WO2011125262A1 - Aimant permanent de terres rares à système r-t-b-m-a et son procédé de production - Google Patents

Aimant permanent de terres rares à système r-t-b-m-a et son procédé de production Download PDF

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WO2011125262A1
WO2011125262A1 PCT/JP2010/072782 JP2010072782W WO2011125262A1 WO 2011125262 A1 WO2011125262 A1 WO 2011125262A1 JP 2010072782 W JP2010072782 W JP 2010072782W WO 2011125262 A1 WO2011125262 A1 WO 2011125262A1
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mass
rare earth
permanent magnet
ppm
alloy
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Japanese (ja)
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喜峰 林
開鴻 丁
思晶 呂
国海 王
京春 于
忠華 李
永杰 王
宮本恭祐
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株式会社 安川電機
煙台首鋼磁性材料株式有限公司
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Priority to JP2011531281A priority Critical patent/JP5943507B2/ja
Publication of WO2011125262A1 publication Critical patent/WO2011125262A1/fr

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus 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
    • H01F41/02—Apparatus 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
    • H01F41/0253—Apparatus 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
    • H01F41/0266—Moulding; Pressing
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/02—Making ferrous alloys by powder metallurgy
    • C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
    • C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/058—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IVa elements, e.g. Gd2Fe14C

Definitions

  • the present invention relates to the field of permanent magnet materials. Specifically, it is an RTB-M-A rare earth permanent magnet material and a method for producing the same, and has a high performance that greatly improves the coercive force of the sintered body without reducing the residual magnetic flux density Br of the magnet.
  • the present invention relates to a rare earth permanent magnet material and a manufacturing method thereof.
  • R is at least one of rare earth elements
  • T is at least one of transition metal elements
  • B is boron
  • High efficiency from medical equipment such as hard disk drive voice coil motor (VCM), CD / DVD pick-up, mobile phone, nuclear magnetic resonance tomography (MRI), which is the area of conventional electronic communication equipment
  • VCM hard disk drive voice coil motor
  • MRI nuclear magnetic resonance tomography
  • the company is expanding into new energy source areas such as wind power generators, which are energy-saving electric fields, compressor motors for air conditioners and refrigerators, and hybrid car motors and generators. Therefore, the demand for high-performance RTB-based permanent magnet materials is increasing, and rare earth permanent magnet materials with high residual magnetic flux density and high coercive force, especially under conditions of high operating temperatures. The demand for is increasing.
  • the main technical indicators of the magnetic characteristics of the RTB permanent magnet material are the residual magnetic flux density and the coercive force.
  • the residual magnetic flux density is mainly 1. 1. Volume ratio of forward ridges 2. volume ratio of main phase (R 2 T 14 B) or magnetic phase; 3. degree of orientation of magnetic grains; It is determined by factors such as the ratio between the actual density and the theoretical density of the sintered magnet.
  • the residual magnetic flux density Br is expressed by the following formula.
  • Br A (1- ⁇ ) (d / d 0 ) cos ⁇ .
  • the coercive force mainly includes the magnetocrystalline anisotropy (Ha), the microstructure of the sintered magnet (eg, grain size, shape, etc.), the quantity and distribution of R-rich phases, and the inverse magnetic factor in the reverse magnetic domain. It is influenced by etc.
  • Hcj cHa ⁇ N eff Ms Ha: magnetocrystalline anisotropy parameter, Ms: saturation magnetization strength c: microstructure parameter Neff: inverse magnetic factor
  • RTB-based sintered permanent magnet materials that do not contain heavy rare earth elements Dy and Tb have a high residual magnetic flux density Br (usually 1.4T) but a low coercive force of only about 960 kA / m. Absent. For this reason, it can be used only in low and stable use environments, and the application area of permanent magnet materials is greatly restricted. In order to increase the coercive force of the RTB-based sintered magnet and expand the range of operating temperature, various improvements have been implemented such as component adjustment and reduction of crystal grains.
  • Nd is substituted with Dy or Tb, which is a heavy rare earth element having higher anisotropy, and the coercive force and operating temperature are improved.
