C, high-temperature aging temperature range is at 800-950 DEG C, low temperature aging temperature range, at 450-650 DEG C, is sent into cooling chamber argon gas or nitrogen rapid cooling after insulation.
Described preheating skimming temp scope is at 200-400 DEG C, the degassed temperature range of Heating Dehydrogenation is at 550-850 DEG C, pre-sintering temperature scope is at 960-1025 DEG C, sintering range is at 1030-1070 DEG C, high-temperature aging temperature range is at 860-940 DEG C, low temperature aging temperature range, at 460-640 DEG C, is sent into cooling chamber argon gas or nitrogen rapid cooling after insulation.
Described presintering vacuum is higher than 5 × 10-1Pa, sintering vacuum is 5 × 10-1Pa to 5 × 10-3Within the scope of Pa.
Described presintering vacuum is higher than 5Pa, and sintering vacuum, in 500Pa to 5000Pa scope, is filled with argon gas when sintering.
The effective width 400-800mm of described sintering bin, the effective width 300-400mm of timeliness bin,
The magnet density scope of described presintering is at 7.2-7.5g/cm3, the magnet density scope of sintering is at 7.5-7.7g/cm3
A kind of continous vacuum presintering equipment of Fe-B rare-earth permanent magnet, its main body is by inlet valve, preparation room, preparation room valve, degreasing chamber, degreasing chamber valve, the first degas chamber, the first degas chamber valve, the second degas chamber, the second degas chamber valve, the 3rd degas chamber, the 3rd degas chamber valve, the first presintering chamber, the first presintering chamber valve, the second presintering chamber, the second presintering chamber valve, cooling chamber and discharge door are formed by connecting, in described preparation room, be provided with heater and live-roller, preparation room is connected with vacuum unit by filter, vacuum unit comprises Roots vaccum pump, oil-sealed rotary pump and valve, in filter, be provided with cold-trap, condenser temperature is lower than 10 DEG C, indoor live-roller, heater, the metallic insulation screen of being provided with of described degreasing, degreasing chamber is connected with vacuum unit by filter, and vacuum unit comprises Roots vaccum pump, oil-sealed rotary pump and valve, is provided with cold-trap in filter, and condenser temperature is lower than 10 DEG C, in described the first degas chamber, the second degas chamber and the 3rd degas chamber, be respectively arranged with live-roller, heater and heat protection screen, the first degas chamber, the second degas chamber and the 3rd degas chamber are connected with vacuum unit respectively, and vacuum unit comprises diffusion pump, Roots vaccum pump, oil-sealed rotary pump and valve, indoor live-roller, heater, the heat protection screen of being respectively arranged with of described the first presintering chamber, the second presintering, the first presintering chamber, the second presintering chamber are connected with vacuum unit respectively, and vacuum unit comprises diffusion pump, Roots vaccum pump, oil-sealed rotary pump and valve, in described cooling chamber, be provided with live-roller, heat exchanger and cooling fan, cooling chamber is connected with vacuum unit, and vacuum unit comprises Roots vaccum pump, oil-sealed rotary pump and valve, and cooling chamber is also connected with gas charging system, and refrigerating gas is argon gas or nitrogen.
The heating-up temperature of described preparation room is the highest 400 DEG C, the heating-up temperature of described degreasing chamber is the highest 500 DEG C, the heating-up temperature of described the first degas chamber, the second degas chamber, the 3rd degas chamber is the highest 900 DEG C, and the first described presintering chamber, the heating-up temperature of the second presintering chamber are the highest 1100 DEG C.
Described continuous vacuum sintering furnace is provided with charging chamber before preparation room, and charging chamber is connected with inlet valve, transmission device is set in charging chamber and has gloves.
Described transmission device comprises roller bearing, and roller bearing is below bin, and the roller bearing of the first degas chamber, the second degas chamber, the 3rd degas chamber, the first presintering chamber, the second presintering chamber is made up of carbon fibre composite, and roller bearing is arranged in heat protection screen.
A kind of Fe-B rare-earth permanent magnet continous vacuum sintering aging furnace, its main body is formed by connecting by feeding gate, preheating chamber, preheating chamber valve, heating clamber, heating clamber valve, agglomerating chamber, agglomerating chamber's valve, high-temperature aging chamber, high-temperature aging chamber valve, fore-cooling room, fore-cooling room's valve, low temperature aging chamber, low temperature aging chamber valve, cooling chamber and discharge door; In described preheating chamber, be provided with guide rail, transfer bogie, timeliness bin, heater, metallic insulation screen, guide rail be arranged on metallic insulation screen above, the roller of transfer bogie rolls on guide rail, and timeliness bin is suspended on the bottom of transfer bogie, and preheating chamber is also connected with vacuum unit; Indoor guide rail, transfer bogie, timeliness bin, heater, the heat protection screen of being respectively arranged with of described heating clamber, agglomerating chamber and high-temperature aging, guide rail be arranged on heat protection screen above, the roller of transfer bogie rolls on guide rail, timeliness bin is suspended on the bottom of transfer bogie, and heating clamber, agglomerating chamber and high-temperature aging chamber are also connected with respectively vacuum unit; In described fore-cooling room, be provided with guide rail, transfer bogie, timeliness bin, heater, heat protection screen, heat exchanger and cooling fan, guide rail be arranged on heat protection screen above, the roller of transfer bogie rolls on guide rail, timeliness bin is suspended on the bottom of transfer bogie, fore-cooling room can heat and can air cooling, when cooling, can be filled with argon gas, fore-cooling room is also connected with vacuum unit; Indoor guide rail, transfer bogie, timeliness bin, heater, the heat protection screen of being provided with of described low temperature aging, guide rail be arranged on heat protection screen above, the roller of transfer bogie rolls on guide rail, and timeliness bin is suspended on the bottom of transfer bogie, and low temperature aging chamber is also connected with vacuum unit; In described cooling chamber, be provided with guide rail, transfer bogie, timeliness bin, heat exchanger and cooling fan, cooling chamber is connected with gas charging system, and refrigerating gas is argon gas or nitrogen, and cooling chamber is also connected with vacuum unit.
The heating-up temperature of described preheating chamber is the highest 600 DEG C; The heating-up temperature of described heating clamber, agglomerating chamber, high-temperature aging chamber is the highest 1100 DEG C; The heating-up temperature of described fore-cooling room is the highest 1100 DEG C, and the heating-up temperature of described low temperature aging chamber is the highest 1100 DEG C;
The effective width of described timeliness bin is within the scope of 260-450mm.
Described agglomerating chamber, high-temperature aging chamber are provided with voltage divider system, and dividing potential drop pressure limit is: 4000-7000Pa.
