CN107321977B - Rare earth permanent magnet vacuum sintering method and vacuum sintering heat treatment equipment - Google Patents
Rare earth permanent magnet vacuum sintering method and vacuum sintering heat treatment equipment Download PDFInfo
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- CN107321977B CN107321977B CN201610275462.3A CN201610275462A CN107321977B CN 107321977 B CN107321977 B CN 107321977B CN 201610275462 A CN201610275462 A CN 201610275462A CN 107321977 B CN107321977 B CN 107321977B
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- 238000010438 heat treatment Methods 0.000 title claims abstract description 99
- 238000005245 sintering Methods 0.000 title claims abstract description 47
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 34
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000009413 insulation Methods 0.000 claims abstract description 158
- 238000001816 cooling Methods 0.000 claims abstract description 54
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000007789 gas Substances 0.000 claims abstract description 28
- 230000000903 blocking effect Effects 0.000 claims abstract description 26
- 229910052786 argon Inorganic materials 0.000 claims abstract description 18
- 239000000112 cooling gas Substances 0.000 claims abstract description 18
- 238000007789 sealing Methods 0.000 claims description 27
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 12
- 238000011049 filling Methods 0.000 claims description 9
- 238000003825 pressing Methods 0.000 claims description 9
- 238000004321 preservation Methods 0.000 claims description 6
- 239000000498 cooling water Substances 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 2
- 239000004917 carbon fiber Substances 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 claims description 2
- 239000000835 fiber Substances 0.000 claims description 2
- 229910021385 hard carbon Inorganic materials 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 2
- 229910045601 alloy Inorganic materials 0.000 description 16
- 239000000956 alloy Substances 0.000 description 16
- 229910001172 neodymium magnet Inorganic materials 0.000 description 10
- -1 neodymium iron boron rare earth Chemical class 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 230000032683 aging Effects 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 238000009694 cold isostatic pressing Methods 0.000 description 3
- 238000010902 jet-milling Methods 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005219 brazing Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000000462 isostatic pressing Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910001004 magnetic alloy Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000013421 nuclear magnetic resonance imaging Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/003—Apparatus, e.g. furnaces
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
- C21D1/773—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material under reduced pressure or vacuum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
The invention provides a rare earth permanent magnet vacuum sintering method and vacuum sintering heat treatment equipment, wherein the equipment comprises a vacuum furnace body, a vacuum heat insulation gate valve, a vacuum heat insulation chamber, a heater and a vacuum gas cooling system, wherein one end of the vacuum heat insulation gate valve is connected with the vacuum furnace body, two side surfaces of the vacuum heat insulation chamber are provided with heat insulation gas baffle valves, and the vacuum gas cooling system is provided with a heat exchanger and a vacuum fan; the air outlet of the heat exchanger is connected with the air suction port of the vacuum fan, and the air inlet is communicated with the cooling gas channel on one side of the vacuum furnace body through a connecting pipe on the side; the exhaust port of the vacuum fan is communicated with the cooling gas channel at the side through a connecting pipe at the other side surface of the vacuum furnace body. The vacuum sintering method comprises the following steps: opening a vacuum heat insulation gate valve, putting the blank into vacuum sintering heat treatment equipment, vacuumizing and heating; and during cooling, argon is filled, the heat insulation air blocking valves on the two sides of the vacuum heat insulation chamber are opened, the two cooling fans are started alternately, and the heat insulation air blocking valves on the two sides are opened alternately or simultaneously.
Description
Technical Field
The invention relates to a rare earth permanent magnet vacuum sintering method and vacuum sintering heat treatment equipment, belonging to the technical field of rare earth permanent magnet manufacturing. The vacuum sintering heat treatment equipment can be used for sintering or aging of rare earth permanent magnet materials, and can also be used for vacuum sintering, heat treatment, brazing and the like of other metal materials.
Background
The neodymium iron boron rare earth permanent magnet material is a novel rare earth permanent magnet material discovered in 1983, is increasingly applied by excellent magnetic performance, and is widely applied to medical nuclear magnetic resonance imaging, computer hard disk drives, vibration motors of mobile phones, electroacoustic devices, hybrid electric vehicle motors, wind driven generators and the like.
At present, the vacuum furnace widely used for neodymium iron boron vacuum sintering and heat treatment in China mostly adopts a front zone, a middle zone and a rear zone along the length direction of a uniform temperature zone for heating in the arrangement of a heater. When the vacuum heat treatment equipment adopting the heater arrangement mode is used for heating under a vacuum condition, the temperature uniformity in the furnace is still enough, but when process gas or protective atmosphere is filled into the vacuum furnace according to the requirement of a heat treatment process, the gas can generate convection, the hot gas flows upwards, the temperature of the upper part in the furnace is increased, and the temperature uniformity in a uniform temperature zone is poor.
On the other hand, for the vacuum heat treatment equipment using gas cooling, the cooling uniformity is the key to determine the quality of the heat-treated product. In the existing air-cooled vacuum heat treatment equipment, an air pipe array type air cooling mode is generally adopted, the cooling uniformity of a workpiece is difficult to ensure in the process, and the process requirement of a high-quality heat treatment product is difficult to meet.