  • a part of Nd is substituted with 5% by mass of Dy. According to this, the coercive force can be improved to 1680 (kA / m), but the residual magnetic flux density Br is reduced to 1.28 (T).
  • Dy and Tb which are heavy rare earths, are scarce resources and are expensive, and this method is not suitable for mass production.
  • the mass of the permanent magnet used for one unit is an average value of 1000 kg or more, which is a major constraint factor in terms of cost.
  • the coercive force performance required for applications with severe operating temperature conditions for example, electric motors for electric vehicles, electric motors for hybrid vehicles, and generators is raised. I could not.
  • the magnet temperature in an electric vehicle or a hybrid vehicle needs to withstand 150 ° C. for an electric vehicle and 200 ° C. for a hybrid vehicle, and in terms of the coercive force of the magnet, it is 1680 (KA / m) or more.
  • the residual magnetic flux density is required to be 1.28 (T) or more.
  • Dy or Tb which is a heavy rare earth element
  • the coercive force performance Hcj can be improved, but the residual magnetic flux density Br is reduced, which results in a reduction in the efficiency of the motor and the generator. Become.
  • the present invention solves these drawbacks and greatly reduces the amount of expensive rare metal materials that cause cost increases, while improving the residual magnetic flux density Br and the magnetic performance Hcj that affect the efficiency of the electric motor and generator, A high-performance rare earth magnet is provided by using abundant materials at low cost.
  • the product according to the present invention can be used in various fields such as a servo motor, a linear motor, and an elevator motor.
  • IPMSM internal permanent magnet synchronous motor
  • IPMSM internal permanent magnet synchronous motor
  • the torque characteristics of the IPMSM are as follows.
  • the current phase angle ⁇ when the horizontal axis is taken with reference to the magnet magnetic flux axis (d axis), and the torque T when the vertical axis is taken as the magnet torque: Tm And reluctance torque: Tr.
  • Tm ⁇ m ⁇ cos ⁇ ( ⁇ m: maximum value of magnet torque Tm)
  • Tr ⁇ r ⁇ sin (2 ⁇ ) ( ⁇ r: maximum value of magnet torque Tr)
  • the feature of this motor is that the constant output characteristic region of the motor is realized by weakening the generated magnetic flux, which is the magnetic energy of the magnet, with the armature magnetic flux.
  • the arrangement of the rare earth magnet is on the magnetic flux axis (d axis), and the rare earth magnet mainly composed of RTB has a relative permeability ⁇ r ⁇ 1.05.
  • the permeability is almost the same as air. Therefore, the d-axis inductance when viewed from the armature is compared with the q-axis inductance of the axis (q-axis) orthogonal to this, Ld ⁇ Lq Are in a relationship.
  • the d-axis inductance is large in order to perform control to weaken the magnet magnetic flux and to keep the voltage across the motor terminal that increases as the speed increases to a constant value. That is, it is better that the thickness Lm of the magnet disposed inside the rotor core is smaller.
  • the magnet thickness Lm is determined from the coercive force performance Hcj at the use temperature tm (use environment temperature) of the magnet to be used and the field weakening field energy Ata of the armature. Since the field weakening energy Ata is determined from the output specification of the electric motor, it depends on how to use a magnet having a high coercive force performance Hcj at the magnet use temperature tm (use environment temperature). That is, if the coercive force performance Hcj is low, it is necessary to increase the magnet thickness Lm in order to withstand the field weakening field energy Ata of the armature (in order to prevent demagnetization).
  • the magnet thickness Lm when the magnet thickness Lm is increased, the d-axis inductance Ld described above is decreased, and in order to obtain a specified output characteristic, it is necessary to pass a large amount of reactive current through the armature.
  • the efficiency characteristics in the constant output region of the above will be significantly impaired.
  • the magnet of the present invention having a high coercive force performance Hcj the magnet thickness Lm can be made thinner than in the case of a conventional magnet, so that the reactive current can be reduced by reducing the armature and improving the efficiency of the constant output region. The big effect that an energy effect can be produced is acquired.
  • the coercive force performance Hcj can be improved by about 25%, and the magnet thickness can be reduced by 25% compared to the prior art.
  • the Joule loss Wj generated in the armature winding can be reduced by about 35%.
