JP6043812B2 - Flexible sintering method of rare earth permanent magnet alloy and sintering equipment thereof - Google Patents

Description

  The present invention relates to a method for treating a rare earth permanent magnet alloy, and more particularly to a flexible sintering method for a neodymium iron boron rare earth permanent magnet alloy and a sintering facility thereof.

  Neodymium iron boron rare earth permanent magnets are widely applied to electronics, motors, hybrid power vehicles, etc., and the future is likely to be applied to a wider area.

  As a conventional neodymium iron boron rare earth permanent magnet alloy sintering facility, reference can be made to Chinese utility model No. 01248403.2. This facility includes a furnace body, a heating chamber provided in the furnace body, and a nozzle provided on the wall of the heating chamber, and a valve is provided on one side of the furnace body, The valve is connected to a sealed glove box provided with a vacuum pipe. Its purpose is to solve problems such as product oxidation, cooling uniformity and uniformity.

  Conventional equipment has a large investment in maintenance, a large occupied area, a low level of automation, and there is a problem that the non-oxidation of the sintering process of the neodymium iron boron rare earth permanent magnet alloy cannot be realized.

    Patent Document 1: Chinese Utility Model No. 01248403.2

  In order to solve the above technical problems, the present invention provides a flexible sintering method for rare earth permanent magnet alloys and a sintering facility thereof.

The following technical method is adopted as the flexible sintering method for the rare earth permanent magnet alloy of the present invention.
Specifically, the following processing steps are performed.
(1) The fine powder of the rare earth permanent magnet alloy is weighed in a compressor in an inert gas, put in a mold, made into a semi-finished product by orientation molding, and this semi-finished product is put in a material container. It arranges on a material mounting board. The second conveyance hermetic box and the compressor are brought into contact with each other, and the flanges of the two separated isolation valves are hermetically locked. After the air between the two isolation valves is exchanged with an inert gas, the two isolation valves are opened, and the material fork in the second transfer sealed box carries the material mounting plate in the compressor into the second transfer sealed box. And close the two isolation valves. While the second transfer sealed box is separated, it comes into contact with the 1 # isolation valve on the 1 # chamber side of the glove box.
(2) Open the two isolation valves abutted after the air between the second transfer sealed box and the 1 # isolation valve of the glove box is exchanged with an inert gas, and the bottom roller in the second transfer sealed box The transfer device carries the material placing plate into the 1 # chamber of the glove box. When the two isolation valves are closed, the second transfer sealed box is released. Open the 2 # isolation valve of the glove box, the material in the 1 # chamber is carried into the 2 # chamber by the bottom roller transport device, and the 2 # isolation valve is closed. In the 2 # chamber, the semi-finished product is manually placed in the graphite material container, and the graphite material container is placed on the material placing plate.
(3) The first transfer sealed box is brought into contact with the 3 # isolation valve on the 2 # chamber side, and the flanges of the two contacted isolation valves are hermetically locked. Open the two isolation valves connected after the air between the two isolation valves is exchanged with the inert gas, start the 2 # chamber and the bottom roller transfer device of the first transfer sealed box, and start the 2 # chamber The material mounting plate is carried into the first transfer sealed box. When the two isolation valves are closed, the first transfer sealed box is released.
(4) The first transfer sealing box and the isolation valve of the sintering furnace are brought into contact with each other, and the contacted flange is hermetically locked. The balance valve is opened after the air between the two isolation valves is exchanged with an inert gas, and when the atmospheric pressure in the furnace and the pressure in the first transfer sealed box are balanced, the two connected isolation valves are opened. . When the feed screw driving device in the first transfer sealed box, the material fork that is moved up and down by the cylinder is activated, the material mounting plate is carried into the sintering furnace, and the two isolation valves are closed, the first transfer sealed box Leave.
(5) When the sintering furnace is evacuated and the degree of vacuum is higher than 50 Pa or protective gas is introduced, heat insulation is performed with a preset processing curve, and sintering is performed at a maximum temperature of 1200 ° C. When nitrogen or argon is introduced to 0.01 to 0.03 MPa, the blower is activated to cool the material container and the rare earth permanent magnet alloy semi-finished product in the material container, and when cooled to 80 ° C. or less, at least about 5 minutes. Stop the blower after placing it. When the pressure inside the furnace becomes the same as the atmospheric pressure, open the 4 # isolation valve of the sintering furnace, take out the material mounting plate with the material fork of the material outlet side car, and then close the 4 # isolation valve, the material outlet The side car leaves.

  The sintering equipment employed by the processing method of the present invention includes a glove box, two transfer sealed boxes, a compressor, a sintering furnace, and a material outlet side wheel. A distribution passage is provided at each end of the glove box, the compressor and the sintering furnace are arranged on one side of each distribution passage, and the two transfer sealed boxes move in the two distribution passages. Isolation valves are respectively provided on the opposing surfaces between the two transporting sealed boxes and the sintering furnace and the compressor, and at both ends of the glove box, and the isolation valves of the glove box, the sintering furnace, and the compressor are provided by the isolation valves. Respectively.

