CN107686947A - A kind of alloy for permanent-magnet material and preparation method thereof - Google Patents

A kind of alloy for permanent-magnet material and preparation method thereof Download PDF

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CN107686947A
CN107686947A CN201710844253.0A CN201710844253A CN107686947A CN 107686947 A CN107686947 A CN 107686947A CN 201710844253 A CN201710844253 A CN 201710844253A CN 107686947 A CN107686947 A CN 107686947A
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alloy
furnace
permanent
preparation
cast strip
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张椿英
赵浩峰
于鹏
莫宏恩
柴阜桐
柴知章
郑建华
黄自成
沈子强
谢二想
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Anhui Institute of Information Engineering
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/005Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/002Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/18Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/32Ferrous alloys, e.g. steel alloys containing chromium with boron
    • 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
    • H01F1/058Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IVa elements, e.g. Gd2Fe14C

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  • Engineering & Computer Science (AREA)
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  • Metallurgy (AREA)
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  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Power Engineering (AREA)
  • Hard Magnetic Materials (AREA)

Abstract

The present invention relates to a kind of alloy II for permanent-magnet material and preparation method thereof, alloy II material compositions and weight percentage are:Ce15~20%, Bi 0.02%~0.06%, P0.06%~0.12%, Pt0.06%~0.10%, Be 0.02%~0.07%, B2~6%, surplus Fe, preparation method step include dispensing, melting, system band, hydrogen it is broken, grinding, it is used to the alloy II of permanent-magnet material using this and combines permanent-magnet alloy prepared by other alloys having that heat endurance is good, and there is good magnetic property, the preparation method technique of permanent-magnet alloy is simple, production cost is low, suitable for industrialized production.

Description

A kind of alloy for permanent-magnet material and preparation method thereof
Technical field
The invention belongs to permanent-magnet material technical field, and in particular to a kind of for the alloy II of permanent-magnet material and its preparation side Method.
Background technology
Permanent-magnet alloy is a kind of important, modern industry and the indispensable functional material of science and technology.People utilize magnetic Magnetic energy can be converted into electric energy or mechanical energy with the interaction of magnetic energy, magnetic energy and electric energy;Using effect of the magnetic field to material, Change the microstructure of material, promote energy-conservation and environmental-protection function etc..Permanent-magnet alloy is all taken in all these devices or device Important function.
CN201610964128.9 discloses a kind of method for improving border structure and preparing high-performance neodymium-iron-boron magnet, the party Method is sunk before Nd-Fe-B powder is orientated die mould using magnetron sputtering or the method for vacuum evaporation on the surface of neodymium iron boron powder particle RM the or MM low-melting alloys that product a layer thickness is 10-100nm, R La, Ce, Pr, Nd, Gd, Tb, Dy, Ho, M Fe, Co, Ni, Cu, Zn, Ga, Al, Sn, Ag, after being orientated die mould, only carry out liquid-phase sintering and Solid Free and sinter, to avoid producing sintering neck, Tempering heat treatment is finally carried out, makes 2:14:1 main phase grain is by low melting point mutually uniformly cladding, realization sufficiently isolation, and obtaining brilliant Particle size finally gives performance Nd Fe B sintered magnet close to the fine grained texture of particle size.But the production method produces Cycle is grown, and combination property is not high.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of alloy II for permanent-magnet material and preparation method thereof, makes It is used to the alloy II of permanent-magnet material with this and combines permanent-magnet alloy prepared by other alloys having that heat endurance is good, and with good Magnetic property, the preparation method technique of permanent-magnet alloy is simple, and production cost is low, suitable for industrialized production.
The technical solution adopted by the present invention is:
A kind of alloy II for permanent-magnet material, its material composition and weight percentage are:Ce15~20%, Bi 0.02%~0.06%, P0.06%~0.12%, Pt0.06%~0.10%, Be 0.02%~0.07%, B2~6% are remaining Measure as Fe;The B is added in the form of ferro-boron intermediate alloy, and B weight/mass percentage composition is 20-25% in ferro-boron intermediate alloy;
The preparation method of alloy II for permanent-magnet material a kind of, step include:
A, it is Ce15~20% by alloying component weight percentage, Bi 0.02%~0.06%, B3~6%, P0.06%~0.12%, Pt0.06%~0.10%, Be 0.02%~0.07%, surplus are that Fe carries out dispensing;The B with The form of ferro-boron intermediate alloy adds, and B weight/mass percentage composition is 20-25% in ferro-boron intermediate alloy.
B, raw material is heated to 1570-1590 DEG C of melting, then cast obtains mother alloy ingot;The melting is in electric arc furnaces Melting in copper crucible, constantly aluminium alloy is stirred with electric arc in fusion process, it is fully melted uniformly;
Mother alloy ingot is heated to 1500~1560 DEG C of fusings in induction furnace, obtain foundry alloy liquid C,;
The method that foundry alloy liquid is got rid of to band in vacuum rapid hardening spun furnace by vacuum rapid hardening prepares alloy Cast Strip D,;Institute State 15~17 microns of the alloy tape thickness of preparation, 8~13mm of width;
E, alloy Cast Strip is put into placement more than 8min in the closed container for fill dry ice, preferably places 30-50min;Institute State the 5-10% that dry ice quality is alloy Cast Strip;The dry ice is cylindric, a diameter of 4mm, length 5-12mm;Then will close Golden Cast Strip, which is taken out, is put into the hydrogen crushing furnace progress broken obtained alloy coarse powder of hydrogen, and the hydrogen crushing furnace reative cell vacuum is 0.06~0.1Pa, Air pressure is 0.8~1.3atm in hydrogen crushing furnace, and in-furnace temperature is 260~310 DEG C, and the hydrogen broken time is 70~80min;
F, alloy coarse powder is put into airflow milling and ground, the alloy fine powder that granularity is 1~8 μm is made, as permanent magnetism The alloy II of material;The airflow milling powder pressure is 6~7atm.