  • the present invention is characterized in that the component range of A, which is a trace element, is optimally determined in an RTBA-MA based rare earth permanent magnet material.
  • the coercive force of the magnet is improved by adding the trace element A in an optimum range in addition to reducing the particle size of the powder in the pulverization step without adding the rare metal.
  • the influence of oxygen “O” and the necessity of the specified range will be described. Since the magnetic particle size of the magnetic powder is very finely controlled, abnormal growth of magnetic crystal grains is likely to occur during the sintering process. Therefore, the content of oxygen “O” in the magnet is strictly controlled in the pulverization step, and an oxide film is formed on the surface of the powder to prevent abnormal growth of crystal grains. Therefore, the oxygen “O” content only for forming the oxide film is important, and it is necessary to determine a certain component defining range. If an excessive amount of oxygen is added, the R-rich phase is oxidized and the coercive force is lowered.
  • the present invention relates to an RTBMA-based rare earth permanent magnet mainly composed of an R 2 T 14 B type compound, wherein R is at least one of rare earth elements, and T is at least one of transition metal elements.
  • B is boron
  • M is at least one selected from the group consisting of Ti, Mn, Ni, Cu, Zn, Al, Si, P, S
  • A is a trace element
  • R is 24 mass% to 34 mass%
  • T is 63 mass% to 74 mass%
  • B 0.5% by mass to 1.5% by mass
  • the rest consists of M and A, A has a C content of 1100 ppm to 2000 ppm, H content is 10 ppm or less, O content is 1300 ppm to 2000 ppm, N content of 150 ppm or less, Consisting of Further, the average particle diameter of the pulverized permanent magnet material is in the range of 2 to 5 ⁇ m, and the magnet material is pulverized in an argon or helium gas atmosphere.
  • the present invention can provide a rare earth magnet with improved coercive force performance Hcj without increasing the material cost and without reducing the residual magnetic flux density Br that affects the efficiency of the motor and generator.
  • the present invention makes the amount of rare metal elements such as Ga, Nb, and Mo small by setting the trace element A within the specified range, thereby reducing the amount of rare earth elements input as much as possible, greatly reducing the stable supply of magnets and reducing costs. Can be improved.
  • Electric motor output characteristics of electric vehicle motors or hybrid vehicle motors Structure diagram of internal permanent magnet synchronous motor (Interior Permanent Magnet type Synchronous Motor) Torque characteristics of IPMSM Correlation diagram between N content and residual magnetic flux density Correlation diagram between N content and coercive force Correlation diagram between pulverized particle size and residual magnetic flux density Correlation diagram between pulverized particle size and coercive force Correlation diagram between O content and residual magnetic flux density Correlation diagram between O content and coercivity Correlation diagram between C content and residual magnetic flux density Correlation diagram between C content and coercivity Correlation diagram between H content and residual magnetic flux density Correlation diagram between H content and coercivity
  • the weight description in a following example is represented by the mass%, and shows the weight ratio in the substance of each element.
  • an average particle diameter is represented as D50 (50% particle diameter) which is a median diameter, and each numerical value is a measured value by a laser diffraction type particle size distribution measuring apparatus.
  • Alloy production Metal or alloy raw materials are melted and refined in an argon gas atmosphere.
  • the alloy is a component of the sintered body RTB-MA, R is Nd: 22.5% by mass, Dy: 3.5% by mass, Pr: 5.0% by mass, T is Fe: 66.6 mass% Co: 1.0% by mass B is B: 1.0% by mass M is Al: 0.3% by mass, Cu: 0.1% by mass,
  • An alloy consisting of The molten alloy was cooled and solidified with a roll by a strip casting (SC) method to obtain a flake alloy.
  • SC strip casting
  • the hydrogen furnace is evacuated to perform a dehydrogenation treatment. Thereafter, the coarsely pulverized alloy is finely pulverized into a powder having an average particle diameter of about 5.0 ⁇ m in a jet meal machine using high-pressure argon gas.
  • a certain amount of oxygen is put into the inert gas for jet meal grinding during the grinding process. Thereafter, the powder is stored in an inert gas.
  • a certain amount of lubricant is added to the powder mixer.
