CN109148139A - A kind of preparation method of high-performance SmCo sintered permanent magnet superelevation autoclaving - Google Patents

A kind of preparation method of high-performance SmCo sintered permanent magnet superelevation autoclaving Download PDF

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CN109148139A
CN109148139A CN201811060403.XA CN201811060403A CN109148139A CN 109148139 A CN109148139 A CN 109148139A CN 201811060403 A CN201811060403 A CN 201811060403A CN 109148139 A CN109148139 A CN 109148139A
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pressure
heat treatment
permanent magnet
super
temperature
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孙威
张鹏杰
李炳山
全小康
张威峰
胡国辉
熊君
刘冬
王峰
刘辉
王继全
王倩
贾立颖
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Beikuang Magnetic Materials (fuyang) Co Ltd
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Beikuang Magnetic Materials (fuyang) Co Ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets

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Abstract

The present invention provides a kind of preparation method of high-performance SmCo sintered permanent magnet superelevation autoclaving, comprising steps of ingredient, molten alloy ingot casting, airflow milling powder, mixed powder, orientation base and heat treatment.The present invention passes through the innovation in powder processed and heat treatment process, the average particle size of powder is set to be down to submicron order, later, using high vacuum pre-burning, super-pressure (900MPa or more) sintering, solid solution, tempering, reduce permanent magnet heat treatment temperature, heat treatment time is shortened simultaneously, thus improve heat treatment efficiency, and, born of the same parents' shape micro-structure integrated degree of the samarium cobalt permanent magnet body of preparation is high, size is suitable, uniformity is good, to make magnet under the premise that remanent magnetism, maximum magnetic energy product remain unchanged, intrinsic coercivity greatly improved.

Description

A kind of preparation method of high-performance SmCo sintered permanent magnet superelevation autoclaving
Technical field
The present invention relates to field of rare-earth permanent magnetic, are exactly a kind of high-performance SmCo sintered permanent magnets.
Background technique
For samarium cobalt rare earth permanent magnet body because of its low remanent magnetism reversible temperature coefficient, corrosion-resistant and high temperature resistant is irreplaceable excellent in this way Gesture has evolved into indispensable important in the fields such as aerospace, electrical engineering, magnetic machinery, microwave communication, instrument and meter One of Metallic Functional Materials.Its feature is coercivity, Curie temperature height, and corrosion resistance is good, and resistant to rust is very competent, institute With compared with neodymium iron boron, samarium cobalt permanent magnet physical efficiency long-term steady operation in high temperature, wet environment is well suited for various for manufacturing High performance magneto and the sufficiently complex application product of working environment.
In recent years, more next to product quality and stability requirement as rare earth permanent-magnetic material application field develops in depth Higher, demand of the market to samarium-cobalt magnet further increases.Such as maximum magnetic energy product (BH)max>=30MGOe, is reached using temperature To -60~350 DEG C, residual magnetism temperature coefficient is better than neodymium iron boron under the alternative hot conditions of high-performance samarium-cobalt magnet of -0.03%/K Magnet.And the Sintered NdFeB magnet used under hot conditions accounts for about the 10%-20% of whole Sintered NdFeB magnets, wherein having It greatly or the samarium-cobalt magnet that will convert, will be more than 1 in the coming years conservative estimation samarium-cobalt magnet overall market capacity Ten thousand tons, market prospects are boundless.Compared with sintered Nd-Fe-B permanent magnetic material, samarium-cobalt permanent-magnetic material production technology content height and work Skill requirement is stringenter, and the coercivity mechanism of samarium cobalt permanent magnet body is domain wall pinning, microstructure is more dependent on, in high temperature (180 DEG C or more), under adverse circumstances, the magnetic property and service life of sintered samarium cobalt permanent-magnet material are significantly larger than Nd-Fe-B permanent magnetic, and nothing It needs to be electroplated.And the sintered neodymium iron boron material used compared to hot conditions, samarium-cobalt permanent-magnetic material without add heavy rare earth element dysprosium, Terbium has highly important strategic importance to the reasonable using playing a positive role of China's heavy rare earth resource.On the other hand, Samarium and praseodymium neodymium are generally associated minerals, and relatively single compared to praseodymium neodymium samarium metal using face, cause largely hoarding for samarium oxide, institute The reasonable utilization of China's light rare earth resource is also beneficial to the production of samarium cobalt permanent magnet body.
