CN107564653B - A kind of magnetic composite and preparation method thereof - Google Patents
A kind of magnetic composite and preparation method thereof Download PDFInfo
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- CN107564653B CN107564653B CN201710844219.3A CN201710844219A CN107564653B CN 107564653 B CN107564653 B CN 107564653B CN 201710844219 A CN201710844219 A CN 201710844219A CN 107564653 B CN107564653 B CN 107564653B
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Abstract
The present invention relates to a kind of magnetic composites, magnetic composite is combined by alloy I, II, III and inorganic composite materials IV, the mass ratio of described alloy I, II, III and inorganic composite materials IV are 1.5:0.8-1:0.2-0.5:0.03, preparation method step includes ingredient, compression moulding, sintering, heat treatment, magnetic composite of the present invention has thermal stability good, and has good magnetic property, the preparation method simple process of permanent-magnet alloy, production cost is low, is suitable for industrialized production.
Description
Technical field
The invention belongs to magnetic field of material technology, and in particular to a kind of magnetic composite and preparation method thereof.
Background technique
CN201611158469.3 provide a kind of low heavy rare earth, high-coercive force permanent-magnet material preparation method, packet
Include and carry out mixing heat treatment with heavy rare earth metal or alloy powder by rare-earth iron-boron alloy powder, heat treatment while constantly into
Row stirring, makes heavy rare earth metal atom diffuse into the surface layer of rare-earth iron-boron alloy powder, obtains mixture；Mixture is placed in
Green compact is made through being orientated die mould in the magnetic field 1.5T or more；Green compact is prepared into sintered rare earth, iron boron forever through high temperature sintering and tempering
Magnetic material.But comprehensive performance is not high.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of magnetic composite and preparation method thereof, the magnetic coupling
Material has thermal stability good, and has good magnetic property, the preparation method simple process of magnetic composite, production cost
It is low, it is suitable for industrialized production.
The technical solution adopted by the present invention is that:
A kind of magnetic composite, raw material is composed of alloy I, II, III and inorganic composite materials IV, described
The mass ratio of alloy I, II, III and inorganic composite materials IV are 1.5:0.8-1:0.2-0.5:0.03；
Described its material composition of alloy I and weight percentage are as follows: Bi0.7~1.2%, Si0.5~0.9%, Ga 0.03
~0.08%, Sb0.01~0.04%, Sc0.05~0.09%, B2~5%, Nd20~24%, surplus Fe；The B is with boron
The form of iron intermediate alloy is added, and the mass percentage of B is 20-25% in ferro-boron intermediate alloy；
Described its material composition of alloy II and weight percentage are as follows: La12~17%, B3~6%, Pb0.02%~
0.08%, V0.03%~0.08%, Os0.03%~0.08%, Au0.001%~0.004%, Be 0.05%~0.09%,
Surplus is Fe；The B is added in the form of ferro-boron intermediate alloy, and the mass percentage of B is 20- in ferro-boron intermediate alloy
25%；
The alloy III, material composition and weight percentage are as follows: Eu2~6%, Al 5~9%, Si5~10%,
Surplus is Fe；
Described its ingredient of inorganic composite materials IV and weight percentage are as follows: Li2O 0.1-0.4%, BaO 3~8%,
Cu2O 0.3-0.8%, Fe3O40.1-0.4%, SiO20.1-0.4%, V2O50.1-0.5%, Sb2O50.2-0.6%, surplus
For Fe2O3。
The preparation method step of the alloy I includes:
A, by alloying component weight percentage be Bi0.7~1.2%, Si0.5~0.9%, Ga 0.03~0.08%,
Sb0.01~0.04%, Sc0.05~0.09%, B2~5%, Nd20~24%, surplus are that Fe carries out ingredient；The B is with ferro-boron
The form of intermediate alloy is added, and the mass percentage of B is 20-25% in ferro-boron intermediate alloy.
B, 1550~1580 DEG C of meltings are heated the raw material to, then casting obtains mother alloy ingot；The melting is in electric arc
Melting in furnace copper crucible constantly stirs aluminium alloy with electric arc in fusion process, melts it sufficiently uniformly；
C, mother alloy ingot is heated to 1510-1540 DEG C of fusing in induction furnace, obtains master alloy liquid；
D, master alloy liquid is prepared into alloy Cast Strip by the method that vacuum rapid hardening gets rid of band in vacuum rapid hardening spun furnace；Institute
17~20 microns of alloy tape thickness for stating preparation, 8~13mm of width；
E, alloy Cast Strip is put into placement 8min or more in the closed container for fill dry ice, preferably placement 30-50min；Institute
State the 5-10% that dry ice quality is alloy Cast Strip；The dry ice is cylindric, diameter 4mm, length 5-12mm；Then it 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 reaction chamber vacuum degree 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 is ground, the alloy fine powder that granularity is 2~5 μm is made, as magnetism
The alloy I of composite material；The airflow milling powder pressure is 6~7atm.
The preparation method step of the alloy II includes:
It A, is La12~17%, B3~6%, Pb0.02%~0.08%, V0.03% by alloying component weight percentage
~0.08%, Os0.03%~0.08%, Au0.001%~0.004%, Be 0.05%~0.09%, surplus are that Fe is matched
Material；The B is added in the form of ferro-boron intermediate alloy, and the mass percentage of B is 20-25% in ferro-boron intermediate alloy.
B, 1550~1580 DEG C of meltings are heated the raw material to, then casting obtains mother alloy ingot；The melting is in electric arc
Melting in furnace copper crucible constantly stirs aluminium alloy with electric arc in fusion process, melts it sufficiently uniformly；
C, mother alloy ingot is heated to 1510-1540 DEG C of fusing in induction furnace, obtains master alloy liquid；
D, master alloy liquid is prepared into alloy Cast Strip by the method that vacuum rapid hardening gets rid of band in vacuum rapid hardening spun furnace；Institute
15~17 microns of alloy tape thickness for stating preparation, 8~13mm of width；
E, alloy Cast Strip is put into placement 8min or more in the closed container for fill dry ice, preferably placement 30-50min；Institute
State the 5-10% that dry ice quality is alloy Cast Strip；The dry ice is cylindric, diameter 4mm, length 5-12mm；Then it 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 reaction chamber vacuum degree 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 is ground, the alloy fine powder that granularity is 1~8 μm is made, as magnetism
The alloy II of composite material；The airflow milling powder pressure is 6~7atm.