  • the process of mixing the lubricant is performed under an argon gas protective atmosphere.
  • Molding Magnetic field molding is performed in an inert gas atmosphere using the fine powder produced by the above method.
  • the molded body molded by the above method is kept at a temperature environment of 400 ° C. or higher for a certain period of time, and thereafter sintered by a sintering process to obtain a sintered body RTB-M-A. obtain.
  • Example 1 After the sintering treatment is completed, the magnet is subjected to an aging treatment. Thereafter, a sample of Example 1 having a diameter of 10 mm and a height of 10 mm was manufactured through machining.
  • Example 2 differs from Example 1 in that helium gas was used as a protective atmosphere in the pulverization, lubricant addition, and molding steps.
  • Example 1 the alloy of the comparative example 1, the comparative example 2, and the comparative example 3 was also produced.
  • Alloy production method of comparative example A metal or alloy raw material is melted and refined in a nitrogen gas atmosphere.
  • the alloy is a component of the sintered body RTB-MA, R is Nd: 21% by mass, Dy: 5.0% by mass Pr: 5.0% by mass, T is Fe: 66.6 mass% Co: 1.0% by mass B is B: 1.0% by mass M is Al: 0.3% by mass, Cu: 0.1% by mass,
  • An alloy consisting of The molten alloy was cooled and solidified with a roll by a strip casting method to obtain a flake alloy.
  • the hydrogen furnace is placed in a vacuum state to perform a dehydrogenation treatment. Thereafter, using the high pressure nitrogen gas, the coarsely pulverized alloy is finely pulverized into a powder having an average particle diameter of about 5.0 ⁇ m in a jet meal machine.
  • a certain amount of oxygen is put into nitrogen gas for jet meal grinding during the grinding process. Thereafter, the powder is stored in nitrogen gas.
  • a certain amount of lubricant is added to the powder mixer.
  • nitrogen gas is put in a protective atmosphere.
  • Molding Magnetic field molding is performed in a nitrogen gas atmosphere using the fine powder produced by the above method.
  • the molded body molded by the above method is first held at a temperature environment of 400 ° C. or higher for a certain time, and then sintered by a sintering process to obtain a sintered body RTMBA-MA. Get.
  • FIG. 4 shows the relationship between the nitrogen N content on the horizontal axis and the residual magnetic flux density on the vertical axis.
  • FIG. 5 shows the relationship between the nitrogen N content on the horizontal axis and the coercive force on the vertical axis. From these figures, it is necessary to reduce the nitrogen N to 150 ppm or less so that the coercive force of 1680 kA / m or more required as a high-performance permanent magnet is obtained. At this time, the residual magnetic flux density is 1.28 T or more. It can be confirmed. Table 1:
  • Example 1 of the present invention although the amount of rare earth metal Dy added was reduced by 30% compared to Comparative Example 1, the residual magnetic flux density was basically unchanged and maintained. There is no great difference in magnetic force. That is, according to the present invention, the expensive rare earth Dy can be reduced by 30%.
  • Pulverization The alloy is coarsely pulverized through a hydrogenation treatment, and a hydrogen furnace is evacuated to perform a dehydrogenation treatment. Thereafter, the coarsely pulverized alloy is pulverized to an average particle size of about 4.0 ⁇ m in a jet meal machine using high-pressure argon gas. In order to prevent abnormal growth of crystal grains, a certain amount of oxygen is put into the jet meal grinding gas during the powder making process, and then the powder is stored in argon gas.
  • An alloy is manufactured by the same manufacturing process as in Example 3, but the coarsely pulverized alloy is pulverized to an average particle size of about 3.0 ⁇ m in a jet meal machine.
  • a certain amount of oxygen is put into the jet meal grinding gas during the powder making process, and then the powder is stored in argon gas.
  • An alloy is produced by the same manufacturing process as in Example 3, but the coarsely pulverized alloy is pulverized to an average particle size of about 2.5 ⁇ m in a jet meal machine.
  • a certain amount of oxygen is put into the jet meal grinding gas during the powder making process, and then the powder is stored in argon gas.
  • Comparative Example 4 samples of Comparative Example 4 and Comparative Example 5 were also produced.
