CN111633212B - Method for processing sintered neodymium iron boron blank - Google Patents

Method for processing sintered neodymium iron boron blank Download PDF

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CN111633212B
CN111633212B CN202010594387.3A CN202010594387A CN111633212B CN 111633212 B CN111633212 B CN 111633212B CN 202010594387 A CN202010594387 A CN 202010594387A CN 111633212 B CN111633212 B CN 111633212B
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sintered
blank
heat treatment
stage heat
temperature
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CN111633212A (en
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曾祥华
李智翔
孔维峰
谢家滨
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Fujian Jinlong Rare Earth Co ltd
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Fujian Changting Jinlong Rare Earth Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
    • C21D1/773—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material under reduced pressure or vacuum
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/78—Combined heat-treatments not provided for above
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D6/00—Heat treatment of ferrous alloys
    • C21D6/007—Heat treatment of ferrous alloys containing Co
    • 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
    • C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
    • 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
    • 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
    • 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
    • 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
    • B22F3/24—After-treatment of workpieces or articles
    • B22F2003/248—Thermal after-treatment

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  • Engineering & Computer Science (AREA)
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  • Metallurgy (AREA)
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  • Crystallography & Structural Chemistry (AREA)
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  • Thermal Sciences (AREA)
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  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
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Abstract

The invention discloses a method for treating a sintered neodymium iron boron blank. The invention discloses a method for treating a sintered neodymium iron boron blank, which comprises the following steps: and carrying out three-stage heat treatment on the sintered neodymium iron boron blank, wherein the temperature of the first-stage heat treatment is 890-920 ℃, the temperature of the second-stage heat treatment is 620-670 ℃, and the temperature of the third-stage heat treatment is 450-540 ℃. The product prepared by the processing method of the invention can improve the remanence or coercive force of the product under the condition of ensuring that the squareness is unchanged or improved.

Description

Treatment method of sintered neodymium iron boron blank
Technical Field
The invention relates to a method for processing a sintered neodymium iron boron blank.
Background
The neodymium iron boron magnet is used as a third-generation rare earth permanent magnet material and has wide application in the fields of energy, transportation, machinery, medical treatment, IT, household appliances and the like. With the progress of science and technology, the performance of the neodymium iron boron functional material is continuously improved, the application of the neodymium iron boron functional material is widened, and the neodymium iron boron functional material brings wider market prospect for the neodymium iron boron industry.
The traditional neodymium iron boron permanent magnet material is generally treated by primary tempering and secondary tempering. Patent application CN108907203A discloses a heat treatment method for improving the consistency of intrinsic coercivity (Hcj) of a neodymium iron boron blank, wherein the average value of intrinsic coercivity of the prepared neodymium iron boron blank is 15.6-16.2KOe. Patent application CN103317132A discloses a novel aging process for sintered neodymium iron boron, wherein the remanence (Br) of the obtained product is 12.98-13.22KGs, and the coercive force is 13-14.2KOe. Patent application CN105489369A discloses a method for improving coercive force of neodymium iron boron magnet, the remanence of the obtained product is 12.28-13.51KGs, and the squareness (Hk/Hcj) is 0.96-0.98.
The phenomenon of high O content is easy to occur in the production process of the neodymium iron boron product, and the remanence, the coercive force or the squareness degree in the product performance is low due to the use of the conventional aging process.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects of poor magnetic properties such as residual magnetism, coercive force, squareness and the like of a product prepared by the existing preparation method of the neodymium iron boron permanent magnetic material, and provides a processing method of a sintered neodymium iron boron blank. The product prepared by the processing method of the invention can improve the remanence or coercive force of the product under the condition of ensuring that the squareness is unchanged or improved.
The invention solves the technical problems through the following technical scheme.
The invention provides a method for processing a sintered neodymium iron boron blank, which comprises the following steps: carrying out three-stage heat treatment on the sintered neodymium iron boron blank, wherein the temperature of the first-stage heat treatment is 890-920 ℃, the temperature of the second-stage heat treatment is 620-670 ℃, and the temperature of the third-stage heat treatment is 450-540 ℃.
In certain embodiments of the invention, the temperature of the first stage heat treatment may be 890 ℃ to 910 ℃, for example 900 ℃.
In certain embodiments of the present invention, the first stage heat treatment may be performed for a period of time ranging from 3 to 5 hours, such as 3 hours.
In certain embodiments of the invention, the degree of vacuum of the first stage heat treatment may be in the range of 0.1Pa to 100Pa, for example 5Pa.
In certain embodiments of the invention, the temperature of the second stage heat treatment may be 630 ℃ to 660 ℃, such as 630 ℃,640 ℃, 650 ℃ or 660 ℃, preferably 635 ℃ to 645 ℃.
In certain embodiments of the present invention, the time period for the second stage heat treatment may be 3 to 5 hours, for example 3 hours.
In certain embodiments of the present invention, the degree of vacuum of the second stage heat treatment may be in the range of 0.1Pa to 100Pa, for example 5Pa.
In certain embodiments of the invention, the temperature of the third stage heat treatment may range from 460 ℃ to 530 ℃, and may also range from 480 ℃ to 500 ℃, for example 490 ℃.