Disclosure of Invention
In view of the above problems, the invention arranges the heaters in the upper, middle and lower three zones, and the two ends of the uniform temperature zone are respectively provided with the independent heaters, thereby overcoming the defect that the temperature uniformity is reduced after the existing equipment is loaded. In addition, a plurality of heat insulation and air blocking valves are respectively arranged on two side walls of the vacuum heat insulation chamber, and are switched alternately, so that gas generates uniform vortex cyclone in a uniform temperature region, uniform cooling of workpieces is realized, and the defects of the existing equipment are overcome.
The invention provides vacuum sintering heat treatment equipment, which mainly comprises a vacuum furnace door, a vacuum furnace body, a vacuum heat insulation gate valve, a vacuum heat insulation chamber, a vacuum heat insulation gate, a heater, a vacuum gas cooling system and a vacuum unit, and is characterized in that: the vacuum furnace door is provided with an observation window, the vacuum furnace body is of a horizontal double-layer water-cooled wall structure, and a front flange and a rear flange are arranged at two ends of the vacuum furnace body; the vacuum heat insulation gate valve is provided with a valve body, a vacuum sealing valve plate and a pneumatic opening and pressing mechanism; the vacuum sealing valve plate is provided with a heat insulation layer; the vacuum furnace door is contacted with a front flange of the vacuum furnace body; one end of a valve body of the vacuum heat insulation gate valve is connected with a rear flange of the vacuum furnace body through a flange; the vacuum furnace door, the vacuum furnace body and the vacuum heat insulation gate valve form a closed vacuum container; the vacuum heat insulation chamber, the vacuum heat insulation door and the heat insulation layer of the vacuum sealing valve plate are arranged in the vacuum container; the vacuum heat insulation chamber is of a horizontal box-shaped structure, the front end of the vacuum heat insulation chamber is in contact with the vacuum heat insulation door, and the rear end of the vacuum heat insulation chamber is in contact with a heat insulation layer of the vacuum sealing valve plate; the vacuum heat insulation chamber is provided with a frame and a heat insulation layer; the heat insulation layer is arranged on the inner side of the frame; more than 1 heat-insulating air blocking valve is respectively arranged on two side surfaces of the vacuum heat-insulating chamber, a cooling gas channel is respectively arranged on two side surfaces of the frame, and the heat-insulating air blocking valves are sealed in the cooling gas channels; in a preferred embodiment, the heat insulation and air blocking valve is respectively provided with 2 valves on each side surface of the vacuum heat insulation chamber; the heater is arranged on the inner wall of the vacuum heat insulation chamber; the vacuum gas cooling system is provided with a heat exchanger and a vacuum fan; the air outlet of the heat exchanger is connected with the air suction port of the vacuum fan, the air inlet of the heat exchanger is connected with a connecting pipe on one side surface of the vacuum furnace body, and the connecting pipe passes through the vacuum furnace body and is communicated with a cooling gas channel on the same side of the vacuum heat insulation chamber; the exhaust port of the vacuum fan is connected with a connecting pipe on the other side surface of the vacuum furnace body, and the connecting pipe passes through the vacuum furnace body and is communicated with a cooling gas channel on the other side of the vacuum heat insulation chamber; the vacuum furnace body is also provided with a vacuumizing interface, and the vacuum unit is connected with the vacuumizing interface.
The vacuum gas cooling system is provided with a heat exchanger and two vacuum fans, air suction ports of the two vacuum fans are respectively connected with an air inlet and an air outlet of the heat exchanger, and exhaust ports of the two vacuum fans are respectively communicated with cooling gas channels on two sides of the vacuum heat insulation chamber through the vacuum furnace body.
The vacuum gas cooling system is characterized in that another vacuum fan is arranged between the air inlet of the heat exchanger and the connecting pipe on one side face of the vacuum furnace body, the air suction port of the other vacuum fan is connected with the air inlet of the heat exchanger, the air exhaust port of the other vacuum fan is connected with the connecting pipe on one side face of the vacuum furnace body, and the connecting pipe penetrates through the vacuum furnace body and is communicated with the cooling gas channel on the same side of the vacuum heat insulation chamber.
The vacuum furnace door is also provided with a hinge for opening and closing the vacuum furnace door and a gear ring for locking the vacuum furnace door, and a sealing ring is also arranged between the vacuum furnace door and a front flange of the vacuum furnace body; the vacuum heat insulation door is connected with the vacuum furnace door and is opened and closed together with the vacuum furnace door.
The vacuum furnace door is also provided with a hinge for opening and closing the vacuum furnace door and a gear ring for locking the vacuum furnace door, an air cylinder for driving the gear ring to rotate is arranged between the gear ring and the vacuum furnace body, an air cylinder for driving the vacuum furnace door to rotate is also arranged between the vacuum furnace door and the vacuum furnace body, and a sealing ring is also arranged between the vacuum furnace door and a front flange of the vacuum furnace body; the vacuum heat insulation door is connected with the vacuum furnace door and is opened and closed together with the vacuum furnace door.
The vacuum furnace body is also provided with temperature measuring thermocouples and a heater power supply leading-in electrode, and the number of the temperature measuring thermocouples is more than 3; the power supply lead-in electrode of the heater is internally provided with cooling water.
The pneumatic valve opening and pressing mechanism drives the vacuum sealing valve plate to move up and down and press the sealing ring.
