CN105513736A - Sintered neodymium-iron-boron magnet - Google Patents

Sintered neodymium-iron-boron magnet Download PDF

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Publication number
CN105513736A
CN105513736A CN201610011160.5A CN201610011160A CN105513736A CN 105513736 A CN105513736 A CN 105513736A CN 201610011160 A CN201610011160 A CN 201610011160A CN 105513736 A CN105513736 A CN 105513736A
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sintered ndfeb
magnet
ndfeb magnet
incubated
mean size
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张宏芳
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NINGBO HONGLEI MAGNETIC INDUSTRY Co Ltd
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NINGBO HONGLEI MAGNETIC INDUSTRY Co Ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets 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
    • H01F1/04Magnets 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
    • H01F1/047Alloys characterised by their composition
    • H01F1/053Alloys characterised by their composition containing rare earth metals
    • H01F1/055Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571Alloys 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02Compacting only
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/1017Multiple heating or additional steps
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets 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
    • H01F1/04Magnets 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
    • H01F1/047Alloys characterised by their composition
    • H01F1/053Alloys characterised by their composition containing rare earth metals
    • H01F1/055Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571Alloys 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
    • H01F1/0575Alloys 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

Abstract

The invention discloses a sintered neodymium-iron-boron magnet. The magnet is prepared from the balance of RxMyBzFe, wherein R is one or more out of La, Ce, Pr, Nd, Gd, Ho and Dy, a total mass fraction of R is x, M is one or more out of Co, Al, Cu, Nb, Zr and Ga, a total mass fraction of M is y, x is equal to 29 to 33 percent by weight, y is equal to 0 to 2 percent by weight, and z is equal to 0.9 to 1.1 percent by weight. By adopting the technical scheme, not only can the coercive force of the magnet be increased, but also the brittleness of the magnet is improved. As an adding element, the crystal boundary of the titanium element is added, so that the titanium element is mainly distributed at the crystal boundary, the structure of the crystal boundary is improved, crystalline grains are refined, and the coercive force is increased; and meanwhile, the titanium element improves the mechanical performance of the crystal boundary neodymium-rich phase, the occurrence and extension of cracks are inhibited, and the brittleness of the magnet is improved.

Description

A kind of Sintered NdFeB magnet
Technical field
The present invention relates to a kind of permanent magnet, particularly a kind of Sintered NdFeB magnet.
Background technology
Neodymium iron boron magnetic body, primarily of the intermetallic compound that rare-earth element R and iron, boron form.The combination of R mainly neodymium or neodymium and other rare earth elements, also replaces part iron with elements such as cobalt, aluminium, vanadium sometimes.Mainly be divided into sintered NdFeB and Agglutinate neodymium-iron-boron two kinds, Agglutinate neodymium-iron-boron all directions are all magnetic, corrosion-resistant; And sintered NdFeB is because of perishable, surface needs coating, generally has zinc-plated, nickel, zinc electroplating bath, environmental protection nickel, ambrose alloy nickel, environmental protection ambrose alloy nickel etc.And sintered NdFeB generally divides axial charging and radial magnetizing, determine according to required working face.
Nd-Fe-Bo permanent magnet material is the permanent magnetic material based on intermetallic compound RE2FE14B.Main component is rare earth (RE), iron (Fe), boron (B).Its middle rare earth ND substitutes to obtain other rare earth metals such as different performance applicable part dysprosium (Dy), praseodymium (Pr), iron also can be substituted by other metallic member such as cobalt (Co), aluminium (Al), the content of boron is less, but formation tetragonal structure intermetallic compound is played an important role, the compound made has high saturation and magnetic intensity, high uniaxial anisotropy and high Curie temperature.
Neodymium iron boron magnetic body is a kind of new permanent-magnet invented by Contemporary Japanese scientist Zuo Chuan true man, and in 29 metal academic discussions in November nineteen eighty-three, is proposed the manufacture of neodymium, iron, boron permanent magnet material by SUMITOMO CHEMICAL particulate metal company at first.It is the alloy magnet primarily of neodymium, iron, boron three kinds of elements composition, is the permanent magnet that present magnetic is the strongest, because neodymium atom is flat, electron cloud limited, makes iron atom offset, thus form constant magnetic force.
