CN106887294A - Many seamless permanent-magnet rare-earth rings of Hard Magnetic principal phase radial orientation and cold-forming process - Google Patents

Many seamless permanent-magnet rare-earth rings of Hard Magnetic principal phase radial orientation and cold-forming process Download PDF

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Publication number
CN106887294A
CN106887294A CN201710143001.5A CN201710143001A CN106887294A CN 106887294 A CN106887294 A CN 106887294A CN 201710143001 A CN201710143001 A CN 201710143001A CN 106887294 A CN106887294 A CN 106887294A
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magnetic
permanent
magnet
phase
rare earth
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CN106887294B (en
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姜瑞姣
朱明刚
李安华
郑立允
郭朝晖
石晓宁
李卫
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Central Iron and Steel Research Institute
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Central Iron and Steel Research Institute
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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
    • 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
    • H01F1/0576Alloys 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 pressed, e.g. hot working
    • 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
    • B22F3/12Both compacting and sintering
    • B22F3/14Both compacting and sintering simultaneously
    • 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
    • B22F3/24After-treatment of workpieces or articles
    • 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
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H01F41/0266Moulding; Pressing
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F7/00Magnets
    • H01F7/02Permanent magnets [PM]
    • 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
    • B22F3/12Both compacting and sintering
    • B22F3/14Both compacting and sintering simultaneously
    • B22F2003/145Both compacting and sintering simultaneously by warm compacting, below debindering temperature

Abstract

A kind of many seamless permanent-magnet rare-earth rings of Hard Magnetic principal phase radial orientation and cold-forming process, belong to permanent-magnet material manufacture field.Raw material magnetic for preparing the permanent-magnetic clamp is by the RE Fe B rapidly quenched magnetic powders without high abundance rare earth element and (RE, RE ' containing high abundance rare earth element1,RE′2,...,RE′n) the single-phase rapidly quenched magnetic powders of Fe B mix by required composition quality proportioning, the mixing magnetic becomes through hot pressing/hot-fluid under the conditions of less than 10~100 DEG C of conventional magnetic Nd-Fe-B ring preparation technology and is made the seamless permanent-magnet rare-earth ring of radial orientation containing many or double Hard Magnetic principal phases.Advantage is that each Hard Magnetic principal phase is flake nano crystal structure in permanent-magnetic clamp microstructure, and structural homogenity and uniformity are good, is increasing high abundance rare earth element, while reduction using elements such as neodymium, praseodymiums, it is ensured that magnet ring magnetic property higher.To reducing medium trade mark magnet ring cost, balanced use rare earth resources improve the applications of the high abundance rare earth element in permanent-magnet material such as La, Ce significant.

Description

Many seamless permanent-magnet rare-earth rings of Hard Magnetic principal phase radial orientation and cold-forming process
Technical field
The invention belongs to rare earth permanent-magnetic material manufacture field, more particularly to a kind of many seamless rare earths of Hard Magnetic principal phase radial orientation Permanent-magnetic clamp and cold-forming process, including double seamless permanent-magnet rare-earth rings of Hard Magnetic principal phase radial orientation.
Background technology
Radial orientation permanent-magnet rare-earth ring has important application in the fields such as Aero-Space, electron and electrician, information technology.At present The permanent-magnet rare-earth ring of preparation is main based on neodymium, praseodymium element, and dysprosium, terbium etc. are adulterated again toward contact in the permanent-magnetic clamp of high-temperature coefficient Rare earth element is improving coercivity.However, nature rare earth elements are often symbiosis and metabiosis, current rare earth resources Consumption s tructure causes that permanent-magnet rare-earth ring preparation cost is high, and the high abundance such as lanthanum, cerium rare earth element is in superfluous state.
In recent years, for balanced use rare earth resources, reduces cost, people with lanthanum and cerium as entry, around high abundance Rare earth element expands balance resource and the research for utilizing.But due to the magnetic moment J of Ce, LaSWith anisotropy field HAIt is very low, use Ce, La replace Pr, Nd to prepare magnet performance obtained in cerium-rich rare earth permanent-magnet material far below Nd-Fe-B magnets.Existing control Ce, La mainly have three kinds to the method that magnet intrinsic magnetic properties can be limited:One is to limit Ce to the substitution amount of Nd, Pr element to control The deterioration of magnet performance;Two is to ensure magnetic property to the heavy rare earth element that adulterated in magnet;Three are sintered by double Hard Magnetic principal phases Method adds auxiliary phase alloy sintering to improve the performance containing Ce magnets.It is limited that first two method saves rare earth effect, it is difficult to changes Existing rare earth consumption s tructure, and sintered magnet preparation process is long and numerous and diverse, and prepare radial orientation by being machined magnet There is the problems such as magnetic field orientating is difficult, and waste of material is serious, machining is difficult in seamless magnet ring.