The vacuum heat insulation chamber is a symmetrical octagonal horizontal box body, and the side lengths of the upper side, the lower side and the two side surfaces are larger than that of 4 bevel edges; and rib plates are welded on the outer side of the frame of the vacuum heat insulation chamber, and the height of each rib plate is less than 200mm.
The inner side of the heat-insulating layer is provided with a molybdenum sheet, and the frame, the heat-insulating layer and the molybdenum sheet are connected together through a molybdenum rod; the heat-insulating layer is made of more than one of ceramic fiber and carbon fiber.
The heat-insulating layer is made of hard carbon felt.
The heater consists of a front heater, a rear heater, an upper heater, a lower heater and 2 side heaters, wherein the front heater and the rear heater are of annular structures and are respectively arranged at the front end and the rear end of the vacuum heat insulation chamber, and the upper heater, the lower heater and the 2 side heaters are respectively arranged on the upper surface, the lower surface and two side surfaces of the vacuum heat insulation chamber; the heater is made of molybdenum or graphite.
A hearth is arranged on the inner side of the lower surface of the vacuum heat insulation chamber, an upright post is connected to the lower surface of the hearth, and the upright post penetrates through the heat insulation layer to be supported on the inner wall of the vacuum furnace body; the lower heater is arranged between the hearth and the inner wall of the lower side of the vacuum heat insulation chamber; the upper part of the hearth is a uniform temperature zone which is positioned in a space formed by an upper heater, a lower heater and 2 side heaters; placing the sintered or heat-treated workpiece on a hearth in a uniform temperature zone; the width of the uniform temperature zone is within the range of 400-1200mm, the height is within the range of 400-1200mm, and the length is within the range of 800-3500 mm; the highest temperature of the temperature equalizing zone is within the range of 500-1400 ℃.
The flange at the other end of the valve body is connected with the glove box; the glove box is provided with a glove box body, a feeding car, a transmission device, a lifting mechanism and a discharge door; the glove box body is provided with an observation window and gloves.
The flange at the other end of the valve body is connected with another plug board valve without a heat insulation layer, the other end of the plug board valve is connected with a movable box, and a feeding car, a transmission device and a lifting mechanism are arranged in the movable box; the movable box and the flashboard valve move together on the guide rail.
The vacuum unit comprises an oil diffusion vacuum pump, a Roots vacuum pump and a mechanical vacuum pump; ultimate vacuum degree higher than 5 × 10 -1 Pa。
A rare earth permanent magnet vacuum sintering method is characterized in that: the rare earth permanent magnet vacuum sintering method comprises the steps of firstly opening a vacuum heat insulation gate valve of vacuum sintering heat treatment equipment, conveying a magnetic field forming blank of the rare earth permanent magnet to a hearth of a vacuum heat insulation chamber under protective atmosphere, closing the vacuum heat insulation gate valve, and vacuumizing to the vacuum degree of 5 multiplied by 10 -1 Continuously vacuumizing and starting heating for 1-30 hours under the condition that the maximum heating temperature is 450-1100 ℃, stopping heating, closing a vacuumizing valve, filling argon, respectively opening heat insulation air blocking valves at two sides of a vacuum heat insulation chamber and alternately starting two cooling fans when the gas pressure exceeds 4000KPa, and then alternately or simultaneously opening or closing the heat insulation air blocking valves at the two sides; and then the cooling fan is stopped.
Before opening a vacuum heat insulation gate valve of rare earth permanent magnet vacuum sintering heat treatment equipment, packaging a blank of a magnetic field forming blank under the protection of nitrogen, then sending the blank into an isostatic pressing machine for cold isostatic pressing, wherein the cold isostatic pressing pressure is 150-300MPa, sending the blank into a glove box connected with a flange at the other end of the vacuum heat insulation gate valve after the cold isostatic pressing, removing the package under the protection of nitrogen in the glove box, filling the blank into a material box, then opening the vacuum heat insulation gate valve, and sending the blank onto a hearth of a vacuum heat insulation chamber under the protection atmosphere.
In another embodiment, before opening the vacuum heat insulation gate valve of the rare earth permanent magnet vacuum sintering heat treatment equipment, the blank formed by the magnetic field is sent into a moving box connected with a gate valve without a heat insulation layer under the protection of nitrogen, the moving box is butted with the vacuum heat insulation gate valve of the rare earth permanent magnet vacuum sintering heat treatment equipment, and then the vacuum heat insulation gate valve is opened to send the blank to a hearth of a vacuum heat insulation chamber.
The heating time is 1-30 hours, the highest heating temperature is 450-1100 ℃, firstly, the blank is heated to 400-600 ℃ within 1-9 hours and is kept warm, then, the blank is heated from 400-600 ℃ to 800-900 ℃ within 1-9 hours and is kept warm, then, the blank is heated from 800-900 ℃ to 1010-1090 ℃ within 1-5 hours and is kept warm, then, the heating is stopped, after argon is filled, a cooling fan is started, heat insulation air blocking valves on two sides of a vacuum heat insulation chamber are alternately opened, and then, two cooling fans are alternately switched on and off every 3-15 minutes.