Neodymium iron boron magnetic body has very strong magnetocrystalline anisotropy and very high saturation magnetization.In permanent magnetic material; sintered nd-fe-b magnet performance is the highest; maximum magnetic energy product (BH) max=360kJ/m3 of commercial product; but the Curie temperature of this magnet lower (314 DEG C); temperature stability and corrosion resistance poor; limit and use at relatively high temperatures, and need as a rule to adopt protective finish.The manufacturing process of neodymium iron boron magnetic body has powder metallurgic method and melt-quenching method.Because magnetic property is excellent, Nd-Fe-B type magnet obtains a wide range of applications, and is mainly used in motor, generator, acoustic wave transducer, various transducer, medicine equipment and magnetic machinery etc.
In order to improve the coercive force of sintered NdFeB, it is more common methods that crystal boundary adds some trace elements, but these elements are the oxide of rare earth or pure rare earth micro mist mostly, by adding these elements, the rich neodymium phase or the magnetic hardening crystal boundary that add crystal boundary reach the coercitive object of raising, and cost is higher simultaneously.Sintered NdFeB belongs to a kind of fragile material simultaneously, and people more and more pay close attention to the machinability of sintered NdFeB, and the sintered NdFeB adopting current technique to prepare is general more crisp, and machinability is poor.
Summary of the invention
For solving the problem, the invention discloses a kind of Sintered NdFeB magnet, in the micro mist of sintered NdFeB, being added the method for titanium valve by crystal boundary, both can improve the coercive force of magnet, also improve the fragility of magnet simultaneously.As a kind of Addition ofelements, the crystal boundary of titanium elements adds, titanium elements is made mainly to be distributed in crystal boundary, improve the structure of crystal boundary, refinement crystal grain, makes coercive force to be improved, and titanium elements also improves the mechanical property of the rich neodymium phase of crystal boundary simultaneously, inhibit generation and the expansion of crackle, so the fragility of magnet is improved.
Sintered NdFeB magnet disclosed by the invention, magnet consist of R xm yb zfe surplus, wherein, R comprises one or more in La, Ce, Pr, Nd, Gd, Ho, Dy, R gross mass mark to be x, M be in Co, Al, Cu, Nb, Zr, Ga one or more, M gross mass mark is y, x=29 ~ 33wt%, y=0 ~ 2wt%, z=0.9 ~ 1.1wt%.
The one of Sintered NdFeB magnet disclosed by the invention is improved, magnet is that raw material obtains through smelting slab, powder process, powder mold pressing base, sinter molding, wherein powder process is after meal slab first being made particle mean size 50-2000 μm, then makes the micro mist of particle mean size 2-4 μm further.
The one of Sintered NdFeB magnet disclosed by the invention is improved, being prepared as of micro mist is pulverized or fine Comminuting Micawith High Pressure Water Jet (fine Comminuting Micawith High Pressure Water Jet technology with airflow milling, capacity usage ratio can be improved, avoid occurring airborne dust, reduce equipment requirement, the feature of environmental protection is better, reduces material loss) obtained.
The one of Sintered NdFeB magnet disclosed by the invention is improved, and also comprises the titanium elements accounting for gross mass 0.1 ~ 0.5wt% in magnet composition.
The one of Sintered NdFeB magnet disclosed by the invention is improved, and titanium elements is row powder mold pressing base again after add mixing with titanium valve form after slab powder process, and wherein the particle mean size of titanium valve is 2-50 μm.The mode of adding in micro mist obtained by slab is mixed by adopting with titanium valve in this programme, the crystal boundary realizing the titanium elements of titanium elements in magnet adds, titanium elements is made mainly to be distributed in crystal boundary, improve the structure of crystal boundary, refinement crystal grain, makes coercive force to be improved, and titanium elements also improves the mechanical property of the rich neodymium phase of crystal boundary simultaneously, inhibit generation and the expansion of crackle, so the fragility of magnet is improved.
The one of Sintered NdFeB magnet disclosed by the invention is improved, and before powder mold pressing base, the screening of 100-300 mesh sieve all crossed by alloy powder.