  Furthermore, the glove box is a two-chamber vacuum or protective gas sealed box, the glove box has two sealed chambers, and a 2 # isolation valve is provided between the two sealed chambers. 1 # and 3 # isolation valves are provided on the end face of the closed chamber. Each chamber is provided with a vacuum pipe, an inert gas introduction pipe, a gas discharge valve pipe, a pressure gauge, and a vacuum gauge, and a balance valve pipe is provided between the two chambers. Balance the pressure in the two chambers with a pipe. In the two chambers, 2 # and 3 # bottom roller conveying devices for placing the material placing plates are respectively provided. The 2 # chamber is provided with a glove box flange module.

  In addition, a 5 # isolation valve is provided at one end of the transport sealed box, and a box door is provided at the other end. When the conveying sealed box and the glove box, sintering furnace or compressor abut, the two flanges on the isolation valve are sealed.

  Further, a 1 # bottom roller transport device for transporting material into the glove box and a material fork structure for transporting material into the sintering furnace are provided inside the transport sealed box, and an omnidirectional roller is disposed at the bottom of the transport sealed box. And a 1 # vacuum pipe, an inert gas introduction pipe, and a 1 # gas discharge valve pipe are connected to the transport sealed box.

  Further, the material fork structure includes a material fork, a roller rail frame, a feed screw drive device, a 1 # motor speed reducer, and a first cylinder. The output shaft of the 1 # motor speed reducer is a feed screw drive device. Connected to one end of the feed screw, the other end of the feed screw driving device is connected to the roller rail frame supported by the first cylinder, and the 1 # bottom roller transport device is attached to the box bottom by the support frame.

  Further, the first cylinder is fixed to the lower side of the box, the piston of the first cylinder is inserted into the box and linked to the roller shaft of the roller rail frame of the material fork, and the roller is a rail of the 1 # roller rail device. Move in.

  In addition, one or more sintering furnaces are provided, one end of which is provided with a 4 # isolation valve located on one side of the distribution passage, and the other end is provided with a furnace door which is locked to a high pressure hermetic lock. It is done. A heating chamber is provided in the furnace of the sintering furnace, a heat shield layer is provided in the heating chamber, and a plurality of sets of heaters and thermocouples are provided in the heat shield layer. The heater is electrically connected to the heating power source box by an electrode provided on the heating chamber and a copper wire provided outside the heating chamber. A plurality of nozzles penetrating the heat shield layer along the warp direction and communicating with each other are provided in the furnace. The outer wall of the sintering furnace has a two-layer structure in which the cooling water is placed, and a cooling water inlet / outlet pipe is provided thereon. An inert gas introduction pipe, a safety valve pipe, a gas discharge valve pipe, and a wind cooling system are connected to the inner chamber of the sintering furnace. The material placing plate is placed on the material placing table in the heating chamber in the furnace by the material fork in the first transfer sealed box.

  Further, a balance valve pipe is connected between the inside of the sintering furnace and the 4 # isolation valve.

  Furthermore, the wind cooling system has an external circulation structure or an internal circulation structure, and includes a blower, a heat exchanger, and a plurality of nozzles provided along the furnace, and is connected to each nozzle. One end of the passage is connected to the blower, and the other end is connected to the heat exchanger.

  Furthermore, when there are a plurality of the sintering furnaces, they are arranged in front of the distribution passage.

  The present invention adopts a parallel flexible production method, and the sintering process time of the neodymium iron boron rare earth permanent magnet alloy takes 24 hours. It takes only 1 hour to manually put the semi-finished product into the graphite material container and place the graphite material container on the material placing plate. As a result, the glove box of the single-chamber sintering furnace can be deleted, and one glove box can be made to correspond to the single-chamber sintering furnace of a plurality of isolation valves, and can be brought into contact with the sintering furnace by a protective gas transfer sealed box. it can.

  The present invention adopts a flexible production method, and abuts against the compressor by a conveyance sealed box, thereby realizing an oxygen-free connection from compression to sintering, effectively improving the characteristics of the magnetic material, The automation level can be greatly improved.

It is a figure which shows the flexible sintering equipment of the rare earth permanent magnet alloy of this invention. It is a figure which shows the conveyance sealed box in FIG. It is a figure which shows the glove box in FIG. It is a figure which shows the sintering furnace in FIG. It is a top view which shows the sintering furnace of FIG. It is a figure which shows the structure of the conveyance sealed box in FIG.

  The present invention will be described in detail below based on the drawings and examples.