The heating time is 1-30 hours, the highest heating temperature is 450-1100 ℃, firstly, the blank is heated to 300-600 ℃ within 1-9 hours and is subjected to heat preservation, and then, the blank is heated from 300-600 ℃ to 1010-1090 ℃ within 1-20 hours and is subjected to heat preservation; stopping heating, reducing the temperature to below 800 ℃, then heating the blank to 800-950 ℃ and preserving the heat; stopping heating, starting a cooling fan after filling argon gas and alternately opening heat insulation air blocking valves at two sides of a vacuum heat insulation chamber, alternately switching on and off the two cooling fans every 3-15 minutes until the temperature is cooled to below 400 ℃ and stopping cooling, continuing heating after vacuumizing, heating the blank to 460-640 ℃ within 1-9 hours and preserving heat, then stopping heating, starting the cooling fan after filling argon gas and alternately opening the heat insulation air blocking valves at two sides of the vacuum heat insulation chamber, and alternately switching on and off the two cooling fans every 3-15 minutes until the temperature is cooled to below 100 ℃ and stopping cooling.
The invention has the beneficial effects that:
1. the heaters are distributed in an upper three-zone area, a middle three-zone area and a lower three-zone area, and the two ends of the uniform temperature area are respectively provided with the independent heaters, so that the heating temperature of the vacuum heat treatment furnace is uniform under the loading condition, and the defect that the temperature uniformity is reduced after the vacuum heat treatment furnace is loaded, particularly after the vacuum heat treatment furnace is inflated, is overcome.
2. The two side walls of the vacuum heat-insulating chamber are respectively provided with a plurality of heat-insulating gas-blocking valves which are alternately switched, so that gas generates uniform vortex cyclone in a uniform temperature region, uniform cooling of a workpiece is realized, and the defects of the existing equipment are overcome; when in heating, the heat insulation gas baffle valve is closed, so that the heating is uniform, the heat leakage is less, the efficiency is high, and the energy is saved; and when the cooling is performed, the heat insulation air blocking valve is alternately switched on and off to reduce wind resistance, and the cooling efficiency and the cooling speed are improved.
3. The double fans realize positive and negative flow of air flow and solve the problem of cooling uniformity in the width direction of the workpiece.
4. The design of the movable box can ensure that the blank is prevented from being oxidized in the vacuum furnace under the protection of nitrogen on the one hand, and on the other hand, the movable box can be flexibly butted with the vacuum furnace and the press through the vacuum gate valve, so that the non-oxidation connection from pressing to sintering is realized, and the magnet performance is obviously improved.
Drawings
FIG. 1 is a schematic front view of an embodiment of a vacuum heat treatment sintering apparatus according to the present invention.
FIG. 2 is a schematic top view of an embodiment of a vacuum heat treatment sintering apparatus according to the present invention.
FIG. 3 is a left side view schematically showing a vacuum heat treatment sintering apparatus in which the other end of the vacuum heat insulation gate valve is connected to a glove box according to the present invention.
FIG. 4 is a schematic left side view of a gate valve without a thermal insulating layer and a moving box connected to the other end of a vacuum thermal insulation gate valve in another embodiment of the vacuum thermal treatment sintering apparatus according to the present invention.
Detailed Description
The invention is further illustrated with reference to the following figures and examples.
As shown in fig. 1-3, the present invention provides a vacuum sintering heat treatment apparatus, which mainly comprises a vacuum furnace door 1, a vacuum furnace body 2, a vacuum heat insulation gate valve 32, a vacuum heat insulation chamber 3, a vacuum heat insulation door 16, a heater, a vacuum gas cooling system 21 and a vacuum unit 7; an observation window 15 is arranged on the vacuum furnace door 1, the vacuum furnace body 2 is of a horizontal double-layer water-cooled wall structure, and a front flange 19 and a rear flange 35 are arranged at two ends of the vacuum furnace body 2; the vacuum heat insulation gate valve 32 is provided with a valve body 33, a vacuum sealing valve plate 28 and a pneumatic open valve pressing mechanism 34; the vacuum sealing valve plate 28 is provided with a heat insulation layer 27; the vacuum furnace door 1 is contacted with a front flange 19 of the vacuum furnace body 2; one end of a valve body 33 of the vacuum heat insulation gate valve 32 is connected with a rear flange 35 of the vacuum furnace body through a flange 36; the vacuum furnace door 1, the vacuum furnace body 2 and the vacuum heat insulation gate valve 32 form a closed vacuum container; the vacuum heat insulation chamber 3, the vacuum heat insulation door 16 and the heat insulation layer 27 of the vacuum sealing valve plate are arranged in the vacuum container; the vacuum heat insulation chamber 3 is a horizontal box-shaped structure, the front end of the vacuum heat insulation chamber 3 is contacted with the vacuum heat insulation door 16, and the rear end is contacted with a heat insulation layer 27 of the vacuum sealing valve plate; the vacuum heat insulation chamber 3 is provided with a frame 4 and a heat insulation layer 5; the heat insulation layer 5 is arranged on the inner side of the frame 4; more than 1 heat insulation air blocking valve 11 is respectively arranged on two side surfaces of the vacuum heat insulation chamber 3, cooling gas channels 29 and 6 are respectively arranged on two side surfaces of the frame 4, and the heat insulation air blocking valves 11 are sealed in the cooling gas channels 29 and 6; in a preferred embodiment, 2 insulating gas dampers 11 are provided on each side of the vacuum insulation chamber 3. The heater is arranged on the inner wall of the vacuum heat insulation chamber 3; the vacuum gas cooling system 21 is provided with a heat exchanger 22 and a vacuum fan 23; the air outlet of the heat exchanger 22 is connected with the air suction port of the vacuum fan 23, the air inlet of the heat exchanger 22 is connected with a connecting pipe 31 on one side surface of the vacuum furnace body 2, and the connecting pipe 31 penetrates through the vacuum furnace body 2 to be communicated with a cooling gas channel 29 on the same side of the vacuum heat insulation chamber 3; an exhaust port of the vacuum fan 23 is connected with a connecting pipe 52 on the other side surface of the vacuum furnace body 2, and the connecting pipe 52 penetrates through the vacuum furnace body 2 to be communicated with a cooling gas channel 6 on the other side of the vacuum heat insulation chamber 3; the vacuum furnace body 2 is also provided with a vacuumizing interface, and the vacuum unit 7 is connected with the vacuumizing interface.
