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WO2015058654A1 - Composition de poudre et procédé de préparation d'un aimant fritté de la série r-fe-b - Google Patents

Composition de poudre et procédé de préparation d'un aimant fritté de la série r-fe-b Download PDF

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Publication number
WO2015058654A1
WO2015058654A1 PCT/CN2014/088848 CN2014088848W WO2015058654A1 WO 2015058654 A1 WO2015058654 A1 WO 2015058654A1 CN 2014088848 W CN2014088848 W CN 2014088848W WO 2015058654 A1 WO2015058654 A1 WO 2015058654A1
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Prior art keywords
magnet
component
powder composition
powder
uniformity
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Chinese (zh)
Inventor
陈国安
赵玉刚
胡伯平
饶晓雷
张瑾
钮萼
陈治安
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SANVAC (BEIJING) MAGNETICS CO Ltd
Beijing Zhong Ke San Huan High Tech Co Ltd
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SANVAC (BEIJING) MAGNETICS CO Ltd
Beijing Zhong Ke San Huan High Tech Co Ltd
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    • 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
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
    • H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/107—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing organic material comprising solvents, e.g. for slip casting
    • 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
    • B22F3/1003—Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007—Atmosphere
    • B22F3/101—Changing atmosphere
    • 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
    • B22F3/1017—Multiple heating or additional steps
    • 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
    • B22F3/1017—Multiple heating or additional steps
    • B22F3/1028—Controlled cooling
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
    • 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
    • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
    • 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
    • C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
    • 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
    • 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
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/20—Ferrous alloys, e.g. steel alloys containing chromium with copper
    • 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
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/28—Ferrous alloys, e.g. steel alloys containing chromium with titanium or zirconium
    • 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
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/30—Ferrous alloys, e.g. steel alloys containing chromium with 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
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/42—Ferrous alloys, e.g. steel alloys containing chromium with nickel with copper
    • 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
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/50—Ferrous alloys, e.g. steel alloys containing chromium with nickel with titanium or zirconium
    • 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
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/52—Ferrous alloys, e.g. steel alloys containing chromium with nickel with cobalt
    • 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

Definitions

  • the present invention relates to a powder composition and method for preparing an R-Fe-B based sintered magnet.
  • a large amount of heavy rare-earth elements RH (Dy( ⁇ ), Tb( ⁇ )) is added to the R-Fe-B based sintered magnet to replace the rare earth element R in the R 2 Fe 14 B phase, and the coercive force of the magnet can be remarkably improved.
  • Dy 2 Fe 14 B or Tb 2 Fe 14 B has a higher magnetocrystalline anisotropy field than Nd 2 Fe 14 B, so that the intrinsic coercive force of the magnet may be further improved.
  • the magnetocrystalline anisotropy field ratio Nd 2 of the solid solution phase (Nd, Dy) 2 Fe 14 B or (Nd, Tb) 2 Fe 14 B formed after the Dy/Tb moiety replaces the Nd in the main phase Nd 2 Fe 14 B
  • the Fe 14 B is large, so that the coercive force of the sintered magnet can be remarkably improved.
  • Patent document CN 200610089124.7 shows a method for preparing high-coercivity Nd-Fe-B sintered magnets by using nano Dy and Tb powders as the second phase and mixing with the main alloy powder. law. Under the same conditions, the method can save the use of heavy rare earth to a certain extent, but the coercive force is less increased and the remanence is significantly reduced.
  • Patent document CN 201110024823.4 provides a method for thermally diffusing a powder of heavy rare earth fluoride, nitrate and phosphate on the surface of a magnet, solving the problem of uneven distribution of molten material remaining on the surface after thermal diffusion of the magnet, thereby solving the coating problem.
  • the composition of the powder and the state of the surface of the magnet and the like may affect the effect of the coercive force very sensitively.
  • an object of the present invention is to provide a powder composition for preparing an R-Fe-B based sintered magnet and a method for producing an R-Fe-B based sintered magnet using the powder composition, having a substantially holding magnet
  • the technical effect of the coercive force of the magnet is remarkably improved by using a very small amount of heavy rare earth Dy ( ⁇ ) or Tb ( ⁇ ).
  • the powder composition for producing an R-Fe-B based sintered magnet provided by the present invention is composed of the component (A), the component (B) and the component (C).
  • the component (A) is one or more powders selected from the group consisting of fluorides, oxides, and oxyfluorides of heavy rare earths.
  • the component (B) is a rare earth-transition intermetallic compound powder having a MgCu 2 crystal structure.
  • the component (C) is selected from one or more of the rare earth hydrated nitrate powders.
  • the component (A) is from 1% to 98% by weight of the powder composition, and the component (B) is from 1% to 98% by weight of the powder composition, the component (C) is from 1% to 98% by weight of the powder composition.
  • the content of the rare earth element is ⁇ 55% by weight, and the weight percentage of the sum of lanthanum, cerium or lanthanum and cerium is ⁇ 10%, and iron, cobalt or iron and cobalt in the transition metal element And the weight percentage is ⁇ 40%, and the balance is at least one selected from the group consisting of copper, titanium, chromium, zinc, and nickel.