The one of Sintered NdFeB magnet disclosed by the invention is improved, sinter molding comprises sintering circuit and aging sequence, described sintering circuit for be incubated 3-6 hour at 1000-1080 DEG C, described aging sequence at least comprises first order timeliness, and described first order timeliness for be incubated 1-4 hour at 800-950 DEG C.
The one of Sintered NdFeB magnet disclosed by the invention is improved, and the second level timeliness that aging sequence performs after being also included in first order timeliness, described second level timeliness for be incubated 3-6 hour at 450-550 DEG C.
The one of Sintered NdFeB magnet disclosed by the invention is improved, and during powder mold pressing base, in environment, oxygen content is less than 1000ppm.
Sintered NdFeB magnet disclosed by the invention, its preparation is simple, and stable performance, by crystal boundary Doped with Titanium element, both can improve the coercive force of magnet, can improve again the fragility of magnet, drastically increase the processing characteristics of magnet.
Embodiment
Below in conjunction with embodiment, illustrate the present invention further, following embodiment should be understood and be only not used in for illustration of the present invention and limit the scope of the invention.
Embodiment 1
In the present embodiment, alloy composition is that (content is weight percentage (PrNd) 27.2Gd4.0Al0.8Cu0.2Co1.0B0.98Febal, wt%), through the melting of vacuum induction slab stove, be prepared into the alloy casting piece of this composition, then through hydrogen break by pure for alloy casting piece meal for particle mean size be the meal of 50 μm, then adopt airflow milling to shatter, meal ground to form the micro mist that particle mean size is 3.3 μm.Micro mist being divided into two groups: first group is the micro mist not adding titanium valve, carries out batch mixing by three-dimensional material mixer, and mixing time is 6 hours, then with order number be 200 object sieving machines sieve powder; The second is add the micro mist of titanium valve, and in micro mist, add the titanium valve that percentage by weight is 0.2wt%, the particle mean size of titanium valve is 15 μm, carries out batch mixing by three-dimensional material mixer, and mixing time is 6 hours, is then 200 object sieving machines sieve powder with order number.Be pressed in two groups of micro mists respectively closed press under nitrogen protection, the specification of pressed compact is the square of 57.5 × 30 × 48, and the oxygen content closed in press requires lower than 1000ppm.Suppress two groups of samples are put into same sintering furnace under nitrogen protection carry out sintering and timeliness, sintering temperature is 1060 DEG C, and be incubated 4.5 hours, first order aging temp is 900 DEG C, and be incubated 2 hours, second level aging temp is 500 DEG C, is incubated 4.5 hours.The magnet prepared is contrasted as follows:
1), by magnet be processed into the sample post of D10 × 10, adopt ATM-4 magnetic measurement instrument to test, contrast magnetic property;
2), by magnet be processed into the sample of 30 × 17.25 × 3,50 respectively, carry out fall-down test, from the height of 1.5 meters, free-electron model is to ground, and the ratio of statistics embrittlement, compares the fragility of magnet with this.
Table 1 does not add titanium valve and adds the sintered NdFeB magnetic property of 0.2wt% titanium valve
Br(KGs) Hcj(KOe) (BH)max(MGO) Hk/Hcj
Do not add titanium valve 12.56 15.51 38.53 96.5%
Add 0.2wt% titanium valve 12.45 16.26 38.12 96.8%
As can be seen from result above, add the titanium valve of 0.2wt%, coercive force improves 0.75kOe, and remanent magnetism merely reduces 0.11kGs.Titanium valve is more significant for the coercitive raising of magnet.
Table 2 does not add titanium valve and adds the Sintered NdFeB magnet fall-down test of 0.2wt% titanium valve
Sample number (pcs) Embrittlement sample number (pcs) Embrittlement percentage
Do not add titanium valve 50 11 22%
Add 0.2wt% titanium valve 50 4 8%
As can be seen from test data above, the magnet adding 0.2wt% titanium valve reduces 14% from the embrittlement percentage of 1.5 meters of height free-electron model than the magnet for adding titanium valve, the interpolation of titanium valve can improve the fragility of magnet.