Hot pressing/hot-fluid has two or more Hard Magnetic principal phase structures simultaneously in becoming many (double) Hard Magnetic principal phase permanent-magnetic clamps, passes through Build new combination interface and ensure that magnet magnetic property higher, give on the basis of rare earth total content is controlled, improve high The effective way of abundance content of rare earth permanent-magnetic clamp performance, solves the problems, such as a newly net forming of high abundance permanent-magnet rare-earth ring, enters One step reduces preparation cost.Patent application CN103714928A provides fast quenching permanent magnetism of the Ce contents higher than total amount of rare earth 50% Powder, preparation method thereof, and point out that the magnetic can be used to prepare hot-pressed magnets, but concrete technology step is not given, it is not related to many (double) Hard Magnetic principal phase permanent-magnetic clamp and preparation method thereof, more not on the rare earth element such as high abundance rare earth La, Y, Sc for preparing The content of many (double) Hard Magnetic principal phase permanent-magnetic clamps.The hot pressing of patent 101202143/hot-fluid becomes method and is prepared for high-performance list Hard Magnetic master Phase permanent-magnetic ring of radial orientation, hot pressing temperature is higher than 600 DEG C, and hot-fluid temperature is higher, and energy ezpenditure is excessive, and preparation technology difficulty increases Plus.Attempt reduction hot pressing temperature is excessively added by rare earth element in patent application 104505207, it is seen that in hot-pressed magnets mistake There is real economy benefit and important research to be worth for the realization of low temperature preparation technique in journey.
The content of the invention
Present invention aim at a kind of many seamless permanent-magnet rare-earth rings of Hard Magnetic principal phase radial orientation of offer and its low temperature moulding side Method, including double seamless permanent-magnet rare-earth rings of Hard Magnetic principal phase radial orientation.Using low-temperature primary newly net forming preparation technology, effectively solve On the premise of relatively low without heavy rare earth element and holding total amount of rare earth, using high abundance rare earth element ce, La, Y or Sc portion Point substituting Nd, Pr element still keeps the magnet ring magnetic property not reduce or reduce little problem, reduces the preparation of permanent-magnet rare-earth ring Cost, meets the performance requirement of the trade mark permanent-magnetic clamp such as city's field alignment, is that balanced use rare earth resources seek new way.
Many seamless permanent-magnet rare-earth rings of Hard Magnetic principal phase radial orientation of the invention, the raw material magnetic for preparing the permanent-magnetic clamp It is by the RE-Fe-B rapidly quenched magnetic powders without high abundance rare earth element and (RE, RE ' containing high abundance rare earth element1,RE ′2,...,RE′n) the single-phase rapidly quenched magnetic powders of-Fe-B by required composition quality proportioning mix, the mixing magnetic is through hot pressing/hot-fluid Change is made the seamless permanent-magnet rare-earth ring of radial orientation containing many or double Hard Magnetic principal phases, wherein, RE is lanthanide series, RE 'nFor La, One or more in Ce, Sc and Y element, n is one or more in the positive integer less than 5.
The permanent-magnetic clamp nominal composition is (RE in mass ratio1-x,(RE′1,RE′2,…,RE′n)x)aFe1-a-b-c- dBbCocTMd, wherein, RE is lanthanide series, RE 'nOne or more in for La, Ce, Sc and Y, during n is the positive integer less than 5 One or more;TM is selected from the one kind in element Ni, Mn, Cr, Al, Sn, Ga, Ti, Co, Zn, Zr, Mo, Ag, W, Nb and Cu Or it is various, 0<x<1;24%≤a≤30%;0.6%≤b≤1.2%;1%≤c≤5%;0≤d≤1%;Fe element mass ratioes It is 60~75%;And in raw material magnetic (RE, RE '1,RE′2,...,RE′n) in-Fe-B, Co ≠ 0.