In recent years, client requires samarium cobalt permanent magnet body properties of product higher and higher, including maximum magnetic energy product and intrinsic coercive Power, and for SmCo sintered permanent magnet, intrinsic coercivity and maximum magnetic energy product are the physical quantitys of conflict.In general, I The magnet of the 32H trade mark of SmCo sintered permanent magnet manufacturer of state preparation, intrinsic coercivity~18kOe are not able to satisfy market day The demand to high intrinsic coercivity that benefit increases.
Summary of the invention
The purpose of the present invention is to the not high disadvantages of existing high-performance SmCo sintered permanent magnet intrinsic coercivity, provide A kind of preparation method of high-performance SmCo sintered permanent magnet superelevation autoclaving.Compared with prior art, the present invention is using high Vacuum pre-burning, ultra-high pressure sintering, solid solution, tempering considerably reduce heat by the super-pressure pressure of the every procedure of strict control Treatment temperature shortens heat treatment time, improves heat treatment efficiency;Meanwhile reducing magnetic powder made from airflow milling process Area average particle size SMD, to further reduced heat treatment temperature.Using the born of the same parents of SmCo sintered permanent magnet prepared by the present invention Shape micro-structure integrated degree is high, size is suitable, uniformity is good, so, the SmCo sintered permanent magnet of preparation is protected in maximum magnetic energy product It holds under constant premise, intrinsic coercivity is greatly improved.
The technical solution of the present invention is as follows: a kind of preparation method of high-performance SmCo sintered permanent magnet superelevation autoclaving, Comprising steps of ingredient, molten alloy ingot casting, airflow milling powder, mixed powder, orientation base and heat treatment, the heat treatment include with Lower step:
(1) after low temperature presintering knot, it is heated to low-temperature sintering temperature, during this, is filled with Ar gas to super-pressure, sintering;
(2) it is cooled to low temperature solid solubility temperature, then controls the pressure of super-pressure, solution treatment;
(3) super-pressure low temperature isothermal annealing is heat-treated, slow cooling, quenching.
Preferably, the preferred He gas of gas that the airflow milling powder in the step uses, the powder area of airflow milling powder Average particle size SMD is 800~990nm.From the point of view of usually, the manufacturing firm of SmCo sintered permanent magnet either uses airflow milling still Stirring ball-milling powder, the SMD of powder are mostly 3~5 μm.The sintering temperature and powder size of studies have shown that SmCo sintered permanent magnet Pressure when size, distribution and sintering is related: granularity is thinner, and heat treatment temperature is lower.
Preferably, pumping high vacuum to less than 1.0*10 in the heat treatment step (1)-5Pa, in 940~945 DEG C of pre-burnings 20 ~30min.
Preferably, super-pressure pressure is 900~1000MPa when heat treatment step (1) low temperature sintering, 1000~ 1010 DEG C of 45~60min of sintering.
Preferably, super-pressure pressure is 1000~1100MPa when low temperature is dissolved in the heat treatment step (2), 980~ 990 DEG C of 60~90min of solid solution.
Preferably, super-pressure pressure is 900~1000MPa when tempering in the heat treatment step (3), with slow cooling into Row, pressure can reduce, and add the device of an accurate control pressure, make-up gas, remains unchanged pressure at any time, 780~790 DEG C isothermal annealing is heat-treated 180~210min, is then cooled to 380~390 DEG C with the cooling rate of 1.5~2 DEG C/min.
Ultra-high pressure sintering: the sintering process of samarium cobalt permanent magnet body belongs to liquid-phase sintering, is broadly divided into three phases: (1) The generation and flowing of liquid phase;(2) dissolution and precipitation;(3) solid-phase sintering.These three stages do not have apparent boundary, intersect With it is overlapping, it may be said that be to carry out simultaneously.Ultra-high pressure sintering can increase capillary power, accelerate in liquid phase generation and flow process In powder particle velocity of displacement, meanwhile, improve dissolution with precipitation process in spherical particle interaction force, moreover, Promote the speed of growth of the sintering neck in solid-phase sintering process.Moreover, it can also significantly reduce sintering temperature and reduce and burn Tie the time.