  Example: As shown in FIG. 1, the equipment of the present invention includes a glove box 1, first and second transfer sealed boxes 2 and 6, a compressor 5, a sintering furnace 3, and a material outlet side vehicle 4. Including. A distribution passage is provided at both ends of the glove box 1, the compressor 5 and the sintering furnace 3 are arranged on one side of each distribution passage, and the first and second transfer sealed boxes 2, 6 each have two You can move in the logistics path. Isolation valves are provided on the opposing surfaces between the first and second transfer sealed boxes 2 and 6 and the sintering furnace 3 and the compressor 5 and on both ends of the glove box 1, respectively. It is connected to the isolation valve of the box 1, the sintering furnace 3 and the compressor 5. When there are a plurality of sintering furnaces 3 and compressors 5, they can be arranged in parallel.

  As shown in FIG. 3, the glove box 1 is a two-chamber vacuum or protective gas sealed box. The glove box of this embodiment has two sealed chambers, that is, a 1 # chamber 32 and a 2 # chamber 38. A 2 # isolation valve 36 is provided between the two sealed chambers, and a 1 # isolation valve 31 and a 3 # isolation valve 43 are provided on the end surfaces of the two sealed chambers, respectively. Each chamber is provided with a vacuum pipe, an inert gas introduction pipe, a gas discharge valve pipe, a pressure gauge, and a vacuum gauge, and a balance valve pipe is provided between the two chambers. Balance the pressure in the two chambers with a pipe. In the two chambers, 2 # and 3 # bottom roller conveying devices 46 and 45 for placing the material placing plate 44 are provided, respectively. In the 2 # chamber 38, a glove box flange module 37 and a 2 # cabinet 39 are provided.

  As shown in FIG. 1, the structures of the first and second transfer sealed boxes 2 and 6 are the same, and a 5 # isolation valve 14 is provided at one end of both, and a box door 7 is provided at the other end. ing. By bringing the first and second transfer sealed boxes 2 and 6 into contact with the glove box 1, the sintering furnace 3, or the compressor 5, the sealing of the flanges of the two isolation valves is ensured. The air between the 5 # isolation valve 14 and the 1 # isolation valve 31 and 3 # isolation valve 43 can be evacuated by the 4 # vacuum pipe 30 of the valve provided in the 5 # isolation valve 14 of the transport sealed box, Or it can replace | exchange by blowing inactive gas with an inert gas introduction pipe.

  As shown in FIG. 2, a 1 # bottom roller transport device for transporting the material to the glove box 1 and a material fork structure for transporting the material to the sintering furnace 3 or the compressor are provided inside the transport sealed box. ing. An omnidirectional roller 19 is provided at the bottom of the transport sealed box, and a 1 # vacuum pipe 12, an inert gas introduction pipe, and a 1 # gas discharge valve pipe 8 are connected to the transport sealed box. ing.

  The material fork structure includes a material fork 17, a roller rail frame 20, a feed screw drive device 29, a 1 # motor speed reducer 18, and a first cylinder 27. 1 # motor speed reducer 18 is fixed on roller rail frame 20, its output shaft is connected to one end of feed screw 21, the other end of feed screw 21 is connected to roller rail frame 20, and first cylinder 27 is a roller. The roller shaft of the rail frame 20 is supported. A feed screw driving device 29 is fixed to the material fork 17. By driving the nut in the feed screw driving device 29 when the feed screw rotates, the roller of the material fork 17 rolls along the roller rail frame 20 and the material fork moves. The 1 # bottom roller transport device 16 is mounted on the box bottom 22 by a support frame 81. The first cylinder 27 is fixed to the lower side of the box, and the piston of the first cylinder 27 is inserted into the box and linked to the roller shaft of the roller rail frame 20 of the material fork. Move along the rail. The 1 #, 2 #, 3 # bottom roller conveying devices 16, 46, 45 have the same structure, and are all fixed in a box by a support frame 81, all of which have a motor, a plurality of roller support frames, a chain wheel, Consists of a chain. The chain wheel is rotated by driving the motor, and the material placing plate 44 thereon is moved. When activated, the first cylinder 27 causes the rollers of the 1 # roller rail device 28 to move up and down along the rails, and the 1 # motor speed reducer 18 drives the feed screw drive 29 to cause the rollers on the material fork 17 to move. Moves horizontally along the rails of the roller rail frame 20. This realizes vertical and horizontal movement.

  As shown in FIGS. 4 and 5, the sintering furnace 3 is one or plural. In the case of a plurality, they are arranged in front of the distribution passage. One end of the sintering furnace 3 is provided with a 4 # isolation valve 56 located on one side of the physical distribution passage, and the other end is provided with a furnace door 53 that is locked to the high-pressure hermetic lock portion 52. A heating chamber is provided in the furnace, a heat shielding layer 59 is provided in the heating chamber, and a plurality of sets of heaters 58 and thermocouples 55 are provided in the heat shielding layer 59. . The heater 58 is electrically connected to the heating power source box 48 by an electrode 54 provided on the heating chamber and a copper wire 49 provided outside the heating chamber. In the furnace, a plurality of nozzles 60 penetrating the heat shield layer 59 along the warp direction and communicating with each other are provided. The outer wall of the sintering furnace has a two-layer structure in which the cooling water is placed, and a cooling water inlet / outlet pipe 57 is provided thereon. An inert gas introduction pipe, a safety valve pipe 67, a gas discharge valve pipe 68, and a wind cooling system are connected to the inner chamber of the sintering furnace. The material placing plate 44 is placed on the material placing table in the heating chamber in the furnace by the material fork 17 in the first transfer sealed box 2. A balance valve pipe 69 is connected between the inside of the sintering furnace 3 and the 4 # isolation valve 56 to balance the pressure.