  • the component (A) has an average particle diameter of ⁇ 50 ⁇ m.
  • the component (B) has an average particle diameter of from 2 to 10 ⁇ m.
  • the component (C) has an average particle diameter of ⁇ 100 ⁇ m.
  • the present invention also provides a method of preparing an R-Fe-B based sintered magnet, comprising the steps of: dissolving the powder composition according to any one of claims 1 to 6 in an organic solvent to prepare a treatment liquid; The treatment liquid is applied to the magnet; and the magnet after the treatment liquid is applied is subjected to vacuum heat treatment.
  • the content of the powder composition in the treatment liquid is 0.01 to 1.0 g/mL.
  • the treatment liquid further includes a dispersant, and the volume ratio of the dispersant to the organic solvent is less than 1%.
  • the organic solvent is selected from the group consisting of alcohols, alkanes or esters having 5 to 16 carbon atoms.
  • the step of applying the treatment liquid to the magnet includes immersing the magnet in the treatment liquid in a stirred state for a immersion time of 1 to 60 minutes.
  • the vacuum heat treatment comprises the steps of: placing the magnet after coating the treatment liquid into a vacuum sintering furnace, evacuating to a vacuum of 10 -2 Pa; heating to 820 to 1050 ° C, and holding for 1 to 8 hours; The argon gas is cooled to below 100 ° C, the cooling is stopped, and the vacuum is evacuated to a vacuum of 10 -2 Pa; the temperature is raised to 450 ° C to 620 ° C, and the temperature is maintained for 1 to 5 hours; and the argon gas is cooled to 80 ° C or less.
  • the present invention also provides an R-Fe-B based sintered magnet comprising a magnet portion and a coating portion on an outer surface of the magnet portion, the coating portion being formed of the above powder composition.
  • the present invention also provides an R-Fe-B based sintered magnet prepared by the above method.
  • component A is one or more powders selected from the group consisting of fluorides, oxides and/or oxyfluorides of cerium and/or cerium
  • component B is a rare earth having a crystal structure of MgCu 2 -
  • the transition metal intermetallic compound powder, component C is one or more selected from the group consisting of rare earth hydrated nitrate powders.
  • Component A is from 1% to 98% by weight of the powder composition
  • Component B is from 1% to 98% by weight of the powder composition
  • Component C is from 1% to 98% by weight of the powder composition.
  • Component A has an average particle diameter of not more than 50 ⁇ m.
  • the content of the rare earth element is not less than 55% by weight, and the weight percentage of the sum of Dy, Tb or Dy and Tb is not less than 10%, and Fe, Co or Fe and Co in the transition metal element
  • the weight percentage is not less than 40%, and the balance is at least one of Cu, Ti, Cr, Zn, Ni, and the like.
  • Component B has an average particle diameter of 2 to 10 ⁇ m.
  • Component C has an average particle diameter of not more than 100 ⁇ m.
  • the structure is uniform, which reduces the amount of heavy rare earth used, thereby saving manufacturing costs.
  • the above powder composition can be processed for different specifications and different grades of magnets, and the powder can be uniformly distributed on the surface of the magnet during the coating process, and no large melt residue remains after the heat treatment is diffused, and the powder can be remarkably improved.
  • Coercive force and almost no reduction of remanence and maximum magnetic energy product, to ensure uniformity and consistency of coercivity improvement of magnets of different specifications and different grades, as well as stability and consistency of coercivity improvement of different batches of products.
  • the uniformity of remanence is ⁇ 0.9%
  • the uniformity of coercive force is ⁇ 2%
  • the uniformity of maximum magnetic energy product is ⁇ 2.5%.
  • uniformity is expressed using (very poor/average value) ⁇ 100 (%), and the larger the numerical value, the lower the uniformity; the smaller the numerical value, the higher the uniformity.
  • the above powder composition was used to prepare an R-Fe-B based sintered magnet by referring to the following process.
  • the components A, B and C are mixed in a certain ratio to prepare a powder composition.
  • the powder composition is stored, configured and used under the protection of an inert gas.
  • the slurry is used as a mixed powder slurry for grain boundary diffusion and permeation, and is coated on a magnet which is subjected to surface cleaning treatment or conversion film treatment such as phosphating or oxidation after machining, without adding metal, non-metal or organic
  • the magnet of the protective layer, and the oxygen content of the magnet is 4000 ppm or less, and the magnetization direction of the magnet (ie, the orientation direction of the magnet) is 10 mm or less.
  • the above organic solvent may be an alcohol or an alkane or an ester having 5 to 16 carbon atoms.
  • the alcohol may be selected from the group consisting of ethanol, propanol, isopropanol, butanol, and butanol.
  • the alkane may be selected from cyclohexane and cyclooctane.
  • the esters may be selected from ethyl acetate and isobutyl acetate.
  • the slurry may be applied to the surface of the magnet by immersing the magnet in a slurry in a stirred state for a immersion time of 1 to 60 minutes. Then, the processed magnet is placed in a metal box and sealed, and the material of the metal box is iron, steel, molybdenum, tungsten, tantalum.