In certain embodiments of the present invention, the time period of the third stage heat treatment may be 3 to 5 hours, for example 3 hours.
In certain embodiments of the present invention, the degree of vacuum of the third stage heat treatment may be in the range of 0.1Pa to 100Pa, for example 5Pa.
In certain embodiments of the invention, the treatment protocol may be any of the following:
scheme (1):
carrying out three-stage heat treatment on the sintered neodymium iron boron blank, wherein the temperature of the first-stage heat treatment is 900 ℃, the time is 3 hours, and the vacuum degree is 5Pa; the temperature of the second-stage heat treatment is 640 ℃, the time is 3 hours, and the vacuum degree is 5Pa; the temperature of the third-stage heat treatment is 490 ℃, the time is 3h, and the vacuum degree is 5Pa;
scheme (2):
carrying out three-stage heat treatment on the sintered neodymium iron boron blank, wherein the temperature of the first-stage heat treatment is 900 ℃, the time is 3 hours, and the vacuum degree is 5Pa; the temperature of the second-stage heat treatment is 620 ℃, the time is 3 hours, and the vacuum degree is 5Pa; the temperature of the third-stage heat treatment is 490 ℃, the time is 3 hours, and the vacuum degree is 5Pa;
scheme (3):
carrying out three-stage heat treatment on the sintered neodymium iron boron blank, wherein the temperature of the first-stage heat treatment is 900 ℃, the time is 3 hours, and the vacuum degree is 5Pa; the temperature of the second-stage heat treatment is 630 ℃, the time is 3 hours, and the vacuum degree is 5Pa; the temperature of the third-stage heat treatment is 490 ℃, the time is 3 hours, and the vacuum degree is 5Pa;
scheme (4):
carrying out three-stage heat treatment on the sintered neodymium iron boron blank, wherein the temperature of the first-stage heat treatment is 900 ℃, the time is 3 hours, and the vacuum degree is 5Pa; the temperature of the second-stage heat treatment is 650 ℃, the time is 3h, and the vacuum degree is 5Pa; the temperature of the third-stage heat treatment is 490 ℃, the time is 3h, and the vacuum degree is 5Pa;
scheme (5):
carrying out three-stage heat treatment on the sintered neodymium iron boron blank, wherein the temperature of the first-stage heat treatment is 900 ℃, the time is 3 hours, and the vacuum degree is 5Pa; the temperature of the second-stage heat treatment is 660 ℃, the time is 3 hours, and the vacuum degree is 5Pa; the temperature of the third-stage heat treatment is 490 ℃, the time is 3 hours, and the vacuum degree is 5Pa;
scheme (6):
carrying out three-stage heat treatment on the sintered neodymium iron boron blank, wherein the temperature of the first-stage heat treatment is 900 ℃, the time is 3 hours, and the vacuum degree is 5Pa; the temperature of the second-stage heat treatment is 670 ℃, the time is 3 hours, and the vacuum degree is 5Pa; the temperature of the third stage heat treatment is 490 ℃, the time is 3h, and the vacuum degree is 5Pa.
In some embodiments of the present invention, the raw material formula of the sintered nd-fe-b blank comprises the following components (1) to (5) in percentage by weight:
(1) 29.00wt.% to 36.00wt.% RE; the RE is a rare earth element including LRE and HRE; the LRE comprises Nd and Pr, and the HRE comprises Dy;
(2) 0.70wt.% to 1.20wt.% of B;
(3) 0.10wt.% to 0.40wt.% Cu;
(4) 0.05wt.% to 0.40wt.% Ga;
(5) 62.00-70.00 wt.% Fe.
In certain embodiments of the present invention, in the raw material formulation of the sintered ndfeb blank, the content of the RE may be 29.00wt.% to 36.00wt.%, or may be 30.20wt.%, 30.40wt.%, 31.68wt.%, or 32.20wt.%.
In some embodiments of the present invention, in the raw material formulation of the sintered ndfeb blank, the content of Nd may be conventional in the art, and may also be 6.20wt.% to 7.50wt.%, and may also be 6.55wt.%, 7.00wt.%, 7.25wt.%, or 7.30wt.%.
In certain embodiments of the present invention, in the raw material formulation of the sintered ndfeb blank, the content of Pr may be conventional in the art, and may also be 19.40wt.% to 22.00wt.%, and may also be 19.64wt.%, 21.00wt.%, 21.75wt.%, or 21.90wt.%.
In some embodiments of the present invention, in the raw material formulation of the sintered Nd-fe-b blank, the addition form of Pr and Nd may be conventional in the art, for example, in the form of PrNd, or in the form of a mixture of Pr and Nd, or in the form of a mixture of PrNd, pr and Nd. When added as PrNd, the weight ratio of Pr to Nd is 25; the content of PrNd may be from 26wt.% to 32wt.%, or from 26wt.% to 29.5wt.%, or may be 26.19wt.%, 28wt.%, 29wt.%, or 29.2wt.%, in weight percent.
In some embodiments of the present invention, in the raw material formulation of the sintered ndfeb blank, the content of Dy may be 0.05wt.% to 7wt.%, or 0.1wt.% to 6.2wt.%, or 0.12wt.%, 0.2wt.%, 1.8wt.%, or 6.01wt.%.