In a preferred embodiment of the present invention, the vacuum gas cooling system 21 is provided with a heat exchanger 22 and two vacuum fans 23 and 30, suction ports of the two vacuum fans 23 and 30 are respectively connected to an air inlet and an air outlet of the heat exchanger 22, and exhaust ports of the two vacuum fans 23 and 30 are respectively communicated with cooling gas passages 29 and 6 on both sides of the vacuum heat insulation chamber 3 through the vacuum furnace body 2.
Further, the vacuum gas cooling system 21 is further provided with another vacuum fan 30 between the air inlet of the heat exchanger 22 and a connecting pipe 31 on one side of the vacuum furnace body 2, the air outlet is connected with the connecting pipe 31 on one side of the vacuum furnace body 2, and the connecting pipe passes through the vacuum furnace body 2 and is communicated with a cooling gas channel 29 on the same side of the vacuum heat insulation chamber 3.
The vacuum furnace door 1 is also provided with a hinge 17 for opening and closing the vacuum furnace door 1 and a gear ring 18 for locking the vacuum furnace door, and a sealing ring 20 is also arranged between the vacuum furnace door 1 and a front flange 19 of a vacuum furnace body; the vacuum heat insulation door 16 is connected to the vacuum oven door 1 and is opened and closed together with the vacuum oven door 1. An air cylinder for driving the gear ring 18 to rotate is arranged between the gear ring 18 and the vacuum furnace body 2, and an air cylinder for driving the vacuum furnace door 1 to rotate is also arranged between the vacuum furnace door 1 and the vacuum furnace body 2. The vacuum furnace body 2 is also provided with temperature thermocouples 9 and a heater power supply leading-in electrode 8, and the number of the temperature thermocouples 9 is more than 3; the heater power supply lead-in electrode 8 is internally provided with cooling water. The vacuum sealing valve plate 28 is filled with cooling water, a sealing ring 37 is arranged between the vacuum sealing valve plate 28 and the valve body 33, the vacuum sealing valve plate 28 is connected with a pneumatic open valve pressing mechanism 34 through a hinge 38, and the pneumatic open valve pressing mechanism 34 drives the vacuum sealing valve plate 28 to move up and down and press the sealing ring 37. The vacuum heat insulation chamber 3 is a symmetrical octagonal horizontal box body, and the side lengths of the upper side, the lower side and the two side surfaces are larger than that of 4 bevel edges; and rib plates are welded on the outer side of the frame 4 of the vacuum heat insulation chamber 3, and the height of each rib plate is less than 200mm. The inner side of the heat preservation layer 5 is provided with a molybdenum sheet, and the frame 4, the heat preservation layer 5 and the molybdenum sheet are connected together through a molybdenum rod.
The heater is composed of a front heater 24, a rear heater 26, an upper heater 10, a lower heater 14 and 2 side heaters 25, wherein the front heater 24 and the rear heater 26 are both ring-shaped structures and are respectively arranged at the front end and the rear end of the vacuum insulation chamber 3, and the upper heater 10, the lower heater 14 and the 2 side heaters 25 are respectively arranged at the upper surface, the lower surface and two side surfaces of the vacuum insulation chamber 3; the heater is made of molybdenum or graphite.
A hearth 12 is arranged on the inner side of the lower surface of the vacuum heat insulation chamber 3, an upright post 13 is connected to the lower surface of the hearth 12, and the upright post 13 penetrates through the heat insulation layer 5 and is supported on the inner wall of the vacuum furnace body 2; the upper part of the hearth 12 is a uniform temperature zone which is positioned in a space formed by the upper heater 10, the lower heater 14 and the 2 side heaters 25; the sintered or heat-treated workpiece is placed on the hearth 12 and is placed in a uniform temperature zone; the width of the uniform temperature zone is within the range of 400-1200mm, the height is within the range of 400-1200mm, and the length is within the range of 800-3500 mm; the highest temperature of the temperature equalizing zone is within the range of 500-1400 ℃.
In one embodiment of the present invention, a flange 39 at the other end of the valve body 33 is connected to a glove box 41; the glove box 41 is provided with a glove box body 40, a feeding car 43, a transmission device 44, a lifting mechanism 45 and a discharge door 42; the glove box body 40 is provided with an observation window and gloves.
In another embodiment of the invention, the flange 39 at the other end of the valve body 33 is connected with another flashboard valve 46 without an insulating layer, the other end of the flashboard valve 46 is connected with a movable box 47, and a feeding cart 48, a transmission device 49 and a lifting mechanism 50 are arranged in the movable box 47; the moving box 47 and the gate valve 46 move together on the guide rail 51.