  The wind cooling system has an external circulation structure or an internal circulation structure, and includes a blower 50, a heat exchanger 51, and a plurality of nozzles 60 provided along a furnace of a sintering furnace. One end of the air passage communicated with each nozzle 60 is connected to the blower 50, and the other end is connected to the heat exchanger 51.

  The vacuum system includes a diffusion pump 64, a roots pump 63, a plunger pump or rotor blade pump 62, and a vacuum pipe connected in series. A high vacuum flap valve 61 is provided in the diffusion pump 64, the roots pump 63, and the plunger pump or the rotary blade pump 62.

  As shown in FIG. 6, each of the isolation valves has a unidirectional sealed plug valve structure, and has a valve body, a second cylinder 70, a water cooling valve plate 75 provided inside, It includes a hinge plate 76, a link 78, a 2 # roller rail device 77, and a contact mass 79. The water cooling valve plate 75 is connected to the hinge plate 76 by a plurality of links 78, and is provided on the guide rail 24 of the 2 # roller rail device 77 in the valve body. A roller 23 that slides along the guide rail 24 is provided on the water cooling valve plate 75 and the hinge plate 76. The second cylinder 70 is placed outside the valve body, and its piston is inserted into the valve body and connected to the hinge plate 76. The contact mass 79 is placed on the valve bottom 25 in the valve body, and a rubber ring 74 is provided at one end of the water cooling valve plate 75 approaching the valve side flange 26. The second cylinder 70 is driven so that the hinge plate 76 moves on the guide rail 24, the water cooling valve plate 75 contacts the contact mass 79, and the plurality of links 78 connect the water cooling valve plate 75 to the valve side flange. 26, the rubber ring 74 has an isolating and sealing action. The water inlet / outlet pipe shaft 72 of the water cooling valve plate 75 and the piston of the second cylinder 70 are linked together by a connecting plate 73. A heat shield plate can be further provided on the water cooling valve plate 75. By further providing an upper flange 80 on the valve body, the water cooling valve plate 75 can be transferred from the valve body through the upper flange 80 when repairing.

  The operation process of the present invention is as follows.

  Check power electricity, power air source, circulating cooling water and medium air source. Inspect all main / auxiliary equipments to ensure that they are not broken and in normal working condition. By adopting a model in which the glove box 1, the sintering furnace 3, the first and second transfer sealed boxes 2, 6, and the compressor 5 all have independent cabinets and are operated separately, Ensure equipment meets production requirements. That is, the vacuum system is activated and locked to each other, and the inert gas valve is opened and adjusted to a predetermined flow rate. Each isolation valve, furnace door and box door are all closed. The heater is not broken.

  The first and second transport sealed boxes 2 and 6 are sealed boxes provided on the transport vehicle. When operating, the box door 7 and the 5 # isolation valve 14 are closed, and the 1 # vacuum pipe 12 is opened to evacuate the transfer sealed box or allow the air in the inert gas exchange box to pass through the transfer sealed box. Can be blown into. The pressure in the transport sealed box is controlled by a 1 # pressure gauge 13. The 1 # observation window 9 is provided symmetrically on the left and right sides of the box, and the 1 # cabinet 10, 2 # observation window 11 and 1 # gas discharge valve pipe 8 are provided on the ceiling, so that the operation is easy. Can be. The second transfer sealed box 6 can be brought into contact with the 1 # isolation valve 31 of the glove box 1 and the compressor 5 by the movement of the omnidirectional roller 19 and can be fixed in position by a position switch. The first transport sealed box 2 can be brought into contact with the 3 # isolation valve 43 of the glove box 1 and the sintering furnace 3 by the movement of the omnidirectional roller 19 and can be fixed in position by a position switch.

  (1) The fine powder of the rare earth permanent magnet alloy is weighed in the compressor 5 in an inert gas, put into a mold, and the semi-finished product formed into the orientation mold is put into the material container 15. The material container 15 is arranged on the material placing plate 44, abuts the second conveyance hermetic box 6 and the compressor 5, and locks the flanges of the two abutting isolation valves. After the air between the two isolation valves is exchanged with inert gas, the two abutting isolation valves are opened (ie, the 4 # vacuum pipe 30 is opened to evacuate the space between the two isolation valves) When the inert gas is introduced through the air introduction pipe and the pressure balance between the second transfer hermetic box 6 and the compressor 5 is balanced, the two isolation valves are opened.) The material fork of the second transport sealed box 6 is activated to take out the material placing plate 44 on which the material container 15 in the compressor is placed, and the material fork carries the material placing plate 44 into the second transport sealed box 6. To do. When the two isolation valves are closed and the contact-locked flange is opened, the second transfer sealing box 6 is separated from the compressor 5 and is in contact with the 1 # isolation valve 31 on the 1 # chamber side of the glove box 1. .