Super-pressure solid solution: in the preparation process of samarium cobalt permanent magnet body, the effect for being dissolved process includes: that (1) makes permanent magnet into one Step densification;(2) most important effect is to make the permanent magnet after being dissolved by single 1:7H phase composition, this is the high coercive of production One of the most critical technique of power SmCo sintered permanent magnet, super-pressure is dissolved the speed that can significantly improve phase transition, while can also Solid solubility temperature is greatly reduced and reduces solution time.
Super-pressure tempering: the tempering process of SmCo sintered permanent magnet is extremely complex, and effect is similar to " spinodal decomposition ", In drawing process, single 1:7H phase is completely converted into 1:5H cell wall phase and 2:17R main phase, is embodied in microstructure, then for The generation of born of the same parents' shape micro-structure, diffusion and ferro element of the simultaneous copper to 1:5H cell wall phase are to 2:17R main phase intracellular Diffusion.Born of the same parents' shape micro-structure integrated degree that super-pressure tempering prepares SmCo sintered permanent magnet is high, size is suitable, uniformity is good, together When, it reduces isothermal annealing heat treatment temperature, reduce isothermal annealing heat treatment time and slow cooling time.
Three above effect collective effect is just able to achieve implementation result of the invention, that is, reduces permanent magnet heat treatment temperature Degree, while heat treatment time is shortened, thus heat treatment efficiency is improved, moreover, magnet is kept not in remanent magnetism, maximum magnetic energy product Under the premise of change, intrinsic coercivity greatly improved.
The coercivity of rare earth permanent-magnetic material is structure sensitive magnetic parameter, and the coercivity mechanism of SmCo sintered permanent magnet is domain wall Pinning, born of the same parents' shape micro-structure integrated degree, size, uniformity are the major influence factors of its intrinsic coercivity.Studies have shown that born of the same parents' shape The size of micro-structure is less than 50nm or is greater than 200nm, and the intrinsic coercivity of magnet is not high.Compared with customary preparation methods, adopt With SmCo sintered permanent magnet born of the same parents shape micro-structure integrated degree prepared by the present invention is high, size suitable (80~100nm of average-size), Uniformity is good, so, the SmCo sintered permanent magnet of preparation has high maximum magnetic energy product and high intrinsic coercivity concurrently.
Compared with prior art, the invention has the advantages that magnet prepared by the present invention is kept not in remanent magnetism, maximum magnetic energy product Under the premise of change, intrinsic coercivity improves 20%~40%;Tempering time of the invention reduces 30%~70%;This hair Bright solution time reduces 30%~40%.
Specific embodiment
With reference to embodiment, the present invention is furture elucidated, it should be understood that following specific embodiments are only used for It is bright the present invention rather than limit the scope of the invention.
Comparative example 1
Ingredient, molten alloy ingot casting, airflow milling powder & mix powder, orientation base and heat treatment.Wherein, heat treatment include with Lower step:
(1) after being pre-sintered, it is heated to sintering temperature, during this, is filled with Ar gas to positive pressure, sintering;
(2) it is cooled to solid solubility temperature, then controls pressure, solution treatment;
(3) isothermal annealing is heat-treated, slow cooling, quenching.
Wherein, the powder area average particle size SMD of airflow milling powder is 4.5 μm.
Pumping high vacuum is to 1.0*10 in heat treatment step (1)-2Pa, in 1185 DEG C of pre-burning 30min.
Pressure is 3atm when sintering in heat treatment step (1), in 1205 DEG C of sintering 90min.
Pressure is 3atm when solid solution in heat treatment step (2), in 1180 DEG C of solid solution 120min.
Pressure is 3atm, the isothermal annealing heat-treatment 20h at 800 DEG C, then with 0.48 when tempering in heat treatment step (3) DEG C/cooling rate of min is cooled to 400 DEG C, 10h is kept the temperature, room temperature is chilled to.
Comparative example 2
Ingredient, molten alloy ingot casting, airflow milling powder & mix powder, orientation base and heat treatment.Wherein, heat treatment include with Lower step:
(1) after being pre-sintered, it is heated to sintering temperature, during this, is filled with Ar gas to positive pressure, sintering;
(2) it is cooled to solid solubility temperature, then controls pressure, solution treatment;
(3) isothermal annealing is heat-treated, slow cooling, quenching.
Wherein, the powder area average particle size SMD of airflow milling powder is 4.7 μm.
Pumping high vacuum is to 1.0*10 in heat treatment step (1)-3Pa, in 1180 DEG C of pre-burning 30min.