The permanent-magnetic clamp is near-net-shape ring, and maximum magnetic energy product reaches more than 50MGOe, is existed simultaneously not in its microstructure RE containing high abundance rare earth element2Fe14B alloys phase and (RE, RE ' containing high abundance rare earth element1,RE′2,...,RE′n)2Fe14B alloy phases, are many or double Hard Magnetic principal phase flake nano crystal structures, and crystal grain length is 0.2~2 micron, thickness about 50~ 300nm。
Preferably, the RE 'nIt is Ce and/or La elements.As RE 'nDuring for Y and/or Sc for element, in raw material magnetic extremely A kind of few single-phase alloy magnetic for also being constituted comprising rare earth element based on Ce and/or La, and this single-phase alloy magnetic is former The amount of material is more than the single-phase alloy magnetic based on Y and/or Sc.
Many or double Hard Magnetic principal phases are flake nano crystal structure in permanent-magnetic clamp microstructure of the invention, structural homogenity and Uniformity is good, is increasing high abundance rare earth element, while reduction using elements such as neodymium, praseodymiums, it is ensured that magnet ring magnetic higher Energy.For balanced use rare earth resources, improving the applications of the high abundance rare earth element in permanent-magnet material such as La, Ce has important meaning Justice.
The purpose of the invention also resides in the low temperature for providing a kind of many (double) Hard Magnetic seamless permanent-magnet rare-earth rings of principal phase radial orientation Forming technique, it is characterised in that smelt the single-phase RE-Fe-B alloy cast ingots without high abundance rare earth element by quality proportioning and contain There are single-phase (RE, RE ' of high abundance rare earth element1,RE′2,...,RE′n)-Fe-B alloy cast ingots, and amorphous nano is produced respectively Brilliant rapid tempering belt, broken screening is made sub-micron magnetic, by required quality proportioning mixing RE-Fe-B magnetics and (RE, RE '1,RE ′2,...,RE′n)-Fe-B magnetics, many (double) the Hard Magnetic principal phase magnets of theoretical density isotropism are hot pressed under high-frequency alternating magnetic field, Reheating rheology is made many (double) Hard Magnetic seamless permanent-magnet rare-earth rings of principal phase radial orientation.Comprise the following steps:
1) by alloying component dispensing, the single-phase RE-Fe-B alloy cast ingots without high abundance rare earth element are smelted respectively and is contained There are single-phase (RE, RE ' of high abundance rare earth element1,RE′2,...,RE′n)-Fe-B alloy cast ingots.
2) by above two or various single-phase alloy ingot castings, melt casting fast quenching on refractory alloy roller obtains two kinds respectively Or various single-phase RE-Fe-B amorphous nano-crystalline strips.
3) each single-phase RE-Fe-B amorphous nano-crystallines strip is carried out into Mechanical Crushing and screening, is calculated according to target component Weigh, be uniformly mixed and made into the dual or multi Hard Magnetic principal phase amorphous nano-crystalline magnetic of isotropism.
4) the dual or multi Hard Magnetic principal phase amorphous nano-crystalline mixing magnetic of isotropism that will be obtained is true under high-frequency alternating magnetic field The dual or multi Hard Magnetic principal phase Re-Fe-B magnets blank of density isotropic is helped in empty hot pressing.
5) the dual or multi Hard Magnetic principal phase magnet blank of the theoretical density isotropism is extruded into hot-fluid in argon gas protection environment lower back Become the seamless rare earth-Fe-B permanent-magnetic clamps of dual or multi Hard Magnetic principal phase of radial orientation.
6) after the completion of hot-fluid becomes, extract hot-fluid out and become pressure head, permanent-magnetic clamp sends out the demoulding by roller-way, cuts off discard, and cooling is obtained The dual or multi seamless permanent-magnet rare-earth ring of Hard Magnetic principal phase of radial orientation;
It is described it is rapid 1) in, RE-Fe-B alloy cast ingots and (RE, RE '1,RE′2,...,RE′n) also contain in-Fe-B alloy cast ingots There is one or more in element Ni, Mn, Cr, Al, Sn, Ga, Ti, Co, Zn, Zr, Mo, Ag, W, Nb and Cu;And (RE, RE ' 1, RE ' 2 ..., RE ' be n) in-Fe-B, Co ≠ 0;2 are respectively provided with the alloy cast ingot that obtains is microcosmic:14:1 permanent-magnet alloy phase;Step 3) The amorphous nano-crystalline magnetic and step 4 of middle acquisition) in obtained isotropic magnet blank microstructure simultaneously containing receiving The RE of metrical scale2Fe14B alloys phase and (RE, RE '1,RE′2,...,RE′n)2Fe14B alloy phases, and may comprising a small amount of amorphous into Point.