The preparation method step of the alloy III includes:
It A, is Eu2~6% by alloying component weight percentage, Al 5~9%, Si5~10%, surplus is that Fe is matched
Material；
B, 1450-1480 DEG C of melting is heated the raw material to, then casting obtains mother alloy ingot；The melting is in electric arc furnaces
Melting in copper crucible constantly stirs aluminium alloy with electric arc in fusion process, melts it sufficiently uniformly；
C, mother alloy ingot is heated to 1410-1440 DEG C of fusing in induction furnace, obtains master alloy liquid；
D, master alloy liquid is prepared into alloy Cast Strip by the method that vacuum rapid hardening gets rid of band in vacuum rapid hardening spun furnace；Institute
3~5 millimeters of alloy tape thickness for stating preparation, width are 5~12mm；
E, it prepares fused salt: pressing FeCl2、MgCl2、KCl、NaCl、NaF、BeF2Molar ratio be 0.1: 0.1: 1:3:1:
0.02-0.06 weighs each constituent element, and fused-salt medium is obtained after mixing, and the powdery that the 11%-15% for accounting for fused-salt medium quality is added is more
Crystal silicon is ground；
F, fused salt is put into salt bath furnace, is heated to 680-770 DEG C, then constant temperature 20-30min does cathode with silicon steel sheet
It immerses in liquid fused salt, logical direct current in liquid fused salt is immersed into as anode in alloy Cast Strip, plating siliconising is carried out to alloy Cast Strip；Institute
Stating logical direct current is pulse to electric mode, average current density 65-75mA/cm2；The alloy Cast Strip in fused salt with
The travel speed of 0.11-0.15m/min carries out uniform motion, and being kept for residence time of the alloy Cast Strip in fused salt is 25-
30min；The mass percentage of silicon is preferably 4-6% in the silicon steel sheet；
G, progress mechanical ball mill to alloy powder partial size in ball grinder will be put into after the alloy Cast Strip coarse crushing after siliconising to reach
To 7-11 μm, the alloy III for magnetic composite is obtained.
The preparation method step of the inorganic composite materials IV includes:
A, inorganic composite materials IV Ingredients Weight percentage composition Li is pressed2O 0.1-0.4%, BaO 3~8%, Cu2O 0.3-
0.8%, Fe3O40.1-0.4%, SiO20.1-0.4%, V2O50.1-0.5%, Sb2O50.2-0.6%, surplus Fe2O3Into
Row ingredient；
B, it dries after the raw material prepared being carried out mixing and breaking up in sand mill, is then sieved；The sieve of the sieving
For 180-220 mesh；The drying temperature is 110-120 DEG C, drying time 2-4h；
C, the raw material after sieving is put into sintering furnace and is sintered, sintering temperature is 1100-1250 DEG C, and soaking time is
2-4h；
D, sintered product is ground to 10-13 microns of partial size in grinder, obtains the nothing for magnetic composite
Machine composite material IV.
A kind of preparation method of magnetic composite, step include:
A, by the mass ratio 1.5 of magnetic composite raw alloy material I, II, III and inorganic composite materials IV:
0.8-1:0.2-0.5:0.03 ingredient is added in three-dimensional mixer and is uniformly mixed, and mixed powder is made；
B, mixed powder is orientated in Magnetic field press, compression moulding；The compression moulding is formed using Bidirectional pressure mode,
Pressure is 150KN, pressure maintaining 10-20S；
C, molded blank is put into sintering furnace to be sintered under protection of argon gas, is first warming up to 500-750 DEG C, keep the temperature 2-
4h then heats to 1150-1180 DEG C of sintering 2-4h, is cooled to room temperature；
D, ageing treatment is carried out after sintered molded blank being carried out double tempering processing, magnetic composite is made；
The temperature of double tempering processing is respectively 890-910 DEG C and 540-570 DEG C of soaking time is respectively 2-4h；At the timeliness
The temperature of reason is 210-250 DEG C, soaking time 20-40h.
Light rare earth forms main phase Nd2Fe14B and time main phase Eu2Fe14B, La2Fe14B in magnetic composite of the present invention
Apparent phase interface, enhances magnetic coupling interaction, so that the existing high coercivity of magnet is in turn avoided remanent magnetism and declines to a great extent, thus
Obtain higher comprehensive magnetic energy.Sb, Bi, Al and Be can reduce the angle of wetting of rich-Nd phase and main phase, inhibit growing up for main phase,
Reduce main phase interface defect density, magnetic reversal farmland is in interface forming core difficulty.Therefore the remanent magnetism of material is improved.
Si, Ga and Pb element can be distributed in around main phase grain to disperse, can be effectively improved the knot of tissue of Grain-Boundary Phase
Structure carries out crystal boundary modified, reinforcing Grain-Boundary Phase to magnet.
The metal oxide complex that inorganic composite materials are formed in magnetic composite is evenly distributed in crystal boundary and rises
To pinning effect, coercivity is improved.And itself be permanent-magnet ferrite, it can equally play enhancing product magnetic property
Effect.
During the sintering process, a small amount of high-melting point alloy element such as third transition system Os, Au is added, can make to analyse in magnet tissue
Cenotype out eliminates the phenomenon that directly contacting between main phase grain, effectively inhibits growing up for main phase grain, is conducive to obtain relatively fine
Uniform grain structure, while the thermal stability of main phase magnet can be improved.
The reason of Sc, V improvement intrinsic coercivity of First Transition system is the intercrystalline pair phase to be formed, and crystal grain is inhibited to cross
Growing up for place's particle, has refined main phase grain, therefore may refrain from the enhancing of their ambient stray fields, and then improves intrinsic rectify
Stupid power.
Products obtained therefrom of the present invention has excellent magnetic energy.Heavy rare earth element is not had in preparation, rare element dosage is few, other
Cost of material is lower；In addition preparing alloy in kind ensure that the uniform of alloying component, tissue and performance by being quickly cooled down
Property, it ensure that the quality of alloy.The alloy preparation technology is easy, and process is simple, and the alloy of production is with good performance, very
It is convenient for industrialized production.Permanent-magnet material prepared by the present invention is suitable for electrical apparatus industry.