  • the difference between Comparative Example 4 and Comparative Example 5 from Example 3-5 is the average particle size of the powder.
  • a sample having an average particle diameter of 6.0 ⁇ m was designated as Comparative Example 4, and a sample having a mean particle diameter of 1.5 ⁇ m was designated as Comparative Example 5.
  • FIG. 6 shows the relationship between the average particle diameter on the horizontal axis and the residual magnetic flux density on the vertical axis.
  • FIG. 7 shows the relationship between the average particle diameter on the horizontal axis and the coercive force on the vertical axis. From these figures, it is necessary to make the average particle diameter 2 to 5 ⁇ m so that the coercive force 1680 kA / m or more required as a high-performance permanent magnet is obtained. At this time, the residual magnetic flux density is 1.28 T or more. It can be confirmed that Table 2:
  • Pulverization The alloy is coarsely pulverized through a hydrogenation treatment, and a hydrogen furnace is placed in a vacuum state to perform dehydrogenation treatment. Thereafter, the coarsely pulverized alloy is pulverized to an average particle size of about 4.0 ⁇ m in a jet meal machine using a high-pressure inert gas. In order to prevent abnormal growth of crystal grains, a certain amount of oxygen is put into the jet meal grinding gas during the powder making process, and then the powder is stored in an inert gas.
  • a certain amount of lubricant is added to the powder mixer.
  • the process of mixing the lubricant is performed under an inert gas protective atmosphere.
  • Example 1 Molding, sintering, and aging treatment A sample is prepared in the same manner as in Example 1. The difference from Example 1 is that a certain amount of oxygen is put into the jet meal grinding gas during the powder making process, and then the powder is added. It is the point which stored in the inert gas and adjusted the amount of oxygen.
  • Example 6 was performed with oxygen O at 1300 ppm.
  • Example 7 is prepared by the same process as 6 described above, except that oxygen O is 1600 ppm.
  • Example 8 is prepared by the same process as 6 described above, except that oxygen O is 2000 ppm.
  • Comparative Examples 6, 7, and 8 from Examples 6, 7, and 8 is that the amount of oxygen in the pulverization step was controlled to the lower limit and the upper limit.
  • FIG. 8 shows the relationship between the oxygen O content on the horizontal axis and the residual magnetic flux density on the vertical axis.
  • FIG. 9 shows the relationship between the oxygen O content on the horizontal axis and the coercive force on the vertical axis. From these figures, it is necessary to make oxygen O 1300 ppm or more and 2000 ppm or less so that the coercive force 1680 kA / m or more required as a high-performance permanent magnet is obtained. At this time, the residual magnetic flux density is 1.28 T or more. It can be confirmed that Table 3:
  • Example 6 Example 7, and Example 8 is superior to that of Comparative Example 8.
  • the coercive force of Example 6, Example 7, and Example 8 was 182 KA / m, 207 KA / m, and 194 KA / m higher than Comparative Example 7, respectively, and 235 KA / m respectively compared with Comparative Example 8. m, 260 KA / m, 267 KA / m higher.
  • the magnet coercive force performance of Examples 6, 7, and 8 is 10% to 20% superior to Comparative Examples 6 to 8.
  • the hydrogen furnace is evacuated to perform a dehydrogenation treatment. Thereafter, the coarsely pulverized alloy is pulverized to an average particle size of about 3.0 ⁇ m in a jet meal machine using high-pressure argon gas.
  • a certain amount of oxygen is put into the jet meal grinding gas during the grinding process, and then the powder is stored in an inert gas.
  • a certain amount of lubricant is added to the powder mixer.
  • the process of mixing the lubricant is performed under an argon gas protective atmosphere.
  • Example 2 Molding, sintering, and aging treatment As in Example 1, a sample having a diameter of 10 mm and a height of 10 mm was produced through machining.
  • Comparative Example 9 Comparative Example 9
  • Comparative Example 10 Comparative Example 11
  • the difference between Comparative Examples 9, 10 and 11 from Example 9 is the amount of lubricant added.