Pressure is 200MPa when sintering in heat treatment step (1), in 1200 DEG C of sintering 60min.
Pressure is 200MPa when solid solution in heat treatment step (2), in 1180 DEG C of solid solution 90min.
Pressure is 200MPa, the isothermal annealing heat-treatment 5h at 835 DEG C when tempering in heat treatment step (3), then with The cooling rate of 0.55 DEG C/min is cooled to 420 DEG C, keeps the temperature 6h, is chilled to room temperature.
Embodiment 1
A kind of preparation method of high-performance SmCo sintered permanent magnet superelevation autoclaving, comprising steps of ingredient, melting are closed Golden ingot casting, airflow milling powder & mix powder, orientation base and heat treatment, wherein heat treatment the following steps are included:
(1) after low temperature presintering knot, it is heated to low-temperature sintering temperature, during this, is filled with Ar gas to super-pressure, sintering;
(2) it is cooled to low temperature solid solubility temperature, then controls the pressure of super-pressure, solution treatment;
(3) low-temperature ultrahigh-pressure isothermal annealing is heat-treated, slow cooling, quenching.
Wherein, the powder area average particle size SMD of airflow milling powder is 800nm.
Pumping high vacuum is to 9.0*10 in heat treatment step (1)-6Pa, in 940 DEG C of pre-burning 27min.
Super-pressure pressure is 930MPa when heat treatment step (1) low temperature sintering, in 1000 DEG C of sintering 60min.
Super-pressure pressure is 1100MPa when low temperature is dissolved in heat treatment step (2), in 980 DEG C of solid solution 90min.
Super-pressure pressure remains 970MPa when tempering in heat treatment step (3), is heat-treated in 780 DEG C of isothermal annealings Then 180min is cooled to 390 DEG C with the cooling rate of 1.7 DEG C/min.
Embodiment 2
A kind of preparation method of high-performance SmCo sintered permanent magnet superelevation autoclaving, comprising steps of ingredient, melting are closed Golden ingot casting, airflow milling powder & mix powder, orientation base and heat treatment, wherein heat treatment the following steps are included:
(1) after low temperature presintering knot, it is heated to low-temperature sintering temperature, during this, is filled with Ar gas to super-pressure, sintering;
(2) it is cooled to low temperature solid solubility temperature, then controls the pressure of super-pressure, solution treatment;
(3) low-temperature ultrahigh-pressure isothermal annealing is heat-treated, slow cooling, quenching.
Wherein, the powder area average particle size SMD of airflow milling powder is 800nm.
Pumping high vacuum is to 9.0*10 in heat treatment step (1)-6Pa, in 940 DEG C of pre-burning 27min.
Super-pressure pressure is 900MPa when heat treatment step (1) low temperature sintering, in 1007 DEG C of sintering 49min.
Super-pressure pressure is 1000MPa when low temperature is dissolved in heat treatment step (2), in 983 DEG C of solid solution 60min.
Super-pressure pressure remains 900MPa when tempering in heat treatment step (3), is heat-treated in 784 DEG C of isothermal annealings Then 210min is cooled to 386 DEG C with the cooling rate of 1.5 DEG C/min.
Embodiment 3
A kind of preparation method of high-performance SmCo sintered permanent magnet superelevation autoclaving, comprising steps of ingredient, melting are closed Golden ingot casting, airflow milling powder & mix powder, orientation base and heat treatment, wherein heat treatment the following steps are included:
(1) after low temperature presintering knot, it is heated to low-temperature sintering temperature, during this, is filled with Ar gas to super-pressure, sintering;
(2) it is cooled to low temperature solid solubility temperature, then controls the pressure of super-pressure, solution treatment;
(3) low-temperature ultrahigh-pressure isothermal annealing is heat-treated, slow cooling, quenching.
Wherein, the powder area average particle size SMD of airflow milling powder is 800nm.
Pumping high vacuum is to 9.0*10 in heat treatment step (1)-6Pa, in 940 DEG C of pre-burning 27min.
Super-pressure pressure is 1000MPa when heat treatment step (1) low temperature sintering, in 1010 DEG C of sintering 45min.
Super-pressure pressure is 1050MPa when low temperature is dissolved in heat treatment step (2), in 990 DEG C of solid solution 72min.