A manufacture method for Fe-B rare-earth permanent magnet, is characterized in that: first raw material fusing is made to rapid hardening alloy sheet, then carry out hydrogen fragmentation, airflow milling powder and pressing under magnetic field pack magnetic patch into magazine after moulding under nitrogen protection, then magazine are contained on sintering bin, and under the drive of transmission device, sintering bin enters the preparation room of continous vacuum pre-burning freezing of a furnace successively, degreasing chamber, the first degas chamber, the second degas chamber, the 3rd degas chamber, the first presintering chamber, the second presintering chamber and cooling chamber carry out preheating degreasing, Heating Dehydrogenation is degassed, presintering and cooling, cooling employing argon gas, cooling rear sintering bin takes out and magazine is installed to timeliness bin again from continous vacuum pre-burning freezing of a furnace, and timeliness bin plays and sends into the preheating chamber of continous vacuum sintering aging furnace, heating clamber, agglomerating chamber, high-temperature aging chamber, fore-cooling room, low temperature aging chamber and cooling chamber carry out sintering, high-temperature aging, pre-cooled, low temperature aging and air cooling fast, make sintered NdFeB rear-earth permanent magnet, and sintered NdFeB rear-earth permanent magnet is made Nd-Fe-B rare-earth permanent magnet device through machining and surface treatment again.
Described preheating skimming temp scope is at 200-400 DEG C, the degassed temperature range of Heating Dehydrogenation is at 400-900 DEG C, pre-sintering temperature scope is at 900-1050 DEG C, sintering range is at 1020-1080 DEG C, high-temperature aging temperature range is at 850-950 DEG C, low temperature aging temperature range, at 460-640 DEG C, is sent into cooling chamber argon gas or nitrogen rapid cooling after insulation.
Described alloy that raw material is smelted into is made rapid hardening alloy sheet, first R-Fe-B-M raw material is heated to more than 500 DEG C under vacuum condition, is filled with afterwards argon gas continuation heating and R-Fe-B-M raw material is melted and be refined into molten alloy, in this process, adds T2O3Oxide micropowder, afterwards by the aluminium alloy of melting by trough casting to being with in water-cooled rotating roller, form alloy sheet;
Wherein R represents more than one in the rare earth element that comprises Nd;
One or more in M representative element Al, Co, Nb, Ga, Zr, Cu, V, Ti, Cr, Ni, Hf element;
T2O3Represent oxide Dy2O3、Tb2O3、Ho2O3、Y2O3、Al2O3、Ti2O3In one or more;
Described T2O3The addition of oxide micropowder: 0≤T2O3≤2%；
Preferred T2O3The addition of oxide micropowder: 0 < T2O3≤0.8%；
Preferred T2O3Oxide micropowder is Al2O3And Dy2O3In more than one;
Further preferred T2O3Oxide micropowder is Al2O3；
Further preferred T again2O3Oxide micropowder is Dy2O3；
Described alloy that raw material is smelted into is made rapid hardening alloy sheet, first by R-Fe-B-M raw material and T2O3Oxide micropowder is heated to more than 500 DEG C under vacuum condition, be filled with afterwards argon gas continuation heating R-Fe-B-M raw material is fused into alloy, after refining by the aluminium alloy of melting by trough casting to being with in water-cooled rotating roller, molten alloy forms alloy sheet after rotating roller is cooling.
Described involutory gold plaque carries out hydrogen fragmentation and first the alloy sheet of preorder is packed in swing roller, after vacuumizing, be filled with hydrogen by absorption hydrogen, control absorption hydrogen temperature at 20-300 DEG C, then swing roller heat and vacuumize dehydrogenation, dehydrogenation holding temperature 500-900 DEG C, temperature retention time 3-15 hour, insulation stops heating after finishing, it is cooling to cylinder to withdraw heating furnace, and continue swing roller and vacuumize, temperature is lower than 500 DEG C, cooling to cylinder water spray.
Described involutory gold plaque carries out the broken broken equipment of continuous hydrogen that adopts of hydrogen, the material frame of RE permanent magnetic alloy sheet is housed, under the driving of transmission device, order is by suction hydrogen chamber, Heating Dehydrogenation chamber, the cooling chamber of the broken equipment of continuous hydrogen, enter discharge chamber by outlet valve, alloy sheet after hydrogen is broken is derived from material frame, falls into the storage tank of discharge chamber bottom, under nitrogen protection, storage tank is encapsulated, material frame shifts out from the discharge door of discharge chamber, again circular flow after charging; The suction hydrogen temperature 50-350 DEG C of described suction hydrogen chamber, described Heating Dehydrogenation chamber is more than one, desorption temperature 600-900 DEG C, described cooling chamber is more than one.
The described broken equipment of continuous hydrogen has two Heating Dehydrogenation chambers, and material frame stops two Heating Dehydrogenation chambers successively, in time of staying of single Heating Dehydrogenation chamber at 2-6 hour; The broken equipment of described continuous hydrogen has two cooling chambers, and material frame stops at two cooling chambers successively, in time of staying of single cooling chamber at 2-6 hour.
Before finishing, described Heating Dehydrogenation is filled with quantitative hydrogen.
Described batch mixer that storage tank is put into carries out, before front batch mixing, lubricant or antioxidant are added to storage tank.
Described batch mixer that storage tank is put into carries out before front batch mixing T2O3Oxide micropowder adds storage tank.
Before described airflow milling powder, the alloy sheet after hydrogen fragmentation is joined to batch mixer and carries out front batch mixing, when front batch mixing, add antioxidant and lubricant more than one.
Before described airflow milling powder, the alloy sheet after hydrogen fragmentation is joined to batch mixer and carries out front batch mixing, when front batch mixing, add oxide micropowder more than one.
Before described airflow milling powder, the alloy sheet after hydrogen fragmentation is joined to batch mixer and carry out front batch mixing, when front batch mixing, add T2O3Oxide micropowder is Y2O3、Al2O3And Dy2O3In more than one.
Before described airflow milling powder, the alloy sheet after hydrogen fragmentation is joined to batch mixer and carry out front batch mixing, when front batch mixing, add T2O3Oxide micropowder is Y2O3。
Before described airflow milling powder, the alloy sheet after hydrogen fragmentation is joined to batch mixer and carry out front batch mixing, when front batch mixing, add T2O3Oxide micropowder is Al2O3。
Before described airflow milling powder, the alloy sheet after hydrogen fragmentation is joined to batch mixer and carry out front batch mixing, when front batch mixing, add T2O3Oxide micropowder is Dy2O3。
Described airflow milling powder, adopt nitrogen protection airflow milling powder, first broken the hydrogen after batch mixing powder is packed into the hopper of feeder, by feeder, powder is joined to mill chamber, utilize the high velocity air of nozzle ejection to carry out grinding, powder after grinding enters centrifugal separation polling powder with air-flow, the meal that does not reach powder process granularity turns back to mill chamber and continues grinding under the effect of centrifugal force, the fine powder that reaches granularity enters cyclone collector after by separation wheel sorting and collects, a small amount of fine powder can be discharged along with the air-flow of cyclone collector blast pipe, entering rear cyclone collector collects again, the gas that rear cyclone collector is discharged enters into the air inlet pipe of nozzle after cooling again through compressor compresses and cooler, nitrogen circulation is used.
The described powder that enters cyclone collector collection is collected in by the valve of alternation switch in the mixed powder machine of cyclone collector bottom, the powder that enters rear cyclone collector collection is also collected in the mixed powder machine of cyclone collector bottom by the valve of alternation switch, and powder packs rewinding tank into after mixing in mixed powder machine.