A kind of permanent-magnet alloy, its raw material are combined by alloy I, II, III and inorganic composite materials IV, the alloy material I, II, III and inorganic composite materials IV mass ratio are 1:1-1.5:0.2-0.6:0.01;
Described its material composition of alloy I and weight percentage are:Cr0.7~1.3%, Ta 3~7%, Ge 0.1~ 0.7%, Ti 0.3~0.6%, Sn0.5~0.9%, B3~6%, Nd21~25%, surplus Fe;The B with ferro-boron among The form of alloy adds, and B weight/mass percentage composition is 20-25% in ferro-boron intermediate alloy;
The alloy III, its material composition and weight percentage are:La 5~8%, P0.04%~0.08%, B0.2 ~0.6%, Al 5~8%, Si7~11%, surplus Fe;The B is added in the form of ferro-boron intermediate alloy, is closed among ferro-boron B weight/mass percentage composition is 20-25% in gold;
Described its composition of inorganic composite materials IV and weight percentage are:SrO 2~6%, BaO 2-7%, K2O 0.1-0.5%, Mn2O30.5-1.2%, Pb3O40.3-0.7%, Sb2O50.3-0.8%, PbO20.1-0.4%, surplus are Fe2O3
The preparation method step of the alloy I includes:
A, it is Cr0.7~1.3%, Ta 3~7%, Ge 0.1~0.7%, Ti 0.3 by alloying component weight percentage ~0.6%, Sn0.5~0.9%, B3~6%, Nd21~25%, surplus are that Fe carries out dispensing;The B is with ferro-boron intermediate alloy Form add, B weight/mass percentage composition is 20-25% in ferro-boron intermediate alloy.
B, raw material is heated to 1570-1590 DEG C of melting, then cast obtains mother alloy ingot;The melting is in electric arc furnaces Melting in copper crucible, constantly aluminium alloy is stirred with electric arc in fusion process, it is fully melted uniformly;
Mother alloy ingot is heated to 1500~1560 DEG C of fusings in induction furnace, obtain foundry alloy liquid C,;
The method that foundry alloy liquid is got rid of to band in vacuum rapid hardening spun furnace by vacuum rapid hardening prepares alloy Cast Strip D,;Institute State 17~20 microns of the alloy tape thickness of preparation, 8~13mm of width;
E, alloy Cast Strip is put into placement more than 8min in the closed container for fill dry ice, preferably places 30-50min;Institute State the 5-10% that dry ice quality is alloy Cast Strip;The dry ice is cylindric, a diameter of 4mm, length 5-12mm;Then will close Golden Cast Strip, which is taken out, is put into the hydrogen crushing furnace progress broken obtained alloy coarse powder of hydrogen, and the hydrogen crushing furnace reative cell vacuum is 0.06~0.1Pa, Air pressure is 0.8~1.3atm in hydrogen crushing furnace, and in-furnace temperature is 260~310 DEG C, and the hydrogen broken time is 70~80min;
F, alloy coarse powder is put into airflow milling and ground, the alloy fine powder that granularity is 2~5 μm is made, as permanent magnetism The alloy I of material;The airflow milling powder pressure is 6~7atm.
The preparation method step of the alloy III includes:
A, it is La 5~8%, P0.04%~0.08%, B0.2~0.6% by alloying component weight percentage, Al 5 ~8%, Si7~11%, surplus are that Fe carries out dispensing;The B is added in the form of ferro-boron intermediate alloy, ferro-boron intermediate alloy Middle B weight/mass percentage composition is 20-25%;
B, raw material is heated to 1470-1490 DEG C of melting, then cast obtains mother alloy ingot;The melting is in electric arc furnaces Melting in copper crucible, constantly aluminium alloy is stirred with electric arc in fusion process, it is fully melted uniformly;
Mother alloy ingot is heated to 1400-1460 DEG C of fusing in induction furnace, obtain foundry alloy liquid C,;
The method that foundry alloy liquid is got rid of to band in vacuum rapid hardening spun furnace by vacuum rapid hardening prepares alloy Cast Strip D,;Institute 3~5 millimeters of the alloy tape thickness of preparation is stated, width is 5~12mm;
E, fused salt is prepared:It is 0.1: 1: 1 by CaCl2, KCl, NaF, CsF mol ratio:0.05-0.09 weighs each constituent element, Fused-salt medium is obtained after mixing, the powdery monocrystalline silicon for the 11%-14% for accounting for fused-salt medium quality is added, is ground;
F, fused salt is put into salt bath furnace, is heated to 690-760 DEG C, constant temperature 20-30min, negative electrode is then done with silicon steel sheet Immerse in liquid fused salt, alloy Cast Strip is immersed into logical direct current in liquid fused salt as anode carries out plating siliconising to alloy Cast Strip;Institute It is pulse to electrically to state logical direct current, average current density 55-65mA/cm2;The alloy Cast Strip in fused salt with 0.10-0.13m/min gait of march carries out uniform motion, and it is 20- to be kept for residence time of the alloy Cast Strip in fused salt 25min;The weight/mass percentage composition of silicon is preferably 4-6% in the silicon steel sheet;
G, the alloy Cast Strip after siliconising is put into progress mechanical ball mill to alloy powder particle diameter in ball grinder and reaches 7-11 μm, The alloy III for permanent-magnet material is made.
The preparation method step of the inorganic composite materials IV includes:
A, by inorganic composite materials IV Ingredients Weight percentage compositions SrO 2~6%, BaO 2-7%, K2O 0.1-0.5%, Mn2O30.5-1.2%, Pb3O40.3-0.7%, Sb2O50.3-0.8%, PbO20.1-0.4%, surplus Fe2O3Carry out dispensing;
B, dry after the raw material prepared being carried out into mixing and breaking up in sand mill, then sieve;The screen cloth of the sieving For 180-220 mesh;The drying temperature is 110-120 DEG C, drying time 1-3h;
C, the raw material after sieving is put into sintering furnace and be sintered, sintering temperature is 1100-1250 DEG C, and soaking time is 1-3h;
D, sintered product is ground to particle diameter 10-13 microns in grinder, that is, be made for the inorganic multiple of permanent-magnet material Condensation material IV.
A kind of preparation method of permanent-magnet alloy, step include:
A, by permanent-magnet alloy raw alloy material I, II, III and inorganic composite materials IV mass ratio 1:1-1.5: 0.2-0.6:0.01 dispensing, it is added in three-dimensional mixer and is well mixed, mixed powder is made;
B, mixed powder is orientated in Magnetic field press, it is compressing;The compressing use Bidirectional pressure mode is molded, Pressure is 150KN, pressurize 10-20S;
C, molded blank is entered into sintering furnace in argon gas protection down to be sintered, is first warming up to 500-750 DEG C, be incubated 1- 3h, 1150-1180 DEG C of sintering 1-3h is then heated to, is cooled to room temperature;
D, Ageing Treatment is carried out after the molded blank after sintering being carried out into double tempering processing, obtained permanent-magnet alloy is made; The temperature of the double tempering processing is respectively 890-910 DEG C and 540-570 DEG C, and soaking time is respectively 1-2h;The timeliness The temperature of processing is 210-250 DEG C, soaking time 10-30h.
It is used for the alloy II of permanent-magnet material using the present invention and combines light rare earth shape in the permanent-magnet alloy of other alloys preparation Into principal phase Nd2Fe14B and time obvious boundary of principal phase Ce2Fe14B, La2Fe14B, magnetic coupling interaction is enhanced, makes magnetic The existing high coercivity of body turn avoid remanent magnetism and decline to a great extent, so as to obtain higher comprehensive magnetic energy.
