CN101028652A - Magnetic-field temperature-pressure formation - Google Patents

Magnetic-field temperature-pressure formation Download PDF

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Publication number
CN101028652A
CN101028652A CN 200710062677 CN200710062677A CN101028652A CN 101028652 A CN101028652 A CN 101028652A CN 200710062677 CN200710062677 CN 200710062677 CN 200710062677 A CN200710062677 A CN 200710062677A CN 101028652 A CN101028652 A CN 101028652A
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magnetic
powder
material powder
permanent
magnetic material
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CN 200710062677
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Inventor
张深根
曲选辉
左志军
田建军
王健
秦明礼
何新波
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University of Science and Technology Beijing USTB
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University of Science and Technology Beijing USTB
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Priority to CN 200710062677 priority Critical patent/CN101028652A/en
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Abstract

A magnetic-field thermo-pressing process for preparing the high-performance magnetic material with magnetic anisotropy includes such steps as preparing the ultra-magnetostrictive RE powder or permanent-magnet NdFeB powder or permanent-magnet SmCo powder in vacuum or inertial gas or organic medium, mixing it with adhesive, coupling agent and lubricant, and thermopressing at 80-350 deg.C under 300-900 MPa in a magnetic field (1.5-2.5T).

Description

A kind of magnetic-field temperature-pressure formation
Technical field
The invention belongs to technical field of material, a kind of magnetic-field temperature-pressure formation particularly is provided, be applicable to that preparation has magnetic anisotropic characteristics, high performance magnetic material, as agglutinate rare earth ultra-magnetostriction material and bonding rare earth permanent magnet material.
Background technology
Press forming is a manufacturing process the most general in the PM technique.Its objective is the pressed compact that obtains definite shape and size, and make it have certain density and intensity.Owing to have only the pressure field effect in this forming process, thereby only be applicable to and make isotropic material, and exist big frictional force to make the inhomogeneous of the density of pressed compact and intensity distributions in the pressing process between powder and powder, powder and the die wall, the powder compaction sclerosis is difficult to factors such as elimination, causes green density to improve difficulty.For further improving green density, adopt isostatic cool pressing or high temperature insostatic pressing (HIP) usually, cause the production cost height.
Magnetic forming is to add an alignment magnetic field on the basis of common mold pressing, is used to have magnetic anisotropy powdered metallurgical material orientation and is shaped the particularly shaping of rare earth permanent-magnetic material.The document of relevant magnetic forming is a lot, announced patent in July 11 calendar year 2001 as Sumitomo Special Metal Co., Ltd: the manufacturing method of pressed body of rare earth alloy powder, building mortion and rare-earth magnet (CN00129884.4), adopt the limit externally-applied magnetic field to be orientated the orientation compression section of exerting pressure to rare earth alloy powder in the limit, obtain pressed compact in the N level with certain degree of orientation.The magnetic forming process is because the rotary resistance of powder orientation is big, the frictional force between powder and powder, powder and the die wall, and factors such as powder sclerosis cause the density of pressed compact, the degree of orientation undesirable.Adopt isostatic cool pressing that green density is increased, but can advance once causing the pressed compact degree of orientation to worsen, influence the performance of material.
For improving powder compact density, U.S. Hoeganaes company has announced temperature-pressure formation in international powder metallurgy in 1994 and granular materials meeting (PM TEC94), it is the manufacturing high density that grows up on conventional moulded technology basis, the low-cost new technology of high-performance powder metallurgy parts.Temperature-pressure formation is exactly that the special powder of employing is heated, powder is carried and mold heating system, be heated to 80~150 ℃ with being added with the pre-alloyed powder of special lubricant and mould etc., simultaneously for guaranteeing good powder flowbility and powder filling behavior, temperature fluctuation range is controlled at ± 2.5 ℃ in, suppress by the conventional powder pressing process then.It can once the compacting, sintering condition under make the density of powdered metal parts and correlated performance obtain bigger raising, for powdered metal parts has found the binding site an of the best, the of paramount importance technological progress in powder metallurgy production technology aspect since being considered to enter the nineties between performance and cost.
For having the magnetic anisotropy powder metallurgy magnetic material, improving the green density and the degree of orientation is to improve the key of material property.The present invention organically combines magnetic forming technology and temperature-pressure formation, and the magnetic material forming process is introduced in pressure field, temperature field and magnetic field jointly, improves the density and the degree of orientation of pressed compact, thereby reaches the low-cost purpose that improves material property.The present invention is applicable to the bonded permanent magnet of preparation high-performance anisotropic, as high-performance agglutinate rare earth ultra-magnetostriction material and cohesive rare earth permanent-magnetic material.
Summary of the invention
The object of the present invention is to provide a kind of magnetic-field temperature-pressure New Forming Process, with magnetic forming and organically combination of warm-pressing formation, be the low cost process that preparation has magnetic anisotropic characteristics, high performance magnetic material, be specially adapted to agglutinate rare earth ultra-magnetostriction material and bonding rare earth permanent magnet material
Technical process of the present invention comprises the steps:
1, prepared sizes are rare earth ultra-magnetostriction material powder or the Nd-Fe-Bo permanent magnet material powder of 40.0 μ m-240.0 μ m or the samarium-cobalt permanent-magnetic material powder of 40.0 μ m-200.0 μ m of 40.0 μ m-550.0 μ m under vacuum or inert gas or organic media protection;
2, magnetic material powder also evenly mixes in proportion with binding agent, coupling agent, lubricant;