The powder that the powder that described cyclone collector is collected and rear cyclone collector are collected imports in rewinding tank by collector.
The described powder that enters rear cyclone collector collection is collected by the rear cyclone collector of 2-6 in parallel.
The described powder that enters rear cyclone collector collection is collected by the rear cyclone collector of 4 in parallel.
After described airflow milling powder, be sent to and on batch mixer, carry out rear batch mixing, the powder mean particle sizes 1.6-2.9 μ m after rear batch mixing.
After described airflow milling powder, be sent to and on batch mixer, carry out rear batch mixing, the powder mean particle sizes 2.1-2.8 μ m after rear batch mixing.
Described pressing under magnetic field method, under nitrogen protection, pack the permanent-magnet rare-earth NdFeB alloy powder of preorder into nitrogen protection lutation magnetic field presser, under nitrogen protection, in lutation magnetic field presser, the material of weighing is put into the mould cavity after assembling, pack seaming chuck into die cavity afterwards, then mould is sent into the orientation space of electromagnet, in alignment magnetic field interval, the alloy powder in mould is pressurizeed and pressurize, then magnetic patch is demagnetized, after demagnetization, hydraulic cylinder resets, afterwards mould is withdrawn into dress powder position, opening mould packs magnetic patch taking-up plastics or gum cover by magnetic patch, and then mould is assembled, cycling, magnetic patch after packaging is put into charging tray and is taken out from lutation magnetic field presser in batches, send into isostatic pressing machine and wait static pressure.
Described semi-automatic pressing under magnetic field, first the batch can that permanent-magnet rare-earth NdFeB alloy powder is housed is docked with the charging aperture of nitrogen protection alignment magnetic field mo(u)ldenpress, after docking by after the Bas Discharged between the charging aperture valve of batch can and semi-automatic press, open the hopper that material inlet valve imports the powder in batch can weighing device, after weighing, powder is sent in the die cavity of mould automatically, after dust feeder leaves, cylinder pressure on press is moved down, enter after die cavity the powder orientation that magnetizes, under magnetic field to powder extrusion forming, afterwards the magnetic patch of moulding is demagnetized and magnetic patch is ejected from die cavity, then magnetic patch is taken out to the material platform of putting into nitrogen protection alignment magnetic field mo(u)ldenpress, magnetic patch is packed with plastics or gum cover by gloves, packaged magnetic patch is put into charging tray and is taken out in batches, send into isostatic pressing machine and wait static pressure.
Described static pressure such as grade is packaged magnetic patch to be placed in to isostatic pressing machine have in a high-pressure chamber, and in cavity, remaining space is full of with hydraulic oil, and after sealing, to hydraulic oil pressurization in cavity, pressurization maximum pressure scope 150-300MPa, after pressure release takes out magnetic patch.
Described isostatic pressing machine has two high-pressure chambers, a cavity is enclosed within the outside of another cavity, form an inner chamber body and an outer chamber, pack into wrapped magnetic patch in the inner chamber body of isostatic pressing machine, in inner chamber body, remaining space is full of liquid medium, the outer chamber of isostatic pressing machine is filled with hydraulic oil, be connected with the device that produces high pressure, the hydraulic fluid pressure of outer chamber by and inner chamber body between spacer pass to inner chamber body, inner chamber body also produces high pressure, the pressure limit 150-300MPa of inner chamber body thereupon.
Described automatic pressing under magnetic field method, first the batch can that permanent-magnet rare-earth NdFeB alloy powder is housed is docked with the charging aperture of nitrogen protection alignment magnetic field mo(u)ldenpress, after docking by after the Bas Discharged between the charging aperture valve of batch can and mo(u)ldenpress, open the hopper that material inlet valve imports the powder in batch can weighing device, after weighing, powder is sent in the die cavity of mould automatically, after dust feeder leaves, cylinder pressure on press is moved down, enter after die cavity the powder orientation that magnetizes, then to powder extrusion forming, afterwards the magnetic patch of moulding is demagnetized and magnetic patch is ejected from die cavity, then magnetic patch is taken out to the magazine of putting into nitrogen protection alignment magnetic field mo(u)ldenpress, magazine after filling closes the lid magazine, again magazine is put on charging tray, after charging tray is filled, the charging tray of filling magazine under nitrogen protection, is sent to transmission seal box by the discharge valve of opening nitrogen protection sealing magnetic field mo(u)ldenpress, then under nitrogen protection, dock with the protection material feeding box of vacuum sintering furnace transmitting seal box, the charging tray of filling magazine is sent into the protection material feeding box of vacuum sintering furnace.
Electromagnet pole and the field coil of described nitrogen protection lutation magnetic field presser are connected with cooling medium, and cooling medium is water, oil or cold-producing medium, and the space temperature of the placement mould being made up of electromagnet pole and field coil when moulding is lower than 25 DEG C.
Described cooling medium is water, oil or cold-producing medium, the space temperature of the placement mould being formed by electromagnet pole and field coil when moulding lower than 5 DEG C higher than-10 DEG C. Described to powder extrusion forming, briquetting pressure scope 100-300MPa.
Described Nd-Fe-B permanent magnet is made up of principal phase and Grain-Boundary Phase, and principal phase has R2（Fe,Co）14B structure, wherein principal phase from the heavy rare earth HR content in inside 1/3 scope of outer rim the heavy rare earth HR content higher than principal phase center, in Grain-Boundary Phase, there is the oxide fine particle of neodymium, R represent comprise Nd rare earth element more than one, HR represents more than one in Dy, Tb, Ho, Y rare earth element.
The structure of described Nd-Fe-B permanent magnet has at R2（Fe1-xCox）14The surrounding of B crystal grain surrounds heavy rare earth content higher than R2（Fe1-xCox）14The ZR of B phase2（Fe1-xCox）14The structure of B phase, ZR2（Fe1-xCox）14B phase and R2（Fe1-xCox）14Between B without Grain-Boundary Phase, ZR2（Fe1-xCox）14Between B phase, connect by Grain-Boundary Phase; In literary composition, ZR is illustrated in the rare earth higher than the phase of the content of the heavy rare earth in average content of rare earth of heavy rare earth content in crystalline phase; 0≤x≤0.5.
More than two ZR in the structure of described Nd-Fe-B permanent magnet2（Fe1-xCox）14The oxide fine particle that has neodymium in the Grain-Boundary Phase of the intersection of B phase crystal grain, the oxygen content of crystal boundary is higher than the oxygen content of principal phase.
The crystallite dimension 5-15 μ m of the sintered Nd-Fe-B permanent magnet that the manufacture method of described sintered Nd-Fe-B permanent magnet is manufactured, preferably 5-9 μ m.
Brief description of the drawings
Fig. 1 is continous vacuum presintering equipment principle schematic front view of the present invention.
Fig. 2 is continous vacuum presintering equipment principle diagrammatic top view of the present invention.
Fig. 3 is continous vacuum sintering aging furnace principle schematic front view of the present invention.