Sn and Ge can reduce rich-Nd phase and the angle of wetting of principal phase, suppress growing up for principal phase, make principal phase interface defect density Reduce, magnetic reversal farmland is difficult in interface forming core.Therefore the remanent magnetism of material is improved.
Bi and P element can be distributed in around main phase grain to disperse, can be effectively improved the institutional framework of Grain-Boundary Phase, right Magnet carries out crystal boundary modified, reinforcing Grain-Boundary Phase.
The metal oxide complex that inorganic composite materials are formed in permanent-magnet alloy is evenly distributed in crystal boundary and plays nail Bundle acts on, and coercivity is improved.And itself be permanent-magnet ferrite, it can equally play the work of enhancing product magnetic property With.
In the preparation method of permanent-magnet alloy of the present invention, in sintering process, a small amount of high-melting point alloy element the such as the 3rd is added Transition system Ta, Pt, it can make to separate out cenotype in magnet tissue, eliminate the phenomenon directly contacted between main phase grain, effectively suppress Main phase grain is grown up, and beneficial to the relatively fine uniform grain structure of acquisition, while can improve the heat endurance of principal phase magnet.
The reason for Ti, Cr improvement HCJ of First Transition system is the intercrystalline parafacies to be formed, and inhibits crystal grain to hand over Particle is grown up at remittance, has refined main phase grain, therefore may refrain from the enhancing of their ambient stray fields, and then is improved intrinsic Coercivity.
Heavy rare earth element is not had in preparation, few using rare element, other costs of material are relatively low;Prepared and closed in kind in addition Gold ensure that the uniformity of alloying component, tissue and performance, ensure that the quality of alloy by quick cooling.It is prepared by the alloy Simple process, process is simple, and the alloy of production has good performance, is highly convenient for industrialized production.The present invention is prepared forever Magnetic material is applied to electrical apparatus industry.
Embodiment
Embodiment 1
A kind of permanent-magnet alloy, its raw material are combined by alloy I, II, III and inorganic composite materials IV, the alloy material I, II, III and inorganic composite materials IV mass ratio are 1:1:0.2:0.01;
Described its material composition of alloy I and weight percentage are:Cr0.7%, Ta3%, Ge 0.1%, Ti0.3%, Sn0.5%, B3%, Nd21%, surplus Fe;The B is added in the form of ferro-boron intermediate alloy, B in ferro-boron intermediate alloy Weight/mass percentage composition is 24%;
Described its material composition of alloy II and weight percentage are:Ce15%, Bi0.02%%, P0.06%, Pt0.06%, Be 0.02%, B2%, surplus Fe;The B is added in the form of ferro-boron intermediate alloy, ferro-boron intermediate alloy Middle B weight/mass percentage composition is 24%;
Described its material composition of alloy III and weight percentage are:La 5%, P0.04%, B0.2%, Al5%, Si7%, surplus Fe;The B is added in the form of ferro-boron intermediate alloy, and B weight/mass percentage composition is in ferro-boron intermediate alloy 22%;
Described its material composition of inorganic composite materials IV and weight percentage are:SrO 2%, BaO 2%, K2O 0.1%, Mn2O30.5%, Pb3O40.3%, Sb2O50.3%, PbO20.1%, surplus Fe2O3
The preparation method step of the alloy I includes:
A, it is Cr0.7%, Ta3%, Ge0.1%, Ti0.3%, Sn0.5% by alloy raw material Ingredients Weight percentage composition, B3%, Nd21%, surplus are that Fe carries out dispensing, and Cr, Ta, Ge, Ti, Sn, Nd, Fe are pure material (content is more than 99.9%); B Added in the form of ferro-boron intermediate alloy, B weight/mass percentage composition is 24% in ferro-boron intermediate alloy.
B, raw material is heated to 1570 DEG C of meltings, then cast obtains mother alloy ingot;The melting is in electric arc furnaces copper earthenware Melting in crucible, constantly aluminium alloy is stirred with electric arc in fusion process, it is fully melted uniformly;
Mother alloy ingot is heated to 1540 DEG C of fusings in induction furnace, obtain foundry alloy liquid C,;
The method that foundry alloy liquid is got rid of to band in vacuum rapid hardening spun furnace by vacuum rapid hardening prepares alloy Cast Strip D,;Institute State remelting tubular type crucible bottom in vacuum rapid hardening spun furnace and be provided with through hole, remelting tubular type crucible top connects nitrogen, nitrogen through valve The pressure of gas is 1.6 atmospheric pressure;The bottom of remelting tubular type crucible is placed on forming furnace runner wheel rim at 3mm, works as foundry alloy After fusing, the valve on remelting tubular type crucible top is opened, melting foundry alloy sprays from the through hole of crucible bottom under nitrogen pressure To the forming furnace runner wheel rim of rotation, continuous alloy strip (17~20 microns of alloy tape thickness, 8~13mm of width) is formed;Weight Fusion tube type crucible internal diameter is 13mm, is highly 260mm, and the through-hole aperture of remelting tubular type crucible bottom is 1.5mm, runner rotational line Speed is 25m/s;
E, alloy Cast Strip is put into the closed container for fill dry ice and places 30min;The dry ice quality is alloy Cast Strip 6%;The dry ice is cylindric, a diameter of 4mm, length 5-12mm;Then the taking-up of alloy Cast Strip is put into hydrogen crushing furnace to enter The broken obtained alloy coarse powder of row hydrogen, the hydrogen crushing furnace reative cell vacuum are 0.08Pa, and air pressure is 1atm in hydrogen crushing furnace, in-furnace temperature For 300 DEG C, the hydrogen broken time is 75min;
F, alloy coarse powder is put into airflow milling and ground, the alloy fine powder that granularity is 2~5 μm is made, as permanent magnetism The alloy I of material;The airflow milling powder pressure is 7atm.
The preparation method step of the alloy II includes:
A, it is Ce15%, Bi0.02%, B3%, P0.06%, Pt0.06% by alloy raw material Ingredients Weight percentage composition, Be 0.02%, surplus are that Fe carries out dispensing;Ce, Bi, P, Pt, Be, Fe are pure material (content is more than 99.9%), and the B is with boron The form of iron intermediate alloy adds, and B weight/mass percentage composition is 24% in ferro-boron intermediate alloy.