In some embodiments of the present invention, in the raw material formulation of the sintered ndfeb blank, the content of B may be 0.93wt.% to 1wt.%, or may be 0.95wt.%, 0.97wt.%, or 0.98wt.%.
In some embodiments of the present invention, in the raw material formulation of the sintered ndfeb blank, the content of Cu may be 0.13wt.% to 0.23wt.%, and may also be 0.15wt.%, 0.2wt.%, or 0.21wt.%.
In some embodiments of the present invention, in the raw material formulation of the sintered ndfeb blank, the content of Ga may be 0.1wt.% to 0.3wt.%, and may also be 0.13wt.%, 0.25wt.%, 0.28wt.%, or 0.29wt.%.
In some embodiments of the present invention, in the raw material formulation of the sintered ndfeb blank, the content of Fe may be 64.00wt.% to 68.00wt.%, and may also be 64.4wt.%, 65.16wt.%, 66.54wt.%, or 67.59wt.%.
In some embodiments of the present invention, in the raw material formulation of the sintered nd-fe-b blank, the HRE may further include Tb.
In some embodiments of the present invention, when the HRE further includes Tb, the content of Tb may be conventional in the art, and may be 0.1wt.% to 1.5wt.%, and may be 0.3wt.% to 1.2wt.%, and may also be 0.4wt.% or 1wt.%, in terms of weight percentage.
In some embodiments of the present invention, in the raw material formulation of the sintered nd-fe-b blank, the HRE may further include Ho.
In certain embodiments of the present invention, when the HRE further includes Ho in the raw material formulation of the sintered ndfeb blank, the Ho content may be conventional in the art, and may be in a range from 1.5wt.% to 3.5wt.%, and may be in a range from 2.3wt.% to 2.7wt.%, and may also be in a range from 2.56wt.%.
In some embodiments of the present invention, the raw material formulation of the sintered nd-fe-b blank may further include Al.
In certain embodiments of the present invention, when the raw material formulation of the sintered ndfeb blank contains Al, the content of Al may be conventional in the art, and may be 0.2wt.% to 0.7wt.%, 0.35wt.% to 0.53wt.%, and may also be 0.39wt.% or 0.5wt.%.
In some embodiments of the present invention, the raw material formulation of the sintered nd-fe-b blank may further include Nb.
In certain embodiments of the present invention, when the raw material formulation of the sintered nd-fe-b blank contains Nb, the content of Nb may be conventional in the art, and may be 0.05wt.% to 0.25wt.%, and may be 0.15wt.% to 0.25wt.%, and may also be 0.2wt.%.
In some embodiments of the present invention, the raw material formulation of the sintered nd-fe-b blank may further include Zr.
In certain embodiments of the present invention, when the raw material formulation of the sintered ndfeb blank contains Zr, the content of Zr may be conventional in the art, and may be 0.1wt.% to 0.4wt.%, and may be 0.13wt.% to 0.29wt.%, and may also be 0.15wt.%, 0.2wt.%, or 0.25wt.%.
In some embodiments of the present invention, the raw material formulation of the sintered nd-fe-b blank may further include Ti.
In certain embodiments of the present invention, when the raw material formulation of the sintered ndfeb blank contains Ti, the content of Ti may be conventional in the art, and may be 0.05wt.% to 0.3wt.%, and may be 0.07wt.% to 0.23wt.%, and may also be 0.1wt.% or 0.19wt.%.
In some embodiments of the present invention, the raw material formulation of the sintered nd-fe-b blank may further include Co.
In certain embodiments of the present invention, when the raw material formulation of the sintered ndfeb blank contains Co, the content of Co may be conventional in the art, and may be 0.5wt.% to 2wt.%, or may be 1wt.% to 1.8wt.%, or may be 1.02wt.%, 1.15wt.%, or 1.62wt.%.
In certain embodiments of the invention, the HRE is Dy.
In certain embodiments of the invention, the HRE is Dy and Tb.
In certain embodiments of the invention, the HRE is Dy and Ho.
In certain embodiments of the invention, the HRE is Dy, tb, and Ho.
In some embodiments of the present invention, the formula of the raw materials of the sintered nd-fe-b blank may be: 26-29.5 wt.% PrNd, 0.1-0.3 wt.% Dy, 0.3-1.2 wt.% Tb, 0.93-1 wt.% B, 0.35-0.53 wt.% Al, 0.13-0.23 wt.% Cu, 0.1-0.3 wt.% Ga, 0.15-0.25 wt.% Nb, the remainder being Fe.
In some embodiments of the present invention, the formula of the sintered nd-fe-b blank may be: 26-29.5 wt.% PrNd, 0.1-0.3 wt.% Dy, 2.3-2.7 wt.% Ho, 1-1.8 wt.% Co, 0.93-1 wt.% B, 0.35-0.53 wt.% Al, 0.13-0.23 wt.% Cu, 0.1-0.3 wt.% Ga, 0.13-0.29 wt.% Zr, the remainder being Fe.
In some embodiments of the present invention, the formula of the raw materials of the sintered nd-fe-b blank may be: 26-29.5 wt.% PrNd, 1.6-2.2 wt.% Dy, 0.3-1.2 wt.% Tb, 1-1.8 wt.% Co, 0.93-1 wt.% B, 0.07-0.23 wt.% Ti, 0.13-0.23 wt.% Cu, 0.1-0.3 wt.% Ga, 0.13-0.29 wt.% Zr, the remainder being Fe.