Embodiment 2
In the present embodiment, alloy composition is that (content is weight percentage (PrNd) 27.2Gd4.0Al0.8Cu0.2Co1.0B0.98Febal, wt%), through the melting of vacuum induction slab stove, be prepared into the alloy casting piece of this composition, then through hydrogen break by pure for alloy casting piece meal for particle mean size be the meal of 100 μm, then adopt airflow milling to shatter, meal ground to form the micro mist that particle mean size is 2.7 μm.In micro mist, add the titanium valve that percentage by weight is 0.2wt%, the particle mean size of titanium valve is 8 μm, carries out batch mixing by three-dimensional material mixer, and mixing time is 6 hours, then with order number be 200 object sieving machines sieve powder.Be pressed in micro mist respectively closed press under nitrogen protection, the specification of pressed compact is the square of 57.5 × 30 × 48, and the oxygen content closed in press requires lower than 930ppm.The sample suppressed is put into same sintering furnace under nitrogen protection carry out sintering and timeliness, sintering temperature is 1060 DEG C, and be incubated 4.5 hours, first order aging temp is 860 DEG C, and be incubated 1.5 hours, second level aging temp is 550 DEG C, is incubated 4.5 hours.
Embodiment 3
In the present embodiment, alloy composition is that (content is weight percentage (PrNd) 27.2Gd4.0Al0.8Cu0.2Co1.0B0.98Febal, wt%), through the melting of vacuum induction slab stove, be prepared into the alloy casting piece of this composition, then through hydrogen break by pure for alloy casting piece meal for particle mean size be the meal of 200 μm, then adopt airflow milling to shatter, meal ground to form the micro mist that particle mean size is 3.8 μm.In micro mist, add the titanium valve that percentage by weight is 0.2wt%, the particle mean size of titanium valve is 47 μm, carries out batch mixing by three-dimensional material mixer, and mixing time is 6 hours, then with order number be 200 object sieving machines sieve powder.Be pressed in micro mist respectively closed press under nitrogen protection, the specification of pressed compact is the square of 57.5 × 30 × 48, and the oxygen content closed in press requires lower than 970ppm.The sample suppressed is put into same sintering furnace under nitrogen protection carry out sintering and timeliness, sintering temperature is 1035 DEG C, and be incubated 4.6 hours, first order aging temp is 850 DEG C, and be incubated 1.7 hours, second level aging temp is 540 DEG C, is incubated 6 hours.
Embodiment 4
In the present embodiment, alloy composition is that (content is weight percentage (PrNd) 27.2Gd4.0Al0.8Cu0.2Co1.0B0.98Febal, wt%), through the melting of vacuum induction slab stove, be prepared into the alloy casting piece of this composition, then through hydrogen break by pure for alloy casting piece meal for particle mean size be the meal of 400 μm, then adopt airflow milling to shatter, meal ground to form the micro mist that particle mean size is 2.7 μm.In micro mist, add the titanium valve that percentage by weight is 0.2wt%, the particle mean size of titanium valve is 34 μm, carries out batch mixing by three-dimensional material mixer, and mixing time is 6 hours, then with order number be 300 object sieving machines sieve powder.Be pressed in micro mist respectively closed press under nitrogen protection, the specification of pressed compact is the square of 57.5 × 30 × 48, and the oxygen content closed in press requires lower than 850ppm.The sample suppressed is put into same sintering furnace under nitrogen protection carry out sintering and timeliness, sintering temperature is 1030 DEG C, and be incubated 5.2 hours, first order aging temp is 820 DEG C, and be incubated 2.6 hours, second level aging temp is 450 DEG C, is incubated 6 hours.
Embodiment 5
In the present embodiment, alloy composition is that (content is weight percentage (PrNd) 27.2Gd4.0Al0.8Cu0.2Co1.0B0.98Febal, wt%), through the melting of vacuum induction slab stove, be prepared into the alloy casting piece of this composition, then through hydrogen break by pure for alloy casting piece meal for particle mean size be the meal of 600 μm, then adopt airflow milling to shatter, meal ground to form the micro mist that particle mean size is 3.2 μm.In micro mist, add the titanium valve that percentage by weight is 0.1wt%, the particle mean size of titanium valve is 26 μm, carries out batch mixing by three-dimensional material mixer, and mixing time is 6 hours, then with order number be 100 object sieving machines sieve powder.Be pressed in micro mist respectively closed press under nitrogen protection, the specification of pressed compact is the square of 57.5 × 30 × 48, and the oxygen content closed in press requires lower than 950ppm.The sample suppressed is put into same sintering furnace under nitrogen protection carry out sintering and timeliness, sintering temperature is 1010 DEG C, and be incubated 3.6 hours, first order aging temp is 880 DEG C, and be incubated 2.7 hours, second level aging temp is 530 DEG C, is incubated 3 hours.