  (2) The second transfer hermetic box 6 is moved to the glove box 1 side and brought into contact with the 1 # isolation valve 31, and the flanges of the two contacted isolation valves are locked. After the air between the 5 # and 1 # isolation valves is exchanged with an inert gas, the two abutting isolation valves are opened (ie, the 4 # vacuum pipe 30 is opened and the 5 #, 1 # isolation valve is opened) 14 and 31 are evacuated, and the vacuum pump is stopped.When an inert gas is introduced by the air introduction pipe and the pressure balance in the second transfer sealed box 6 and the 1 # chamber 32 is balanced, 5 #, 1 # Open isolation valves 14, 31). The 1 # bottom roller transport device 16 and the 2 # bottom roller transport device 46 are activated to carry the material placement plate 44 on which the material container 15 is placed into the 1 # chamber 32, and the 5 #, 1 # isolation valve. When the 14 and 31 are closed and the flanges of the two abutment-locked isolation valves are opened, the second transfer sealed box 6 is separated. When the pressure balance between the 1 # chamber 32 and the 2 # chamber 38 is taken, the 2 # isolation valve 36 of the glove box 1 is opened, the 2 # bottom roller transport device 46 and the 3 # bottom roller transport device 45 are activated, and the material The material placement plate 44 on which the container 15 is placed is carried from the 1 # chamber 32 to the 2 # chamber 38, and the 2 # isolation valve 36 is closed. In the 2 # chamber, the semi-finished product is manually placed in the graphite material container, and the graphite material container is placed on the material placing plate 44.

  (3) The first transfer sealed box 2 is moved to the 2 # chamber side of the glove box 1 and brought into contact with the 3 # isolation valve 43, and the flanges of the two contacted isolation valves are locked. After the air between the two isolation valves is exchanged with an inert gas, the connected 5 #, 3 # isolation valve is opened (ie, the 4 # vacuum pipe 30 is opened and the 5 #, 3 # isolation valve 14 is opened. , 43 is evacuated, and the vacuum pump is stopped, and an inert gas is introduced by the air introduction pipe, and when the pressure balance in the first transfer sealed box 2 and the 2 # chamber 38 is balanced, 5 #, 3 # Open isolation valves 14 and 43.) The 1 # bottom roller transport device 16 and 3 # bottom roller transport device 45 in the 2 # chamber are activated, and the material placement plate 44 for placing the material container 15 in the 2 # chamber is placed in the first transport sealed box 2. When the 5 # and 3 # isolation valves 14 and 43 are closed, and the flanges of the 5 # and 3 # isolation valves that are in lock contact are opened, the first transfer sealed box 2 is separated.

  (4) The first transfer hermetic box 2 is moved to the sintering furnace 3 side and brought into contact with the 4 # isolation valve 56, and the flanges of the contacted 5 # and 4 # isolation valves 14 and 56 are locked. The balance valve is opened after the air between the 5 #, 4 # isolation valves 14, 56 is exchanged with an inert gas. When the pressure in the furnace and the pressure in the first transfer sealed box are balanced, the connected 5 #, 4 # isolation valves 14, 56 are opened (ie, the 4 # vacuum pipe 30 is opened, 5 #, 4 # is opened). # Vacuum the space between the isolation valves 14 and 56 and stop the vacuum pump.When the inert gas is introduced by the air introduction pipe and the pressure balance in the first transfer sealed box 2 and the sintering furnace 3 is balanced, Open the two isolation valves 14, 56). The 1 # motor speed reducer 18 is activated, and the material fork 17 is inserted into the sintering furnace 3 by the feed screw driving device 29, and the material fork 17 is moved down along the 1 # roller rail device 28 by the first cylinder 27. Try to move. The material mounting plate 44 is placed on the material mounting table of the sintering furnace 3, and the material fork 17 is returned into the first transfer sealed box 2. When the 4 # isolation valve 56 and the 5 # isolation valve 14 are closed and the flanges of the 5 # and 4 # isolation valves 14 and 56 that are locked against contact are opened, the first transfer sealed box 2 is released.