Fig. 4 is continous vacuum sintering aging furnace principle diagrammatic top view of the present invention.
In figure: 1, inlet valve; 2, preparation room; 3, preparation room valve; 4, dewaxing chamber; 5, dewaxing chamber valve; 6, the first degas chamber; 7, the first degas chamber valve; 8, the second degas chamber; 9, the second degas chamber valve; 10, the 3rd degas chamber; 11, the 3rd degas chamber valve; 12, the first presintering chamber; 13, the first presintering chamber valve; 14, the second presintering chamber; 15, the second presintering chamber valve; 16, cooling chamber; 17, discharge door; 18,21,24,27,30,33,36 is heater; 19,20,23,26,29,32,35,38 is live-roller; 22, metallic insulation screen; 25,28,31,34,37 is heat protection screen; 39, heat exchanger; 40, cooling fan; 41, feeding gate; 42, preheating chamber; 43, preheating chamber valve; 44, heating clamber; 45, heating clamber valve; 46, agglomerating chamber; 47, agglomerating chamber's valve; 48, high-temperature aging chamber; 49, high-temperature aging chamber valve; 50, fore-cooling room; 51, fore-cooling room's valve; 52, low temperature aging chamber; 53, low temperature aging chamber valve; 54, cooling chamber; 55, discharge door; 56,60,65,70,75,82,87 is guide rail; 57,61,66,71,76,83,88 is transfer bogie; 58,62,67,72,77,84,89 is timeliness bin; 59,63,68,73,80,85 is heater; 64,69,74,81,86 is heat protection screen; 78,90 is heat exchanger; 79,91 is cooling fan; 92 is metallic insulation screen.
A kind of continous vacuum presintering equipment of Fe-B rare-earth permanent magnet, its main body is by inlet valve 1, preparation room 2, preparation room valve 3, degreasing chamber 4, degreasing chamber valve 5, the first degas chamber 6, the first degas chamber valve 7, the second degas chamber 8, the second degas chamber valve 9, the 3rd degas chamber 10, the 3rd degas chamber valve 11, the first presintering chamber 12, the first presintering chamber valve 13, the second presintering chamber 14, the second presintering chamber valve 15, cooling chamber 16 and discharge door 17 are formed by connecting, in described preparation room 1, be provided with heater 18 and live-roller 19, preparation room is connected with vacuum unit by filter, vacuum unit comprises Roots vaccum pump, oil-sealed rotary pump and valve, in filter, be provided with cold-trap, condenser temperature is lower than 10 DEG C, indoor live-roller 20, heater 21, the metallic insulation screen 22 of being provided with of described degreasing, degreasing chamber 4 is connected with vacuum unit by filter, vacuum unit comprises Roots vaccum pump, oil-sealed rotary pump and valve, is provided with cold-trap in filter, and condenser temperature is lower than 10 DEG C, in the first described degas chamber 6, be provided with live-roller 23, heater 24 and heat protection screen 25, the first degas chambers 6 and be connected with vacuum unit, vacuum unit comprises diffusion pump, Roots vaccum pump, oil-sealed rotary pump and valve, in the second described degas chamber 8, be provided with live-roller 26, heater 27, heat protection screen 28, the second degas chambers 8 and be connected with vacuum unit, vacuum unit comprises diffusion pump, Roots vaccum pump, oil-sealed rotary pump and valve, in the 3rd described degas chamber 10, be provided with live-roller 29, heater 30, heat protection screen 31, the three degas chambers 10 and be connected with vacuum unit, vacuum unit comprises diffusion pump, Roots vaccum pump, oil-sealed rotary pump and valve, in the first described presintering chamber 12, be provided with live-roller 32, heater 33, heat protection screen 34, the first presintering chambers 12 and be connected with vacuum unit, vacuum unit comprises diffusion pump, Roots vaccum pump, oil-sealed rotary pump and valve, in the second described presintering chamber 14, be provided with live-roller 35, heater 36, heat protection screen 37, the second presintering chambers 14 and be connected with vacuum unit, vacuum unit comprises diffusion pump, Roots vaccum pump, oil-sealed rotary pump and valve, in described cooling chamber 16, be provided with live-roller 38, heat exchanger 39 and cooling fan 40, cooling chamber 16 is connected with vacuum unit, vacuum unit comprises Roots vaccum pump, oil-sealed rotary pump and valve, and cooling chamber 16 is also connected with gas charging system, and refrigerating gas is argon gas or nitrogen.
A kind of Fe-B rare-earth permanent magnet continous vacuum sintering aging furnace, its main body is formed by connecting by feeding gate 41, preheating chamber 42, preheating chamber valve 43, heating clamber 44, heating clamber valve 45, agglomerating chamber 46, agglomerating chamber's valve 47, high-temperature aging chamber 48, high-temperature aging chamber valve 49, fore-cooling room 50, fore-cooling room's valve 51, low temperature aging chamber 52, low temperature aging chamber valve 53, cooling chamber 54 and discharge door 55; In described preheating chamber 42, be provided with guide rail 56, transfer bogie 57, timeliness bin 58, heater 59, metallic insulation screen 92, guide rail 56 be arranged on metallic insulation screen 92 above, the roller of transfer bogie 57 rolls on guide rail 56, timeliness bin 58 is suspended on the bottom of transfer bogie 57, and preheating chamber 42 is also connected with vacuum unit; In described heating clamber 44, be provided with guide rail 60, transfer bogie 61, timeliness bin 62, heater 63, heat protection screen 64, guide rail 60 be arranged on heat protection screen 64 above, the roller of transfer bogie 61 rolls on guide rail 60, timeliness bin 62 is suspended on the bottom of transfer bogie 61, and heating clamber 44 is also connected with vacuum unit; In described agglomerating chamber 46, be provided with guide rail 65, transfer bogie 66, timeliness bin 67, heater 68, heat protection screen 69, guide rail 65 be arranged on heat protection screen 69 above, the roller of transfer bogie 66 rolls on guide rail 65, timeliness bin 67 is suspended on the bottom of transfer bogie 66, and agglomerating chamber 46 is also connected with vacuum unit; In described high-temperature aging chamber 48, be provided with guide rail 70, transfer bogie 71, timeliness bin 72, heater 73, heat protection screen 74, guide rail 70 be arranged on heat protection screen 74 above, the roller of transfer bogie 71 rolls on guide rail 70, timeliness bin 72 is suspended on the bottom of transfer bogie 71, and high-temperature aging chamber 48 is also connected with vacuum unit; In described fore-cooling room 50, be provided with guide rail 75, transfer bogie 76, timeliness bin 77, heater 80, heat protection screen 81, heat exchanger 78 and cooling fan 79, guide rail 75 be arranged on heat protection screen 81 above, the roller of transfer bogie 76 rolls on guide rail 75, timeliness bin 77 is suspended on the bottom of transfer bogie 76, fore-cooling room 50 can heat and can air cooling, when cooling, can be filled with argon gas, fore-cooling room 50 is also connected with vacuum unit; In described low temperature aging chamber 52, be provided with guide rail 82, transfer bogie 83, timeliness bin 84, heater 85, heat protection screen 86, guide rail 82 be arranged on heat protection screen 86 above, the roller of transfer bogie 83 rolls on guide rail 82, timeliness bin 84 is suspended on the bottom of transfer bogie 83, and low temperature aging chamber 52 is also connected with vacuum unit; In described cooling chamber 54, be provided with guide rail 87, transfer bogie 88, timeliness bin 89, heat exchanger 90 and cooling fan 91, cooling chamber 54 is connected with gas charging system, and refrigerating gas is argon gas or nitrogen, and cooling chamber 54 is also connected with vacuum unit.