Specific embodiment
Embodiment 1
A kind of magnetic composite, raw material is composed of alloy I, II, III and inorganic composite materials IV, described
The mass ratio of alloy material I, II, III and inorganic composite materials IV are 1.5:0.8:0.2:0.03；
Described its material composition of alloy I and weight percentage are as follows: Bi0.7%, Si0.5%, Ga 0.03%,
Sb0.01%, Sc0.05%, B2%, Nd20%, surplus Fe；The B is in the form of ferro-boron intermediate alloy (FeB23C0.05)
It is added, the mass percentage of B is 23% in ferro-boron intermediate alloy；
Described its material composition of alloy II and weight percentage are as follows: La12%, B3%, Pb0.02%, V0.03%,
Os0.03%, Au0.001%, Be 0.05%, surplus Fe；The B is added in the form of ferro-boron intermediate alloy, among ferro-boron
The mass percentage of B is 23% in alloy；
Described its material composition of alloy III and weight percentage are as follows: Eu2%, Al 5%, Si5%, surplus Fe；
Described its material composition of inorganic composite materials IV and weight percentage are as follows: Li2O 0.1%, BaO 3%, Cu2O
0.3%, Fe3O40.1%, SiO20.1%, V2O50.1%, Sb2O50.2%, surplus Fe2O3。
The preparation method step of the alloy I includes:
A, by alloy raw material Ingredients Weight percentage composition be Bi0.7%, Si0.5%, Ga 0.03%, Sb0.01%,
Sc0.05%, B2%, Nd20%, surplus are that Fe carries out ingredient, and Bi, Si, Ga, Sb, Sc, Nd, Fe are that (content is greater than pure material
99.9%)；B is added in the form of ferro-boron intermediate alloy, and the mass percentage of B is 23% in ferro-boron intermediate alloy.
B, 1550 DEG C of meltings are heated the raw material to, then casting obtains mother alloy ingot；The melting is in electric arc furnaces copper earthenware
Melting in crucible constantly stirs aluminium alloy with electric arc in fusion process, melts it sufficiently uniformly；
C, mother alloy ingot is heated to 1510 DEG C of fusings in induction furnace, obtains master alloy liquid；
D, master alloy liquid is prepared into alloy Cast Strip by the method that vacuum rapid hardening gets rid of band in vacuum rapid hardening spun furnace；Institute
It states remelting tubular type crucible bottom in vacuum rapid hardening spun furnace and is equipped 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 master alloy
After fusing, the valve on remelting tubular type crucible top is opened, melting master alloy is sprayed 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) are 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 35min；The dry ice quality is alloy Cast Strip
6%；The dry ice is cylindric, diameter 4mm, length 5-12mm；Then by alloy Cast Strip take out be put into hydrogen crushing furnace into
The broken obtained alloy coarse powder of row hydrogen, the hydrogen crushing furnace reaction chamber vacuum degree are 0.08Pa, and air pressure is 1atm, in-furnace temperature in hydrogen crushing furnace
It is 300 DEG C, the hydrogen broken time is 75min；
F, alloy coarse powder is put into airflow milling and is ground, the alloy fine powder that granularity is 2~5 μm is made, as magnetism
The alloy I of composite material；The airflow milling powder pressure is 7atm.
The preparation method step of the alloy II includes:
A, by alloy raw material Ingredients Weight percentage composition be La12%, B3%, Pb0.02%, V0.03%, Os0.03%,
Au0.001%, Be 0.05%, surplus are that Fe carries out ingredient；La, Pb, V, Os, Au, Be, Fe are that (content is greater than pure material
99.9%), the B is added in the form of ferro-boron intermediate alloy, and the mass percentage of B is 23% in ferro-boron intermediate alloy.
B, 1550 DEG C of meltings are heated the raw material to, then casting obtains mother alloy ingot；The melting is in electric arc furnaces copper earthenware
Melting in crucible constantly stirs aluminium alloy with electric arc in fusion process, melts it sufficiently uniformly；
C, mother alloy ingot is heated to 1510 DEG C of fusings in induction furnace, obtains master alloy liquid；
D, master alloy liquid is prepared into alloy Cast Strip by the method that vacuum rapid hardening gets rid of band in vacuum rapid hardening spun furnace；Institute
It states remelting tubular type crucible bottom in vacuum rapid hardening spun furnace and is equipped 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 master alloy
After fusing, the valve on remelting tubular type crucible top is opened, melting master alloy is sprayed 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) are 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
6%；The dry ice is cylindric, diameter 4mm, length 5-12mm；Then by alloy Cast Strip take out be put into hydrogen crushing furnace into
The broken obtained alloy coarse powder of row hydrogen, the hydrogen crushing furnace reaction chamber vacuum degree are 0.08Pa, and air pressure is 1atm, in-furnace temperature in hydrogen crushing furnace
It is 300 DEG C, the hydrogen broken time is 75min；
F, alloy coarse powder is put into airflow milling and is ground, the alloy fine powder that granularity is 1~8 μm is made, as magnetism
The alloy II of composite material；The airflow milling powder pressure is 7atm.