B, raw material is heated to 1580 DEG C of meltings, then cast obtains mother alloy ingot;The melting is in electric arc furnaces copper earthenware Melting in crucible, constantly aluminium alloy is stirred with electric arc in fusion process, it is fully melted uniformly;
Mother alloy ingot is heated to 1550 DEG C of fusings in induction furnace, obtain foundry alloy liquid C,;
The method that foundry alloy liquid is got rid of to band in vacuum rapid hardening spun furnace by vacuum rapid hardening prepares alloy Cast Strip D,;Institute State remelting tubular type crucible bottom in vacuum rapid hardening spun furnace and be provided with through hole, remelting tubular type crucible top connects nitrogen, nitrogen through valve The pressure of gas is 1.6 atmospheric pressure;The bottom of remelting tubular type crucible is placed on forming furnace runner wheel rim at 3mm, works as foundry alloy After fusing, the valve on remelting tubular type crucible top is opened, melting foundry alloy sprays from the through hole of crucible bottom under nitrogen pressure To the forming furnace runner wheel rim of rotation, continuous alloy strip (15~17 microns of alloy tape thickness, 8~13mm of width) is formed;Weight Fusion tube type crucible internal diameter is 13mm, is highly 260mm, and the through-hole aperture of remelting tubular type crucible bottom is 1.5mm, runner rotational line Speed is 28m/s;
E, alloy Cast Strip is put into the closed container for fill dry ice and places 45min;The dry ice quality is alloy Cast Strip 8%;The dry ice is cylindric, a diameter of 4mm, length 5-12mm;Then the taking-up of alloy Cast Strip is put into hydrogen crushing furnace to enter The broken obtained alloy coarse powder of row hydrogen, the hydrogen crushing furnace reative cell vacuum are 0.06Pa, and air pressure is 1atm in hydrogen crushing furnace, temperature in stove Spend for 300 DEG C, the hydrogen broken time is 75min;
F, alloy coarse powder is put into airflow milling and ground, the alloy fine powder that granularity is 1~8 μm is made, as permanent magnetism The alloy II of material;The airflow milling powder pressure is 7atm.
The preparation method step of the alloy III includes:
A, it is La5%, P0.04%, B0.2%, Al5%, Si7% by alloy raw material Ingredients Weight percentage composition, surplus is Fe carries out dispensing;La, P, Al, Si, Fe are pure material (content is more than 99.9%), and the B is added in the form of ferro-boron intermediate alloy Enter, B weight/mass percentage composition is 22% in ferro-boron intermediate alloy;
B, raw material is heated to 1480 DEG C of meltings, then cast obtains mother alloy ingot;The melting is in electric arc furnaces copper earthenware Melting in crucible, constantly aluminium alloy is stirred with electric arc in fusion process, it is fully melted uniformly;
Mother alloy ingot is heated to 1430 DEG C of fusings in induction furnace, obtain foundry alloy liquid C,;
The method that foundry alloy liquid is got rid of to band in vacuum rapid hardening spun furnace by vacuum rapid hardening prepares alloy Cast Strip D,;Institute State remelting tubular type crucible bottom in vacuum rapid hardening spun furnace and be provided with through hole, remelting tubular type crucible top connects nitrogen, nitrogen through valve The pressure of gas is 1.6 atmospheric pressure;The bottom of remelting tubular type crucible is placed on forming furnace runner wheel rim at 3mm, works as foundry alloy After fusing, the valve on remelting tubular type crucible top is opened, melting foundry alloy sprays from the through hole of crucible bottom under nitrogen pressure To the forming furnace runner wheel rim of rotation, form continuous alloy strip (3~5 millimeters of alloy tape thickness, width are 5~12mm);Weight Fusion tube type crucible internal diameter is 13mm, is highly 260mm, and the through-hole aperture of remelting tubular type crucible bottom is 1.5mm, runner rotational line Speed is 24m/s;
E, fused salt is prepared:It is 0.1: 1: 1 by CaCl2, KCl, NaF, CsF mol ratio:0.06 weighs each constituent element, after mixing Fused-salt medium is obtained, the 12% powdery monocrystalline silicon for accounting for fused-salt medium quality is added, is ground (CaCl2, NaCl, NaF, CsF Purity with powdery monocrystalline silicon is 99.99%, and each material first is dried into 8h at 200 DEG C before preparing);
F, fused salt is put into salt bath furnace, is heated to 730 DEG C, constant temperature 30min, is then done with the silicon steel sheet containing 4.5%Si Negative electrode is immersed in liquid fused salt, is immersed using alloy Cast Strip as anode in liquid fused salt and is led to direct current to alloy Cast Strip progress Permeation in Electroplating Silicon;The logical direct current is given electrically for pulse, average current density 60mA/cm2;The alloy Cast Strip in fused salt with 0.12m/min gait of march carries out uniform motion, and it is 25min to be kept for residence time of the alloy Cast Strip every in fused salt;
G, the alloy Cast Strip after siliconising is put into progress mechanical ball mill to alloy powder particle diameter in ball grinder and reaches 7-11 μm, The alloy III for permanent-magnet material is made.
The preparation method step of the inorganic composite materials IV includes:
A, by inorganic composite materials material composition weight percentage SrO 2%, BaO 2%, K2O 0.1%, Mn2O30.5%, Pb3O40.3%, Sb2O50.3%, PbO20.1%, surplus Fe2O3Carry out dispensing;Each raw material components purity is equal More than 99.9%;
B, dry after the raw material prepared being carried out into mixing and breaking up in sand mill, then sieve;The screen cloth of the sieving For 200 mesh;The drying temperature is 120 DEG C, drying time 1.5h;
C, the raw material after sieving is put into sintering furnace and be sintered, sintering temperature is 1150 DEG C, soaking time 1.5h;
D, sintered product is ground to particle diameter 10-13 microns in grinder, that is, be made for the inorganic multiple of permanent-magnet material Condensation material IV.
A kind of preparation method of permanent-magnet alloy, step include:
A, by permanent-magnet alloy raw alloy material I, II, III and inorganic composite materials IV mass ratio 1:1:0.2: 0.01 dispensing, it is added in three-dimensional mixer and is well mixed, mixed powder is made;
B, mixed powder is orientated in Magnetic field press, be molded (pressure 150KN, pressurize 15 seconds) with Bidirectional pressure mode;
C, molded blank is entered into sintering furnace in argon gas protection down to be sintered, is first warming up to 700 DEG C, be incubated 3h, then 1160 DEG C of sintering 3h are warming up to, are cooled to room temperature;
D, Ageing Treatment is carried out after the molded blank after sintering being carried out into double tempering processing, obtained permanent-magnet alloy is made; The temperature of the double tempering processing is respectively 900 DEG C, and 550 DEG C, soaking time is respectively 1h, 1.5h;The Ageing Treatment Temperature is 240 DEG C, soaking time 12h.