  • the vacuum heat treatment can be carried out in the following manner. First, the cartridge was placed in a vacuum sintering furnace and evacuated to a vacuum of 10 -2 Pa. Next, the temperature was raised to 820 to 1050 ° C, and the temperature was kept for 1 to 8 hours. Then, when the argon gas was cooled to below 100 ° C, the cooling was stopped, and the vacuum was evacuated until the degree of vacuum reached 10 -2 Pa. The temperature was raised again to 450 ° C to 620 ° C, and the temperature was kept for 1 to 5 hours. After that, it was cooled by argon gas to below 80 °C.
  • the above powder composition is used as a diffusion permeation source, which can significantly improve the coercive force of the magnet, and is advantageous for controlling the stability and consistency of the coercivity between batches.
  • the reproducibility of the diffusion process to achieve the purpose of industrial preparation.
  • Component A cesium fluoride powder having an average particle diameter of 10 ⁇ m.
  • Component B Rare earth-transition intermetallic compound powder having a MgCu 2 crystal structure having an average particle diameter of 2 ⁇ m, specific components and weight percentages are 15% Nd, 12% Pr, 30% Dy, 42% Fe, 1% Cu .
  • Component C cerium nitrate pentahydrate powder having an average particle diameter of 100 ⁇ m.
  • the powder composition was dispersed in ethanol at a ratio of 0.01 g/mL to form a slurry, that is, 0.01 g of the powder composition was mixed per 1 mL of ethanol.
  • the sintered NdFeB blank machine without aging treatment is processed into a circular magnetic piece having a diameter of 10 mm and a height of 3.5 mm, and then subjected to conventional degreasing treatment, pickling in a 5% (volume%) concentration of nitric acid, ultrasonic cleaning and Blow dry.
  • the treated magnetic sheet was completely immersed in the slurry in a stirred state for 1 minute, and the impregnated magnet was placed in a tinplate box to be sealed.
  • the cartridge was placed in a vacuum sintering furnace, evacuated, and heated to 820 ° C when the degree of vacuum reached 10 -2 Pa or more, and kept for 3 hours. Then the heating was stopped and the argon gas was cooled to below 100 °C. After that, the cooling was stopped, and the vacuum was evacuated to 10 -2 Pa, and then heated to 450 ° C for 3 hours. Then, the heating was stopped and argon gas was charged, and the mixture was cooled to 80 ° C or lower.
  • control magnet 1 was prepared, except that the slurry impregnation magnet was not used, and the other process steps were the same as those of the magnet of Example 1.
  • Component A cerium oxide powder having an average particle diameter of 20 ⁇ m.
  • Component B Rare earth-transition intermetallic compound powder having a MgCu 2 crystal structure having an average particle diameter of 6 ⁇ m, specific components and weight percentages of 10% Nd, 12% Pr, 35% Dy, 41% Fe and 2% Co .
  • Component C cerium nitrate hexahydrate powder having an average particle diameter of 50 ⁇ m.
  • the powder composition was dispersed in pentanol at a ratio of 0.05 g/mL to form a slurry, that is, 0.05 g of the above powder composition was dispersed per 1 mL of pentanol.
  • the sintered NdFeB blank without aging treatment is machined into a magnetic piece having a diameter of 10 mm and a height of 5 mm, and the magnetic piece is subjected to conventional degreasing, pickling in a 5% (volume%) concentration of nitric acid, ultrasonic cleaning and drying. .
  • the treated magnetic sheet was completely immersed in the slurry in a stirred state for 60 minutes, and the impregnated magnet was placed in a stainless steel container and sealed.
  • the cartridge was placed in a vacuum sintering furnace, evacuated, and heated to 1050 ° C when the degree of vacuum reached 10 -2 Pa or more, and kept for 1 hour. Then the heating was stopped and the argon gas was cooled to below 100 °C. After that, the cooling was stopped, and the vacuum was applied to 10 -2 Pa, heated to 620 ° C, and kept for 1 hour. Next, the heating was stopped, argon gas was charged, and the temperature was cooled to below 80 °C.
  • control magnet 2 was prepared, and the other process steps were the same as those of the magnet of Example 2 except that the slurry was not impregnated with the slurry containing the powder composition.
  • Component A bismuth oxyfluoride powder having an average particle diameter of 30 ⁇ m.
  • Component B Rare earth-transition intermetallic compound powder having a MgCu 2 crystal structure having an average particle diameter of 3 ⁇ m, specific components and weight percentages of 10% Nd, 15% Pr, 25% Dy, 7% Tb, 41.9% Fe , 1% Co and 0.1% Cu.
  • Component C 3.5 hydrate cerium nitrate powder having an average particle diameter of 30 ⁇ m.
  • the powder composition was dispersed in isopropyl alcohol in a ratio of 0.1 g/mL to form a slurry, that is, 0.1 g of the powder composition was mixed per 1 mL of isopropyl alcohol.