The preparation method step of the alloy III includes:
It A, is Eu2%, Al 5%, Si5% by alloy raw material Ingredients Weight percentage composition, surplus is that Fe carries out ingredient；Eu,
Al, Fe are pure material (content is greater than 99.9%)；
B, 1450 DEG C of meltings are heated the raw material to, then casting obtains mother alloy ingot；The melting is in electric arc furnaces copper earthenware
Melting in crucible constantly stirs aluminium alloy with electric arc in fusion process, melts it sufficiently uniformly；
C, mother alloy ingot is heated to 1420 DEG C of fusings in induction furnace, obtains master alloy liquid；
D, master alloy liquid is prepared into alloy Cast Strip by the method that vacuum rapid hardening gets rid of band in vacuum rapid hardening spun furnace；Institute
It states remelting tubular type crucible bottom in vacuum rapid hardening spun furnace and is equipped 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 master alloy
After fusing, the valve on remelting tubular type crucible top is opened, melting master alloy is sprayed from the through-hole of crucible bottom under nitrogen pressure
To the forming furnace runner wheel rim of rotation, continuous alloy strip (3~5 millimeters of alloy tape thickness, width is 5~12mm) are 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, it prepares fused salt: pressing FeCl2、MgCl2、KCl、NaCl、NaF、BeF2Molar ratio be 0.1: 0.1: 1: 3:1:0.03
Each constituent element is weighed, fused-salt medium is obtained after mixing, the 12% powdery monocrystalline silicon for accounting for fused-salt medium quality is added, is ground
(FeCl2、MgCl2、KCl、NaCl、NaF、BeF2Purity with powdery monocrystalline silicon is 99.99%, and first each material exists before preparing
200 DEG C of drying 8h)；
F, fused salt is put into salt bath furnace, is heated to 750 DEG C, then constant temperature 30min is done with the silicon steel sheet containing 5.5%Si
Cathode immerses in liquid fused salt, immerses in liquid fused salt using alloy Cast Strip as anode and leads to direct current to alloy Cast Strip progress Permeation in Electroplating
Silicon；The logical direct current is pulse to electric mode, average current density 65mA/cm2；The alloy Cast Strip in fused salt with
The travel speed of 0.12m/min carries out uniform motion, and being kept for residence time of the alloy Cast Strip every in fused salt is 30min；
G, the alloy Cast Strip after siliconising is put into progress mechanical ball mill to alloy powder partial size in ball grinder and reaches 7-11 μm,
Obtain the alloy III for magnetic composite.
The preparation method step of the inorganic composite materials IV includes:
A, inorganic composite materials material composition weight percentage Li is pressed2O 0.1%, BaO 3%, Cu2O 0.3%,
Fe3O40.1-0.4%, SiO20.1%, V2O50.1%, Sb2O50.2%, surplus Fe2O3Carry out ingredient；Each raw material component is pure
Degree is all larger than 99.9%；
B, it dries after the raw material prepared being carried out mixing and breaking up in sand mill, is then sieved；The sieve of the sieving
For 200 mesh；The drying temperature is 120 DEG C, drying time 3h；
C, the raw material after sieving is put into sintering furnace and is sintered, sintering temperature is 1150 DEG C, soaking time 2h；
D, sintered product is ground to 10-13 microns of partial size in grinder, obtains the nothing for magnetic composite
Machine composite material IV.
A kind of preparation method of magnetic composite, step include:
A, by the mass ratio 1.5 of magnetic composite raw alloy material I, II, III and inorganic composite materials IV:
0.8:0.2:0.03 ingredient is added in three-dimensional mixer and is uniformly mixed, and mixed powder is made；
B, mixed powder is orientated in Magnetic field press, compression moulding；The compression moulding is formed using Bidirectional pressure mode,
Pressure is 150KN, pressure maintaining 20S；
C, molded blank is put into sintering furnace to be sintered under protection of argon gas, is first warming up to 700 DEG C, keep the temperature 3h, then
1160 DEG C of sintering 4h are warming up to, are cooled to room temperature；
D, ageing treatment is carried out after sintered molded blank being carried out double tempering processing, obtained magnetic coupling material is made
Material；The temperature of the double tempering processing is respectively 900 DEG C, and 550 DEG C, soaking time is respectively 2h, 2.5h；The ageing treatment
Temperature be 240 DEG C, soaking time 30h.
Embodiment 2
A kind of magnetic composite, raw material is composed of alloy I, II, III and inorganic composite materials IV, described
The mass ratio of alloy material I, II, III and inorganic composite materials IV are 1.5:1:0.5:0.03；
Described its material composition of alloy I and weight percentage are as follows: Bi1.2%, Si0.9%, Ga 0.08%,
Sb0.04%, Sc0.09%, B5%, Nd24%, surplus Fe；The B is added in the form of ferro-boron intermediate alloy, among ferro-boron
The mass percentage of B is 23% in alloy；
Described its material composition of alloy II and weight percentage are as follows: La17%, B6%, Pb0.08%, V0.08%,
Os0.08%, Au0.004%, Be 0.09%, surplus Fe；The B is added in the form of ferro-boron intermediate alloy, among ferro-boron
The mass percentage of B is 23% in alloy；
Described its material composition of alloy III and weight percentage are as follows: Eu6%, Al 9%, Si10%, surplus Fe；
Described its material composition of inorganic composite materials IV and weight percentage are as follows: Li2O 0.4%, BaO 8%, Cu2O
0.8%, Fe3O40.4%, SiO20.4%, V2O50.4%, Sb2O50.6%, surplus Fe2O3。
The preparation method step of the alloy I includes:
A, by alloy raw material Ingredients Weight percentage composition be Bi1.2%, Si0.9%, Ga 0.08%, Sb0.04%,
Sc0.09%, B5%, Nd24%, surplus are that Fe carries out ingredient, and Bi, Si, Ga, Sb, Sc, Nd, Fe are that (content is greater than pure material
99.9%)；B is added in the form of ferro-boron intermediate alloy, and the mass percentage of B is 23% in ferro-boron intermediate alloy.
B, 1575 DEG C of meltings are heated the raw material to, then casting obtains mother alloy ingot；The melting is in electric arc furnaces copper earthenware
Melting in crucible constantly stirs aluminium alloy with electric arc in fusion process, melts it sufficiently uniformly；
C, mother alloy ingot is heated to 1540 DEG C of fusings in induction furnace, obtains master alloy liquid；
D, master alloy liquid is prepared into alloy Cast Strip by the method that vacuum rapid hardening gets rid of band in vacuum rapid hardening spun furnace；Institute
It states remelting tubular type crucible bottom in vacuum rapid hardening spun furnace and is equipped 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 master alloy
After fusing, the valve on remelting tubular type crucible top is opened, melting master alloy is sprayed 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) are 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 15min；The dry ice quality is alloy Cast Strip
8%；The dry ice is cylindric, diameter 4mm, length 5-12mm；Then by alloy Cast Strip take out be put into hydrogen crushing furnace into
The broken obtained alloy coarse powder of row hydrogen, the hydrogen crushing furnace reaction chamber vacuum degree are 0.06Pa, and air pressure is 1.2atm, temperature in furnace in hydrogen crushing furnace
Degree is 270 DEG C, and the hydrogen broken time is 80min；
F, alloy coarse powder is put into airflow milling and is ground, the alloy fine powder that granularity is 2~5 μm is made, as magnetism
The alloy I of composite material；The airflow milling powder pressure is 6atm.