  • the lubricant is selected from one of methyl acetate, methyl caprylate, zinc stearate, and lithium stearate. These lubricants are organic substances containing carbon “C”. Therefore, in Comparative Examples 9, 10, and 11, the amount of the lubricant is controlled in the sintered body, and the carbon C content is varied.
  • FIG. 10 shows the relationship between the carbon C content on the horizontal axis and the residual magnetic flux density on the vertical axis.
  • FIG. 11 shows a relationship between the carbon C content on the horizontal axis and the coercive force on the vertical axis. From these figures, it is necessary to make carbon C 1100 ppm or more and 2000 ppm or less so that the coercive force 1680 kA / m or more required as a high-performance permanent magnet is obtained. At this time, the residual magnetic flux density is 1.28 T It can be confirmed that this is the case.
  • Table 4 shows the residual magnetic flux density
  • Example 9 the magnet residual magnetic flux density Br is higher by 0.08T and 0.07T than Comparative Examples 9 and 10, respectively. Compared with Comparative Example 11, the magnet coercivity is 249 KA / m higher.
  • the hydrogen furnace is dehydrogenated in a vacuum state. Thereafter, the coarsely pulverized alloy is pulverized to an average particle size of about 5.0 ⁇ m in a jet meal machine using high-pressure argon gas.
  • argon gas In order to prevent abnormal growth of crystal grains, a certain amount of oxygen is added to the jet meal grinding gas during the powder making process, and then the powder is stored in argon gas.
  • the hydrogen content was 2 ppm. This is achieved by adjusting the degree of vacuum after dehydrogenation.
  • a certain amount of lubricant is added to the material mixer.
  • the process of mixing the lubricant is an argon gas protective atmosphere.
  • Example 11 was prepared in the same process as Example 10, but the hydrogen content was 5 ppm.
  • Example 12 was prepared in the same process as Example 10, but the hydrogen content was 9 ppm.
  • Comparative Example 12 is prepared in the same manner as in Example 10, but the difference is the hydrogen content, which is achieved by adjusting the degree of vacuum after dehydrogenation.
  • FIG. 12 shows the relationship between the hydrogen H content on the horizontal axis and the residual magnetic flux density on the vertical axis.
  • FIG. 13 shows the relationship between the hydrogen H content on the horizontal axis and the coercive force on the vertical axis. From these figures, it is necessary to make hydrogen H 10 ppm or less so that the coercive force 1680 kA / m or more required as a high-performance permanent magnet is obtained. At this time, the residual magnetic flux density is 1.28 T or more. Can be confirmed. Table 5:
  • Pulverization The alloy is coarsely pulverized through a hydrogenation treatment, and a hydrogen furnace is evacuated to perform a dehydrogenation treatment. Thereafter, the coarsely pulverized alloy is pulverized to an average particle size of about 3.5 ⁇ m in a jet meal machine using high-pressure argon gas. In order to prevent abnormal growth of crystal grains, a certain amount of oxygen is put into the jet meal grinding gas during the powder making process, and then the powder is stored in argon gas.
  • a certain amount of lubricant is added to the material mixer.
  • the process of mixing the lubricant is performed under an argon gas protective atmosphere.
  • Example 2 Molding, sintering, and aging treatment As in Example 1, a sample having a diameter of 10 mm and a height of 10 mm is prepared through machining.
  • Comparative Example 13 and Comparative Example 14 are also produced. Alloy Production Method of Comparative Example 13
  • a metal or alloy raw material is melted and refined in a vacuum or an inert gas (argon gas optimum) atmosphere.
  • the alloy is a component of the sintered body RTB-MA, R is Nd: 22.5% by mass, Dy: 3.5% by mass, Pr: 5.0% by mass, T is Fe: 66.35 mass% Co: 1.0% by mass, B is B: 1.0% by mass M is Al: 0.3% by mass, Cu: 0.1% by mass As other Ga: 0.15% by mass, Nb: 0.05% by mass, Mo: 0.05 mass%
  • An alloy consisting of The molten alloy is cooled and solidified with a roll by a strip casting method to obtain a flake alloy.
  • the hydrogen furnace is evacuated to perform a dehydrogenation treatment. Thereafter, using the high-pressure nitrogen gas, the coarsely pulverized alloy is finely pulverized into a powder having an average particle diameter of about 6.0 ⁇ m in a jet meal machine.