Embodiment 6
In the present embodiment, alloy composition is that (content is weight percentage (PrNd) 27.2Gd4.0Al0.8Cu0.2Co1.0B0.98Febal, wt%), through the melting of vacuum induction slab stove, be prepared into the alloy casting piece of this composition, then through hydrogen break by pure for alloy casting piece meal for particle mean size be the meal of 800 μm, then adopt airflow milling to shatter, meal ground to form the micro mist that particle mean size is 2.3 μm.In micro mist, add the titanium valve that percentage by weight is 0.5wt%, the particle mean size of titanium valve is 50 μm, carries out batch mixing by three-dimensional material mixer, and mixing time is 6 hours, then with order number be 150 object sieving machines sieve powder.Be pressed in micro mist respectively closed press under nitrogen protection, the specification of pressed compact is the square of 57.5 × 30 × 48, and the oxygen content closed in press requires lower than 500ppm.The sample suppressed is put into same sintering furnace under nitrogen protection carry out sintering and timeliness, sintering temperature is 1045 DEG C, and be incubated 5.5 hours, first order aging temp is 870 DEG C, and be incubated 3 hours, second level aging temp is 450 DEG C, is incubated 3 hours.
Embodiment 7
In the present embodiment, alloy composition is that (content is weight percentage (PrNd) 27.2Gd4.0Al0.8Cu0.2Co1.0B0.98Febal, wt%), through the melting of vacuum induction slab stove, be prepared into the alloy casting piece of this composition, then through hydrogen break by pure for alloy casting piece meal for particle mean size be the meal of 2000 μm, then adopt airflow milling to shatter, meal ground to form the micro mist that particle mean size is 4 μm.In micro mist, add the titanium valve that percentage by weight is 0.4wt%, the particle mean size of titanium valve is 40 μm, carries out batch mixing by three-dimensional material mixer, and mixing time is 6 hours, then with order number be 250 object sieving machines sieve powder.Be pressed in micro mist respectively closed press under nitrogen protection, the specification of pressed compact is the square of 57.5 × 30 × 48, and the oxygen content closed in press requires lower than 600ppm.Put into same sintering furnace under nitrogen protection by suppress two groups to carry out sintering and timeliness, sintering temperature is 1050 DEG C, and be incubated 5 hours, first order aging temp is 830 DEG C, and be incubated 3.5 hours, second level aging temp is 480 DEG C, is incubated 3.7 hours.
Embodiment 8
In the present embodiment, alloy composition is that (content is weight percentage (PrNd) 27.2Gd4.0Al0.8Cu0.2Co1.0B0.98Febal, wt%), through the melting of vacuum induction slab stove, be prepared into the alloy casting piece of this composition, then through hydrogen break by pure for alloy casting piece meal for particle mean size be the meal of 1800 μm, then adopt airflow milling to shatter, meal ground to form the micro mist that particle mean size is 2 μm.In micro mist, add the titanium valve that percentage by weight is 0.25wt%, the particle mean size of titanium valve is 30 μm, carries out batch mixing by three-dimensional material mixer, and mixing time is 6 hours, then with order number be 220 object sieving machines sieve powder.Be pressed in micro mist respectively closed press under nitrogen protection, the specification of pressed compact is the square of 57.5 × 30 × 48, and the oxygen content closed in press requires lower than 700ppm.Put into same sintering furnace under nitrogen protection by suppress two groups to carry out sintering and timeliness, sintering temperature is 1040 DEG C, and be incubated 6 hours, first order aging temp is 800 DEG C, and be incubated 4 hours, second level aging temp is 530 DEG C, is incubated 5.6 hours.