Detailed description of the invention
Further illustrate remarkable result of the present invention below by the contrast of embodiment.
Embodiment 1
Press composition Nd30Dy1Co1.2Cu0.1Ｂ0.9Al0.1FeSurplusChoose raw material 600Kg heat fused, add oxide Dy2O3Micro mist, under molten condition by alloy casting to being with cooling formation alloy sheet on water-cooled rotation copper roller, use the broken equipment hydrogen of continuous hydrogen broken, first the R-Fe-B-M alloy sheet of preorder is packed into the charging basket playing, order is sent into the suction hydrogen chamber of continuous hydrogen crushing furnace, Heating Dehydrogenation chamber, cooling chamber is inhaled respectively hydrogen, Heating Dehydrogenation and cooling, then the alloy after hydrogen is broken under protective atmosphere packs storage tank into, after hydrogen fragmentation, carry out batch mixing, after batch mixing, adopt nitrogen protection airflow milling to carry out airflow milling powder, under nitrogen protection with delivering to the moulding of nitrogen protection lutation magnetic field presser after batch mixer batch mixing, magnetic patch size 62 × 52 × 42mm, differently-oriented directivity is 42 dimensional directions, after shaping, in guard box, encapsulate, then take out and wait static pressure, carry out afterwards vacuum presintering, described vacuum presintering is to carry out at continous vacuum pre-burning freezing of a furnace, the magazine that magnetic patch after moulding is housed is contained on sintering bin, and under the drive of transmission device, sintering bin enters the preparation room of continous vacuum pre-burning freezing of a furnace successively, degreasing chamber, the first degas chamber, the second degas chamber, the 3rd degas chamber, the first presintering chamber, the second presintering chamber and cooling chamber carry out preheating degreasing, Heating Dehydrogenation is degassed, presintering and cooling, cooling employing argon gas, cooling rear sintering bin takes out and magazine is installed to timeliness bin again from continous vacuum pre-burning freezing of a furnace, and timeliness bin plays and sends into the preheating chamber of continous vacuum sintering aging furnace, heating clamber, agglomerating chamber, high-temperature aging chamber, fore-cooling room, low temperature aging chamber and cooling chamber carry out sintering, high-temperature aging, pre-cooled, low temperature aging and air cooling fast. make sintered Nd-Fe-B permanent magnet, take out and carry out machining afterwards, be processed into square piece 50 × 30 × 20mm, after electroplating, make rare earth permanent magnet device, test result is listed table one in.
Embodiment 2
Press composition Nd30Dy1Co1.2Cu0.1Ｂ0.9Al0.1FeSurplusChoose alloy 600Kg heat fused, under molten condition by alloy casting to being with cooling formation alloy sheet on water-cooled rotation copper roller; Use the broken equipment of continuous hydrogen to carry out hydrogen fragmentation, after hydrogen fragmentation, carry out batch mixing, when batch mixing, add oxide Y2O3Micro mist and lubricant, the nitrogen protection airflow milling that adopts the present invention to have cyclone collector after 3 after batch mixing is carried out airflow milling powder, under nitrogen protection, seal magnetic field semi-automatic press moulding with delivering to nitrogen protection after batch mixer batch mixing, magnetic patch size 62 × 52 × 42mm, differently-oriented directivity is 42 dimensional directions, after shaping, in guard box, encapsulate, then take out and wait static pressure, carry out afterwards vacuum presintering, described vacuum presintering is to carry out preheating degreasing at continous vacuum pre-burning freezing of a furnace, Heating Dehydrogenation is degassed, presintering and cooling, send into again afterwards continous vacuum sintering aging furnace and carry out sintering, high-temperature aging, pre-cooled, low temperature aging and air cooling fast, described preheating skimming temp scope is at 210-290 DEG C, the degassed temperature range of Heating Dehydrogenation is at 610-690 DEG C, pre-sintering temperature scope is at 960-990 DEG C, sintering range is at 1020-1045 DEG C, high-temperature aging temperature range is at 850-950 DEG C, low temperature aging temperature range is at 450-650 DEG C, after insulation, send into cooling chamber argon gas rapid cooling, make sintered Nd-Fe-B permanent magnet, take out and carry out machining afterwards, be processed into square piece 50 × 30 × 20mm, after electroplating, make rare earth permanent magnet device, test result is listed table one in.
Embodiment 3
Press composition Nd30Dy1Co1.2Cu0.1Ｂ0.9Al0.1FeSurplusChoose raw material 600Kg heat fused, under molten condition by alloy casting to being with cooling formation alloy sheet on water-cooled rotation copper roller; Use vacuum hydrogen crushing furnace hydrogen broken, after hydrogen fragmentation, carry out batch mixing, when batch mixing, add oxide Al2O3Micro mist, the nitrogen protection airflow milling that adopts the present invention to have cyclone collector after 4 after batch mixing is carried out airflow milling powder, airflow milling atmosphere oxygen content 0-20ppm, under nitrogen protection, seal magnetic field mo(u)ldenpress moulding with delivering to nitrogen protection after batch mixer batch mixing, oxygen content 0-20ppm in guard box, alignment magnetic field 1.9T, mould cavity temperature 0-4 DEG C, magnetic patch size 62 × 52 × 42mm, differently-oriented directivity is 42 dimensional directions, after shaping, carry out vacuum presintering, described vacuum presintering is to carry out preheating degreasing at continous vacuum pre-burning freezing of a furnace, Heating Dehydrogenation is degassed, presintering and cooling, send into again afterwards continous vacuum sintering aging furnace and carry out sintering, high-temperature aging, pre-cooled, low temperature aging and air cooling fast, described preheating skimming temp scope is at 310-340 DEG C, the degassed temperature range of Heating Dehydrogenation is at 610-640 DEG C, pre-sintering temperature scope is at 1010-1030 DEG C, sintering range is at 1055-1075 DEG C, high-temperature aging temperature range is at 910-940 DEG C, low temperature aging temperature range is at 460-640 DEG C, after insulation, send into cooling chamber argon gas rapid cooling, make sintered Nd-Fe-B permanent magnet, take out and carry out machining afterwards, be processed into square piece 50 × 30 × 20mm, after electroplating, make rare earth permanent magnet device, test result is listed table one in.