Preferably, step 1) in, composition is (RE, RE '1,RE′2,...,RE′n)-Fe-B alloy cast ingot at least one Plant amount of the ingot casting containing RE ' and account for more than the 50% of its total rare earth (TRE) amount.
The step 4) and step 5) in do lubricated before hot pressing/hot-fluid becomes, by outer die casing inwall, gasket surface, Position spraying lubricant or cushioning graphite material that pressure head end face etc. may be contacted with magnetic or hot-pressed magnets blank.And step 4) Middle hot pressing is completed in high-frequency alternating magnetic field, and hot pressing temperature is lower than conventional magnetic Nd-Fe-B ring hot pressing temperature 10~100 DEG C.
The step 5) in, hot-fluid temperature is lower than conventional magnetic Nd-Fe-B ring hot-fluid temperature 10~50 DEG C, becomes in hot-fluid Before process terminates, an about 0.1~0.8MPa is downwardly applied on magnet ring top by the movable annular seaming chuck (5) of additional high temperature resistant Slight pressure.
The step 4) in, outer die casing is made of Talide, and it is the alloy system of H13 that pressure head uses the trade mark Into;Step 5) in, outer die casing and pressure head are made of Talide.
The beneficial effects of the present invention are:
The present invention is using uniform by quality proportioning after various or two kinds of alloy amorphous nanocrystalline rapid tempering belt powder of single-phase permanent Mixing, new many or double Hard Magnetic principal phase slotless design rare earths are prepared in high-frequency alternating magnetic field by hot pressing/hot-fluid change technique Permanent-magnetic clamp, maintains nanocrystalline microstructure, and magnetic property is excellent.
The present invention using without high abundance rare earth element RE-Fe-B rapid tempering belts and containing high abundance rare earth element (RE, RE′1,RE′2,...,RE′n)-Fe-B magnetics many (double) the Hard Magnetic principal phase permanent-magnetic clamps of mixed powder hot-pressing thermal rheology preparation, with other methods The high abundance permanent magnet of preparation is compared, and the method is not simply to substitute neodymium, praseodymium with the high abundance such as La, Ce, Sc, Y rare earth element Element, but construct novel interfacial in hot-fluid becomes permanent-magnetic clamp and combine, form RE2Fe14B and (RE '1,RE′2,...,RE ′n)2Fe14Many (double) Hard Magnetic principal phase structures that B phases coexist, (RE1-x,(RE′1,RE′2,...,RE′n)x)aFe1-a-b-c-dBbCocTMd Only nominal composition, in the case where not increasing or increasing total amount of rare earth on a small quantity, largely adds high abundance elements, and reduction is used The elements such as neodymium, praseodymium, have remained in that permanent-magnetic clamp magnetic property higher, can meet the need of the trade mark permanent-magnetic clamp such as city's field alignment Ask, greatly reduce production cost, open the new way of balanced use rare earth resources.
The present invention by largely add low melting point high abundance rare earth elements reduce two step heat pressing process temperature, realize compared with Prepared by the near-net-shape of the seamless permanent-magnet rare-earth ring of (double) Hard Magnetic principal phases many under low temperature, technological process is short, and energy resource consumption is low, subsequently Processing is simple, improves rare earth permanent-magnetic material utilization rate.
Brief description of the drawings
Fig. 1 be many seamless permanent-magnet rare-earth ring forming method steps 4 of Hard Magnetic principal phase radial orientation of the invention) in hot pressing die Structural representation.
Fig. 2 be many seamless permanent-magnet rare-earth ring forming method steps 5 of Hard Magnetic principal phase radial orientation of the invention) in hot-fluid become before Mould structure schematic diagram.
Fig. 3 be many seamless permanent-magnet rare-earth ring forming method steps 5 of Hard Magnetic principal phase radial orientation of the invention) in hot-fluid become after Mould structure schematic diagram.