Embodiment 9
In the present embodiment, alloy composition is that (content is weight percentage (PrNd) 27.2Gd4.0Al0.8Cu0.2Co1.0B0.98Febal, wt%), through the melting of vacuum induction slab stove, be prepared into the alloy casting piece of this composition, then through hydrogen break by pure for alloy casting piece meal for particle mean size be the meal of 1500 μm, then adopt airflow milling to shatter, meal ground to form the micro mist that particle mean size is 2.5 μm.In micro mist, add the titanium valve that percentage by weight is 0.32wt%, the particle mean size of titanium valve is 10 μm, carries out batch mixing by three-dimensional material mixer, and mixing time is 6 hours, then with order number be 280 object sieving machines sieve powder.Be pressed in micro mist respectively closed press under nitrogen protection, the specification of pressed compact is the square of 57.5 × 30 × 48, and the oxygen content closed in press requires lower than 800ppm.The sample suppressed is put into same sintering furnace under nitrogen protection carry out sintering and timeliness, sintering temperature is 1080 DEG C, and be incubated 3.5 hours, first order aging temp is 930 DEG C, and be incubated 1.5 hours, second level aging temp is 480 DEG C, is incubated 3.6 hours.
Embodiment 10
In the present embodiment, alloy composition is that (content is weight percentage (PrNd) 27.2Gd4.0Al0.8Cu0.2Co1.0B0.98Febal, wt%), through the melting of vacuum induction slab stove, be prepared into the alloy casting piece of this composition, then through hydrogen break by pure for alloy casting piece meal for particle mean size be the meal of 1300 μm, then adopt airflow milling to shatter, meal ground to form the micro mist that particle mean size is 3 μm.In micro mist, add the titanium valve that percentage by weight is 0.14wt%, the particle mean size of titanium valve is 20 μm, carries out batch mixing by three-dimensional material mixer, and mixing time is 6 hours, then with order number be 160 object sieving machines sieve powder.Be pressed in micro mist respectively closed press under nitrogen protection, the specification of pressed compact is the square of 57.5 × 30 × 48, and the oxygen content closed in press requires lower than 900ppm.The sample suppressed is put into same sintering furnace under nitrogen protection carry out sintering and timeliness, sintering temperature is 1000 DEG C, and be incubated 6 hours, first order aging temp is 950 DEG C, and be incubated 1 hour, second level aging temp is 540 DEG C, is incubated 4.5 hours.
Embodiment 11
In the present embodiment, alloy composition is that (content is weight percentage (PrNd) 27.2Gd4.0Al0.8Cu0.2Co1.0B0.98Febal, wt%), through the melting of vacuum induction slab stove, be prepared into the alloy casting piece of this composition, then through hydrogen break by pure for alloy casting piece meal for particle mean size be the meal of 1100 μm, then adopt airflow milling to shatter, meal ground to form the micro mist of particle mean size 3.5 μm.In micro mist, add the titanium valve that percentage by weight is 0.46wt%, the particle mean size of titanium valve is 2 μm, carries out batch mixing by three-dimensional material mixer, and mixing time is 6 hours, then with order number be 140 object sieving machines sieve powder.Be pressed in micro mist respectively closed press under nitrogen protection, the specification of pressed compact is the square of 57.5 × 30 × 48, and the oxygen content closed in press requires lower than 1000ppm.The sample suppressed is put into same sintering furnace under nitrogen protection carry out sintering and timeliness, sintering temperature is 1080 DEG C, and be incubated 3 hours, first order aging temp is 900 DEG C, is incubated 2 hours.
In above embodiment, the composition of alloy can also for including, without being limited to situation arbitrary (surplus is Fe, no longer indicates in following table) as in the table below:
The technical scope midrange non-limit part that this place embodiment is protected application claims and in embodiment technical scheme to the new technical scheme that the equal replacement of single or multiple technical characteristic is formed, equally all in the scope of protection of present invention; Simultaneously in all embodiments enumerated or do not enumerate of the present invention program, parameters in the same embodiment only represents an example (i.e. a kind of feasible scheme) of its technical scheme, and between parameters, there is not strict cooperation and qualified relation, wherein each parameter can be replaced, except special declaration mutually when stating ask without prejudice to axiom and the present invention.