Embodiment 4
Press composition Nd30Dy1Co1.2Cu0.1Ｂ0.9Al0.1FeSurplusChoose raw material 600Kg heat fused, under molten condition by alloy casting to being with cooling formation alloy sheet on water-cooled rotation copper roller; Use vacuum hydrogen crushing furnace hydrogen broken, after hydrogen fragmentation, carry out batch mixing, when batch mixing, add oxide Dy2O3Micro mist, the nitrogen protection airflow milling that adopts the present invention to have cyclone collector after 5 after batch mixing is carried out airflow milling powder, airflow milling atmosphere oxygen content 0-18ppm, under nitrogen protection with delivering to the moulding of nitrogen protection lutation magnetic field presser after batch mixer batch mixing, magnetic patch size 62 × 52 × 42mm, differently-oriented directivity is 42 dimensional directions, after shaping, in guard box, encapsulate, then take out and wait static pressure, after hydrostatic pressure 240-300MPa, carry out vacuum presintering, described vacuum presintering is to carry out preheating degreasing at continous vacuum pre-burning freezing of a furnace, Heating Dehydrogenation is degassed, presintering and cooling, send into again afterwards continous vacuum sintering aging furnace and carry out sintering, high-temperature aging, pre-cooled, low temperature aging and air cooling fast, described preheating skimming temp scope is at 320-340 DEG C, the degassed temperature range of Heating Dehydrogenation is at 660-690 DEG C, pre-sintering temperature scope is at 1010-1040 DEG C, sintering range is at 1050-1085 DEG C, high-temperature aging temperature range is at 850-940 DEG C, low temperature aging temperature range is at 460-640 DEG C, after insulation, send into cooling chamber argon gas rapid cooling, make sintered Nd-Fe-B permanent magnet, take out and carry out machining afterwards, be processed into square piece 50 × 30 × 20mm, after electroplating, make rare earth permanent magnet device, test result is listed table one in.
Embodiment 5
Press composition Nd30Dy1Co1.2Cu0.1Ｂ0.9Al0.1FeSurplusChoose raw material 600Kg heat fused, under molten condition by alloy casting to being with cooling formation alloy sheet on water-cooled rotation copper roller, adopt the fragmentation of vacuum hydrogen crushing furnace, hydrogen fragmentation adopts the present invention to have the nitrogen protection airflow milling powder of cyclone collector after 6 afterwards, airflow milling atmosphere oxygen content 0-20ppm, under nitrogen protection, seal magnetic field mo(u)ldenpress moulding with delivering to nitrogen protection after batch mixer batch mixing, oxygen content 10-150ppm in guard box, alignment magnetic field 1.8T, mould cavity temperature 0-14 DEG C, magnetic patch size 62 × 52 × 42mm, differently-oriented directivity is 42 dimensional directions, after shaping, in guard box, encapsulate, then take out and wait static pressure, after hydrostatic pressure 210-240MPa, carry out vacuum presintering, described vacuum presintering is to carry out preheating degreasing at continous vacuum pre-burning freezing of a furnace, Heating Dehydrogenation is degassed, presintering and cooling, send into again afterwards continous vacuum sintering aging furnace and carry out sintering, high-temperature aging, pre-cooled, low temperature aging and air cooling fast, described preheating skimming temp scope is at 355-390 DEG C, the degassed temperature range of Heating Dehydrogenation is at 710-790 DEG C, pre-sintering temperature scope is at 1010-1020 DEG C, sintering range is at 1030-1085 DEG C, high-temperature aging temperature range is at 860-940 DEG C, low temperature aging temperature range is at 460-640 DEG C, after insulation, send into cooling chamber argon gas rapid cooling, make sintered Nd-Fe-B permanent magnet, take out and carry out machining afterwards, be processed into square piece 50 × 30 × 20mm, after electroplating, make rare earth permanent magnet device, test result is listed table one in.
Comparative example
Press composition Nd30Dy1Co1.2Cu0.1Ｂ0.9Al0.1FeSurplusChoose alloy 600Kg heat fused, under molten condition by alloy casting to cooling formation alloy sheet on the chill roll with water-cooled rotation, then use the involutory gold plaque of vacuum hydrogen crushing furnace to carry out coarse crushing, after hydrogen fragmentation, carry out the airflow milling of prior art, deliver to afterwards the pressing under magnetic field press-molding of current techique, magnetic patch size 62 × 52 × 42mm, differently-oriented directivity is 42 dimensional directions, after shaping, in guard box, encapsulate, then take out and wait static pressure, hydrostatic pressure 210MPa, carries out sintering and timeliness afterwards, makes sintered Nd-Fe-B permanent magnet; Take out and carry out machining afterwards, be processed into square piece 50 × 30 × 20mm, after electroplating, make rare earth permanent magnet device.
The performance measurement result of table one, embodiment and comparative example:
By relatively further illustrating of embodiment and comparative example, adopt technology and equipment of the present invention obviously to improve magnetic property and the decay resistance of magnet, be the technology and equipment technology that has very much development.
Claims (19)
1. the vacuum presintering method of a Fe-B rare-earth permanent magnet, it is characterized in that: described vacuum presintering is to carry out at continous vacuum presintering equipment, the magazine that magnetic patch after moulding is housed is contained on sintering bin, under the drive of transmission device, sintering bin enters the preparation room of continous vacuum presintering equipment successively, degreasing chamber, the first degas chamber, the second degas chamber, the 3rd degas chamber, the first presintering chamber, the second presintering chamber and cooling chamber carry out preheating degreasing, Heating Dehydrogenation is degassed, presintering and cooling, cooling rear sintering bin takes out and magazine is installed to timeliness bin again from continous vacuum presintering equipment, timeliness bin plays and sends into the preheating chamber of continous vacuum sintering aging furnace, heating clamber, agglomerating chamber, high-temperature aging chamber, fore-cooling room, low temperature aging chamber and cooling chamber carry out sintering, high-temperature aging, pre-cooled, low temperature aging and air cooling fast,
Preheating skimming temp scope is at 200-400 DEG C, the degassed temperature range of Heating Dehydrogenation is at 400-900 DEG C, pre-sintering temperature scope is at 900-1050 DEG C, sintering range is at 1010-1085 DEG C, high-temperature aging temperature range is at 800-950 DEG C, low temperature aging temperature range, at 450-650 DEG C, is sent into cooling chamber argon gas or nitrogen rapid cooling after insulation.
2. the vacuum presintering method of a kind of Fe-B rare-earth permanent magnet according to claim 1, it is characterized in that: described preheating skimming temp scope is at 200-400 DEG C, the degassed temperature range of Heating Dehydrogenation is at 550-850 DEG C, pre-sintering temperature scope is at 960-1025 DEG C, sintering range is at 1030-1070 DEG C, high-temperature aging temperature range is at 860-940 DEG C, and low temperature aging temperature range, at 460-640 DEG C, is sent into cooling chamber argon gas or nitrogen rapid cooling after insulation.
3. the vacuum presintering method of a kind of Fe-B rare-earth permanent magnet according to claim 1, is characterized in that: described presintering vacuum is higher than 5 × 10-1Pa, sintering vacuum is 5 × 10-1Pa to 5 × 10-3Within the scope of Pa.