In figure, pressed on hot pressing core bar 1, hot pressing outer die casing 2, many Hard Magnetic major phase raw materials magnetics 3, circular gasket 4, additional annular First 5, hot-fluid becomes outer die casing 6, hot-fluid change pressure head 7, hot-fluid change many (double) the Hard Magnetic principal phase blanks 9, hot-fluid of die cavity 8, hot pressing and becomes many (double) Hard Magnetic principal phase permanent-magnetic clamp 10.
Specific embodiment
The RE-Fe-B alloy cast ingots of chemical composition proportion ingredient, vacuum metling without high abundance rare earth element as shown in table 1 With (RE, RE ' containing high abundance rare earth element1,RE′2,...,RE′n)-Fe-B alloy cast ingots.
The single-phase alloy ingot chemistry (wt.%) of the embodiment of the present invention of table 1
Ingot casting is numbered Nd Fe B Ga Co Al Ce La Y Sc
1-1# 28.5 66.16 0.92 0.42 4 / / / / /
1-2# / 65.93 0.92 0.65 4 / 29 / / /
2-1# 28.5 68.18 0.9 0.42 2 / / / / /
2-2# / 65.68 0.9 0.42 4 / 28.5 / / /
3-1# 29.7 68.85 0.98 0.65 0 / / / / /
3-2# 9 64.62 0.98 0.4 4 / / 21 / /
4-1# 24 73.58 1.02 0.3 0 0.2 / / / /
4-2# / 65.97 0.9 0.4 4 / 29 / / /
4-3# / 65.87 0.9 0.4 2 0.1 / / 31 /
4-4# / 67.87 0.9 0.4 2 0.1 / / / 29
* in table 1 "/" represent without.
Above-mentioned alloy cast ingot is crushed into shove charge respectively, vacuum is pumped to higher than 10-3Argon gas is filled with during Pa, induction melting makes Melt casting fast quenching on refractory alloy roller obtains single-phase nano crystalline crystallite strip (strip may include part amorphous structure). The rapid tempering belt of acquisition is carried out into Mechanical Crushing respectively, the magnetic that particle diameter is 0.2~0.45 μm is filtered out, according to 164.99:5.01 Quality proportioning weigh the corresponding single-phase alloy magnetic of numbering 1-1# and 1-2# alloy cast ingot, be uniformly mixed into preparation 1# samples institute Double Hard Magnetic principal phase magnetic powder materials;It is 2-1# that will number and the rapid tempering belt that is made of the alloy cast ingot of 2-2# crushes sieve powder respectively, According to 85.74:84.26 quality proportioning claims powder to be uniformly mixed into the double Hard Magnetic principal phase magnetic powder materials prepared used by 2# samples.According to Secondary to analogize, just numbering is that the rapid tempering belt that is made of alloy cast ingot of 4-1#, 4-2#, 4-3# and 4-4# crushes sieve powder respectively, according to 109.87:45.46:7.09:7.58 quality proportioning claims powder to be uniformly mixed into many Hard Magnetic principal phase magnetics prepared used by 4# samples Raw material, many (double) the Hard Magnetic principal phase isotropism magnetic powder materials nominal compositions for obtaining are (RE in mass ratio1-x,(RE′1,RE ′2,...,RE′n)x)aFe1-a-b-c-dBbCocTMd, as shown in table 3.
Single-phase alloy magnetic and its consumption used by the embodiment of the present invention magnetic powder materials of table 2
Lubricant is sprayed to hot pressing die outer die casing, pressure head bottom surface and pad upper surface, the isotropism that will be obtained is more It is 45mm that (double) Hard Magnetic principal phase magnetic powder materials load internal diameter, and during external diameter is for the cylindrical mold of 75mm, being pumped to vacuum is higher than 10-2Pa, connects high-frequency alternating magnetic field, and hot pressing helps close under the conditions of less than 10~100 DEG C of conventional neodymium iron boron magnetic body hot pressing temperature Degree many (double) the Hard Magnetic principal phase permanent-magnetic clamp blanks of isotropism, are quickly cooled to the room temperature demoulding.
Many (double) the Hard Magnetic principal phase magnet blanks of the theoretical density isotropism are warming up to conventional neodymium iron boron under argon gas protection 10~50 DEG C below magnet hot-fluid temperature, preheating 10s~2min back extruding hot-fluids become many (double) Hard Magnetics of radial orientation Principal phase rare earth-Fe-B permanent-magnetic clamps, heating rate 150~250 DEG C/min, 100~250MPa of pressure, rate of deformation 10-4~10- 1mm/S-1.Before hot Rheologic terminates, by additional high temperature resistant can rotating ring 5 magnet ring top be downwardly applied to one about 0.1~ The slight pressure of 0.8MPa.