The preparation method step of the alloy II includes:
A, by alloy raw material Ingredients Weight percentage composition be La17%, B6%, Pb0.08%, V0.08%, Os0.08%,
Au0.004%, Be 0.09%, surplus are that Fe carries out ingredient；La, Pb, V, Os, Au, Be, Fe are that (content is greater than pure material
99.9%), the B is added in the form of ferro-boron intermediate alloy, and the mass percentage of B is 23% in ferro-boron intermediate alloy.
B, 1570 DEG C of meltings are heated the raw material to, then casting obtains mother alloy ingot；The melting is in electric arc furnaces copper earthenware
Melting in crucible constantly stirs aluminium alloy with electric arc in fusion process, melts it sufficiently uniformly；
C, mother alloy ingot is heated to 1540 DEG C of fusings in induction furnace, obtains master alloy liquid；
D, master alloy liquid is prepared into alloy Cast Strip by the method that vacuum rapid hardening gets rid of band in vacuum rapid hardening spun furnace；Institute
It states remelting tubular type crucible bottom in vacuum rapid hardening spun furnace and is equipped 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 master alloy
After fusing, the valve on remelting tubular type crucible top is opened, melting master alloy is sprayed 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) are 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
10%；The dry ice is cylindric, diameter 4mm, length 5-12mm；Then by alloy Cast Strip take out be put into hydrogen crushing furnace into
The broken obtained alloy coarse powder of row hydrogen, the hydrogen crushing furnace reaction chamber vacuum degree are 0.1Pa, and air pressure is 1.2atm, temperature in furnace in hydrogen crushing furnace
Degree is 270 DEG C, and the hydrogen broken time is 80min；
F, alloy coarse powder is put into airflow milling and is ground, the alloy fine powder that granularity is 1~8 μm is made, as magnetism
The alloy II of composite material；The airflow milling powder pressure is 6atm.
The preparation method step of the alloy III includes:
It A, is Eu6%, Al 9%, Si10% by alloy raw material Ingredients Weight percentage composition, surplus is that Fe carries out ingredient；
Eu, Al, Fe are pure material (content is greater than 99.9%)；
B, 1480 DEG C of meltings are heated the raw material to, then casting obtains mother alloy ingot；The melting is in electric arc furnaces copper earthenware
Melting in crucible constantly stirs aluminium alloy with electric arc in fusion process, melts it sufficiently uniformly；
C, mother alloy ingot is heated to 1440 DEG C of fusings in induction furnace, obtains master alloy liquid；
D, master alloy liquid is prepared into alloy Cast Strip by the method that vacuum rapid hardening gets rid of band in vacuum rapid hardening spun furnace；Institute
It states remelting tubular type crucible bottom in vacuum rapid hardening spun furnace and is equipped 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 master alloy
After fusing, the valve on remelting tubular type crucible top is opened, melting master alloy is sprayed from the through-hole of crucible bottom under nitrogen pressure
To the forming furnace runner wheel rim of rotation, continuous alloy strip (3~5 millimeters of alloy tape thickness, width is 5~12mm) are 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, it prepares fused salt: pressing FeCl2、MgCl2、KCl、NaCl、NaF、BeF2Molar ratio be 0.1: 0.1: 1: 3:1:0.06
Each constituent element is weighed, fused-salt medium is obtained after mixing, the 15% powdery monocrystalline silicon for accounting for fused-salt medium quality is added, is ground
(FeCl2、MgCl2、KCl、NaCl、NaF、BeF2Purity with powdery monocrystalline silicon is 99.99%, and first each material exists before preparing
200 DEG C of drying 8h)；
F, fused salt is put into salt bath furnace, is heated to 700 DEG C, then constant temperature 25min is done with the silicon steel sheet containing 5.5%Si
Cathode immerses in liquid fused salt, immerses in liquid fused salt using alloy Cast Strip as anode and leads to direct current to alloy Cast Strip progress Permeation in Electroplating
Silicon；The logical direct current is pulse to electric mode, average current density 75mA/cm2；The alloy Cast Strip in fused salt with
The travel speed of 0.15m/min carries out uniform motion, and being kept for residence time of the alloy Cast Strip every in fused salt is 25min；
G, the alloy Cast Strip after siliconising is put into progress mechanical ball mill to alloy powder partial size in ball grinder and reaches 7-11 μm,
Obtain the alloy III for magnetic composite.
The preparation method step of the inorganic composite materials IV includes:
A, inorganic composite materials material composition weight percentage Li is pressed2O 0.4%, BaO 8%, Cu2O 0.8%,
Fe3O40.4%, SiO20.4%, V2O50.4%, Sb2O50.6%, surplus Fe2O3Carry out ingredient；Each raw material component purity
It is all larger than 99.9%；
B, it dries after the raw material prepared being carried out mixing and breaking up in sand mill, is then sieved；The sieve of the sieving
For 200 mesh；The drying temperature is 110 DEG C, drying time 3h；
C, the raw material after sieving is put into sintering furnace and is sintered, sintering temperature is 1250 DEG C, soaking time 3h；
D, sintered product is ground to 10-13 microns of partial size in grinder, obtains the nothing for magnetic composite
Machine composite material IV.
A kind of preparation method of magnetic composite, step include:
A, by the mass ratio 1.5:1 of magnetic composite raw alloy material I, II, III and inorganic composite materials IV:
0.5:0.03 ingredient is added in three-dimensional mixer and is uniformly mixed, and mixed powder is made；
B, mixed powder is orientated in Magnetic field press, compression moulding；The compression moulding is formed using Bidirectional pressure mode,
Pressure is 150KN, pressure maintaining 15S；
C, molded blank is put into sintering furnace to be sintered under protection of argon gas, is first warming up to 600 DEG C, keep the temperature 4h, then
1180 DEG C of sintering 3h are warming up to, are cooled to room temperature；
D, ageing treatment is carried out after sintered molded blank being carried out double tempering processing, obtained magnetic coupling material is made
Material；The temperature of the double tempering processing is respectively 910 DEG C, and 560 DEG C, soaking time is respectively 2h, 2h；The ageing treatment
Temperature is 210 DEG C, soaking time 25h.