In some embodiments of the present invention, the formula of the raw materials of the sintered nd-fe-b blank may be: 26-29.5 wt.% PrNd, 5.8-6.2 wt.% Dy, 1-1.8 wt.% Co, 0.93-1 wt.% B, 0.07-0.23 wt.% Ti, 0.35-0.53 wt.% Al, 0.13-0.23 wt.% Cu, 0.1-0.3 wt.% Ga, 0.13-0.29 wt.% Zr, the remainder being Fe.
In some embodiments of the present invention, the formula of the sintered nd-fe-b blank may be: 29.2-PrNd, 0.2-Dy, 1-Tb, 0.98-B, 0.5-Al, 0.2-Cu, 0.13-Ga, 0.2-Nb, the remainder Fe.
In some embodiments of the present invention, the formula of the raw materials of the sintered nd-fe-b blank may be: 29% PrNd, 0.12% Dy, 2.56% Ho, 1.02% Co, 0.95% B, 0.5% Al, 0.21% Cu, 0.28% Ga, 0.2% Zr, and the balance Fe.
In some embodiments of the present invention, the formula of the raw materials of the sintered nd-fe-b blank may be: 28-PrNd, 1.8-Dy, 0.4-Tb, 1.62-Co, 0.95-B, 0.1-The-Ti, 0.15-Cu, 0.29-Ga, 0.15-Zr, the remainder Fe.
In some embodiments of the present invention, the formula of the raw materials of the sintered nd-fe-b blank may be: 26.19% PrNd, 6.01% Dy, 1.15% Co, 0.97% B, 0.19% Ti, 0.39% Al, 0.2% Cu, 0.25% Ga, 0.25% Zr, the remainder Fe.
The sintered neodymium iron boron blank contains inevitable impurities, such as carbon elements.
The sintered nd-fe-b blank according to the present invention may be a sintered nd-fe-b blank conventionally understood by those skilled in the art, which may be obtained by conventional methods in the art, such as smelting, hydrogen fracturing, jet milling, orientation molding, sintering, etc.
In some embodiments of the present invention, the preparation of the sintered nd-fe-b blank may include the following steps: sequentially carrying out smelting, hydrogen breaking, jet milling, orientation forming, isostatic pressing treatment and sintering on the raw materials.
The smelting conditions and operations may be those conventional in the art. The smelting can be carried out under the vacuum condition, and the vacuum degree can be less than or equal to 30Pa. The smelting can be carried out in a protective gas atmosphere, and the protective gas can be argon. After the smelting is finished, the thickness of the obtained alloy sheet can be 0.2-0.4mm.
The hydrogen fracturing conditions and operations may be those conventional in the art.
The conditions and operation of the jet mill may be those conventional in the art. The oxygen supplementation of the jet mill may be in the range 20 to 120ppm, for example 20ppm, 40ppm, 60ppm, 80ppm, 100ppm or 120ppm, preferably 40 to 100ppm, more preferably 60 to 80ppm. After the jet milling is finished, the grain diameter of the obtained magnetic powder can be 3-5 μm and can also be 3.9-4.2 μm.
The conditions and operations for the described orientation molding may be those conventional in the art. The magnetic field strength for the orientation molding can be more than 1.4T.
The conditions and operations of the isostatic pressing process may be those conventional in the art. The isostatic pressure may be 160-200MPa, e.g. 180MPa.
The conditions and operations of the sintering may be those conventional in the art. The sintering may be vacuum sintering. The vacuum degree of the vacuum sintering can be less than 0.1Pa. The sintering temperature can be 1050-1100 ℃, such as 1075-1082 ℃. The sintering holding time can be 4-8h, such as 6h.
The invention also provides a neodymium iron boron material which is prepared by the treatment method in any scheme.
On the basis of the common knowledge in the field, the above preferred conditions can be combined randomly to obtain the preferred embodiments of the invention.
The reagents and starting materials used in the present invention are commercially available.
The positive progress effects of the invention are as follows: the product prepared by the processing method of the invention can improve the remanence or coercive force of the product under the condition of ensuring that the squareness is unchanged or improved.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the invention thereto. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.