  • the sintered NdFeB blank without aging treatment was machined into a magnetic piece having a diameter of 10 mm and a height of 10 mm, and then subjected to a conventional degreasing treatment, pickled in a 5% (by volume) concentration of nitric acid, ultrasonically washed, and blown dry.
  • the treated magnetic sheet was completely immersed in the slurry under stirring for 15 minutes, and the impregnated magnet was placed in a molybdenum cartridge and sealed.
  • the cartridge was placed in a vacuum sintering furnace, evacuated, and heated to 950 ° C when the degree of vacuum reached 10 -2 Pa or more, and kept for 8 hours. Then the heating was stopped and the argon gas was cooled to below 100 °C. After that, the cooling was stopped, the vacuum was applied to 10 -2 Pa, and the mixture was heated to 500 ° C for 5 hours. Then, the heating was stopped, argon gas was charged, and the temperature was cooled to 80 ° C or lower.
  • a control magnet 3 was prepared, and the other process steps were the same as those of the magnet of Example 3, except that the slurry was not impregnated with the slurry containing the powder composition.
  • Component A cesium fluoride or cerium oxide powder having an average particle diameter of 5 ⁇ m.
  • Component B Rare earth-transition intermetallic compound powder having a MgCu 2 crystal structure with an average particle diameter of 4 ⁇ m, specific composition and weight percentage of 28% Nd, 25% Dy, 3% Ho, 42.7% Fe, 1% Co , 0.1% Cu, 0.1% Ga and 0.1% Zr.
  • Component C cerium nitrate trihydrate powder having an average particle diameter of 20 ⁇ m.
  • the sintered NdFeB blank without aging treatment is machined into a magnetic piece having a diameter of 10 mm and a height of 2 mm, and the magnetic piece is subjected to conventional degreasing treatment, pickled in a 5% (by volume) concentration of nitric acid, ultrasonically washed and blown. dry.
  • the treated magnetic sheet was completely immersed in the slurry under stirring for 25 minutes, and the impregnated magnet was placed in a tungsten box and sealed.
  • the cartridge was placed in a vacuum sintering furnace, evacuated, and heated to 920 ° C when the degree of vacuum reached 10 -2 Pa or more, and kept for 4 hours. Then the heating was stopped and the argon gas was cooled to below 100 °C. After that, the cooling was stopped, and the vacuum was evacuated to 10 -2 Pa, and then heated to 550 ° C for 3 hours. Then, the heating was stopped, and the argon gas was cooled to 80 ° C or lower.
  • a control magnet 4 was prepared, and the other process steps were the same as those of the magnet of Example 4, except that the slurry was not impregnated with the slurry containing the powder composition.
  • Component A cesium fluoride, cerium oxide, cerium oxyfluoride powder having an average particle diameter of 1 ⁇ m.
  • Component B Rare earth-transition intermetallic compound powder having a MgCu 2 crystal structure with an average particle diameter of 5 ⁇ m, specific composition and weight percentage of 22% Pr, 30% Dy, 6% Ho, 38.1% Fe, 3% Co , 0.5% Cu, 0.2% Ga, 0.1% Cr and 0.1% Mn.
  • Component C cerium nitrate hexahydrate powder having an average particle diameter of 20 ⁇ m.
  • the powder composition was dispersed in ethyl acetate at a ratio of 1 g/mL to form a slurry, that is, 1 g of the above powder composition was mixed per 1 mL of ethyl acetate.
  • the sintered NdFeB blank without aging treatment is machined to a diameter of 10 mm and height A magnetic sheet of 1 mm was subjected to conventional degreasing treatment, pickled in a 5% (by volume) concentration of nitric acid, ultrasonically washed and blown dry.
  • the treated magnetic sheet was completely immersed in the slurry under stirring for 40 minutes, and the impregnated magnet was placed in a stainless steel case and sealed.
  • the cartridge was placed in a vacuum sintering furnace, evacuated, and heated to 1000 ° C when the degree of vacuum reached 10 -2 Pa or more, and kept for 5 hours. Then the heating was stopped and the argon gas was cooled to below 100 °C. After that, the cooling was stopped, and the vacuum was evacuated to 10 -2 Pa, and then heated to 480 ° C for 2.5 hours. Next, the heating was stopped, and the argon gas was cooled to 80 ° C or lower.
  • control magnet 5 was simultaneously prepared, and the other process steps were the same as those of the magnet of Example 5 except that the slurry was not impregnated with the slurry containing the powder composition.
  • Component A cesium fluoride or cerium oxide powder having an average particle diameter of 1 ⁇ m.
  • Component B Rare earth-transition intermetallic compound powder having a MgCu 2 crystal structure having an average particle diameter of 2 ⁇ m, specific components and weight percentages of 3% La, 1% Ce, 7% Pr, 11% Nd, 21% Dy 6% Tb, 6% Ho, 41% Fe, 3% Co, 0.5% Cu, 0.1% Ni, 0.2% Ga, 0.1% Cr and 0.1% Ti.
  • Component C cerium nitrate hexahydrate or cerium nitrate pentahydrate powder having an average particle diameter of 10 ⁇ m.