Example 1
Firstly, preparing neodymium iron boron rare earth permanent magnet alloy, preparing the alloy into alloy powder through hydrogen crushing and jet milling, molding the alloy powder by using a press to prepare rare earth permanent magnet blank, and then conveying the rare earth permanent magnet blank into a vacuum heat treatment furnace to perform the following vacuum sintering process:
vacuumizing to the vacuum degree of 5 multiplied by 10 -1 Heating at a temperature above Pa, heating the blank to 440 ℃ for 1 hour, preserving heat for 2 hours, heating the blank to 850 ℃ for 3 hours, preserving heat for 2 hours, heating the blank to 1070 ℃ for 2.5 hours, preserving heat for 2.5 hours, stopping heating, introducing argon, starting a vacuum fan and alternately opening heat insulation air blocking valves at two sides of a vacuum heat insulation chamber when the pressure in the furnace exceeds 4000Pa, and then performing two vacuum heat insulation for 5 minutesThe fan is switched on and off alternately once until the temperature is cooled to be below 100 ℃, and the vacuum fan is switched off to stop cooling.
And after sintering, taking the sintered blank out of the vacuum heat treatment furnace, putting the sintered blank into a common vacuum heat treatment furnace (three zones in front, middle and back of a heater, and air-cooling in an air duct type), carrying out vacuum aging treatment at 900 ℃ for 2 hours and at 500 ℃ for 3 hours, and respectively carrying out argon filling and air cooling after 900 ℃ and 500 ℃ are insulated to prepare the neodymium-iron-boron rare earth permanent magnet material P1.
Example 2
Firstly, preparing neodymium iron boron rare earth permanent magnetic alloy, preparing the alloy into alloy powder through hydrogen crushing and jet milling, molding the alloy powder by using a press to prepare rare earth permanent magnetic blank, and then sending the rare earth permanent magnetic blank into a vacuum heat treatment furnace to perform the following vacuum sintering and heat treatment procedures:
vacuumizing to the vacuum degree of 5 multiplied by 10 -1 Heating is started when the pressure is higher than Pa, the blank is heated to 440 ℃ for 1 hour, the blank is kept warm for 2 hours, then the blank is heated to 1070 ℃ for 5 hours after 2.5 hours, then the heating is stopped, the temperature is reduced to below 800 ℃, then the blank is heated to 900 ℃, the heating is stopped for 2 hours, then the heating is stopped, argon gas is filled, when the pressure in the furnace exceeds 4000Pa, a vacuum fan is started and heat insulation air blocking valves on the two sides of the vacuum heat insulation chamber are opened and closed alternately for one time after 5 minutes until the temperature is cooled to 300 ℃, the vacuum fan is turned off and stopped cooling, then the blank is heated to 500 ℃, the temperature is kept for 3 hours after vacuumizing, then the heating is stopped, one vacuum fan is started after the argon gas is filled, the heat insulation air blocking valves on the two sides of the vacuum heat insulation chamber are opened alternately, the two vacuum fans are turned on and closed alternately for one time after 5 minutes until the temperature is cooled to below 100 ℃, and the vacuum fan is turned off and stopped cooling is stopped, and the neodymium iron boron rare earth permanent magnet material P2 is prepared.
Example 3
Firstly, preparing neodymium iron boron rare earth permanent magnet alloy, performing hydrogen crushing and airflow milling on the alloy to prepare alloy powder, molding the alloy powder by using a press to prepare rare earth permanent magnet blank, then conveying the rare earth permanent magnet blank into a common vacuum sintering furnace (three zones in front, middle and back of a heater, and air cooling in an air duct type), and performing the following vacuum sintering process:
vacuumizing to the vacuum degree of 5 multiplied by 10 -1 Heating is started when the temperature is higher than Pa, the blank is firstly heated to 440 ℃ for 1 hour, the temperature is kept for 2 hours, then the blank is heated to 1070 ℃ for 2.5 hours, the temperature is kept for 5 hours, argon is filled for air cooling, and the vacuum fan is turned off until the temperature is cooled to be lower than 100 ℃ to stop cooling.
Then taking out the sintered blank and putting the sintered blank into a vacuum heat treatment furnace of the invention for vacuum aging treatment: heating the blank to 900 ℃, preserving heat for 2 hours, stopping heating, filling argon, starting a vacuum fan and alternately opening heat insulation air blocking valves at two sides of a vacuum heat insulation chamber when the pressure in the furnace exceeds 4000Pa, alternately switching on and off the two vacuum fans once in 5 minutes until the temperature is cooled to 300 ℃, stopping cooling the vacuum fan, vacuumizing, continuing heating, heating the blank to 500 ℃, preserving heat for 3 hours, then stopping heating, starting a vacuum fan and alternately opening heat insulation air blocking valves at two sides of the vacuum heat insulation chamber after filling argon, alternately switching on and off the two vacuum fans once in 5 minutes until the temperature is cooled to be below 100 ℃, and stopping cooling by switching off the vacuum fans to prepare the neodymium iron boron rare earth permanent magnet material P3.