Embodiment 2
A kind of permanent-magnet alloy, its raw material are combined by alloy I, II, III and inorganic composite materials IV, the alloy material I, II, III and inorganic composite materials IV mass ratio are 1:1.5:0.6:0.01;
Described its material composition of alloy I and weight percentage are:Cr 1.3%, Ta 7%, Ge 0.7%, Ti 0.6%, Sn 0.9%, B 6%, Nd 25%, surplus Fe;The B is added in the form of ferro-boron intermediate alloy, among ferro-boron B weight/mass percentage composition is 24% in alloy;
Described its material composition of alloy II and weight percentage are:Ce 20%, Bi 00.06%, P 0.12%, Pt 0.10%, Be 0.07%, B 6%, surplus Fe;The B is added in the form of ferro-boron intermediate alloy, in ferro-boron intermediate alloy B weight/mass percentage composition is 24%;
Described its material composition of alloy III and weight percentage are:La 8%, P 0.08%, B 0.6%, Al 8%, Si 11%, surplus Fe;The B is added in the form of ferro-boron intermediate alloy, B weight/mass percentage composition in ferro-boron intermediate alloy For 22%;
Described its material composition of inorganic composite materials IV and weight percentage are:SrO 6%, BaO 7%, K2O 0.5%, Mn2O31.2%, Pb3O40.7%, Sb2O50.8%, PbO20.4%, surplus Fe2O3
The preparation method step of the alloy I includes:
A, it is Cr 1.3%, Ta 7%, Ge 0.7%, Ti 0.6%, Sn by alloy raw material Ingredients Weight percentage composition 0.9%, B 6%, Nd 25%, surplus are that Fe carries out dispensing, and Cr, Ta, Ge, Ti, Sn, Nd, Fe are that (content is more than pure material 99.9%);B is added in the form of ferro-boron intermediate alloy, and B weight/mass percentage composition is 24% in ferro-boron intermediate alloy.
B, raw material is heated to 1590 DEG C of meltings, then cast obtains mother alloy ingot;The melting is in electric arc furnaces copper earthenware Melting in crucible, constantly aluminium alloy is stirred with electric arc in fusion process, it is fully melted uniformly;
Mother alloy ingot is heated to 1550 DEG C of fusings in induction furnace, obtain foundry alloy liquid C,;
The method that foundry alloy liquid is got rid of to band in vacuum rapid hardening spun furnace by vacuum rapid hardening prepares alloy Cast Strip D,;Institute State remelting tubular type crucible bottom in vacuum rapid hardening spun furnace and be provided with through hole, remelting tubular type crucible top connects nitrogen, nitrogen through valve The pressure of gas is 1.6 atmospheric pressure;The bottom of remelting tubular type crucible is placed on forming furnace runner wheel rim at 3mm, works as foundry alloy After fusing, the valve on remelting tubular type crucible top is opened, melting foundry alloy sprays from the through hole of crucible bottom under nitrogen pressure To the forming furnace runner wheel rim of rotation, continuous alloy strip (17~20 microns of alloy tape thickness, 8~13mm of width) is formed;Weight Fusion tube type crucible internal diameter is 13mm, is highly 260mm, and the through-hole aperture of remelting tubular type crucible bottom is 1.5mm, runner rotational line Speed is 25m/s;
E, alloy Cast Strip is put into the closed container for fill dry ice and places 50min;The dry ice quality is alloy Cast Strip 10%;The dry ice is cylindric, a diameter of 4mm, length 5-12mm;Then the taking-up of alloy Cast Strip is put into hydrogen crushing furnace to enter The broken obtained alloy coarse powder of row hydrogen, the hydrogen crushing furnace reative cell vacuum are 0.07Pa, and air pressure is 1.2atm in hydrogen crushing furnace, temperature in stove Spend for 290 DEG C, the hydrogen broken time is 75min;
F, alloy coarse powder is put into airflow milling and ground, the alloy fine powder that granularity is 2~5 μm is made, as permanent magnetism The alloy I of material;The airflow milling powder pressure is 6atm.
The preparation method step of the alloy II includes:
A, it is Ce 20%, Bi 00.06%, B 6%, P 0.12%, Pt by alloy raw material Ingredients Weight percentage composition 0.10%, Be 0.07%, surplus are that Fe carries out dispensing;Ce, Bi, P, Pt, Be, Fe are pure material (content is more than 99.9%), The B is added in the form of ferro-boron intermediate alloy, and B weight/mass percentage composition is 24% in ferro-boron intermediate alloy.
B, raw material is heated to 1580 DEG C of meltings, then cast obtains mother alloy ingot;The melting is in electric arc furnaces copper earthenware Melting in crucible, constantly aluminium alloy is stirred with electric arc in fusion process, it is fully melted uniformly;
Mother alloy ingot is heated to 1520 DEG C of fusings in induction furnace, obtain foundry alloy liquid C,;
The method that foundry alloy liquid is got rid of to band in vacuum rapid hardening spun furnace by vacuum rapid hardening prepares alloy Cast Strip D,;Institute State remelting tubular type crucible bottom in vacuum rapid hardening spun furnace and be provided with through hole, remelting tubular type crucible top connects nitrogen, nitrogen through valve The pressure of gas is 1.6 atmospheric pressure;The bottom of remelting tubular type crucible is placed on forming furnace runner wheel rim at 3mm, works as foundry alloy After fusing, the valve on remelting tubular type crucible top is opened, melting foundry alloy sprays from the through hole of crucible bottom under nitrogen pressure To the forming furnace runner wheel rim of rotation, continuous alloy strip (15~17 microns of alloy tape thickness, 8~13mm of width) is formed;Weight Fusion tube type crucible internal diameter is 13mm, is highly 260mm, and the through-hole aperture of remelting tubular type crucible bottom is 1.5mm, runner rotational line Speed is 28m/s;
E, alloy Cast Strip is put into the closed container for fill dry ice and places 12min;The dry ice quality is alloy Cast Strip 8%;The dry ice is cylindric, a diameter of 4mm, length 5-12mm;Then the taking-up of alloy Cast Strip is put into hydrogen crushing furnace to enter The broken obtained alloy coarse powder of row hydrogen, the hydrogen crushing furnace reative cell vacuum are 0.07Pa, and air pressure is 1.2atm in hydrogen crushing furnace, in stove Temperature is 290 DEG C, and the hydrogen broken time is 75min;
F, alloy coarse powder is put into airflow milling and ground, the alloy fine powder that granularity is 1~8 μm is made, as permanent magnetism The alloy II of material;The airflow milling powder pressure is 6atm.