Embodiment 3
A kind of magnetic composite, raw material is composed of alloy I, II, III and inorganic composite materials IV, described
The mass ratio of alloy material I, II, III and inorganic composite materials IV are 1.5:0.9:0.4:0.03；
Described its material composition of alloy I and weight percentage are as follows: Bi0.9%, Si0.79%, Ga 0.05%,
Sb0.03%, Sc0.07%, B3%, Nd22%, surplus Fe；The B is added in the form of ferro-boron intermediate alloy, among ferro-boron
The mass percentage of B is 23% in alloy；
Described its material composition of alloy II and weight percentage are as follows: La15%, B5%, Pb0.06%, V0.05%,
Os0.06%, Au0.003%, Be 0.06%, surplus Fe；The B is added in the form of ferro-boron intermediate alloy, among ferro-boron
The mass percentage of B is 23% in alloy；
Described its material composition of alloy III and weight percentage are as follows: Eu4%, Al 7%, Si7%, surplus Fe；
Described its material composition of inorganic composite materials IV and weight percentage are as follows: Li2O 0.3%, BaO 7%, Cu2O
0.6%, Fe3O40.3%, SiO20.3%, V2O50.3%, Sb2O50.4%, surplus Fe2O3。
The preparation method step of the alloy I includes:
A, by alloy raw material Ingredients Weight percentage composition be Bi0.9%, Si0.79%, Ga 0.05%, Sb0.03%,
Sc0.07%, B3%, Nd22%, surplus are that Fe carries out ingredient, and Bi, Si, Ga, Sb, Sc, Nd, Fe are that (content is greater than pure material
99.9%)；B is added in the form of ferro-boron intermediate alloy, and the mass percentage of B is 23% in ferro-boron intermediate alloy.
B, 1570 DEG C of meltings are heated the raw material to, then casting obtains mother alloy ingot；The melting is in electric arc furnaces copper earthenware
Melting in crucible constantly stirs aluminium alloy with electric arc in fusion process, melts it sufficiently uniformly；
C, mother alloy ingot is heated to 1530 DEG C of fusings in induction furnace, obtains master alloy liquid；
D, master alloy liquid is prepared into alloy Cast Strip by the method that vacuum rapid hardening gets rid of band in vacuum rapid hardening spun furnace；Institute
It states remelting tubular type crucible bottom in vacuum rapid hardening spun furnace and is equipped 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 master alloy
After fusing, the valve on remelting tubular type crucible top is opened, melting master alloy is sprayed 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) are 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 26m/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
8%；The dry ice is cylindric, diameter 4mm, length 5-12mm；Then by alloy Cast Strip take out be put into hydrogen crushing furnace into
The broken obtained alloy coarse powder of row hydrogen, the hydrogen crushing furnace reaction chamber vacuum degree are 0.07Pa, and air pressure is 0.9atm, temperature in furnace in hydrogen crushing furnace
Degree is 290 DEG C, and the hydrogen broken time is 80min；
F, alloy coarse powder is put into airflow milling and is ground, the alloy fine powder that granularity is 2~5 μm is made, as magnetism
The alloy I of composite material；The airflow milling powder pressure is 6atm.
The preparation method step of the alloy II includes:
A, by alloy raw material Ingredients Weight percentage composition be La15%, B5%, Pb0.06%, V0.05%, Os0.06%,
Au0.003%, Be 0.06%, surplus are that Fe carries out ingredient；La, Pb, V, Os, Au, Be, Fe are that (content is greater than pure material
99.9%), the B is added in the form of ferro-boron intermediate alloy, and the mass percentage of B is 23% in ferro-boron intermediate alloy.
B, 1560 DEG C of meltings are heated the raw material to, then casting obtains mother alloy ingot；The melting is in electric arc furnaces copper earthenware
Melting in crucible constantly stirs aluminium alloy with electric arc in fusion process, melts it sufficiently uniformly；
C, mother alloy ingot is heated to 1530 DEG C of fusings in induction furnace, obtains master alloy liquid；
D, master alloy liquid is prepared into alloy Cast Strip by the method that vacuum rapid hardening gets rid of band in vacuum rapid hardening spun furnace；Institute
It states remelting tubular type crucible bottom in vacuum rapid hardening spun furnace and is equipped 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 master alloy
After fusing, the valve on remelting tubular type crucible top is opened, melting master alloy is sprayed 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) are 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 29m/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
8%；The dry ice is cylindric, diameter 4mm, length 5-12mm；Then by alloy Cast Strip take out be put into hydrogen crushing furnace into
The broken obtained alloy coarse powder of row hydrogen, the hydrogen crushing furnace reaction chamber vacuum degree are 0.1Pa, and air pressure is 1.2atm, temperature in furnace in hydrogen crushing furnace
Degree is 280 DEG C, and the hydrogen broken time is 75min；
F, alloy coarse powder is put into airflow milling and is ground, the alloy fine powder that granularity is 1~8 μm is made, as magnetism
The alloy II of composite material；The airflow milling powder pressure is 6atm.
The preparation method step of the alloy III includes:
It A, is Eu4%, Al 7%, Si7% by alloy raw material Ingredients Weight percentage composition, surplus is that Fe carries out ingredient；Eu,
Al, Fe are pure material (content is greater than 99.9%)；
B, 1460 DEG C of meltings are heated the raw material to, then casting obtains mother alloy ingot；The melting is in electric arc furnaces copper earthenware
Melting in crucible constantly stirs aluminium alloy with electric arc in fusion process, melts it sufficiently uniformly；
C, mother alloy ingot is heated to 1430 DEG C of fusings in induction furnace, obtains master alloy liquid；
D, master alloy liquid is prepared into alloy Cast Strip by the method that vacuum rapid hardening gets rid of band in vacuum rapid hardening spun furnace；Institute
It states remelting tubular type crucible bottom in vacuum rapid hardening spun furnace and is equipped 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 master alloy
After fusing, the valve on remelting tubular type crucible top is opened, melting master alloy is sprayed from the through-hole of crucible bottom under nitrogen pressure
To the forming furnace runner wheel rim of rotation, continuous alloy strip (3~5 millimeters of alloy tape thickness, width is 5~12mm) are 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 26m/s；
E, it prepares fused salt: pressing FeCl2、MgCl2、KCl、NaCl、NaF、BeF2Molar ratio be 0.1: 0.1: 1: 3:1:0.05
Each constituent element is weighed, fused-salt medium is obtained after mixing, the 14% powdery monocrystalline silicon for accounting for fused-salt medium quality is added, is ground
(FeCl2、MgCl2、KCl、NaCl、NaF、BeF2Purity with powdery monocrystalline silicon is 99.99%, and first each material exists before preparing
200 DEG C of drying 8h)；
F, fused salt is put into salt bath furnace, is heated to 720 DEG C, then constant temperature 20min is done with the silicon steel sheet containing 5.5%Si
Cathode immerses in liquid fused salt, immerses in liquid fused salt using alloy Cast Strip as anode and leads to direct current to alloy Cast Strip progress Permeation in Electroplating
Silicon；The logical direct current is pulse to electric mode, average current density 70mA/cm2；The alloy Cast Strip in fused salt with
The travel speed of 0.13m/min carries out uniform motion, and being kept for residence time of the alloy Cast Strip every in fused salt is 25min；
G, the alloy Cast Strip after siliconising is put into progress mechanical ball mill to alloy powder partial size in ball grinder and reaches 7-11 μm,
Obtain the alloy III for magnetic composite.