3, the powder that mixes being carried out magnetic-field temperature-pressure is shaped, shaping pressure 300MPa-900MPa, alignment magnetic field is 1.5T-2.5T, and forming temperature is 80 ℃-180 ℃ (rare earth ultra-magnetostriction materials) or be 80 ℃-280 ℃ (Nd-Fe-Bo permanent magnet materials) or be 80 ℃-350 ℃ (samarium-cobalt permanent-magnetic materials);
4, the relative density of agglutinate rare earth ultra-magnetostriction material is that 70.0%-88.0%, magnetostriction coefficient λ are 600ppm-1200ppm after solidifying; The relative density of binding Nd-Fe-B permanent magnetic material is 65.0%-85.0%, maximum magnetic energy product (BH) after solidifying MaxReach 96.0kJ/m 3-155.0kJ/m 3, remanent magnetism Br reaches 0.70T-0.95T; The relative density of bonding samarium-cobalt permanent-magnetic material is 65.0%-90.0%, maximum magnetic energy product (BH) after solidifying MaxReach 68.0kJ/m 3-120.0kJ/m 3, remanent magnetism Br reaches 0.65T-0.85T.
Magnetic material powder of the present invention is: rare earth ultra-magnetostriction material powder, Nd-Fe-Bo permanent magnet material powder or samarium-cobalt permanent-magnetic material powder.Described binding agent is: epoxy resin, phenolic resins, nylon, maleic anhydride or both mixtures wherein.Described coupling agent is: KH550 silane, titanate esters or both mixtures.Described lubricant is: paraffin, zinc stearate or both mixtures.
Of the present inventionly be a little, in forming process to powder exert pressure simultaneously, magnetic field and temperature field; Pressure field and temperature field acting in conjunction can obtain high green density in powder; Thereby magnetic field and temperature field acting in conjunction can reduce the degree of orientation that the powder rotary resistance improves pressed compact.With magnetic forming and organically combination of warm-pressing formation, be the low cost process that preparation has magnetic anisotropic characteristics, high performance magnetic material, be specially adapted to agglutinate rare earth ultra-magnetostriction material and bonding rare earth permanent magnet material.In forming process to powder exert pressure simultaneously, magnetic field and temperature field; Pressure field and temperature field acting in conjunction can obtain high green density in powder; Thereby magnetic field and temperature field acting in conjunction can reduce the degree of orientation that the powder rotary resistance improves pressed compact.
The specific embodiment
Embodiment 1
Prepared sizes are the rare earth ultra-magnetostriction material powder of 40.0 μ m under vacuum or inert gas or organic media protection, evenly mix with the epoxy adhesive of powder weight 1%, 0.1% KH550 silane coupler, 0.1% zinc stearate lubricant in the glove box of high-purity argon gas protection.The powder that mixes is carried out magnetic-field temperature-pressure be shaped, shaping pressure 300MPa, alignment magnetic field are 1.5T, and forming temperature is 80 ℃.Pressed compact obtains agglutinate rare earth ultra-magnetostriction material after solidifying, relative density is 70.0% (6470kg/m 3), magnetostriction coefficient λ is 600ppm.
Embodiment 2
Prepared sizes are the rare earth ultra-magnetostriction material powder of 550.0 μ m under vacuum or inert gas or organic media protection, evenly mix with the epoxy adhesive of powder weight 5%, 3% KH550 silane coupler, 2% zinc stearate lubricant in the glove box of high-purity argon gas protection.The powder that mixes is carried out magnetic-field temperature-pressure be shaped, shaping pressure 900MPa, alignment magnetic field are 2.5T, and forming temperature is 180 ℃.Pressed compact obtains agglutinate rare earth ultra-magnetostriction material after solidifying, relative density is 88.0% (8140kg/m 3), magnetostriction coefficient λ is 1200ppm.
Embodiment 3
Prepared sizes are the NdFeB material powder of 40.0 μ m under vacuum or inert gas or organic media protection, and the lubricant that the binding agent that mixes with the epoxy resin and the maleic anhydride (2: 1) of powder weight 2% in the glove box of high-purity argon gas protection, 0.1% KH550 silane coupler, 0.1% paraffin and zinc stearate (1: 1) mix evenly mixes.The powder that mixes is carried out magnetic-field temperature-pressure be shaped, shaping pressure 300MPa, alignment magnetic field are 1.5T, and forming temperature is 80 ℃.Pressed compact obtains the Agglutinate neodymium-iron-boron material after solidifying, relative density is 65.0% (4875kg/m 3), maximum magnetic energy product (BH) MaxReach 96.0kJ/m 3, remanent magnetism Br reaches 0.70T.
Embodiment 4
Prepared sizes are the NdFeB material powder of 240.0 μ m under vacuum or inert gas or organic media protection, and the lubricant that the binding agent that mixes with the epoxy resin and the maleic anhydride (1: 1) of powder weight 4% in the glove box of high-purity argon gas protection, 2% titanate coupling agent, 2% paraffin and zinc stearate (1: 1) mix evenly mixes.The powder that mixes is carried out magnetic-field temperature-pressure be shaped, shaping pressure 900MPa, alignment magnetic field are 2.5T, and forming temperature is 280 ℃.Pressed compact obtains the Agglutinate neodymium-iron-boron material after solidifying, relative density is 85.0% (6375kg/m 3), maximum magnetic energy product (BH) MaxReach 155.0kJ/m 3, remanent magnetism Br reaches 0.95T.
Embodiment 5
Prepared sizes are the samarium-cobalt material powder of 40.0 μ m under vacuum or inert gas or organic media protection, and the lubricant that the binding agent that mixes with the epoxy resin and the maleic anhydride (1: 1) of powder weight 1% in the glove box of high-purity argon gas protection, 0.1% KH550 silane coupler, 0.2% paraffin and zinc stearate (1: 1) mix evenly mixes.The powder that mixes is carried out magnetic-field temperature-pressure be shaped, shaping pressure 300MPa, alignment magnetic field are 1.5T, and forming temperature is 80 ℃.Pressed compact obtains the samarium-cobalt material that bonds after solidifying, relative density is 65.0% (5525kg/m 3), maximum magnetic energy product (BH) MaxReach 68.0kJ/m 3, remanent magnetism Br reaches 0.65T.
Embodiment 6
Prepared sizes are the samarium-cobalt material powder of 200.0 μ m under vacuum or inert gas or organic media protection, and the lubricant that the binding agent that mixes with the epoxy resin and the maleic anhydride (2: 1) of powder weight 4% in the glove box of high-purity argon gas protection, 3% KH550 silane coupler, 3% paraffin and zinc stearate (3: 1) mix evenly mixes.The powder that mixes is carried out magnetic-field temperature-pressure be shaped, shaping pressure 900MPa, alignment magnetic field are 2.5T, and forming temperature is 350 ℃.Pressed compact obtains the samarium-cobalt material that bonds after solidifying, relative density is 90.0% (7650kg/m 3), maximum magnetic energy product (BH) MaxReach 120.0kJ/m 3, remanent magnetism Br reaches 0.85T.