  • the powder composition was dispersed in cyclooctane at a ratio of 0.2 g/mL to form a slurry, that is, 0.2 g of the above powder composition was mixed per 1 mL of cyclooctane.
  • the sintered NdFeB blank without aging treatment is machined to a diameter of 10 mm and height A 3.5 mm magnetic piece was subjected to conventional degreasing treatment, pickled in a 5% (by volume) concentration of nitric acid, ultrasonically washed, and blown dry.
  • the treated magnetic sheet was completely immersed in the slurry under stirring for 5 minutes, and the impregnated magnet was placed in a stainless steel cartridge and sealed.
  • the cartridge was placed in a vacuum sintering furnace, evacuated, and heated to 850 ° C when the degree of vacuum reached 10 -2 Pa or more, and kept for 2.5 hours. Then the heating was stopped and the argon gas was cooled to below 100 °C. After that, the cooling was stopped, and the vacuum was evacuated to 10 -2 Pa, and then heated to 490 ° C for 2 hours. Next, the heating was stopped, and the argon gas was cooled to 80 ° C or lower.
  • a control magnet 6 was prepared, and the other process steps were the same as those of the magnet of Example 6, except that the slurry was not impregnated with the slurry containing the powder composition.
  • Component A bismuth oxyfluoride powder having an average particle diameter of 40 ⁇ m.
  • Component B Rare earth-transition intermetallic compound powder having a MgCu 2 crystal structure having an average particle diameter of 3 ⁇ m, specific components and weight percentages of 0.5% La, 3.5% Ce, 17% Pr, 30% Dy, 5% Ho 41.2% Fe, 2.5% Co, 0.3% Cu.
  • Component C cerium nitrate trihydrate, cerium nitrate hexahydrate, cerium nitrate pentahydrate having an average particle diameter of 5 ⁇ m.
  • the powder composition was dispersed in isobutyl acetate in a ratio of 0.3 g/mL to form a slurry, that is, 0.3 g of the above powder composition was mixed per 1 mL of isobutyl acetate.
  • the sintered NdFeB blank without aging treatment is machined into a magnetic piece having a diameter of 10 mm and a height of 1.0 mm, and the magnetic piece is subjected to conventional degreasing treatment at a concentration of 5% by volume.
  • the nitric acid is pickled, ultrasonically cleaned and blown dry.
  • the treated magnetic sheet was completely immersed in the slurry under stirring for 10 minutes, and the impregnated magnet was placed in a stainless steel cartridge and sealed.
  • the cartridge was placed in a vacuum sintering furnace, and a vacuum was applied.
  • the degree of vacuum reached 10 -2 Pa or more
  • the temperature was raised to 820 ° C and the temperature was maintained for 8 hours.
  • the heating was stopped and the argon gas was cooled to below 100 °C.
  • the cooling was stopped, and the vacuum was applied to 10 -2 Pa, and then heated to 510 ° C for 3 hours.
  • the heating was stopped, and the argon gas was cooled to 80 ° C or lower.
  • a control magnet 7 was prepared, and the other process steps were the same as those of the magnet of Example 7, except that the slurry was not impregnated with the slurry containing the powder composition.
  • Component A cerium oxide powder having an average particle diameter of 15 ⁇ m.
  • Component B Rare earth-transition intermetallic compound powder having a MgCu 2 crystal structure with an average particle diameter of 4 ⁇ m, specific components and weight percentages of 2% Ce, 22% Nd, 16% Dy, 15% Tb, 2% Ho 40.8% Fe, 1% Co, 0.1% Cu, 0.5% Ni, 0.2% Ga, 0.2% Cr and 0.2% Ti.
  • Component C cerium nitrate pentahydrate or cerium nitrate hexahydrate having an average particle diameter of 80 ⁇ m.
  • the powder composition was dispersed in propanol at a ratio of 0.6 g/mL to form a slurry, that is, 0.6 g of the above powder composition was mixed per 1 mL of propanol.
  • the sintered NdFeB blank without aging treatment is machined into a magnetic piece having a diameter of 10 mm and a height of 5.0 mm, and the magnetic piece is subjected to conventional degreasing treatment, pickled in a 5% (by volume) concentration of nitric acid, and ultrasonically cleaned. Blow dry.
  • the treated magnetic sheet was completely immersed in the slurry under stirring for 30 minutes, and the impregnated magnet was placed in a stainless steel case and sealed.
  • the cartridge was placed in a vacuum sintering furnace, evacuated, and the temperature was raised to 830 ° C when the degree of vacuum reached 10 -2 Pa or more, and the temperature was maintained for 7 hours. Then the heating was stopped and the argon gas was cooled to below 100 °C. After that, the cooling was stopped, and the vacuum was evacuated to 10 -2 Pa, and then heated to 520 ° C for 4 hours. Next, the heating was stopped, and the argon gas was cooled to 80 ° C or lower.
  • a control magnet 8 was prepared, and the other process steps were the same as those of the magnet of Example 8, except that the slurry was not impregnated with the slurry containing the powder composition.
  • Component A cerium oxide having an average particle diameter of 25 ⁇ m, cerium oxide powder.