  • a certain amount of oxygen is put into the inert gas for jet meal grinding during the grinding process. Thereafter, the powder is stored in nitrogen gas.
  • a certain amount of lubricant is added to the powder mixer.
  • the process of mixing the lubricant is performed under an argon gas protective atmosphere.
  • Alloy Preparation Method of Comparative Example 14 A metal or alloy raw material is melted and refined in a vacuum or an inert gas (argon gas optimum) atmosphere.
  • the alloy is a component of the sintered body RTB-MA, R is Nd: 21.5% by mass, Dy: 4.5% by mass, Pr: 5.0% by mass, T is Fe: 66.45 mass% Co: 1.0% by mass B is B: 1.0% by mass M is Al: 0.3% by mass, Cu: 0.1% by mass, As other Ga: 0.05 mass%, Nb: 0.05% by mass, Mo: 0.05 mass%
  • An alloy consisting of The molten alloy is cooled and solidified with a roll by a strip casting method to obtain a flake alloy.
  • the hydrogen furnace is placed in a vacuum state to perform a dehydrogenation treatment. Thereafter, using the high-pressure nitrogen gas, the coarsely pulverized alloy is pulverized into a powder having an average particle diameter of about 8.0 ⁇ m in a jet meal machine.
  • a certain amount of oxygen is put into the inert gas for jet meal grinding during the grinding process. Thereafter, the powder is stored in nitrogen gas.
  • a certain amount of lubricant is added to the powder mixer.
  • the process of mixing the lubricant is performed under an argon gas protective atmosphere.
  • Table 7 As shown in Table 7, the effect of this example is Regarding rare metal elements (Ga, Nb, Mo), Ga can be reduced to 1/40 to 1/150 or less, Nb is 1/50 or less, and Mo is 1/5 or less, as compared with the comparative example. There is a merit that can be reduced.
  • the expensive rare earth element Dy has a reduction effect of about 20%.

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Abstract

L'invention concerne un aimant permanent de terres rares à système R-T-B-M-A. Se distinguant par son faible coût, cet aimant offre une coercivité améliorée (Hcj) sans pour autant être affecté par une diminution de la densité du flux magnétique résiduel (Br) grâce à un contrôle de l'azote (N), du carbone (C), de l'oxygène (O) et de l'hydrogène (H) à des quantités appropriées. L'invention divulgue en particulier un matériau de terres rares pour aimant permanent qui a principalement la configuration d'un composé R2T14B lequel présente une teneur en R de 24-34 % par masse, en T de 63-74 % par masse et en B de 0,5-1,5 % par masse, le restant étant constitué de M et de A. Les éléments-traces A s'établissent à 1.100-2.000 ppm de C, à 10 ppm au maximum de H, à 1.300-2.000 ppm de O et à 150 ppm au maximum de N. Le matériau de terres rares pour aimant permanent est soumis à un processus de pulvérisation dans une atmosphère à gaz inerte et le diamètre moyen des particules est de 2-5 μm.
PCT/JP2010/072782 2010-04-02 2010-12-17 Aimant permanent de terres rares à système r-t-b-m-a et son procédé de production WO2011125262A1 (fr)

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JP2014145129A (ja) * 2013-01-29 2014-08-14 Yantai Shougang Magnetic Materials Inc Ｒ−ｔ−ｂ−ｍ−ｃ系焼結磁石の製造方法、当該方法で製造された磁石、及びその製造装置
EP3185252A4 (fr) * 2014-08-18 2017-08-30 Intermetallics Co. Ltd. AIMANT FRITTÉ À BASE DE RFeB

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JP6003452B2 (ja) * 2012-09-20 2016-10-05 トヨタ自動車株式会社 希土類磁石の製造方法
CN103258634B (zh) * 2013-05-30 2015-11-25 烟台正海磁性材料股份有限公司 一种制备高性能R-Fe-B系烧结磁体方法
CN110993232B (zh) * 2019-12-04 2021-03-26 厦门钨业股份有限公司 一种r-t-b系永磁材料、制备方法和应用

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