Examples 1 to 6
(1) The method comprises the steps of carrying out traditional melting, vacuumizing, heating and baking on 29.2wt.% of PrNd (Pr 25%, nd 75%), 0.2wt.% of Dy, 1wt.% of Tb, 0.98wt.% of B, 0.5wt.% of Al, 0.2wt.% of Cu, 0.13wt.% of Ga, 0.2wt.% of Nb and the balance of Fe according to a formula, vacuumizing to be less than or equal to 30Pa, and carrying out melting, casting and cooling under the protection of argon environment to obtain a silvery white quick-setting melt-spun alloy sheet with the thickness of 0.2-0.4mm;
(2) Preparing 3.9-4.2 μm magnetic powder by hydrogen-breaking jet milling, and supplementing 20-120ppm oxygen by jet milling to make the magnet contain different oxygen contents;
(3) Pressing into green compact with a sampling forming press, wherein the oriented magnetic field intensity is more than 1.4T, and the green compact is pressed by isostatic pressing under the pressure of 180MPa;
(4) Vacuum sintering is adopted, the sintering temperature is 1075-1082 ℃, the temperature is kept for 6h, and the vacuum degree is less than 0.1Pa;
(5) Carrying out three-stage heat treatment on the sintered blank: the temperature of the first-stage heat treatment is 900 ℃, the temperature is maintained at 900 ℃ for 3h, and the vacuum degree is 5Pa; the temperature of the second-stage heat treatment is 640 ℃, the temperature is kept at 640 ℃ for 3h, and the vacuum degree is 5Pa; the temperature of the third-stage heat treatment is 490 ℃, the temperature is kept at 490 ℃ for 3h, and the vacuum degree is 5Pa. Magnetic properties the magnetic properties were measured with a NIN pulsed magnetic field magnetometer.
Example 1 Example 2 Example 3 Example 4 Example 5 Example 6
Oxygen supplement/ppm 20 40 60 80 100 120
Br/kGs 14.2 14.2 14.1 14.0 13.9 13.7
Hcj/kOe 17.3 17.8 18.2 18.1 18.1 17.5
Hk/Hcj/％ 96 98 99 99 98 97
Examples 7 to 11
(1) The method comprises the steps of carrying out traditional melting, vacuumizing, heating and baking on 29.2wt.% of PrNd (Pr 25%, nd 75%), 0.2wt.% of Dy, 1wt.% of Tb, 0.98wt.% of B, 0.5wt.% of Al, 0.2wt.% of Cu, 0.13wt.% of Ga, 0.2wt.% of Nb and the balance of Fe according to a formula, vacuumizing to be less than or equal to 30Pa, and carrying out melting, casting and cooling under the protection of argon environment to obtain a silvery white quick-setting melt-spun alloy sheet with the thickness of 0.2-0.4mm;
(2) Preparing magnetic powder with the particle size of 3.9-4.2 mu m by hydrogen-breaking jet milling, and supplementing oxygen by 60ppm by the jet milling;
(3) Pressing into green compact with a sampling forming press, wherein the oriented magnetic field intensity is more than 1.4T, and the green compact is pressed by isostatic pressing under the pressure of 180MPa;
(4) Vacuum sintering is adopted, the sintering temperature is 1075-1082 ℃, the heat preservation is carried out for 6 hours, and the vacuum degree is less than 0.1Pa;
(5) Carrying out three-stage heat treatment on the sintered blank: the temperature of the first-stage heat treatment is 900 ℃, the heat is preserved for 3 hours, and the vacuum degree is 5Pa; the temperature of the second-stage heat treatment is 620-670 ℃, the temperature is kept for 3h, and the vacuum degree is 5Pa; the temperature of the third-stage heat treatment is 490 ℃, the heat preservation is 3 hours, and the vacuum degree is 5Pa. Magnetic properties the magnetic properties were measured with a NIN pulsed magnetic field magnetometer.
Figure BDA0002556938930000101
Examples 12 to 14
(1) Adopting the following formula (Pr: nd =25 in PrNd);
(2) Preparing 3.9-4.2 μm magnetic powder by hydrogen-breaking jet mill, and supplementing oxygen by jet mill;
(3) Pressing into green compact with a sampling forming press, wherein the oriented magnetic field intensity is more than 1.4T, and the green compact is pressed by isostatic pressing under the pressure of 180MPa;
(4) Vacuum sintering is adopted, the sintering temperature is 1075-1082 ℃, the temperature is kept for 6h, and the vacuum degree is less than 0.1Pa;
(5) Carrying out three-stage heat treatment on the sintered blank: the temperature of the first-stage heat treatment is 900 ℃, the heat is preserved for 3 hours, and the vacuum degree is 5Pa; the temperature of the second-stage heat treatment is 640 ℃, the heat preservation is carried out for 3 hours, and the vacuum degree is 5Pa; the temperature of the third-stage heat treatment is 490 ℃, the heat preservation is carried out for 3 hours, and the vacuum degree is 5Pa; magnetic properties the magnetic properties were measured with a NIN pulsed magnetic field magnetometer.
Figure BDA0002556938930000102
Figure BDA0002556938930000111
Comparative example 1
(1) According to the formula, 29.2wt.% of PrNd (Pr 25%, nd 75%), 0.2wt.% of Dy, 1wt.% of Tb, 0.98wt.% of B, 0.5wt.% of Al, 0.2wt.% of Cu, 0.13wt.% of Ga, 0.2wt.% of Nb and the balance of Fe are adopted, traditional smelting, vacuumizing, heating and baking are carried out, vacuumizing is carried out until the pressure is less than or equal to 30Pa, and argon environment protection is carried out in the processes of melting, casting and cooling, so that a silvery white quick-setting melt-spun alloy sheet is obtained, wherein the thickness of the sheet is 0.2-0.4mm;
(2) Preparing 3.9-4.2 μm magnetic powder by hydrogen-breaking jet milling, and supplementing 60ppm oxygen by jet milling to make the magnet contain different oxygen contents;
(3) Pressing into green compact with a sampling forming press, wherein the oriented magnetic field intensity is more than 1.4T, and the green compact is pressed by isostatic pressing under the pressure of 180MPa;
(4) Vacuum sintering is adopted, the sintering temperature is 1075-1082 ℃, the temperature is kept for 6h, and the vacuum degree is less than 0.1Pa;
(5) And (3) carrying out secondary heat treatment on the sintered blank: the temperature of the first-stage heat treatment is 900 ℃, the heat is preserved for 3 hours, and the vacuum degree is 5Pa; the temperature of the second-stage heat treatment is 490 ℃, the heat preservation is carried out for 3 hours, and the vacuum degree is 5Pa; magnetic properties were measured with a NIN pulsed magnetic field magnetometer with a mean Br =14.2kgs, hcj =17.2koe, hk/Hcj =88.8%.