Comparative example:
firstly, preparing neodymium iron boron rare earth permanent magnet alloy, performing hydrogen crushing and airflow milling on the alloy to prepare alloy powder, molding the alloy powder by using a press to prepare rare earth permanent magnet blank, then sending the rare earth permanent magnet blank into a common vacuum sintering furnace (three zones in front, middle and back of a heater, and air cooling by an air pipe), and performing the following vacuum sintering process:
vacuumizing to the vacuum degree of 5 multiplied by 10 -1 Heating at above Pa, heating blank to 440 deg.C for 1 hr, holding for 2 hr, heating blank to 1070 deg.C for 5 hr, stopping heating to reduce temperature to below 800 deg.C, heating blank to 900 deg.C, holding for 2 hr, stopping heating, introducing argon gas, air cooling, cooling to below 100 deg.C, stopping vacuum blower, stopping heating, and coolingAnd (6) cooling.
And then taking out the sintered blank, putting the sintered blank into a common vacuum heat treatment furnace, heating to 500 ℃, preserving heat for 3 hours, and then filling argon for air cooling for vacuum aging treatment to prepare the neodymium iron boron rare earth permanent magnet material C1.
Through detection, on the premise of the same alloy components, the intrinsic coercive forces of P2 and P3 are respectively 940Oe and 560Oe higher than C1, the maximum magnetic energy products are respectively 2MGOe and 0.8MGOe higher than C1, the intrinsic coercive force of P1 is 300Oe higher than C1, the maximum magnetic energy products are 1.2MGOe higher than C1, and the performance consistency of P2 subjected to vacuum sintering and vacuum aging treatment in the vacuum heat treatment equipment is obviously better than that of C1, P1 and P3.
Claims (11)
1. The utility model provides a vacuum sintering heat treatment equipment, mainly includes vacuum furnace door, vacuum furnace body, the thermal-insulated push-pull valve in vacuum, vacuum heat insulation chamber, vacuum heat insulation door, heater, vacuum gas cooling system and vacuum unit, its characterized in that: the vacuum furnace door is provided with an observation window, the vacuum furnace body is of a horizontal double-layer water-cooled wall structure, and a front flange and a rear flange are arranged at two ends of the vacuum furnace body; the vacuum heat insulation gate valve is provided with a valve body, a vacuum sealing valve plate and a pneumatic opening and pressing mechanism; the vacuum sealing valve plate is provided with a heat insulation layer; the vacuum furnace door is contacted with a front flange of the vacuum furnace body; one end of a valve body of the vacuum heat insulation gate valve is connected with a rear flange of the vacuum furnace body through a flange; the vacuum furnace door, the vacuum furnace body and the vacuum heat insulation gate valve form a closed vacuum container; the vacuum heat insulation chamber, the vacuum heat insulation door and the heat insulation layer of the vacuum sealing valve plate are arranged in the vacuum container; the vacuum heat insulation chamber is of a horizontal box-shaped structure, the front end of the vacuum heat insulation chamber is in contact with the vacuum heat insulation door, and the rear end of the vacuum heat insulation chamber is in contact with a heat insulation layer of the vacuum sealing valve plate; the vacuum heat insulation chamber is provided with a frame and a heat insulation layer; the heat insulation layer is arranged on the inner side of the frame; more than 1 heat insulation air blocking valve is respectively arranged on two side surfaces of the vacuum heat insulation chamber, cooling gas channels are respectively arranged on two side surfaces of the frame, and the heat insulation air blocking valves are sealed in the cooling gas channels; the heater is arranged on the inner wall of the vacuum heat insulation chamber; the vacuum gas cooling system is provided with a heat exchanger and two vacuum fans, air suction ports of the two vacuum fans are respectively connected with an air inlet and an air outlet of the heat exchanger, and exhaust ports of the two vacuum fans are respectively communicated with cooling gas channels on two sides of the vacuum heat insulation chamber through the vacuum furnace body; the air inlet of the heat exchanger is connected with a connecting pipe on one side surface of the vacuum furnace body, and the connecting pipe passes through the vacuum furnace body and is communicated with a cooling gas channel on the same side of the vacuum heat insulation chamber; the vacuum furnace body is also provided with a vacuumizing interface, and the vacuum unit is connected with the vacuumizing interface; the vacuum sealing valve plate is connected with the pneumatic open valve pressing mechanism through a hinge; the heater consists of a front heater, a rear heater, an upper heater, a lower heater and 2 side heaters, wherein the front heater and the rear heater are of annular structures and are respectively arranged at the front end and the rear end of the vacuum heat insulation chamber, and the upper heater, the lower heater and the 2 side heaters are respectively arranged at the upper side, the lower side and two side surfaces of the vacuum heat insulation chamber; the heater is made of molybdenum or graphite; a hearth is arranged on the inner side below the vacuum heat insulation chamber, and an upright post is connected below the hearth; the upper part of the hearth is a uniform temperature zone which is positioned in a space formed by an upper heater, a lower heater and 2 side heaters; the sintered or heat-treated workpiece is placed on a hearth and is placed in a uniform temperature zone; the width of the temperature equalizing zone is within the range of 400-1200mm, the height is within the range of 400-1200mm, and the length is within the range of 800-3500 mm.
2. A vacuum sintering heat treatment apparatus as set forth in claim 1, wherein: the heat insulation air baffle valves are respectively provided with 2 on each side surface of the vacuum heat insulation chamber.