Super-pressure pressure remains 1000MPa when tempering in heat treatment step (3), is heat-treated in 790 DEG C of isothermal annealings Then 195min is cooled to 380 DEG C with the cooling rate of 2.0 DEG C/min.
Embodiment 4
A kind of preparation method of high-performance SmCo sintered permanent magnet superelevation autoclaving, comprising steps of ingredient, melting are closed Golden ingot casting, airflow milling powder & mix powder, orientation base and heat treatment, wherein heat treatment the following steps are included:
(1) after low temperature presintering knot, it is heated to low-temperature sintering temperature, during this, is filled with Ar gas to super-pressure, sintering;
(2) it is cooled to low temperature solid solubility temperature, then controls the pressure of super-pressure, solution treatment;
(3) low-temperature ultrahigh-pressure isothermal annealing is heat-treated, slow cooling, quenching.
Wherein, the powder area average particle size SMD of airflow milling powder is 847nm.
Pumping high vacuum is to 8.3*10 in heat treatment step (1)-6Pa, in 946 DEG C of pre-burning 20min.
Super-pressure pressure is 930MPa when heat treatment step (1) low temperature sintering, in 1000 DEG C of sintering 60min.
Super-pressure pressure is 1000MPa when low temperature is dissolved in heat treatment step (2), in 983 DEG C of solid solution 60min.
Super-pressure pressure remains 1000MPa when tempering in heat treatment step (3), is heat-treated in 790 DEG C of isothermal annealings Then 195min is cooled to 380 DEG C with the cooling rate of 2.0 DEG C/min.
Embodiment 5
A kind of preparation method of high-performance SmCo sintered permanent magnet superelevation autoclaving, comprising steps of ingredient, melting are closed Golden ingot casting, airflow milling powder & mix powder, orientation base and heat treatment, wherein heat treatment the following steps are included:
(1) after low temperature presintering knot, it is heated to low-temperature sintering temperature, during this, is filled with Ar gas to super-pressure, sintering;
(2) it is cooled to low temperature solid solubility temperature, then controls the pressure of super-pressure, solution treatment;
(3) low-temperature ultrahigh-pressure isothermal annealing is heat-treated, slow cooling, quenching.
Wherein, the powder area average particle size SMD of airflow milling powder is 847nm.
Pumping high vacuum is to 8.3*10 in heat treatment step (1)-6Pa, in 946 DEG C of pre-burning 20min.
Super-pressure pressure is 900MPa when heat treatment step (1) low temperature sintering, in 1007 DEG C of sintering 49min.
Super-pressure pressure is 1050MPa when low temperature is dissolved in heat treatment step (2), in 990 DEG C of solid solution 72min.
Super-pressure pressure remains 970MPa when tempering in heat treatment step (3), is heat-treated in 780 DEG C of isothermal annealings Then 180min is cooled to 390 DEG C with the cooling rate of 1.7 DEG C/min.
Embodiment 6
A kind of preparation method of high-performance SmCo sintered permanent magnet superelevation autoclaving, comprising steps of ingredient, melting are closed Golden ingot casting, airflow milling powder & mix powder, orientation base and heat treatment, wherein heat treatment the following steps are included:
(1) after low temperature presintering knot, it is heated to low-temperature sintering temperature, during this, is filled with Ar gas to super-pressure, sintering;
(2) it is cooled to low temperature solid solubility temperature, then controls the pressure of super-pressure, solution treatment;
(3) low-temperature ultrahigh-pressure isothermal annealing is heat-treated, slow cooling, quenching.
Wherein, the powder area average particle size SMD of airflow milling powder is 847nm.
Pumping high vacuum is to 8.3*10 in heat treatment step (1)-6Pa, in 946 DEG C of pre-burning 20min.
Super-pressure pressure is 1000MPa when heat treatment step (1) low temperature sintering, in 1010 DEG C of sintering 45min.
Super-pressure pressure is 1100MPa when low temperature is dissolved in heat treatment step (2), in 980 DEG C of solid solution 90min.
Super-pressure pressure remains 900MPa when tempering in heat treatment step (3), is heat-treated in 784 DEG C of isothermal annealings Then 210min is cooled to 386 DEG C with the cooling rate of 1.5 DEG C/min.