Claims (55)

1. The method for processing the sintered neodymium-iron-boron blank is characterized by comprising the following steps of: carrying out three-stage heat treatment on the sintered neodymium iron boron blank, wherein the temperature of the first-stage heat treatment is 890-920 ℃, the temperature of the second-stage heat treatment is 620-670 ℃, the temperature of the third-stage heat treatment is 480-500 ℃, and the vacuum degree of the third-stage heat treatment is 0.1-100 Pa; the time of the third-stage heat treatment is 3-5h;
the treatment method of the sintered neodymium iron boron blank further comprises the following steps: sequentially carrying out smelting, hydrogen breaking, jet milling, orientation forming, isostatic pressing and sintering on the raw materials to obtain a sintered neodymium iron boron blank;
the oxygen supplement amount of the jet mill is 40-100ppm;
the formula of the raw materials of the sintered neodymium iron boron blank comprises the following components (1) to (5) in percentage by weight:
(1) 29.00wt.% to 36.00wt.% RE; the RE is a rare earth element including LRE and HRE; the LRE comprises Nd and Pr, and the HRE comprises Dy;
(2) 0.70wt.% to 1.20wt.% of B;
(3) 0.10wt.% to 0.40wt.% Cu;
(4) 0.05wt.% to 0.40wt.% Ga;
(5) 62.00wt.% to 70.00wt.% Fe;
the content of Nd is 6.20-7.50 wt.% in percentage by weight;
the content of Pr is 19.40wt.% to 22.00wt.% in percentage by weight;
the Dy content is 0.05-1.8 wt% in percentage by weight.
2. The method for processing the sintered NdFeB blank as claimed in claim 1 wherein the temperature of the first stage heat treatment is 890-910 ℃.
3. The method for processing the sintered nd-fe-b blank according to claim 2, wherein the temperature of the first stage heat treatment is 900 ℃.
4. The processing method for sintering neodymium iron boron blank according to claim 1, characterized in that the time of the first stage heat treatment is 3-5h.
5. The processing method for sintering neodymium iron boron blank according to claim 1, characterized in that the vacuum degree of the first stage heat treatment is 0.1Pa-100Pa.
6. The method for processing sintered NdFeB blanks as recited in claim 1 in which the temperature of the second stage heat treatment is 630 ℃ -660 ℃.
7. The method for processing sintered nd-fe-b blanks as claimed in claim 6, wherein the temperature of the second stage heat treatment is 635-645 ℃.
8. The method of processing sintered neodymium iron boron blank according to claim 7, characterized in that the temperature of the second stage heat treatment is 640 ℃.
9. The method for processing sintered NdFeB blanks as recited in claim 1 in which the time of the second heat treatment is 3-5 hours.
10. The method for processing sintered NdFeB blanks as recited in claim 1, wherein the degree of vacuum of the second stage heat treatment is 0.1Pa-100Pa.
11. The method for processing sintered neodymium-iron-boron blank according to claim 1, characterized in that the temperature of the third stage heat treatment is 490 ℃.
12. The treatment method for the sintered nd-fe-b blank according to claim 2, characterized in that it is any of the following solutions:
scheme (1):
carrying out three-stage heat treatment on the sintered neodymium iron boron blank, wherein the temperature of the first-stage heat treatment is 900 ℃, the time is 3 hours, and the vacuum degree is 5Pa; the temperature of the second-stage heat treatment is 640 ℃, the time is 3 hours, and the vacuum degree is 5Pa; the temperature of the third-stage heat treatment is 490 ℃, the time is 3h, and the vacuum degree is 5Pa;
scheme (2):
carrying out three-stage heat treatment on the sintered neodymium iron boron blank, wherein the temperature of the first-stage heat treatment is 900 ℃, the time is 3 hours, and the vacuum degree is 5Pa; the temperature of the second-stage heat treatment is 620 ℃, the time is 3 hours, and the vacuum degree is 5Pa; the temperature of the third-stage heat treatment is 490 ℃, the time is 3 hours, and the vacuum degree is 5Pa;
scheme (3):
carrying out three-stage heat treatment on the sintered neodymium iron boron blank, wherein the temperature of the first-stage heat treatment is 900 ℃, the time is 3 hours, and the vacuum degree is 5Pa; the temperature of the second-stage heat treatment is 630 ℃, the time is 3h, and the vacuum degree is 5Pa; the temperature of the third-stage heat treatment is 490 ℃, the time is 3 hours, and the vacuum degree is 5Pa;
scheme (4):
carrying out three-stage heat treatment on the sintered neodymium iron boron blank, wherein the temperature of the first-stage heat treatment is 900 ℃, the time is 3 hours, and the vacuum degree is 5Pa; the temperature of the second-stage heat treatment is 650 ℃, the time is 3 hours, and the vacuum degree is 5Pa; the temperature of the third-stage heat treatment is 490 ℃, the time is 3 hours, and the vacuum degree is 5Pa;
scheme (5):
carrying out three-stage heat treatment on the sintered neodymium iron boron blank, wherein the temperature of the first-stage heat treatment is 900 ℃, the time is 3 hours, and the vacuum degree is 5Pa; the temperature of the second-stage heat treatment is 660 ℃, the time is 3 hours, and the vacuum degree is 5Pa; the temperature of the third-stage heat treatment is 490 ℃, the time is 3h, and the vacuum degree is 5Pa;
scheme (6):
carrying out three-stage heat treatment on the sintered neodymium iron boron blank, wherein the temperature of the first-stage heat treatment is 900 ℃, the time is 3 hours, and the vacuum degree is 5Pa; the temperature of the second-stage heat treatment is 670 ℃, the time is 3 hours, and the vacuum degree is 5Pa; the temperature of the third stage heat treatment is 490 ℃, the time is 3h, and the vacuum degree is 5Pa.