  • Component B Rare earth-transition intermetallic compound powder having a MgCu 2 crystal structure with an average particle diameter of 5 ⁇ m, specific components and weight percentages of 3% La, 1% Ce, 7% Pr, 30% Nd, 15% Dy , 42.5% Fe, 1.5% Co.
  • Component C cerium nitrate hexahydrate or cerium nitrate pentahydrate powder having an average particle diameter of 60 ⁇ m.
  • the powder composition was dispersed in butanol at a ratio of 0.7 g/mL to form a slurry, that is, 0.7 g of the above powder composition was mixed per 1 mL of butanol.
  • the sintered NdFeB blank without aging treatment is machined into a magnetic piece having a diameter of 10 mm and a height of 8.0 mm, and the magnetic piece is subjected to conventional degreasing treatment, pickled in a 5% (by volume) concentration of nitric acid, and ultrasonically cleaned. Blow dry.
  • the treated magnetic sheet was completely immersed in the slurry under stirring for 50 minutes, and the impregnated magnet was placed in a stainless steel container and sealed.
  • the cartridge was placed in a vacuum sintering furnace, vacuum was applied, and the temperature was raised to 920 ° C when the degree of vacuum reached 10 -2 Pa or more, and the temperature was maintained for 6.5 hours. Then the heating was stopped and the argon gas was cooled to below 100 °C. After that, the cooling was stopped, and the vacuum was evacuated to 10 -2 Pa, and then heated to 610 ° C for 5 hours. Next, the heating was stopped, and the argon gas was cooled to 80 ° C or lower.
  • a control magnet 9 was prepared, and the other process steps were the same as those of the magnet of Example 9, except that the slurry was not impregnated with the slurry containing the powder composition.
  • Component A cesium fluoride powder having an average particle diameter of 3 ⁇ m.
  • Component B Rare earth-transition intermetallic compound powder having a MgCu 2 crystal structure with an average particle diameter of 6 ⁇ m, specific components and weight percentages are 25% Nd, 25% Dy, 5% Tb, 1% Ho, 43% Fe , 0.5% Co, 0.1% Cu, 0.1% Ga, 0.2% Cr and 0.1% Ti.
  • Component C cerium nitrate pentahydrate, cerium nitrate trihydrate, cerium nitrate hexahydrate having an average particle diameter of 2 ⁇ m.
  • the powder composition was dispersed in pentanol at a ratio of 0.8 g/mL to form a slurry, that is, 0.8 g of the above powder composition was mixed per 1 mL of pentanol.
  • the sintered NdFeB blank without aging treatment is machined into a magnetic piece having a diameter of 10 mm and a height of 2.0 mm, and the magnetic piece is subjected to conventional degreasing treatment, pickled in a 5% (by volume) concentration of nitric acid, and ultrasonically cleaned. Blow dry.
  • the treated magnetic sheet was completely immersed in the slurry under stirring for 25 minutes, and the impregnated magnet was placed in a stainless steel case and sealed.
  • the cartridge was placed in a vacuum sintering furnace, evacuated, and heated to 930 ° C when the degree of vacuum reached 10 -2 Pa or more, and kept for 5 hours. Then the heating was stopped and the argon gas was cooled to below 100 °C. After that, the cooling was stopped, and the vacuum was evacuated to 10 -2 Pa, and then heated to 485 ° C for 6 hours. Next, the heating was stopped, and the argon gas was cooled to 80 ° C or lower.
  • control magnet 10 was prepared, except that the slurry was impregnated with the slurry containing the powder composition, and the other process steps were the same as those of the magnet of Example 10.
  • the coercive force of the magnet can be remarkably improved while substantially maintaining the remanence and the maximum magnetic energy product.
  • Component A cerium oxide powder having an average particle diameter of 20 ⁇ m.
  • Component B Rare earth-transition intermetallic compound powder having a MgCu 2 crystal structure having an average particle diameter of 6 ⁇ m, specific components and weight percentages of 10% Nd, 12% Pr, 35% Dy, 41% Fe and 2% Co .
  • Component C cerium nitrate hexahydrate powder having an average particle diameter of 50 ⁇ m.
  • the mixed powder composition was dispersed in pentanol at a ratio of 0.05 g/mL to form a slurry, that is, 0.05 g of the above mixed powder was dispersed per 1 mL of pentanol.
  • the N48M sintered NdFeB blank machine without aging treatment was processed into a D10mm ⁇ 5mm wafer and a 10mm ⁇ 10mm ⁇ 5mm square piece, and the magnetic sheet was subjected to conventional degreasing at a concentration of 5% (volume percent) nitric acid. Pickled, ultrasonically cleaned and blown dry.
  • the treated magnetic sheet was completely immersed in the slurry in a stirred state for 60 minutes, and the impregnated magnet was placed in a stainless steel container and sealed.
  • a control magnet 11 was prepared, and the above-mentioned N48M magnetic sheet was selected as a coating substrate of 10 mm*10 mm*5 mm, except that the magnet was impregnated with a slurry of cerium nitrate, and other process steps were the same as those of the magnet of Example 11.