The preparation method step of the inorganic composite materials IV includes:
A, inorganic composite materials material composition weight percentage Li is pressed2O 0.3%, BaO 7%, Cu2O 0.6%,
Fe3O40.3%, SiO20.3%, V2O50.3%, Sb2O50.4%, surplus Fe2O3Carry out ingredient；Each raw material component purity is equal
Greater than 99.9%；
B, it dries after the raw material prepared being carried out mixing and breaking up in sand mill, is then sieved；The sieve of the sieving
For 200 mesh；The drying temperature is 110 DEG C, drying time 3h；
C, the raw material after sieving is put into sintering furnace and is sintered, sintering temperature is 1190 DEG C, soaking time 3h；
D, sintered product is ground to 10-13 microns of partial size in grinder, obtains the nothing for magnetic composite
Machine composite material IV.
A kind of preparation method of magnetic composite, step include:
A, by the mass ratio 1.5 of magnetic composite raw alloy material I, II, III and inorganic composite materials IV:
0.9:0.4:0.03 ingredient is added in three-dimensional mixer and is uniformly mixed, and mixed powder is made；
B, mixed powder is orientated in Magnetic field press, compression moulding；The compression moulding is formed using Bidirectional pressure mode,
Pressure is 150KN, pressure maintaining 15S；
C, molded blank is put into sintering furnace to be sintered under protection of argon gas, is first warming up to 700 DEG C, keep the temperature 3h, then
1150 DEG C of sintering 4h are warming up to, are cooled to room temperature；
D, ageing treatment is carried out after sintered molded blank being carried out double tempering processing, obtained magnetic coupling material is made
Material；The temperature of the double tempering processing is respectively 890 DEG C, and 550 DEG C, soaking time is respectively 2.5h, 3h；The ageing treatment
Temperature be 230 DEG C, soaking time 25h.
The magnetic composite performance of embodiment 1-3 preparation is as shown in table 1:
Table 1 implements the magnetic composite mechanical property of embodiment 1-3 preparation
| Embodiment | 1 | 2 | 3 |
| Remanent magnetism (kGs) | 15.1 | 15.8 | 15.4 |
| Coercivity (kOe) | 23.4 | 24.1 | 23.9 |
| Maximum magnetic energy product (MGOe) | 48.5 | 49.7 | 49.1 |
Claims (11)
1. a kind of magnetic composite, raw material is composed of alloy I, II, III and inorganic composite materials IV, the conjunction
The mass ratio of golden I, II, III and inorganic composite materials IV are 1.5:0.8-1:0.2-0.5:0.03；
Described its material composition of alloy I and weight percentage are as follows: Bi0.7~1.2%, Si0.5~0.9%, Ga 0.03~
0.08%, Sb0.01~0.04%, Sc0.05~0.09%, B2~5%, Nd20~24%, surplus Fe；
Described its material composition of alloy II and weight percentage are as follows: La12~17%, B3~6%, Pb0.02%~0.08%,
V0.03%~0.08%, Os0.03%~0.08%, Au0.001%~0.004%, Be 0.05%~0.09%, surplus are
Fe；
The alloy III, material composition and weight percentage are as follows: Eu2~6%, Al 5~9%, Si5~10%, surplus
For Fe；
Described its ingredient of inorganic composite materials IV and weight percentage are as follows: Li2O 0.1-0.4%, BaO 3~8%, Cu2O
0.3-0.8%, Fe3O40.1-0.4%, SiO20.1-0.4%, V2O50.1-0.5%, Sb2O50.2-0.6%, surplus are
Fe2O3。
2. magnetic composite as described in claim 1, it is characterised in that: B is in described alloy I, II with ferro-boron intermediate alloy
Form be added, the mass percentage of B is 20-25% in ferro-boron intermediate alloy.
3. magnetic composite as described in claim 1, it is characterised in that:
The preparation method step of the alloy I includes:
A, by alloying component weight percentage be Bi0.7~1.2%, Si0.5~0.9%, Ga 0.03~0.08%,
Sb0.01~0.04%, Sc0.05~0.09%, B2~5%, Nd20~24%, surplus are that Fe carries out ingredient；The B is with ferro-boron
The form of intermediate alloy is added, and the mass percentage of B is 20-25% in ferro-boron intermediate alloy；
B, 1550~1580 DEG C of meltings are heated the raw material to, then casting obtains mother alloy ingot；The melting is in electric arc furnaces copper
Melting in crucible constantly stirs aluminium alloy with electric arc in fusion process, melts it sufficiently uniformly；
C, mother alloy ingot is heated to 1510-1540 DEG C of fusing in induction furnace, obtains master alloy liquid；
D, master alloy liquid is prepared into alloy Cast Strip by the method that vacuum rapid hardening gets rid of band in vacuum rapid hardening spun furnace；The system
17~20 microns of standby alloy tape thickness, 8~13mm of width；
E, alloy Cast Strip is put into placement 8min or more in the closed container for fill dry ice；The dry ice quality is alloy Cast Strip
5-10%；The dry ice is cylindric, diameter 4mm, length 5-12mm；Then by alloy Cast Strip take out be put into hydrogen crushing furnace into
The broken obtained alloy coarse powder of row hydrogen, the hydrogen crushing furnace reaction chamber vacuum degree are 0.06~0.1Pa, in hydrogen crushing furnace air pressure be 0.8~
1.3atm, in-furnace temperature are 260~310 DEG C, and the hydrogen broken time is 70~80min；
F, alloy coarse powder is put into airflow milling and is ground, the alloy fine powder that granularity is 2~5 μm is made, is as used for magnetic coupling
The alloy I of material；The airflow milling powder pressure is 6~7atm.