13. The processing method for sintering neodymium iron boron blank according to claim 1, wherein Pr and Nd are added in PrNd form, or mixture of Pr and Nd, or mixture of PrNd, pr and Nd.
14. The method for processing sintered nd-fe-B blanks as claimed in claim 1, wherein the amount of B is in the range of 0.93wt.% to 1wt.% in terms of weight percentage.
15. The processing method for the sintered neodymium-iron-boron blank as claimed in claim 1, wherein the content of Cu is 0.13wt.% to 0.23wt.% in terms of weight percentage.
16. The processing method for the sintered neodymium-iron-boron blank according to claim 1, wherein the content of Ga is 0.1wt.% to 0.3wt.% in percentage by weight.
17. The method for processing sintered neodymium-iron-boron blank according to claim 1, wherein the content of Fe is 64.00wt.% to 68.00wt.% in terms of weight percentage.
18. The processing method for sintering neodymium iron boron blank according to claim 1, wherein the HRE further comprises Tb.
19. The method of processing sintered neodymium-iron-boron blank as claimed in claim 1, wherein the HRE further comprises Ho.
20. The processing method of the sintered nd-fe-b blank according to claim 1, wherein the raw material formulation of the sintered nd-fe-b blank further comprises Al.
21. The processing method of sintered nd-fe-b blank according to claim 1, wherein the raw material formulation of sintered nd-fe-b blank further comprises Nb.
22. The processing method of the sintered nd-fe-b blank according to claim 1, wherein the raw material formulation of the sintered nd-fe-b blank further comprises Zr.
23. The processing method of the sintered nd-fe-b blank as claimed in claim 1, wherein the raw material formulation of the sintered nd-fe-b blank further comprises Ti.
24. The processing method of the sintered nd-fe-b blank as claimed in claim 1, wherein the raw material formulation of the sintered nd-fe-b blank further comprises Co.
25. The processing method for sintering neodymium iron boron blank according to claim 13, wherein when Pr and Nd are added in the form of PrNd, the weight ratio of Pr to Nd is 25.
26. The processing method of sintered Nd-fe-b blank according to claim 13, wherein when Pr and Nd are added as PrNd, the PrNd content is 26-32 wt.% in weight percentage.
27. The method of processing a sintered neodymium-iron-boron blank according to claim 26, characterized in that, when Pr and Nd are added in the form of PrNd, the content of PrNd is 26wt.% to 29.5wt.% in terms of weight percentage.
28. The processing method for sintering neodymium iron boron blank according to claim 18, wherein when the HRE further comprises Tb, the content of Tb is 0.1wt.% to 1.5wt.% in terms of weight percentage.
29. The processing method of sintered nd-fe-b blank as claimed in claim 28 wherein when the HRE further includes Tb, the Tb content is 0.3wt.% to 1.2wt.% in weight percent.
30. The processing method of sintered nd-fe-b blank as claimed in claim 19 wherein when the HRE further includes Ho, the Ho is present in an amount of 1.5wt.% to 3.5wt.% in weight percent.
31. The method of processing sintered neodymium-iron-boron blank according to claim 30, wherein when the HRE further includes Ho, the Ho is present in an amount of 2.3wt.% to 2.7wt.% in terms of weight percent.
32. The method of claim 20, wherein when the sintered nd-fe-b blank comprises Al, the Al content is 0.2wt.% to 0.7wt.% in terms of weight percentage.
33. The processing method of the sintered nd-fe-b blank according to claim 32, wherein when the raw material formulation of the sintered nd-fe-b blank contains Al, the content of Al is 0.35wt.% to 0.53wt.% in terms of weight percentage.
34. The processing method of sintered nd-fe-b blank according to claim 21, wherein when the raw material formulation of sintered nd-fe-b blank contains Nb, the content of Nb is 0.05wt.% to 0.25wt.% in terms of weight percentage.