3. The vacuum sintering heat treatment apparatus according to claim 1, wherein: the vacuum furnace door is also provided with a hinge for opening and closing the vacuum furnace door and a gear ring for locking the vacuum furnace door, and a sealing ring is also arranged between the vacuum furnace door and a front flange of the vacuum furnace body; the vacuum heat insulation door is connected with the vacuum furnace door and is opened and closed together with the vacuum furnace door.
4. A vacuum sintering heat treatment apparatus as set forth in claim 1, wherein: the vacuum furnace body is also provided with temperature measuring thermocouples and a heater power supply leading-in electrode, and the number of the temperature measuring thermocouples is more than 3; the power supply lead-in electrode of the heater is internally provided with cooling water.
5. A vacuum sintering heat treatment apparatus as set forth in claim 1, wherein: the pneumatic open valve pressing mechanism drives the vacuum sealing valve plate to move up and down and press the sealing ring.
6. A vacuum sintering heat treatment apparatus as set forth in claim 1, wherein: the vacuum heat insulation chamber is a symmetrical octagonal horizontal box body, and the side lengths of the upper side, the lower side and the two side surfaces are larger than that of 4 bevel edges; and rib plates are welded on the outer side of the frame of the vacuum heat insulation chamber, and the height of each rib plate is less than 200mm.
7. A vacuum sintering heat treatment apparatus as set forth in claim 1, wherein: the inner side of the heat-insulating layer is provided with a molybdenum sheet, and the frame, the heat-insulating layer and the molybdenum sheet are connected together through a molybdenum rod; the heat-insulating layer is made of more than one of ceramic fiber and carbon fiber.
8. A vacuum sintering heat treatment apparatus as set forth in claim 1, wherein: the heat-insulating layer is made of hard carbon felt.
9. A rare earth permanent magnet vacuum sintering method comprises the following steps:
a heating procedure: opening a vacuum heat insulation gate valve of vacuum sintering heat treatment equipment, conveying the blank formed by the magnetic field of the rare earth permanent magnet to a hearth of a vacuum heat insulation chamber under protective atmosphere, closing the vacuum heat insulation gate valve, and vacuumizing to the vacuum degree of 5 multiplied by 10 - 1 Continuously vacuumizing and heating for 1-30 hours at the maximum heating temperature of 450-110 PaWithin 0 ℃, and then stopping heating;
a cooling process: argon is filled, when the gas pressure exceeds 4000Pa, the heat insulation air blocking valves at two sides of the vacuum heat insulation chamber are respectively opened, the two vacuum fans are alternately started, and then the heat insulation air blocking valves at two sides are alternately or simultaneously opened and closed.
10. The vacuum sintering method of rare earth permanent magnet according to claim 9, characterized in that: in the heating procedure, firstly, the blank is heated to 400-600 ℃ within 1-9 hours and is kept warm, then the blank is heated from 400-600 ℃ to 800-900 ℃ within 1-9 hours and is kept warm, then the blank is heated from 800-900 ℃ to 1010-1090 ℃ within 1-5 hours and is kept warm, and then the heating is stopped; in the cooling procedure, after argon is filled, one vacuum fan is started, the heat insulation air blocking valves on two sides of the vacuum heat insulation chamber are opened alternately, and then the two vacuum fans are switched on and off alternately every 3-15 minutes.
11. The vacuum sintering method of rare earth permanent magnet according to claim 9, characterized in that: in the heating procedure, firstly, the blank is heated to 300-600 ℃ within 1-9 hours and is subjected to heat preservation, and then the blank is heated from 300-600 ℃ to 1010-1090 ℃ within 1-20 hours and is subjected to heat preservation; stopping heating, reducing the temperature to below 800 ℃, then heating the blank to 800-950 ℃, preserving heat, and then stopping heating; in the cooling procedure, after argon is filled, a vacuum fan is started, heat insulation air blocking valves on two sides of a vacuum heat insulation chamber are alternately opened, then two vacuum fans are alternately switched on and off every 3-15 minutes, and the vacuum fans are switched off and stop cooling until the temperature is cooled to be below 400 ℃;
and then vacuumizing and heating again, heating the blank to 460-640 ℃ within 1-9 hours, preserving heat, stopping heating, filling argon, starting a vacuum fan, alternately opening heat insulation air blocking valves at two sides of a vacuum heat insulation chamber, and alternately switching on and off the two vacuum fans every 3-15 minutes until the temperature is cooled to be below 100 ℃, and switching off the vacuum fans to stop cooling.
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| CN108788360A (en) * | 2018-05-22 | 2018-11-13 | 滁州华海中谊工业炉有限公司 | A kind of vacuum high-temperature soldering oven being quickly cooled down |
| CN110243188B (en) * | 2019-06-20 | 2020-07-14 | 信丰县包钢新利稀土有限责任公司 | Neodymium iron boron vacuum sintering furnace |
| CN110695359B (en) * | 2019-10-30 | 2022-07-19 | 钢研昊普科技有限公司 | Hot isostatic pressing device and production process of densified product |
| JP7338818B2 (en) * | 2019-11-28 | 2023-09-05 | 島津産機システムズ株式会社 | heat treatment furnace |
| CN112414141B (en) * | 2020-11-26 | 2023-04-07 | 东莞市中汉磁材科技有限公司 | Sintering furnace for producing strong magnetic products and using method thereof |
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