The preparation method step of the alloy III includes:
A, it is La 8%, P 0.08%, B 0.6%, Al 8%, Si 11% by alloy raw material Ingredients Weight percentage composition, Surplus is that Fe carries out dispensing;La, P, Al, Si, Fe are pure material (content is more than 99.9%), and the B is with ferro-boron intermediate alloy Form adds, and B weight/mass percentage composition is 22% in ferro-boron intermediate alloy;
B, raw material is heated to 1470 DEG C of meltings, then cast obtains mother alloy ingot;The melting is in electric arc furnaces copper earthenware Melting in crucible, constantly aluminium alloy is stirred with electric arc in fusion process, it is fully melted uniformly;
Mother alloy ingot is heated to 1440 DEG C of fusings in induction furnace, obtain foundry alloy liquid C,;
The method that foundry alloy liquid is got rid of to band in vacuum rapid hardening spun furnace by vacuum rapid hardening prepares alloy Cast Strip D,;Institute State remelting tubular type crucible bottom in vacuum rapid hardening spun furnace and be provided with through hole, remelting tubular type crucible top connects nitrogen, nitrogen through valve The pressure of gas is 1.6 atmospheric pressure;The bottom of remelting tubular type crucible is placed on forming furnace runner wheel rim at 3mm, works as foundry alloy After fusing, the valve on remelting tubular type crucible top is opened, melting foundry alloy sprays from the through hole of crucible bottom under nitrogen pressure To the forming furnace runner wheel rim of rotation, form continuous alloy strip (3~5 millimeters of alloy tape thickness, width are 5~12mm);Weight Fusion tube type crucible internal diameter is 13mm, is highly 260mm, and the through-hole aperture of remelting tubular type crucible bottom is 1.5mm, runner rotational line Speed is 26m/s;
E, fused salt is prepared:It is 0.1 by CaCl2, KCl, NaF, CsF mol ratio:1:1:0.08 weighs each constituent element, after mixing Obtain fused-salt medium, add the 13% powdery monocrystalline silicon for accounting for fused-salt medium quality, be ground (CaCl2, NaCl, NaF, The purity of CsF and powdery monocrystalline silicon is 99.99%, and each material first is dried into 8h at 200 DEG C before preparing);
F, fused salt is put into salt bath furnace, is heated to 700 DEG C, constant temperature 30min, is then done with the silicon steel sheet containing 4.5%Si Negative electrode is immersed in liquid fused salt, is immersed using alloy Cast Strip as anode in liquid fused salt and is led to direct current to alloy Cast Strip progress Permeation in Electroplating Silicon;The logical direct current is given electrically for pulse, average current density 58mA/cm2;The alloy Cast Strip in fused salt with 0.12m/min gait of march carries out uniform motion, and it is 20min to be kept for residence time of the alloy Cast Strip every in fused salt;
G, the alloy Cast Strip after siliconising is put into progress mechanical ball mill to alloy powder particle diameter in ball grinder and reaches 7-11 μm, The alloy III for permanent-magnet material is made.
The preparation method step of the inorganic composite materials IV includes:
A, by inorganic composite materials material composition weight percentage SrO 6%, BaO 7%, K2O 0.5%, Mn2O31.2%, Pb3O40.7%, Sb2O50.8%, PbO20.4%, surplus Fe2O3Carry out dispensing;Each raw material components purity is equal More than 99.9%;
B, dry after the raw material prepared being carried out into mixing and breaking up in sand mill, then sieve;The screen cloth of the sieving For 200 mesh;The drying temperature is 110 DEG C, drying time 1.5h;
C, the raw material after sieving is put into sintering furnace and be sintered, sintering temperature is 1250 DEG C, soaking time 1.5h;
D, sintered product is ground to particle diameter 10-13 microns in grinder, that is, be made for the inorganic multiple of permanent-magnet material Condensation material IV.
A kind of preparation method of permanent-magnet alloy, step include:
A, by permanent-magnet alloy raw alloy material I, II, III and inorganic composite materials IV mass ratio 1:1.5:0.6: 0.01 dispensing, it is added in three-dimensional mixer and is well mixed, mixed powder is made;
B, mixed powder is orientated in Magnetic field press, be molded (pressure 150KN, pressurize 20 seconds) with Bidirectional pressure mode;
C, molded blank is entered into sintering furnace in argon gas protection down to be sintered, is first warming up to 550 DEG C, be incubated 4h, then 1180 DEG C of sintering 3h are warming up to, are cooled to room temperature;
D, Ageing Treatment is carried out after the molded blank after sintering being carried out into double tempering processing, obtained permanent-magnet alloy is made; The temperature of the double tempering processing is respectively 910 DEG C, and 560 DEG C, soaking time is respectively 1.0h, 1.5h;The Ageing Treatment Temperature be 220 DEG C, soaking time 15h.
Embodiment 3
A kind of permanent-magnet alloy, its raw material are combined by alloy I, II, III and inorganic composite materials IV, the alloy material I, II, III and inorganic composite materials IV mass ratio are 1:1.3:0.4:0.01;
Described its material composition of alloy I and weight percentage are:Cr0.9%, Ta 5%, Ge 0.5%, Ti 0.4%, Sn0.7%, B5%, Nd23%, surplus Fe;The B is added in the form of ferro-boron intermediate alloy, B in ferro-boron intermediate alloy Weight/mass percentage composition is 24%;
Described its material composition of alloy II and weight percentage are:Ce18%, Bi 0.04%, B4%, P0.09%, Pt0.08%, Be 0.05%, surplus Fe;The B is added in the form of ferro-boron intermediate alloy, B in ferro-boron intermediate alloy Weight/mass percentage composition is 24%;
Described its material composition of alloy III and weight percentage are:La 5%, P0.06%, B0.4%, Al 6%, Si9%, surplus Fe;The B is added in the form of ferro-boron intermediate alloy, and B weight/mass percentage composition is in ferro-boron intermediate alloy 22%;
Described its material composition of inorganic composite materials IV and weight percentage are:SrO 4%, BaO 5%, K2O 0.3%, Mn2O30.9%, Pb3O40.5%, Sb2O50.5%, PbO20.2%, surplus Fe2O3
The preparation method step of the alloy I includes:
A, it is Cr0.9%, Ta 5%, Ge 0.5%, Ti 0.4%, Sn0.7% by alloying component weight percentage, B5%, Nd23%, surplus are that Fe carries out dispensing, and Cr, Ta, Ge, Ti, Sn, Nd, Fe are pure material (content is more than 99.9%); B Added in the form of ferro-boron intermediate alloy, B weight/mass percentage composition is 24% in ferro-boron intermediate alloy.