After the completion of hot-fluid becomes, extract hot-fluid out using drawbench and become pressure head, many (double) Hard Magnetic principal phase permanent-magnet rare-earth rings are by roller-way Send out upwards, complete the demoulding, be down to room temperature, cut off discard, obtain the seamless rare earth permanent magnet of many (double) Hard Magnetic principal phases of radial orientation Ring.
Gained permanent-magnet rare-earth ring is near-net-shape pipe, and external diameter is 45mm, and internal diameter is 35mm, ring about 35mm high, each in gained The small column magnet of Φ 6 × 3 is intercepted on anisotropy magnet ring, maximum magnetic energy product is measured as shown in table 3.
Many (double) Hard Magnetic principal phase permanent-magnetic ring of radial orientation maximum magnetic energy products prepared by the embodiment of the present invention of table 3
The present invention is only carried out explanation to preferred scheme, using this technology, by feed change composition, fast quenching speed Degree, pressuring method, die size and shape, prepare heterogeneity, shape and size the seamless rare earth of many (double) Hard Magnetic principal phases forever Magnet ring (including prepare be entirely free of the seamless permanent-magnet rare-earth ring of many (double) Hard Magnetic principal phases of high abundance rare earth element) or by sawing Magnet ring obtains rare-earth permanent magnetic tile and belongs to the scope of the present invention.

Claims (8)

1. the principal phase radial orientation of Hard Magnetic more than is seamless permanent-magnet rare-earth ring, it is characterised in that the raw material magnetic for preparing the permanent-magnetic clamp Powder is by the RE-Fe-B rapidly quenched magnetic powders without high abundance rare earth element and (RE, RE ' containing high abundance rare earth element1,RE ′2,...,RE′n) the single-phase rapidly quenched magnetic powders of-Fe-B by required composition quality proportioning mix, the mixing magnetic is in high-frequency alternating magnetic Become through hot pressing/hot-fluid in and be made the seamless permanent-magnet rare-earth ring of radial orientation containing many or double Hard Magnetic principal phases, wherein, RE is group of the lanthanides Element, RE 'nIt it is one or more in element La, Ce, Sc and Y, n is one or more in the positive integer less than 5.
2. many seamless permanent-magnet rare-earth rings of Hard Magnetic principal phase radial orientation as claimed in claim 1, it is characterised in that permanent-magnetic clamp name Adopted composition is (RE in mass ratio1-x,(RE′1,RE′2,…,RE′n)x)aFe1-a-b-c-dBbCocTMd, wherein, RE is lanthanide series, RE′nIt it is one or more in element La, Ce, Sc and Y, n is one or more in the positive integer less than 5;TM is selected from unit One or more in plain Ni, Mn, Cr, Al, Sn, Ga, Ti, Co, Zn, Zr, Mo, Ag, W, Nb and Cu;0<x<1;24%≤a≤ 30%;0.6%≤b≤1.2%;1%≤c≤5%;0≤d≤1%;Fe elements mass ratio is 60~75%;And in raw material magnetic Powder (RE, RE '1,RE′2,...,RE′n) in-Fe-B, Co ≠ 0.
3. many seamless permanent-magnet rare-earth rings of Hard Magnetic principal phase radial orientation as claimed in claim 1, it is characterised in that should near net into Shape ring, maximum magnetic energy product reaches more than 50MGOe, and its microstructure has the RE without high abundance rare earth element simultaneously2Fe14B alloys Phase and (RE, RE ' containing high abundance rare earth element1,RE′2,...,RE′n)2Fe14B alloy phases, are many or double Hard Magnetic principal phase pieces Shape nanocrystalline structure, crystal grain length is 0.2~2 micron, thickness about 50~300nm.
4. many seamless permanent-magnet rare-earth rings of Hard Magnetic principal phase radial orientation as claimed in claim 1, it is characterised in that RE 'nPreferably La and/or Ce elements.As RE 'nDuring for Y and/or Sc elements, at least also it is with Ce and/or La comprising one kind in raw material magnetic The single-phase alloy magnetic that main rare earth element is constituted, and the amount of this single-phase alloy magnetic powder materials is more than based on Y and/or Sc Single-phase alloy magnetic.