  (5) When the sintering furnace 3 is evacuated and the degree of vacuum is higher than 50 Pa or a protective gas is introduced, it is heated and kept at a preset processing curve, sintered at a maximum temperature of 1200 ° C., and an inert gas ( Nitrogen or argon) is introduced to 0.01 to 0.03 MPa, and the blower 50 is activated to cool the material container 15 and the rare earth permanent magnet alloy semi-finished product in the material container 15. The cooling gas is directed to the material container 15 by the nozzle 60 of the air pipe, and the heated gas is circulated and cooled by the wind of the blower 50 and the efficient heat exchange of the heat exchanger 51. The 2 # cabinet 39 performs electrical control on the sintering furnace 3. After cooling to 80 ° C. or lower, leave it for at least 5 minutes before turning off the blower. Air is introduced into the furnace through a gas discharge valve pipe 68, and when the pressure in the furnace becomes the same as the atmospheric pressure, the 4 # isolation valve of the sintering furnace 3 is opened, and the material is loaded with the material fork of the material outlet side car 4. After the placing plate 44 is taken out of the sintering furnace 3, when the 4 # isolation valve is closed, the material outlet side wheel 4 is separated.

  During production, the external control system continuously checks the status of the equipment, and the equipment is automatically operated by preset software. All operations are performed by human computer interaction.

  The display panel of the external control system can display the following information. For example, operation status of vacuum pump, vacuum valve and vacuum pipe vacuum degree; conveyance and operation status of conveyance sealed box; drive and indication of operation status of isolation valve; glove box 1, sintering furnace 3, first , The pressure of the second transfer sealed box 2, 6 and 5 # isolation valve 14 and the temperature of the sintering furnace 3; the operation status of the inert gas, the status of the safety valve; the actual cooling water, the pressure of the power air, the alarm management; Display all relevant processing parameters (set values and actual values); enter parameters; display and store conventional processing parameters / data. All main parts of the facility can be operated on the display panel.

  A comparison of the quality of products produced by the processing method of the present invention and the current processing method is as follows.

  Ratio adjustment: 18% Nd by weight percentage ratio, 8.5% Pr, 3% Dy, 1.02% B, 0.3% Al, and the remainder is Fe. Semi-finished products manufactured by melting, hydrogen crushing, airflow polishing, and magnetic field molding manufacture are placed in a single-chamber sintering furnace having a protective glove box and vacuum sintered. When the temperature is raised to 430 ° C., the temperature is kept for 3 hours for heat insulation and deaeration, and the vacuum is higher than 1 Pa. After this heat retention, the temperature is raised to 850 ° C. and kept for 2 hours. Next, the temperature is raised to 1080 ° C., vacuum sintering is maintained for 2 hours, and the degree of vacuum reaches E-2 Pa. Next, aging is performed at 900 ° C. for 2 hours and aging is performed at 500 ° C. for 4 hours.

  Example 1: A material ratio similar to the ratio adjustment is adopted, and sintering is performed by the sintering method of the present invention. Vacuum is applied before the temperature is raised, and when the degree of vacuum becomes higher than 1 Pa, heating is started up to 400 ° C. and the temperature is kept for 3 hours. When the temperature in the heating furnace is raised from 400 ° C. to 850 ° C., a plurality of heating and holding steps are performed, and when it is 850 ° C., the temperature is kept for 2 hours, and the degree of vacuum reaches 3E-2 Pa. When the temperature rise is continued and the heating temperature reaches 1080 ° C., sintering is performed for 2 hours, and the degree of vacuum reaches E-2 Pa. Aging is performed by an aging method during the ratio adjustment.

  Example 2: A material ratio similar to the ratio adjustment is adopted, and sintering is performed by the sintering method of the present invention. Evacuation is started before the temperature is raised, and when the degree of vacuum becomes higher than 1 Pa, heating to 450 ° C. is started and the temperature is kept for 3 hours. When the temperature in the heating furnace rises from 450 ° C. to 850 ° C., a plurality of heating and holding steps are performed, and when it is 850 ° C., the temperature is kept for 2 hours, and the degree of vacuum reaches 3E-2 Pa. When the temperature rise is continued and the heating temperature reaches 1080 ° C., sintering is performed for 2 hours, and the degree of vacuum reaches E-2 Pa. Aging is performed by an aging method during the ratio adjustment.

  Example 3: A material ratio similar to the ratio adjustment is adopted, and sintering is performed by the sintering method of the present invention. Evacuation is started before the temperature is raised, and when the degree of vacuum becomes higher than 1 Pa, heating to 400 ° C. is started and the temperature is kept for 3 hours. When the temperature in the heating furnace is raised from 400 ° C. to 900 ° C., a plurality of temperature raising and holding steps are performed. When the temperature rise is continued and the heating temperature reaches 1080 ° C., sintering is performed for 2 hours, and the degree of vacuum reaches E-2 Pa. Aging is performed by an aging method during the ratio adjustment.