Claims (5)

1, a kind of magnetic-field temperature-pressure formation is characterized in that, technology is:
(1) prepared sizes are rare earth ultra-magnetostriction material powder or the Nd-Fe-Bo permanent magnet material powder of 40.0 μ m-240.0 μ m or the samarium-cobalt permanent-magnetic material powder of 40.0 μ m-200.0 μ m of 40.0 μ m-550.0 μ m under vacuum or inert gas or organic media protection;
(2) magnetic material powder also evenly mixes in proportion with binding agent, coupling agent, lubricant;
(3) powder that mixes is carried out magnetic-field temperature-pressure and be shaped, shaping pressure 300MPa-900MPa, alignment magnetic field are 1.5T-2.5T, and forming temperature is 80 ℃-350 ℃.
According to the described technology of claim 1, it is characterized in that 2, described magnetic material powder is: rare earth ultra-magnetostriction material powder, Nd-Fe-Bo permanent magnet material powder or samarium-cobalt permanent-magnetic material powder; Described binding agent is: epoxy resin, maleic anhydride or both mixtures; Described coupling agent is: KH550 silane, titanate esters or both mixtures.Described lubricant is: paraffin, zinc stearate or both mixtures.
According to claim 1 or 2 described technologies, it is characterized in that 3, the forming temperature of preparation agglutinate rare earth ultra-magnetostriction material is 80 ℃-180 ℃; The relative density of c, agglutinate rare earth ultra-magnetostriction material is that 70.0%-88.0%, magnetostriction coefficient λ are 600ppm-1200ppm.
4, technology according to claim 1 and 2 is characterized in that, the forming temperature of preparation binding Nd-Fe-B permanent magnetic material is 80 ℃-280 ℃; The relative density of binding Nd-Fe-B permanent magnetic material is 65.0%-85.0%, maximum magnetic energy product (BH) MaxReach 96.0kJ/m 3-155.0kJ/m 3, remanent magnetism Br reaches 0.70T-0.95T.
5, technology according to claim 1 and 2 is characterized in that, the forming temperature of preparation bonding samarium-cobalt permanent-magnetic material is 80 ℃-350 ℃; The relative density of bonding samarium-cobalt permanent-magnetic material is 65.0%-90.0%, maximum magnetic energy product (BH) MaxReach 68.0kJ/m 3-120.0kJ/m 3, remanent magnetism Br reaches 0.65T-0.85T.
CN 200710062677 2007-01-12 2007-01-12 Magnetic-field temperature-pressure formation Pending CN101028652A (en)