B, raw material is heated to 1590 DEG C of meltings, then cast obtains mother alloy ingot;The melting is in electric arc furnaces copper earthenware Melting in crucible, constantly aluminium alloy is stirred with electric arc in fusion process, it is fully melted uniformly;
Mother alloy ingot is heated to 1550 DEG C of fusings in induction furnace, obtain foundry alloy liquid C,;
The method that foundry alloy liquid is got rid of to band in vacuum rapid hardening spun furnace by vacuum rapid hardening prepares alloy Cast Strip D,;Institute State remelting tubular type crucible bottom in vacuum rapid hardening spun furnace and be provided with through hole, remelting tubular type crucible top connects nitrogen, nitrogen through valve The pressure of gas is 1.6 atmospheric pressure;The bottom of remelting tubular type crucible is placed on forming furnace runner wheel rim at 3mm, works as foundry alloy After fusing, the valve on remelting tubular type crucible top is opened, melting foundry alloy sprays from the through hole of crucible bottom under nitrogen pressure To the forming furnace runner wheel rim of rotation, continuous alloy strip (17~20 microns of alloy tape thickness, 8~13mm of width) is formed;Weight Fusion tube type crucible internal diameter is 13mm, is highly 260mm, and the through-hole aperture of remelting tubular type crucible bottom is 1.5mm, runner rotational line Speed is 25m/s;
E, alloy Cast Strip is put into the closed container for fill dry ice and places 40min;The dry ice quality is alloy Cast Strip 7%;The dry ice is cylindric, a diameter of 4mm, length 5-12mm;Then the taking-up of alloy Cast Strip is put into hydrogen crushing furnace to enter The broken obtained alloy coarse powder of row hydrogen, the hydrogen crushing furnace reative cell vacuum are 0.07Pa, and air pressure is 1.2atm in hydrogen crushing furnace, temperature in stove Spend for 300 DEG C, the hydrogen broken time is 75min;
F, alloy coarse powder is put into airflow milling and ground, the alloy fine powder that granularity is 2~5 μm is made, as permanent magnetism The alloy I of material;The airflow milling powder pressure is 6atm.
The preparation method step of the alloy II includes:
A, it is Ce18%, Bi 0.04%, B4%, P0.09%, Pt0.08% by alloy raw material Ingredients Weight percentage composition, Be 0.05%, surplus are that Fe carries out dispensing;Ce, Bi, P, Pt, Be, Fe are pure material (content is more than 99.9%), and the B is with boron The form of iron intermediate alloy adds, and B weight/mass percentage composition is 24% in ferro-boron intermediate alloy.
B, raw material is heated to 1580 DEG C of meltings, then cast obtains mother alloy ingot;The melting is in electric arc furnaces copper earthenware Melting in crucible, constantly aluminium alloy is stirred with electric arc in fusion process, it is fully melted uniformly;
Mother alloy ingot is heated to 1530 DEG C of fusings in induction furnace, obtain foundry alloy liquid C,;
The method that foundry alloy liquid is got rid of to band in vacuum rapid hardening spun furnace by vacuum rapid hardening prepares alloy Cast Strip D,;Institute State remelting tubular type crucible bottom in vacuum rapid hardening spun furnace and be provided with through hole, remelting tubular type crucible top connects nitrogen, nitrogen through valve The pressure of gas is 1.6 atmospheric pressure;The bottom of remelting tubular type crucible is placed on forming furnace runner wheel rim at 3mm, works as foundry alloy After fusing, the valve on remelting tubular type crucible top is opened, melting foundry alloy sprays from the through hole of crucible bottom under nitrogen pressure To the forming furnace runner wheel rim of rotation, continuous alloy strip (15~17 microns of alloy tape thickness, 8~13mm of width) is formed;Weight Fusion tube type crucible internal diameter is 13mm, is highly 260mm, and the through-hole aperture of remelting tubular type crucible bottom is 1.5mm, runner rotational line Speed is 28m/s;
E, alloy Cast Strip is put into the closed container for fill dry ice and places 30min;The dry ice quality is alloy Cast Strip 8%;The dry ice is cylindric, a diameter of 4mm, length 5-12mm;Then the taking-up of alloy Cast Strip is put into hydrogen crushing furnace to enter The broken obtained alloy coarse powder of row hydrogen, the hydrogen crushing furnace reative cell vacuum are 0.07Pa, and air pressure is 1.2atm in hydrogen crushing furnace, in stove Temperature is 2900 DEG C, and the hydrogen broken time is 75min;
F, alloy coarse powder is put into airflow milling and ground, the alloy fine powder that granularity is 1~8 μm is made, as permanent magnetism The alloy II of material;The airflow milling powder pressure is 6atm.
The preparation method step of the alloy III includes:
A, it is La 5%, P0.06%, B0.4% by alloy raw material Ingredients Weight percentage composition, Al 6%, Si9%, surplus Dispensing is carried out for Fe;La, P, Al, Si, Fe are pure material (content is more than 99.9%), and the B is in the form of ferro-boron intermediate alloy Add, B weight/mass percentage composition is 22% in ferro-boron intermediate alloy;
B, raw material is heated to 1480 DEG C of meltings, then cast obtains mother alloy ingot;The melting is in electric arc furnaces copper earthenware Melting in crucible, constantly aluminium alloy is stirred with electric arc in fusion process, it is fully melted uniformly;
Mother alloy ingot is heated to 1420 DEG C of fusings in induction furnace, obtain foundry alloy liquid C,;
The method that foundry alloy liquid is got rid of to band in vacuum rapid hardening spun furnace by vacuum rapid hardening prepares alloy Cast Strip D,;Institute State remelting tubular type crucible bottom in vacuum rapid hardening spun furnace and be provided with through hole, remelting tubular type crucible top connects nitrogen, nitrogen through valve The pressure of gas is 1.6 atmospheric pressure;The bottom of remelting tubular type crucible is placed on forming furnace runner wheel rim at 3mm, works as foundry alloy After fusing, the valve on remelting tubular type crucible top is opened, melting foundry alloy sprays from the through hole of crucible bottom under nitrogen pressure To the forming furnace runner wheel rim of rotation, form continuous alloy strip (3~5 millimeters of alloy tape thickness, width are 5~12mm);Weight Fusion tube type crucible internal diameter is 13mm, is highly 260mm, and the through-hole aperture of remelting tubular type crucible bottom is 1.5mm, runner rotational line Speed is m/s;
E, fused salt is prepared:It is 0.1 by CaCl2, KCl, NaF, CsF mol ratio:1:1:0.06 weighs each constituent element, after mixing Obtain fused-salt medium, add the 13% powdery monocrystalline silicon for accounting for fused-salt medium quality, be ground (CaCl2, NaCl, NaF, The purity of CsF and powdery monocrystalline silicon is 99.99%, and each material first is dried into 8h at 200 DEG C before preparing);
F, fused salt is put into salt bath furnace, is heated to 750 DEG C, constant temperature 30min, is then done with the silicon steel sheet containing 4.5%Si Negative electrode is immersed in liquid fused salt, is immersed using alloy Cast Strip as anode in liquid fused salt and is led to direct current to alloy Cast Strip progress Permeation in Electroplating Silicon;The logical direct current is given electrically for pulse, average current density 65mA/cm2;The alloy Cast Strip in fused salt with 0.11m/min gait of march carries out uniform motion, and it is 20min to be kept for residence time of the alloy Cast Strip every in fused salt;
G, the alloy Cast Strip after siliconising is put into progress mechanical ball mill to alloy powder particle diameter in ball grinder and reaches 7-11 μm, The alloy III for permanent-magnet material is made.