4. the vacuum presintering method of a kind of Fe-B rare-earth permanent magnet according to claim 1, is characterized in that: described presintering vacuum is higher than 5Pa, and sintering vacuum, in 500Pa to 5000Pa scope, is filled with argon gas when sintering.
5. the vacuum presintering method of a kind of Fe-B rare-earth permanent magnet according to claim 1, is characterized in that: the effective width 400-800mm of described sintering bin, the effective width 300-400mm of timeliness bin.
6. the vacuum presintering method of a kind of Fe-B rare-earth permanent magnet according to claim 1, is characterized in that: the magnet density scope of described presintering is at 7.2-7.5g/cm3, the magnet density scope of sintering is at 7.5-7.7g/cm3。
7. the continous vacuum presintering equipment of a Fe-B rare-earth permanent magnet, it is characterized in that: its main body is formed by connecting by inlet valve, preparation room, preparation room valve, degreasing chamber, degreasing chamber valve, the first degas chamber, the first degas chamber valve, the second degas chamber, the second degas chamber valve, the 3rd degas chamber, the 3rd degas chamber valve, the first presintering chamber, the first presintering chamber valve, the second presintering chamber, the second presintering chamber valve, cooling chamber and discharge door, in described preparation room, be provided with heater and live-roller, preparation room is connected with vacuum unit by filter; Indoor live-roller, heater, the metallic insulation screen of being provided with of described degreasing, degreasing chamber is connected with vacuum unit by filter; In described the first degas chamber, the second degas chamber and the 3rd degas chamber, be respectively arranged with live-roller, heater and heat protection screen, the first degas chamber, the second degas chamber and the 3rd degas chamber are connected with vacuum unit respectively; Indoor live-roller, heater, the heat protection screen of being respectively arranged with of described the first presintering chamber, the second presintering, the first presintering chamber, the second presintering chamber are connected with vacuum unit respectively; In described cooling chamber, be provided with live-roller, heat exchanger and cooling fan, cooling chamber is connected and is connected with gas charging system with vacuum unit respectively, and refrigerating gas is argon gas or nitrogen.
8. the continous vacuum presintering equipment of a kind of Fe-B rare-earth permanent magnet according to claim 7, it is characterized in that: the heating-up temperature of described preparation room is the highest 400 DEG C, the heating-up temperature of described degreasing chamber is the highest 500 DEG C, the heating-up temperature of described the first degas chamber, the second degas chamber, the 3rd degas chamber is the highest 900 DEG C, and the first described presintering chamber, the heating-up temperature of the second presintering chamber are the highest 1100 DEG C.
9. the continous vacuum presintering equipment of a kind of Fe-B rare-earth permanent magnet according to claim 7, it is characterized in that: described continous vacuum presintering equipment is provided with charging chamber before preparation room, charging chamber is connected with preparation room by valve, and transmission device and gloves are set in charging chamber.
10. the continous vacuum presintering equipment of a kind of Fe-B rare-earth permanent magnet according to claim 7, it is characterized in that: the vacuum unit of described preparation room comprises Roots vaccum pump, oil-sealed rotary pump and valve, in filter, be provided with cold-trap, condenser temperature is lower than 10 DEG C; The vacuum unit of described degreasing chamber comprises Roots vaccum pump, oil-sealed rotary pump and valve, is provided with cold-trap in filter, and condenser temperature is lower than 10 DEG C; The vacuum unit of described the first degas chamber, the second degas chamber and the 3rd degas chamber comprises diffusion pump, Roots vaccum pump, oil-sealed rotary pump and valve; The first described presintering chamber, the vacuum unit of the second presintering chamber comprise diffusion pump, Roots vaccum pump, oil-sealed rotary pump and valve; The vacuum unit of described cooling chamber comprises Roots vaccum pump, oil-sealed rotary pump and valve.
11. 1 kinds of Fe-B rare-earth permanent magnet continous vacuum sintering aging furnaces, is characterized in that: its main body is formed by connecting by feeding gate, preheating chamber, preheating chamber valve, heating clamber, heating clamber valve, agglomerating chamber, agglomerating chamber's valve, high-temperature aging chamber, high-temperature aging chamber valve, fore-cooling room, fore-cooling room's valve, low temperature aging chamber, low temperature aging chamber valve, cooling chamber and discharge door; In described preheating chamber, be provided with guide rail, transfer bogie, timeliness bin, heater, guide rail be arranged on metallic insulation screen above, the roller of transfer bogie rolls on guide rail, and timeliness bin is suspended on the bottom of transfer bogie, and preheating chamber is also connected with vacuum unit; Indoor guide rail, transfer bogie, timeliness bin, heater, the heat protection screen of being respectively arranged with of described heating clamber, agglomerating chamber and high-temperature aging, guide rail be arranged on heat protection screen above, the roller of transfer bogie rolls on guide rail, timeliness bin is suspended on the bottom of transfer bogie, and heating clamber, agglomerating chamber and high-temperature aging chamber are also connected with respectively vacuum unit; In described fore-cooling room, be provided with guide rail, transfer bogie, timeliness bin, heater, heat protection screen, heat exchanger and cooling fan, guide rail be arranged on heat protection screen above, the roller of transfer bogie rolls on guide rail, timeliness bin is suspended on the bottom of transfer bogie, fore-cooling room can heat and can air cooling, when cooling, be filled with argon gas, fore-cooling room is also connected with vacuum unit; Indoor guide rail, transfer bogie, timeliness bin, heater, the heat protection screen of being provided with of described low temperature aging, guide rail be arranged on heat protection screen above, the roller of transfer bogie rolls on guide rail, and timeliness bin is suspended on the bottom of transfer bogie, and low temperature aging chamber is also connected with vacuum unit; In described cooling chamber, be provided with guide rail, transfer bogie, timeliness bin, heat exchanger and cooling fan, cooling chamber is connected with vacuum unit with gas charging system respectively, and refrigerating gas is argon gas or nitrogen.
12. a kind of Fe-B rare-earth permanent magnet continous vacuum sintering aging furnaces according to claim 11, is characterized in that: the heating-up temperature of described preheating chamber is the highest 600 DEG C; The heating-up temperature of described heating clamber, agglomerating chamber, high-temperature aging chamber is the highest 1100 DEG C; The heating-up temperature of described fore-cooling room is the highest 1100 DEG C, and the heating-up temperature of described low temperature aging chamber is the highest 1100 DEG C.
13. a kind of Fe-B rare-earth permanent magnet continous vacuum sintering aging furnaces according to claim 11, is characterized in that: the effective width of described timeliness bin is within the scope of 260-450mm.
14. a kind of Fe-B rare-earth permanent magnet continous vacuum sintering aging furnaces according to claim 11, is characterized in that: described agglomerating chamber, high-temperature aging chamber are provided with voltage divider system, and dividing potential drop pressure limit is: 4000-7000Pa.