Embodiment 7
A kind of preparation method of high-performance SmCo sintered permanent magnet superelevation autoclaving, comprising steps of ingredient, melting are closed Golden ingot casting, airflow milling powder & mix powder, orientation base and heat treatment, wherein heat treatment the following steps are included:
(1) after low temperature presintering knot, it is heated to low-temperature sintering temperature, during this, is filled with Ar gas to super-pressure, sintering;
(2) it is cooled to low temperature solid solubility temperature, then controls the pressure of super-pressure, solution treatment;
(3) low-temperature ultrahigh-pressure isothermal annealing is heat-treated, slow cooling, quenching.
Wherein, the powder area average particle size SMD of airflow milling powder is 990nm.
Pumping high vacuum is to 9.0*10 in heat treatment step (1)-6Pa, in 950 DEG C of pre-burning 30min.
Super-pressure pressure is 930MPa when heat treatment step (1) low temperature sintering, in 1000 DEG C of sintering 60min.
Super-pressure pressure is 1050MPa when low temperature is dissolved in heat treatment step (2), in 990 DEG C of solid solution 72min.
Super-pressure pressure remains 900MPa when tempering in heat treatment step (3), is heat-treated in 784 DEG C of isothermal annealings Then 210min is cooled to 386 DEG C with the cooling rate of 1.5 DEG C/min.
Embodiment 8
A kind of preparation method of high-performance SmCo sintered permanent magnet superelevation autoclaving, comprising steps of ingredient, melting are closed Golden ingot casting, airflow milling powder & mix powder, orientation base and heat treatment, wherein heat treatment the following steps are included:
(1) after low temperature presintering knot, it is heated to low-temperature sintering temperature, during this, is filled with Ar gas to super-pressure, sintering;
(2) it is cooled to low temperature solid solubility temperature, then controls the pressure of super-pressure, solution treatment;
(3) low-temperature ultrahigh-pressure isothermal annealing is heat-treated, slow cooling, quenching.
Wherein, the powder area average particle size SMD of airflow milling powder is 990nm.
Pumping high vacuum is to 9.0*10 in heat treatment step (1)-6Pa, in 950 DEG C of pre-burning 30min.
Super-pressure pressure is 900MPa when heat treatment step (1) low temperature sintering, in 1007 DEG C of sintering 49min.
Super-pressure pressure is 1100MPa when low temperature is dissolved in heat treatment step (2), in 980 DEG C of solid solution 90min.
Super-pressure pressure remains 1000MPa when tempering in heat treatment step (3), is heat-treated in 790 DEG C of isothermal annealings Then 195min is cooled to 380 DEG C with the cooling rate of 2.0 DEG C/min.
Embodiment 9
A kind of preparation method of high-performance SmCo sintered permanent magnet superelevation autoclaving, comprising steps of ingredient, melting are closed Golden ingot casting, airflow milling powder & mix powder, orientation base and heat treatment, wherein heat treatment the following steps are included:
(1) after low temperature presintering knot, it is heated to low-temperature sintering temperature, during this, is filled with Ar gas to super-pressure, sintering;
(2) it is cooled to low temperature solid solubility temperature, then controls the pressure of super-pressure, solution treatment;
(3) low-temperature ultrahigh-pressure isothermal annealing is heat-treated, slow cooling, quenching.
Wherein, the powder area average particle size SMD of airflow milling powder is 990nm.
Pumping high vacuum is to 9.0*10 in heat treatment step (1)-6Pa, in 950 DEG C of pre-burning 30min.
Super-pressure pressure is 1000MPa when heat treatment step (1) low temperature sintering, in 1010 DEG C of sintering 45min.
Super-pressure pressure is 1000MPa when low temperature is dissolved in heat treatment step (2), in 983 DEG C of solid solution 60min.
Super-pressure pressure remains 970MPa when tempering in heat treatment step (3), is heat-treated in 780 DEG C of isothermal annealings Then 180min is cooled to 390 DEG C with the cooling rate of 1.7 DEG C/min.