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101934371A (en) * 2010-09-13 2011-01-05 华南理工大学 Permanent magnet material forming method and device under multi-external field coupling effect
CN102240805A (en) * 2011-07-27 2011-11-16 湖南航天工业总公司 Method for preparing anisotropic bonded rare-earth permanent magnet
CN101593590B (en) * 2009-04-10 2012-03-28 华中科技大学 Method for preparing warm compaction molding phenolic resin bonded Nd-Fe-B magnet
CN102412043A (en) * 2011-07-28 2012-04-11 横店集团东磁股份有限公司 Manufacturing method of anisotropic NdFeB radial orientation magnet ring
CN102969116A (en) * 2012-07-20 2013-03-13 横店集团东磁股份有限公司 UV (ultraviolet) solidified bonding magnet and preparation method thereof
CN104377028A (en) * 2009-08-28 2015-02-25 因太金属株式会社 Method and device for producing sintered NdFeB magnet, and sintered NdFeB magnet produced by the production method
CN107993828A (en) * 2017-11-24 2018-05-04 周慧媛 A kind of preparation process of permanent magnet alloy material
CN110942881A (en) * 2018-09-21 2020-03-31 丰田自动车株式会社 Rare earth magnet and method for producing same
CN115020098A (en) * 2022-05-16 2022-09-06 华北电力大学 Nano-coating integrated processing method of amorphous magnetic core
CN116693281A (en) * 2023-05-15 2023-09-05 集美大学 Preparation method for improving magnetostriction coefficient of cobalt ferrite material and cobalt ferrite product prepared by using preparation method

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101593590B (en) * 2009-04-10 2012-03-28 华中科技大学 Method for preparing warm compaction molding phenolic resin bonded Nd-Fe-B magnet
CN104377028A (en) * 2009-08-28 2015-02-25 因太金属株式会社 Method and device for producing sintered NdFeB magnet, and sintered NdFeB magnet produced by the production method
CN101934371A (en) * 2010-09-13 2011-01-05 华南理工大学 Permanent magnet material forming method and device under multi-external field coupling effect
CN102240805A (en) * 2011-07-27 2011-11-16 湖南航天工业总公司 Method for preparing anisotropic bonded rare-earth permanent magnet
CN102412043A (en) * 2011-07-28 2012-04-11 横店集团东磁股份有限公司 Manufacturing method of anisotropic NdFeB radial orientation magnet ring
CN102412043B (en) * 2011-07-28 2015-07-08 横店集团东磁股份有限公司 Manufacturing method of anisotropic NdFeB radial orientation magnet ring
CN102969116B (en) * 2012-07-20 2015-05-27 横店集团东磁股份有限公司 UV (ultraviolet) solidified bonding magnet and preparation method thereof
CN102969116A (en) * 2012-07-20 2013-03-13 横店集团东磁股份有限公司 UV (ultraviolet) solidified bonding magnet and preparation method thereof
CN107993828A (en) * 2017-11-24 2018-05-04 周慧媛 A kind of preparation process of permanent magnet alloy material
CN110942881A (en) * 2018-09-21 2020-03-31 丰田自动车株式会社 Rare earth magnet and method for producing same
CN110942881B (en) * 2018-09-21 2021-10-08 丰田自动车株式会社 Rare earth magnet and method for producing same
CN115020098A (en) * 2022-05-16 2022-09-06 华北电力大学 Nano-coating integrated processing method of amorphous magnetic core
CN116693281A (en) * 2023-05-15 2023-09-05 集美大学 Preparation method for improving magnetostriction coefficient of cobalt ferrite material and cobalt ferrite product prepared by using preparation method

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