The manufacture method of 15. 1 kinds of Fe-B rare-earth permanent magnets, is characterized in that: first raw material fusing is made to rapid hardening alloy sheet, then carry out hydrogen fragmentation, airflow milling powder and pressing under magnetic field pack magnetic patch into magazine after moulding under nitrogen protection, then magazine are contained on sintering bin, and under the drive of transmission device, sintering bin enters the preparation room of continous vacuum pre-burning freezing of a furnace successively, degreasing chamber, the first degas chamber, the second degas chamber, the 3rd degas chamber, the first presintering chamber, the second presintering chamber and cooling chamber carry out preheating degreasing, Heating Dehydrogenation is degassed, presintering and cooling, cooling employing argon gas, cooling rear sintering bin takes out and magazine is installed to timeliness bin again from continous vacuum pre-burning freezing of a furnace, and timeliness bin plays and sends into the preheating chamber of continous vacuum sintering aging furnace, heating clamber, agglomerating chamber, high-temperature aging chamber, fore-cooling room, low temperature aging chamber and cooling chamber carry out sintering, high-temperature aging, pre-cooled, low temperature aging and air cooling fast, make sintered NdFeB rear-earth permanent magnet, and sintered NdFeB rear-earth permanent magnet is made Nd-Fe-B rare-earth permanent magnet device through machining and surface treatment again,
Preheating skimming temp scope is at 200-400 DEG C, the degassed temperature range of Heating Dehydrogenation is at 400-900 DEG C, pre-sintering temperature scope is at 900-1050 DEG C, sintering range is at 1020-1080 DEG C, high-temperature aging temperature range is at 850-950 DEG C, low temperature aging temperature range, at 460-640 DEG C, is sent into cooling chamber argon gas or nitrogen rapid cooling after insulation.
The manufacture method of 16. a kind of Fe-B rare-earth permanent magnets according to claim 15; it is characterized in that: described pressing under magnetic field is the powder of preorder to be sent under nitrogen protection to nitrogen protection lutation magnetic field presser; magnetic field orientating pressure forming under nitrogen protection; after packaging, take out from nitrogen protection lutation magnetic field presser; send into again isostatic pressing machine and wait static pressure; with packaging, magnetic patch is sent into prevention nitrogen gas protection box Deng after static pressure; under nitrogen protection, magnetic patch is removed to packaging; pack sintering magazine into, send into continous vacuum pre-burning freezing of a furnace sintering.
The manufacture method of 17. a kind of Fe-B rare-earth permanent magnets according to claim 15, is characterized in that: described Nd-Fe-B permanent magnet is made up of principal phase and Grain-Boundary Phase, and principal phase has R2（Fe,Co）14B structure, wherein principal phase from the heavy rare earth HR content in inside 1/3 scope of outer rim the heavy rare earth HR content higher than principal phase center, in Grain-Boundary Phase, there is the oxide fine particle of neodymium, R represent comprise Nd rare earth element more than one, HR represents more than one in Dy, Tb, Ho, Y rare earth element.
The manufacture method of 18. a kind of Fe-B rare-earth permanent magnets according to claim 15, is characterized in that: the structure of described Nd-Fe-B permanent magnet has at R2（Fe1-xCox）14The surrounding of B crystal grain surrounds heavy rare earth content higher than R2（Fe1-xCox）14The ZR of B phase2（Fe1-xCox）14The structure of B phase, ZR2（Fe1-xCox）14B phase and R2（Fe1-xCox）14Between B without Grain-Boundary Phase, ZR2（Fe1-xCox）14Between B phase, connect by Grain-Boundary Phase; In literary composition, ZR is illustrated in the rare earth higher than the phase of the content of the heavy rare earth in average content of rare earth of heavy rare earth content in crystalline phase; 0≤x≤0.5.
The manufacture method of 19. a kind of Fe-B rare-earth permanent magnets according to claim 15, is characterized in that: more than two ZR in the structure of described Nd-Fe-B permanent magnet2（Fe1-xCox）14The oxide fine particle that has neodymium in the Grain-Boundary Phase of the intersection of B phase crystal grain, the oxygen content of crystal boundary is higher than the oxygen content of principal phase.
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| CN201410194946.6A Active CN103996521B (en) | 2014-05-11 | 2014-05-11 | A kind of vacuum presintering method and apparatus of Fe-B rare-earth permanent magnet |
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| JP6852351B2 (en) * | 2016-10-28 | 2021-03-31 | 株式会社Ihi | Manufacturing method of rare earth permanent magnets |
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| WO2019148882A1 (en) * | 2018-02-01 | 2019-08-08 | 福建省长汀金龙稀土有限公司 | Device and method for continuous heat treatment of alloy workpiece or metal workpiece |
| CN112179128A (en) * | 2020-10-11 | 2021-01-05 | 江西开源自动化设备有限公司 | Continuous vacuum sintering furnace |
| CN112837878A (en) * | 2020-12-31 | 2021-05-25 | 横店集团东磁股份有限公司 | Rare earth-iron metal magnetic powder and preparation method thereof |
| CN117079961A (en) * | 2023-07-07 | 2023-11-17 | 燕山大学 | Anisotropic Nd 2 Fe 14 Preparation method of B/alpha-Fe block nanocrystalline composite permanent magnet material |
| CN117146580B (en) * | 2023-11-01 | 2023-12-29 | 沈阳广泰真空科技股份有限公司 | Eight-chamber vacuum continuous sintering furnace control method and eight-chamber vacuum continuous sintering furnace |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3188290A (en) * | 1958-06-03 | 1965-06-08 | Philips Corp | Method of manufacturing a magnet core for use as a memory element |
| CN101320609A (en) * | 2008-03-21 | 2008-12-10 | 浙江大学 | Grain boundary phase-reconstructed high-corrosion resistance Sintered NdFeB magnet and preparation method thereof |
| CN103123843A (en) * | 2011-11-21 | 2013-05-29 | 中国科学院宁波材料技术与工程研究所 | Preparation method for fine grain anisotropy densified neodymium iron boron permanent magnet |
| CN103212710A (en) * | 2013-05-05 | 2013-07-24 | 沈阳中北真空磁电科技有限公司 | Manufacturing method of NdFeB rare earth permanent magnetic material |
| CN103572083A (en) * | 2012-07-18 | 2014-02-12 | 三环瓦克华（北京）磁性器件有限公司 | Sintering method for neodymium iron boron magnet |
-
2014
- 2014-05-11 CN CN201410194946.6A patent/CN103996521B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3188290A (en) * | 1958-06-03 | 1965-06-08 | Philips Corp | Method of manufacturing a magnet core for use as a memory element |
| CN101320609A (en) * | 2008-03-21 | 2008-12-10 | 浙江大学 | Grain boundary phase-reconstructed high-corrosion resistance Sintered NdFeB magnet and preparation method thereof |
| CN103123843A (en) * | 2011-11-21 | 2013-05-29 | 中国科学院宁波材料技术与工程研究所 | Preparation method for fine grain anisotropy densified neodymium iron boron permanent magnet |
| CN103572083A (en) * | 2012-07-18 | 2014-02-12 | 三环瓦克华（北京）磁性器件有限公司 | Sintering method for neodymium iron boron magnet |
| CN103212710A (en) * | 2013-05-05 | 2013-07-24 | 沈阳中北真空磁电科技有限公司 | Manufacturing method of NdFeB rare earth permanent magnetic material |
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