35. The processing method of sintered nd-fe-b blank according to claim 34, wherein when the raw material formulation of sintered nd-fe-b blank contains Nb, the content of Nb is 0.15wt.% to 0.25wt.%.
36. The processing method of the sintered nd-fe-b blank according to claim 22, wherein when the raw material formulation of the sintered nd-fe-b blank contains Zr, the content of Zr is 0.1wt.% to 0.4 wt.%.
37. The method of processing the sintered nd-fe-b blank of claim 36, wherein when the raw material formulation of the sintered nd-fe-b blank includes Zr, the Zr content is 0.13wt.% to 0.29wt.%.
38. The method of claim 23, wherein when the raw material formulation of the sintered nd-fe-b blank includes Ti, the Ti content is 0.05wt.% to 0.3wt.% in terms of weight percentage.
39. The processing method of the sintered nd-fe-b blank as claimed in claim 38 wherein when the raw material formulation of the sintered nd-fe-b blank includes Ti, the Ti content is 0.07wt.% to 0.23 wt.%.
40. The processing method of the sintered nd-fe-b blank according to claim 24, wherein when the raw material formulation of the sintered nd-fe-b blank contains Co, the Co content is 0.5wt.% to 2wt.% in terms of weight percentage.
41. The processing method of the sintered nd-fe-b blank as claimed in claim 40 wherein when the raw material formulation of the sintered nd-fe-b blank contains Co, the content of Co is 1wt.% to 1.8 wt.%.
42. The method of processing sintered neodymium iron boron blank as claimed in claim 25, wherein the HRE is any one of the following conditions:
（1）Dy；
(2) Dy and Tb;
(3) Dy and Ho;
(4) Dy, tb and Ho.
43. The processing method of the sintered nd-fe-b blank according to claim 25, wherein the formula of the raw materials of the sintered nd-fe-b blank is any one of the following schemes:
scheme 1:
26 -29.5wt.% PrNd, 0.1wt.% to 0.3wt.% Dy, 0.3wt.% to 1.2wt.% Tb, 0.93wt.% to 1wt.% B, 0.35wt.% to 0.53wt.% Al, 0.13wt.% to 0.23wt.% Cu, 0.1wt.% to 0.3wt.% Ga, 0.15wt.% to 0.25wt.% Nb, the remainder being Fe;
scheme 2:
26wt. -29.5wt.% PrNd, 0.1wt. -0.3wt.% Dy, 2.3wt.% Ho, 1wt. -1.8wt.% Co, 0.93wt. -1wt.% B, 0.35wt.% to 0.53wt.% Al, 0.13wt.% to 0.23wt.% Cu, 0.1wt.% to 0.3wt.% Ga, 0.13wt.% to 0.29wt.% Zr, the remainder being Fe;
scheme 5:
29.2% PrNd, 0.2% Dy, 1% Tb, 0.98% B, 0.5% Al, 0.2% Cu, 0.13% Ga, 0.2% Nb, the remainder Fe;
scheme 6:
29% PrNd, 0.12% Dy, 2.56% Ho, 1.02% Co, 0.95% B, 0.5% Al, 0.21% Cu, 0.28% Ga, 0.2% Zr, the remainder Fe;
scheme 7:
28-PrNd, 1.8-Dy, 0.4-Tb, 1.62-Co, 0.95-B, 0.1-The-Ti, 0.15-Cu, 0.29-Ga, 0.15-Zr, the remainder Fe.
44. The processing method of the sintered nd-fe-b blank according to claim 1, characterized in that the smelting is carried out under vacuum condition with vacuum degree less than or equal to 30Pa.
45. The processing method for sintering neodymium iron boron blank according to claim 1, characterized in that the smelting is carried out in protective gas atmosphere.
46. The processing method of the sintered nd-fe-b blank according to claim 1, wherein after the smelting is finished, the thickness of the obtained alloy sheet is 0.2-0.4mm.
47. The method for treating sintered NdFeB blanks as recited in claim 1, wherein the jet mill has oxygen supplement amount of 60-80ppm.
48. The method for processing the sintered NdFeB blank as claimed in claim 1, wherein the particle size of the obtained magnetic powder is 3-5 μm after the jet milling is finished.
49. The processing method of sintered nd-fe-b blank according to claim 48, wherein after the air-jet milling is finished, the grain size of the obtained magnetic powder is 3.9-4.2 μm.
50. The method for processing sintered NdFeB blanks as recited in claim 1 wherein the magnetic field strength for said orienting is > 1.4T.
51. The method of processing sintered neodymium iron boron blank according to claim 1, characterized in that the isostatic pressure is 160-200Mpa.
52. The processing method for sintering neodymium iron boron blank according to claim 1, characterized in that the sintering is vacuum sintering, and the vacuum degree of the vacuum sintering is less than 0.1Pa.
53. The processing method for sintering neodymium iron boron blank according to claim 1, wherein the sintering temperature is 1050 ℃ -1100 ℃.
54. The processing method for the sintered NdFeB blank as claimed in claim 1, wherein the heat preservation time for sintering is 4-8h.
55. A neodymium iron boron material prepared by the treatment method of any one of claims 1-54.
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Address after: 366300 new industrial zone, Changting Economic Development Zone, Longyan City, Fujian Province

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