5. the cold-forming process of the principal phase radial orientation of Hard Magnetic more than is seamless permanent-magnet rare-earth ring, it is characterised in that comprise the following steps:
1) by alloying component dispensing, the single-phase RE-Fe-B alloy cast ingots without high abundance rare earth element are smelted respectively and contains height Single-phase (RE, RE ' of abundance rare earth element1,RE′2,...,RE′n)-Fe-B alloy cast ingots;
2) by above two or various single-phase alloy ingot castings, melt casting fast quenching on refractory alloy roller obtains two kinds or many respectively Plant single-phase RE-Fe-B amorphous nano-crystalline strips;
3) by each single-phase RE-Fe-B amorphous nano-crystalline strip Mechanical Crushings and screen, calculated by required quality proportioning and weighed, It is even to be mixed and made into the dual or multi Hard Magnetic principal phase amorphous nano-crystalline magnetic of isotropism;
4) the dual or multi Hard Magnetic principal phase amorphous nano-crystalline magnetic of isotropism that will be obtained Vacuum Heat compacting under high-frequency alternating magnetic field Help the dual or multi Hard Magnetic principal phase Re-Fe-B magnets blank of density isotropic;
5) the dual or multi Hard Magnetic principal phase magnet blank of the theoretical density isotropism is become in argon gas protection environment lower back extruding hot-fluid Seamless rare earth-Fe-B the permanent-magnetic clamps of dual or multi Hard Magnetic principal phase of radial orientation;
6) after the completion of hot-fluid becomes, extract hot-fluid out and become pressure head, permanent-magnetic clamp sends out the demoulding by roller-way, cuts off discard, and cooling obtains radial The dual or multi seamless permanent-magnet rare-earth ring of Hard Magnetic principal phase of orientation.
6. method as claimed in claim 5, it is characterised in that:The step 1) in, RE-Fe-B alloy cast ingots and (RE, RE '1, RE′2,...,RE′n) in-Fe-B alloy cast ingots also containing element Ni, Mn, Cr, Al, Sn, Ga, Ti, Co, Zn, Zr, Mo, Ag, W, One or more in Nb and Cu;And (RE, RE ' 1, RE ' 2 ..., RE ' be n) in-Fe-B, Co ≠ 0;The alloy cast ingot for obtaining is micro- 2 are respectively provided with sight:14:1 permanent-magnet alloy phase;Step 3) in the amorphous nano-crystalline magnetic that obtains and step 4) in it is obtained each to same The RE containing nanoscale simultaneously in property magnet blank microstructure2Fe14B alloys phase and (RE, RE '1,RE′2,...,RE ′n)2Fe14B alloy phases, and comprising a small amount of amorphous component.
7. method as claimed in claim 5, it is characterised in that:The step 4) and step 5) in become in hot pressing/hot-fluid and advance Row lubricated, in the position spraying that outer die casing inwall, gasket surface, pressure head end face etc. may be contacted with magnetic/magnet blank Lubricant or cushioning graphite material;And step 4) in, hot pressing is completed in high-frequency alternating magnetic field, and hot pressing temperature is than conventional neodymium iron boron The hot pressing temperature of magnet ring is low 10~100 DEG C.
8. method as claimed in claim 6, it is characterised in that:The step 5) in, hot-fluid temperature is than conventional neodymium-iron-boron The hot-fluid temperature of ring is low 10~50 DEG C, before hot Rheologic terminates, is existed by adding movable high-temperature resistant ring-shaped seaming chuck (5) Magnet ring top is downwardly applied to a pressure of 0.1~0.8MPa.
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CN109346258A (en) * 2018-09-08 2019-02-15 江西理工大学 A kind of nano double main phase magnet and preparation method thereof
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CN109166720A (en) * 2018-08-22 2019-01-08 浙江东阳东磁稀土有限公司 A kind of method of continous way production hot extrusion radiation ring
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CN114334418A (en) * 2021-12-29 2022-04-12 钢铁研究总院 Combined type extrusion forming device and method suitable for neodymium iron boron permanent magnet ring
CN114334418B (en) * 2021-12-29 2022-10-11 钢铁研究总院 Combined type extrusion forming device and method suitable for neodymium iron boron permanent magnet ring

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