The preparation method step of the inorganic composite materials IV includes:
A, by inorganic composite materials material composition weight percentage SrO 4%, BaO 5%, K2O 0.3%, Mn2O30.9%, Pb3O40.5%, Sb2O50.5%, PbO20.2%, surplus Fe2O3Carry out dispensing;Each raw material components purity is equal More than 99.9%;
B, dry after the raw material prepared being carried out into mixing and breaking up in sand mill, then sieve;The screen cloth of the sieving For 200 mesh;The drying temperature is 110 DEG C, drying time 1.5h;
C, the raw material after sieving is put into sintering furnace and be sintered, sintering temperature is 1250 DEG C, soaking time 1.5h;
D, sintered product is ground to particle diameter 10-13 microns in grinder, that is, be made for the inorganic multiple of permanent-magnet material Condensation material IV.
A kind of preparation method of permanent-magnet alloy, step include:
A, by permanent-magnet alloy raw alloy material I, II, III and inorganic composite materials IV mass ratio 1:1.3:0.4: 0.01 dispensing, it is added in three-dimensional mixer and is well mixed, mixed powder is made;
B, mixed powder is orientated in Magnetic field press, be molded (pressure 150KN, pressurize 15 seconds) with Bidirectional pressure mode;
C, molded blank is entered into sintering furnace in argon gas protection down to be sintered, is first warming up to 550 DEG C, be incubated 4h, then 1180 DEG C of sintering 3h are warming up to, are cooled to room temperature;
D, Ageing Treatment is carried out after the molded blank after sintering being carried out into double tempering processing, obtained permanent-magnet alloy is made; The temperature of the double tempering processing is respectively 910 DEG C, and 560 DEG C, soaking time is respectively 1h, 1.5h;The Ageing Treatment Temperature is 220 DEG C, soaking time 24h.
Permanent-magnet alloy performance prepared by embodiment 1-3 is as shown in table 1:
Table 1 implements permanent-magnet alloy mechanical property prepared by embodiment 1-3
Embodiment 1 2 3
Coercivity (kOe) 24 27 26

Claims (7)

1. a kind of alloy II for permanent-magnet material, its material composition and weight percentage are:Ce15~20%, Bi 0.02%~0.06%, P0.06%~0.12%, Pt0.06%~0.10%, Be 0.02%~0.07%, B2~6% are remaining Measure as Fe.
2. alloy I as claimed in claim 1, it is characterised in that:The B is added in the form of ferro-boron intermediate alloy, in ferro-boron Between in alloy B weight/mass percentage composition be 20-25%.
3. the preparation method of alloy II for permanent-magnet material a kind of, step include:
A, it is Ce15~20%, Bi 0.02%~0.06%, B3~6% by alloying component weight percentage, P0.06%~ 0.12%, Pt0.06%~0.10%, Be 0.02%~0.07%, surplus are that Fe carries out dispensing;The B is with conjunction among ferro-boron The form of gold adds, and B weight/mass percentage composition is 20-25% in ferro-boron intermediate alloy.
B, raw material is heated to 1570-1590 DEG C of melting, then cast obtains mother alloy ingot;The melting is in electric arc furnaces copper earthenware Melting in crucible, constantly aluminium alloy is stirred with electric arc in fusion process, it is fully melted uniformly;
Mother alloy ingot is heated to 1500~1560 DEG C of fusings in induction furnace, obtain foundry alloy liquid C,;
The method that foundry alloy liquid is got rid of to band in vacuum rapid hardening spun furnace by vacuum rapid hardening prepares alloy Cast Strip D,;
E, alloy Cast Strip is put into placement more than 8min in the closed container for fill dry ice;The dry ice quality is alloy Cast Strip 5-10%;Then alloy Cast Strip is taken out and is put into the hydrogen crushing furnace progress broken obtained alloy coarse powder of hydrogen, the hydrogen crushing furnace reative cell vacuum To spend for 0.06~0.1Pa, air pressure is 0.8~1.3atm in hydrogen crushing furnace, and in-furnace temperature is 260~310 DEG C, the hydrogen broken time is 70~ 80min。
4. preparation method as claimed in claim 3, it is characterised in that:
Also include step after the step E processed
F, alloy coarse powder is put into airflow milling and ground, the alloy fine powder that granularity is 1~8 μm is made, as permanent-magnet material Alloy II;The airflow milling powder pressure is 6~7atm.
5. preparation method as claimed in claim 3, it is characterised in that:
15~17 microns of the alloy tape thickness prepared described in the step D, 8~13mm of width.
6. preparation method as claimed in claim 3, it is characterised in that:Alloy Cast Strip is put into the step E and fills dry ice Closed container in place 30-50min.
7. preparation method as claimed in claim 3, it is characterised in that:The dry ice is cylindric, a diameter of 4mm, and length is 5-12mm。
CN201710844253.0A 2017-09-15 2017-09-15 A kind of alloy for permanent-magnet material and preparation method thereof Pending CN107686947A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108922712A (en) * 2018-08-16 2018-11-30 安徽信息工程学院 Magnetic composite and preparation method thereof

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CN1033900A (en) * 1987-12-26 1989-07-12 中国科学院三环新材料研究开发公司 Mishmetal-iron-base permanent magnetic material and preparation method thereof
CN1066146A (en) * 1991-04-20 1992-11-11 北京科技大学 The preparation method of rare-earth-iron-boron permanent-magnet powder
US6302939B1 (en) * 1999-02-01 2001-10-16 Magnequench International, Inc. Rare earth permanent magnet and method for making same
CN105913989A (en) * 2016-04-22 2016-08-31 山西三益强磁业股份有限公司 High-remanence material and preparation method

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CN1033900A (en) * 1987-12-26 1989-07-12 中国科学院三环新材料研究开发公司 Mishmetal-iron-base permanent magnetic material and preparation method thereof
CN1066146A (en) * 1991-04-20 1992-11-11 北京科技大学 The preparation method of rare-earth-iron-boron permanent-magnet powder
US6302939B1 (en) * 1999-02-01 2001-10-16 Magnequench International, Inc. Rare earth permanent magnet and method for making same
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