Magnetic property is tested to the SmCo sintered permanent magnet of comparative example 1, comparative example 2 and embodiment 1-9 preparation, it is as a result as follows Table:
Serial number Remanent magnetism kGs Maximum magnetic energy product MGOe Intrinsic coercivity kOe
Comparative example 1 11.30 31.62 17.72
Comparative example 2 11.32 31.71 17.31
Embodiment 1 11.28 31.65 25.02
Embodiment 2 11.24 31.51 24.56
Embodiment 3 11.37 31.73 24.77
Embodiment 4 11.41 31.69 25.12
Embodiment 5 11.19 31.21 24.95
Embodiment 6 11.25 31.40 24.83
Embodiment 7 11.34 31.55 24.71
Embodiment 8 11.31 31.48 24.62
Embodiment 9 11.26 31.52 24.34
This place embodiment is not exhaustive claimed midpoint of technical range and in embodiment technology In scheme to single or multiple technical characteristics it is same replacement be formed by new technical solution, equally all the present invention claims In the range of protection;Simultaneously the present invention program it is all enumerate or unlisted embodiment in, in the same embodiment each Parameter is merely representative of an example (i.e. a kind of feasible scheme) for its technical solution, and not existence anduniquess between parameters Cooperation and qualified relation, wherein each parameter can be replaced mutually when stating and asking without prejudice to axiom and the present invention, special declaration Except.

Claims (5)

1. a kind of preparation method of high-performance SmCo sintered permanent magnet superelevation autoclaving, comprising steps of ingredient, molten alloy Ingot casting, airflow milling powder, mixed powder, orientation base and heat treatment, it is characterised in that: the heat treatment the following steps are included:
(1) after low temperature presintering knot, it is heated to low-temperature sintering temperature, during this, is filled with Ar gas to super-pressure, sintering;
(2) it is cooled to low temperature solid solubility temperature, then controls the pressure of super-pressure, solution treatment;
(3) low-temperature ultrahigh-pressure isothermal annealing is heat-treated, slow cooling, quenching.
2. a kind of preparation method of high-performance SmCo sintered permanent magnet superelevation autoclaving according to claim 1, Be characterized in that: the powder area average particle size SMD of the airflow milling powder is 800~990nm.
3. a kind of preparation method of high-performance SmCo sintered permanent magnet superelevation autoclaving according to claim 1, Be characterized in that: super-pressure pressure is 900~1000MPa when heat treatment step (1) low temperature sintering.
4. a kind of preparation method of high-performance SmCo sintered permanent magnet superelevation autoclaving according to claim 1, Be characterized in that: super-pressure pressure is 1000~1100MPa when low temperature is dissolved in the heat treatment step (2).
5. a kind of preparation method of high-performance SmCo sintered permanent magnet superelevation autoclaving according to claim 1, Be characterized in that: super-pressure pressure remains 900~1000MPa when tempering in the heat treatment step (3).
CN201811060403.XA 2018-09-12 2018-09-12 A kind of preparation method of high-performance SmCo sintered permanent magnet superelevation autoclaving Pending CN109148139A (en)

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CN110473703A (en) * 2019-07-24 2019-11-19 北矿磁材(阜阳)有限公司 A kind of high HkThe preparation method of SmCo agglomeration permanent magnetic material
CN113436874A (en) * 2021-05-27 2021-09-24 北矿科技股份有限公司 Sm2Co17Molded high-temperature magnet and preparation method thereof
CN114420432A (en) * 2021-12-23 2022-04-29 中国科学院宁波材料技术与工程研究所 Preparation method for improving magnetic property of samarium cobalt permanent magnet material

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CN103515049A (en) * 2012-06-20 2014-01-15 信越化学工业株式会社 Cylindrical magnetic circuit and producing method thereof
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Publication number Priority date Publication date Assignee Title
CN110473703A (en) * 2019-07-24 2019-11-19 北矿磁材(阜阳)有限公司 A kind of high HkThe preparation method of SmCo agglomeration permanent magnetic material
CN110473703B (en) * 2019-07-24 2021-07-27 北矿磁材(阜阳)有限公司 High HkPreparation method of samarium cobalt sintered permanent magnet material
CN113436874A (en) * 2021-05-27 2021-09-24 北矿科技股份有限公司 Sm2Co17Molded high-temperature magnet and preparation method thereof
CN113436874B (en) * 2021-05-27 2023-04-18 北矿科技股份有限公司 Sm 2 Co 17 Molded high-temperature magnet and preparation method thereof
CN114420432A (en) * 2021-12-23 2022-04-29 中国科学院宁波材料技术与工程研究所 Preparation method for improving magnetic property of samarium cobalt permanent magnet material
CN114420432B (en) * 2021-12-23 2024-03-26 中国科学院宁波材料技术与工程研究所 Preparation method for improving magnetic performance of samarium cobalt permanent magnet material

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