  • the heat treatment process conditions are as follows: the cartridge is placed in a vacuum sintering furnace, vacuum is applied, and the temperature is raised to 1050 ° C when the degree of vacuum reaches 10 -2 Pa or more, and the temperature is maintained for 1 hour. Then the heating was stopped and the argon gas was cooled to below 100 °C. After that, the cooling was stopped, and the vacuum was applied to 10 -2 Pa, heated to 620 ° C, and kept for 1 hour. Next, the heating was stopped, argon gas was charged, and the temperature was cooled to below 80 °C.
  • the magnetic properties of the square magnets of the uncoated and heat-treated square magnets, the square magnet of Example 11, and the magnetic specimen of Comparative Magnetic Example 11 were averaged and the calculated range was compared. The results are shown in Table 11-1. . At the same time, the average results of the magnetic properties of the 30 pieces of the wafer and the square piece after the first batch treatment and the extremely poor results are shown in Table 11-2. The magnetic performance results and the extremely poor results of the five batches of treated square sheets are shown in Table 11-3.
  • uniformity is expressed using (very poor/average value) ⁇ 100 (%), and the larger the numerical value, the lower the uniformity; the smaller the numerical value, the higher the uniformity.
  • the values in parentheses below the range are (very poor/average) ⁇ 100 (%), which are used to indicate uniformity.
  • the technical solution of the present invention not only improves the magnet Hcj well, but also reduces the Br and the magnetic energy product, and improves the product consistency of batch production of different batches and different specifications. And uniformity.
  • Component A cesium fluoride or cerium oxide powder having an average particle diameter of 1 ⁇ m.
  • Component B Rare earth-transition intermetallic compound powder having a MgCu 2 crystal structure having an average particle diameter of 2 ⁇ m, specific components and weight percentages of 3% La, 1% Ce, 7% Pr, 11% Nd, 21% Dy, 6% Tb, 6% Ho, 41% Fe, 3% Co, 0.5% Cu, 0.1% Ni, 0.2% Ga, 0.1% Cr and 0.1% Ti.
  • Component C cerium nitrate hexahydrate or cerium nitrate pentahydrate powder having an average particle diameter of 10 ⁇ m.
  • the mixed powder composition was dispersed in pentanol at a ratio of 0.05 g/mL to form a slurry, that is, 0.05 g of the above mixed powder was dispersed per 1 mL of pentanol.
  • the N35SH sintered NdFeB blank machine without aging treatment was processed into a D10 mm ⁇ 5 mm wafer, the magnetic sheet was subjected to conventional degreasing, pickled in a 5% (volume percent) concentration of nitric acid, ultrasonically washed and blown dry.
  • the treated magnetic sheet was completely immersed in the slurry in a stirred state for 60 minutes, and the impregnated magnet was placed in a stainless steel container and sealed.
  • a comparative example magnet 12 was prepared, except that the magnet was impregnated with a slurry of cesium fluoride, and the other process steps were the same as those of the magnet of Example 12.
  • the D10 mm ⁇ 5 mm wafer magnet of Example 12 and the D10 mm * 5 mm wafer magnet of Comparative Example 12 were placed together in the same vacuum sintering furnace for heat treatment. Further, the wafer magnet of Example 12 was separately selected, and a total of 5 batches of heat treatment were performed for each batch of 2000 sheets. The heat treatment process conditions for all batches are consistent as shown below.
  • 30 sheets were each selected for measurement of magnetic properties. Batches of the examples were separately processed. 30 magnets were selected per batch for magnetic performance measurements. In addition, 30 pieces of N35SH disk magnets which were not coated and heat-treated were selected for magnetic property measurement.
  • the magnetic properties of the comparative examples were different from those of the uncoated magnets and the comparative examples. Performance consistency of products between different batches of the example. The average value and the extreme difference of the measured values of the magnetic properties of each batch of magnets were compared. The results are shown in Table 12-1 and Table 12-2.
  • Heat treatment process conditions The material box is placed in a vacuum sintering furnace, vacuum is applied, and the temperature is raised to 1050 ° C when the degree of vacuum reaches 10 -2 Pa or more, and the temperature is kept for 1 hour. Then the heating was stopped and the argon gas was cooled to below 100 °C. After that, the cooling was stopped, and the vacuum was applied to 10 -2 Pa, heated to 620 ° C, and kept for 1 hour. Next, the heating was stopped, argon gas was charged, and the temperature was cooled to below 80 °C.
  • the technical solution of the present invention can not only improve the magnet Hcj, and Br and magnetic properties are reduced less, and can improve the consistency and uniformity of products in batch production.
  • Component A cesium fluoride, cerium oxide, cerium oxyfluoride powder having an average particle diameter of 1 ⁇ m.
  • Component B a rare earth-transition intermetallic compound powder having a MgCu 2 crystal structure having an average particle diameter of 5 ⁇ m, specific components and weight percentages of 22% Pr, 30% Dy, 6% Ho, 38.1% Fe, 3% Co, 0.5% Cu, 0.2% Ga, 0.1% Cr and 0.1% Mn.