Include, without being limited to above-mentioned cited embodiment scheme, technical solution of the present invention implements the magnet obtained, and magnetic coercive force and magnet fragility are all significantly improved, and the titanium elements of crystal boundary interpolation in addition, has all had significant raising to the magnetic property of magnet.
Technological means disclosed in the present invention program is not limited only to the technological means disclosed in above-mentioned technological means, also comprises the technical scheme be made up of above technical characteristic combination in any.The above is the specific embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.

Claims (9)

1. a Sintered NdFeB magnet, is characterized in that: described magnet consist of R xm yb zfe surplus, wherein, R comprises one or more in La, Ce, Pr, Nd, Gd, Ho, Dy, R gross mass mark to be x, M be in Co, Al, Cu, Nb, Zr, Ga one or more, M gross mass mark is y, x=29 ~ 33wt%, y=0 ~ 2wt%, z=0.9 ~ 1.1wt%.
2. Sintered NdFeB magnet according to claim 1, it is characterized in that: described magnet is that raw material obtains through smelting slab, powder process, powder mold pressing base, sinter molding, wherein powder process is after meal slab first being made particle mean size 50-2000 μm, then makes the micro mist of particle mean size 2-4 μm further.
3. Sintered NdFeB magnet according to claim 1, is characterized in that: being prepared as with airflow milling pulverizing of described micro mist is obtained.
4. Sintered NdFeB magnet according to claim 1, is characterized in that: also comprise the titanium elements accounting for gross mass 0.1 ~ 0.5wt% in described magnet composition.
5. Sintered NdFeB magnet according to claim 4, is characterized in that: described titanium elements is row powder mold pressing base again after add mixing with titanium valve form after slab powder process, and wherein the particle mean size of titanium valve is 2-50 μm.
6. the Sintered NdFeB magnet according to claim 2 or 5, is characterized in that: before described powder mold pressing base, the screening of 100-300 mesh sieve all crossed by alloy powder.
7. Sintered NdFeB magnet according to claim 2, it is characterized in that: described sinter molding comprises sintering circuit and aging sequence, described sintering circuit for be incubated 3-6 hour at 1000-1080 DEG C, described aging sequence at least comprises first order timeliness, and described first order timeliness for be incubated 1-4 hour at 800-950 DEG C.
8. Sintered NdFeB magnet according to claim 7, is characterized in that: the second level timeliness that described aging sequence performs after being also included in first order timeliness, and described second level timeliness for be incubated 3-6 hour at 450-550 DEG C.
9. the Sintered NdFeB magnet according to claim 2 or 5, is characterized in that: during described powder mold pressing base, in environment, oxygen content is less than 1000ppm.
CN201610011160.5A 2016-01-08 2016-01-08 Sintered neodymium-iron-boron magnet Withdrawn CN105513736A (en)

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CN110428947A (en) * 2019-07-31 2019-11-08 厦门钨业股份有限公司 A kind of rare earth permanent-magnetic material and its feedstock composition, preparation method and application

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CN103996519A (en) * 2014-05-11 2014-08-20 沈阳中北通磁科技股份有限公司 Manufacturing method for high-performance NdFeB rare earth permanent magnet devices
CN104575904A (en) * 2014-11-26 2015-04-29 宁波宏垒磁业有限公司 NdFeB magnet formed by sintering NdFeB recycling waste and preparation method of NdFeB magnet

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CN101266857A (en) * 2007-12-24 2008-09-17 中国石油大学(华东) Method for improving sintered neodymium-iron-boron coercive force and working temperature based on nano Ti powder modification
CN103996519A (en) * 2014-05-11 2014-08-20 沈阳中北通磁科技股份有限公司 Manufacturing method for high-performance NdFeB rare earth permanent magnet devices
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108154986A (en) * 2016-12-06 2018-06-12 中国科学院宁波材料技术与工程研究所 A kind of rare-earth permanent magnet of high abundance containing Y and preparation method thereof
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CN110428947A (en) * 2019-07-31 2019-11-08 厦门钨业股份有限公司 A kind of rare earth permanent-magnetic material and its feedstock composition, preparation method and application
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