  Example 4: A material ratio similar to the ratio adjustment is adopted, and sintering is performed by the sintering method of the present invention. Evacuation is started before the temperature is raised, and when the degree of vacuum becomes higher than 1 Pa, heating to 400 ° C. is started and the temperature is kept for 3 hours. When the temperature in the heating furnace is raised from 400 ° C. to 900 ° C., a plurality of temperature raising and holding steps are performed, and when the temperature reaches 900 ° C., the temperature is kept for 2 hours, and the degree of vacuum is set to 3E-2 Pa. When the temperature rise is continued and the heating temperature reaches 1070 ° C., sintering is performed for 3 hours, and the degree of vacuum reaches E-2 Pa. Aging is performed by an aging method during the ratio adjustment.

  Example 5: A material ratio similar to the ratio adjustment is adopted, and sintering is performed by the sintering method of the present invention. Evacuation is started before the temperature is raised, and when the degree of vacuum becomes higher than 1 Pa, heating is started to 500 ° C. and the temperature is kept for 3 hours. When the temperature in the heating furnace is raised from 500 ° C. to 900 ° C., a plurality of temperature raising and holding steps are performed, and when the temperature reaches 900 ° C., the temperature is kept for 2 hours, and the degree of vacuum is set to 3E-2 Pa. When the temperature rise is continued and the heating temperature reaches 1070 ° C., sintering is performed for 3 hours, and the degree of vacuum reaches E-2 Pa. Aging is performed by an aging method during the ratio adjustment.

  As shown in each row above, the parallel flexible production method of the present invention eliminates the glove box of a single chamber sintering furnace and replaces one glove box with a single chamber sintering furnace of a plurality of isolation valves. Correspondingly, since it can be brought into contact with the sintering furnace and the compressor by means of the protective gas carrying hermetically sealed box, an oxygen-free connection from compression to sintering can be realized. When compared with the production method of a conventional sintering furnace provided with a glove box, the present invention can effectively improve the quality of the magnetic material and greatly improve the level of automation of production.

  A general engineer in this technical field can understand the technical matters of the present invention, and can make various modifications to the specific embodiments without departing from the scope of the claims. . For example, a plurality of sintering furnaces can be provided.

DESCRIPTION OF SYMBOLS 1 Glove box 2 1st conveyance sealed box 3 Sintering furnace 4 Material exit side vehicle 5 Compressor 6 2nd conveyance sealed box 7 Box door 8 1 # Pipe for gas release valve 9 1 # Observation window 10 1 # Cabinet 11 2 # Observation window 12 1 # Vacuum pipe 13 1 # Pressure gauge 14 5 # Isolation valve 15 Material container 16 1 # Bottom roller transport device 17 Material fork 18 1 # Motor speed reducer 19 Omni-directional roller 20 Roller rail frame 21 Feed screw 22 Box bottom 23 Roller 24 Guide rail 25 Valve bottom 26 Valve side flange 27 First cylinder 28 1 # Roller rail device 29 Feed screw drive device 30 4 # Vacuum pipe 31 1 # Isolation valve 32 1 # chamber 33 2 # Pipe for gas release valve 34 2 # Vacuum pipe 35 2 # Pressure gauge 36 2 # isolation valve 37 glove box flange module 38 2 # chamber 39 2 # cabinet 40 3 # pipe for gas release valve 41 3 # vacuum pipe 42 3 # pressure gauge 43 3 # isolation valve 44 material mounting plate 45 3 # bottom roller Conveying device 46 2 # Bottom roller conveying device 47 3 # Cabinet 48 Heating power supply box 49 Copper wire 50 Blower 51 Heat exchanger 52 High-pressure hermetic lock part 53 Furnace door 54 Electrode 55 Thermocouple
56 4 # Isolation valve 57 Cooling water inlet / outlet pipe 58 Heater 59 Heat shield layer 60 Nozzle 61 High vacuum flap valve 62 Plunger pump or rotary blade type pump 63 Roots pump 64 Diffusion pump 65 Cold trap 66 Electrical connection point pressure gauge 67 Safety valve Pipe 68 for gas release valve 69 Pipe for balance valve 70 Second cylinder 71 Magnetic switch 72 Water inlet / outlet pipe shaft 73 Connecting plate 74 Rubber ring 75 Water cooling valve plate 76 Hinge plate 77 2 # Roller rail device 78 Link 79 Contact Mass 80 Upper flange 81 Support frame

Claims (7)