  • Component C cerium nitrate hexahydrate powder having an average particle diameter of 20 ⁇ m.
  • the mixed powder composition was dispersed in pentanol at a ratio of 0.05 g/mL to form a slurry, that is, 0.05 g of the above mixed powder was dispersed per 1 mL of pentanol.
  • the N40H sintered NdFeB blank machine without aging treatment was processed into a D10 mm ⁇ 5 mm wafer, the magnetic sheet was subjected to conventional degreasing, pickled in a 5% (volume percent) concentration of nitric acid, ultrasonically washed and blown dry.
  • the treated magnetic sheet was completely immersed in the slurry in a stirred state for 60 minutes, and the impregnated magnet was placed in a stainless steel container and sealed.
  • control magnet 13 was prepared, except that the magnet was impregnated with only the slurry of the component B, and the other process steps were the same as those of the magnet of Example 13.
  • the D10 mm ⁇ 5 mm wafer magnet of Example 13 and the D10 mm * 5 mm wafer magnet of Comparative Example 13 were placed together in the same vacuum sintering furnace for heat treatment. Further, the wafer magnet of Example 13 was separately selected, and a total of 5 batches of heat treatment were performed for each batch of 2000 sheets. The heat treatment process conditions for all batches are consistent as shown below.
  • 30 sheets were each selected for measurement of magnetic properties. Batches of the examples were separately processed. 30 magnets were selected per batch for magnetic performance measurements. In addition, 30 pieces of N40H disk magnets which were not coated and heat-treated were selected for magnetic property measurement.
  • the magnetic properties of the comparative examples were different from those of the uncoated magnets and the comparative examples, and the performance consistency of the products between the different batches of the examples.
  • the average value and the extreme difference of the measured values of the magnetic properties of each batch of magnets were compared. The results are shown in Table 13-1 and Table 13-2.
  • Heat treatment process conditions The material box is placed in a vacuum sintering furnace, vacuum is applied, and the temperature is raised to 1050 ° C when the degree of vacuum reaches 10 -2 Pa or more, and the temperature is kept for 1 hour. Then the heating was stopped and the argon gas was cooled to below 100 °C. After that, the cooling was stopped, and the vacuum was applied to 10 -2 Pa, heated to 620 ° C, and kept for 1 hour. Next, the heating was stopped, argon gas was charged, and the temperature was cooled to below 80 °C.
  • the technical solution of the present invention can not only improve the Hcj of the magnet, but also reduce the Br and magnetic properties less, and can improve the consistency and uniformity of the product in batch production.

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Abstract

La présente invention concerne une composition de poudre et un procédé de préparation d'un aimant fritté de la série R-Fe-B. La composition de poudre consiste en un composant (A), un composant (B) et un composant (C). Le composant (A) est sélectionné parmi un ou plusieurs des éléments suivants : une poudre de fluorure, une poudre d'oxyde et une poudre d'oxyfluorure d'une terre rare lourde. Le composant (B) est une poudre de composé intermétallique de transition de terre rare ayant une structure cristalline MgCu2 Le composant (C) est sélectionné parmi une ou plusieurs poudres de nitrate hydraté de terre rare. Le procédé de préparation d'un aimant fritté de la série R-Fe-B selon la présente invention consiste à : revêtir l'aimant d'un liquide de conditionnement contenant la composition de poudre, ce qui a pour effet technique, au moyen d'une toute petite quantité de terres rares lourdes, le dysprosium (Dy) ou le terbium (Tb), d'améliorer sensiblement la coercivité de l'aimant avec l'idée du maintien, pour l'essentiel, de la rémanence et d'un produit d'énergie magnétique maximal de l'aimant fritté de la série R-Fe-B.
PCT/CN2014/088848 2013-10-22 2014-10-17 Composition de poudre et procédé de préparation d'un aimant fritté de la série r-fe-b Ceased WO2015058654A1 (fr)

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CN106158347B (zh) * 2016-08-31 2017-10-17 烟台正海磁性材料股份有限公司 一种制备R‑Fe‑B类烧结磁体的方法
CN109003799B (zh) * 2018-07-06 2021-02-12 杭州永磁集团振泽磁业有限公司 一种高矫顽力钕铁硼磁体的制备方法

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CN101694796A (zh) * 2005-09-21 2010-04-14 株式会社日立制作所 磁铁、磁铁用磁性材料、涂膜形成处理液及旋转机
CN102610355A (zh) * 2011-01-24 2012-07-25 北京中科三环高技术股份有限公司 一种稀土永磁体及其制备方法
CN102768898A (zh) * 2011-05-02 2012-11-07 信越化学工业株式会社 稀土永磁体及其制备方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101694796A (zh) * 2005-09-21 2010-04-14 株式会社日立制作所 磁铁、磁铁用磁性材料、涂膜形成处理液及旋转机
CN102610355A (zh) * 2011-01-24 2012-07-25 北京中科三环高技术股份有限公司 一种稀土永磁体及其制备方法
CN102768898A (zh) * 2011-05-02 2012-11-07 信越化学工业株式会社 稀土永磁体及其制备方法

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