In the flexible sintering method of rare earth permanent magnet alloy,
(1) The fine powder of rare earth permanent magnet alloy is weighed in a compressor in an inert gas, put into a mold, made into a semi-finished product by orientation molding, and this semi-finished product is put into a material container. Arranged on the mounting plate, abuts the second transport sealed box and the compressor, and seals the flanges of the two separated isolation valves, and the air between the two isolation valves is an inert gas. After opening the two isolation valves, the material fork in the second transfer sealed box carries the material mounting plate in the compressor into the second transfer sealed box and closes the two isolation valves. A step of contacting the first isolation valve on the first chamber side of the glove box while the conveyance sealed box is separated;
(2) Open the two isolation valves abutted after the air between the second transfer sealed box and the first isolation valve of the glove box is exchanged with an inert gas, and the bottom roller in the second transfer sealed box The transfer device carries the material mounting plate into the first chamber of the glove box, and when the two isolation valves are closed, the second transfer sealed box is separated; the second isolation valve of the glove box is opened and the material in the first chamber is Carrying into the second chamber by the bottom roller transport device, closing the second isolation valve; manually placing the semi-finished product into the graphite material container in the second chamber, and placing the graphite material container on the material mounting plate;
(3) The first transfer sealing box is brought into contact with the third isolation valve on the second chamber side, and the flanges of the two isolation valves in contact with each other are hermetically locked; the air between the two isolation valves is an inert gas Open the two isolation valves connected after the replacement, and activate the second chamber and the bottom roller transport device of the first transport sealed box to place the material mounting plate in the second chamber in the first transport sealed box When the two isolation valves are closed, the first transfer sealed box is separated;
(4) The first transfer sealed box and the isolation valve of the sintering furnace are brought into contact with each other, and the contacted flange is hermetically locked; the balance valve after the air between the two isolation valves is exchanged with an inert gas When the pressure in the furnace and the pressure in the first transfer sealed box are balanced, the two connected isolation valves are opened, the feed screw drive in the first transfer sealed box, and the material fork that moves up and down by the cylinder , And after bringing the material mounting plate into the sintering furnace, closing the two isolation valves causes the first transfer sealed box to leave,
(5) When the sintering furnace is evacuated and less than 50 Pa, which is the upper limit of the degree of vacuum, or when a protective gas is introduced, heat insulation is performed based on a preset heat insulation, and the maximum temperature is 1200 ° C. Sintering; When nitrogen or argon is introduced to 0.01 to 0.03 MPa, the blower is activated to cool the material container and the rare earth permanent magnet alloy semi-finished product in the material container, and when cooled to 80 ° C. or lower After at least 5 minutes, stop the blower; when the pressure in the furnace becomes the same as the atmospheric pressure, open the 4th isolation valve of the sintering furnace and take out the material mounting plate with the material fork of the material outlet side car. A method of flexible sintering of a rare earth permanent magnet alloy, comprising: performing a treatment process including: a step of separating a material outlet side vehicle when the isolation valve is closed. A sintering facility,
It is used for the flexible sintering method of the rare earth permanent magnet alloy according to claim 1,
A glove box, two conveying sealed boxes, a compressor, a sintering furnace, and a material outlet side vehicle; distribution passages are provided at both ends of the glove box, and the compressor and the sintering furnace are respectively Arranged on one side of each logistics passage, the two transport sealed boxes each move in the two logistics passages,
An isolation valve is provided at one end on the side of the sintering furnace of the one of the transfer sealed boxes,
An isolation valve is provided at one end on the compressor side of the other transport sealed box,
An isolation valve is provided at both ends of the glove box, and the glove box is connected to the isolation valve of the sintering furnace / compressor by the isolation valve.   The glove box is a two-chamber vacuum or two-chamber protective gas sealed box, the glove box has two sealed chambers, and a second isolation valve is provided between the two sealed chambers. No. 1 and No. 3 isolation valves are provided at the end face of the sealed chamber; each chamber has a vacuum pipe, an inert gas introduction pipe, a gas discharge valve pipe, a pressure gauge, and a vacuum gauge. A balance valve pipe is provided between the two chambers, and the pressure balance of the two chambers is balanced by this balance valve pipe; the second and third bottom rollers for placing the material placing plate in the two chambers The sintering equipment according to claim 2, wherein a conveying device is provided; a glove box flange module is provided in the second chamber. The transport sealed box has one isolation valve at one end and a box door at the other end,
The sintering equipment according to claim 2, wherein when the conveyance sealed box and the glove box, the sintering furnace, or the compressor come into contact with each other, sealing of the two flanges on the isolation valve is ensured.   The inside of the conveyance sealed box is provided with a first bottom roller conveyance device for carrying the material into the glove box and a material fork structure for carrying the material into the sintering furnace, and an omnidirectional roller is provided at the bottom of the conveyance sealed box The sintering equipment according to claim 2, wherein a first vacuum pipe, an inert gas introduction pipe, and a first gas discharge valve pipe are connected to the transport sealed box.   The material fork structure includes a material fork, a roller rail frame, a feed screw driving device, a No. 1 motor speed reduction device, and a first cylinder. An output shaft of the No. 1 motor speed reduction device is a feed screw of the feed screw driving device. The other end of the feed screw driving device is connected to a roller rail frame supported by the first cylinder, and the bottom roller transporting device is attached to the bottom of the box by a support frame. Item 6. The sintering facility according to Item 5.   The first cylinder is fixed to the lower side of the box, the piston of the first cylinder is inserted into the box and linked to the roller shaft of the roller rail frame of the material fork, and the roller is in the rail of the first roller rail device. The sintering equipment according to claim 6, wherein the sintering equipment is moved at a high speed.