4. magnetic composite as claimed in claim 3, it is characterised in that: standing time is 30-50min in the step E.
5. magnetic composite as described in claim 1, it is characterised in that:
The preparation method step of the alloy II includes:
A, by alloying component weight percentage be La12~17%, B3~6%, Pb0.02%~0.08%, V0.03%~
0.08%, Os0.03%~0.08%, Au0.001%~0.004%, Be 0.05%~0.09%, surplus are that Fe is matched
Material；The B is added in the form of ferro-boron intermediate alloy, and the mass percentage of B is 20-25% in ferro-boron intermediate alloy；
B, 1550~1580 DEG C of meltings are heated the raw material to, then casting obtains mother alloy ingot；The melting is in electric arc furnaces copper
Melting in crucible constantly stirs aluminium alloy with electric arc in fusion process, melts it sufficiently uniformly；
C, mother alloy ingot is heated to 1510-1540 DEG C of fusing in induction furnace, obtains master alloy liquid；
D, master alloy liquid is prepared into alloy Cast Strip by the method that vacuum rapid hardening gets rid of band in vacuum rapid hardening spun furnace；The system
15~17 microns of standby alloy tape thickness, 8~13mm of width；
E, alloy Cast Strip is put into placement 8min or more in the closed container for fill dry ice；The dry ice quality is alloy Cast Strip
5-10%；The dry ice is cylindric, diameter 4mm, length 5-12mm；Then by alloy Cast Strip take out be put into hydrogen crushing furnace into
The broken obtained alloy coarse powder of row hydrogen, the hydrogen crushing furnace reaction chamber vacuum degree are 0.06~0.1Pa, in hydrogen crushing furnace air pressure be 0.8~
1.3atm, in-furnace temperature are 260~310 DEG C, and the hydrogen broken time is 70~80min；
F, alloy coarse powder is put into airflow milling and is ground, the alloy fine powder that granularity is 1~8 μm is made, is as used for magnetic coupling
The alloy II of material；The airflow milling powder pressure is 6~7atm.
6. magnetic composite as claimed in claim 5, it is characterised in that: standing time is 30-50min in the step E.
7. magnetic composite as described in claim 1, it is characterised in that:
The preparation method step of the alloy III includes:
It A, is Eu2~6% by alloying component weight percentage, Al5~9%, Si5~10%, surplus is that Fe carries out ingredient；
B, 1450-1480 DEG C of melting is heated the raw material to, then casting obtains mother alloy ingot；The melting is in electric arc furnaces copper earthenware
Melting in crucible constantly stirs aluminium alloy with electric arc in fusion process, melts it sufficiently uniformly；
C, mother alloy ingot is heated to 1410-1440 DEG C of fusing in induction furnace, obtains master alloy liquid；
D, master alloy liquid is prepared into alloy Cast Strip by the method that vacuum rapid hardening gets rid of band in vacuum rapid hardening spun furnace；The system
3~5 millimeters of standby alloy tape thickness, width are 5~12mm；
E, it prepares fused salt: pressing FeCl2、MgCl2、KCl、NaCl、NaF、BeF2Molar ratio be 0.1: 0.1: 1: 3: 1: 0.02-
0.06 weighs each constituent element, and fused-salt medium is obtained after mixing, and the powdery polysilicon for accounting for the 11%-15% of fused-salt medium quality is added,
It is ground；
F, fused salt is put into salt bath furnace, is heated to 680-770 DEG C, then constant temperature 20-30min does cathode immersion with silicon steel sheet
In liquid fused salt, logical direct current in liquid fused salt is immersed into as anode in alloy Cast Strip, plating siliconising is carried out to alloy Cast Strip；It is described logical
Direct current is pulse to electric mode, average current density 65-75mA/cm2；The alloy Cast Strip is in fused salt with 0.11-
The travel speed of 0.15m/min carries out uniform motion, and being kept for residence time of the alloy Cast Strip in fused salt is 25-30min；
G, it will be put into progress mechanical ball mill to alloy powder partial size in ball grinder after the alloy Cast Strip coarse crushing after siliconising and reach 7-
11 μm, obtain the alloy III for magnetic composite.
8. magnetic composite as claimed in claim 7, it is characterised in that: in the step F in silicon steel sheet silicon quality hundred
Dividing content is 4-6%.
9. magnetic composite as described in claim 1, it is characterised in that:
The preparation method step of the inorganic composite materials IV includes:
A, inorganic composite materials IV Ingredients Weight percentage composition Li is pressed2O 0.1-0.4%, BaO 3~8%, Cu2O 0.3-
0.8%, Fe3O40.1-0.4%, SiO20.1-0.4%, V2O50.1-0.5%, Sb2O50.2-0.6%, surplus Fe2O3Into
Row ingredient；
B, it dries after the raw material prepared being carried out mixing and breaking up in sand mill, is then sieved；The sieve of the sieving is
180-220 mesh；The drying temperature is 110-120 DEG C, drying time 2-4h；
C, the raw material after sieving is put into sintering furnace and is sintered, sintering temperature is 1100-1250 DEG C, soaking time 2-
4h；
D, sintered product is ground to 10-13 microns of partial size in grinder, obtained for the inorganic multiple of magnetic composite
Condensation material IV.
10. the preparation method of magnetic composite as claimed in claims 1-9, step include:
A, by the mass ratio 1.5:0.8-1 of magnetic composite raw alloy material I, II, III and inorganic composite materials IV:
0.2-0.5:0.03 ingredient is added in three-dimensional mixer and is uniformly mixed, and mixed powder is made；
B, mixed powder is orientated in Magnetic field press, compression moulding；
C, molded blank is put into sintering furnace to be sintered under protection of argon gas, is first warming up to 500-750 DEG C, keep the temperature 2-4h, so
After be warming up to 1150-1180 DEG C of sintering 2-4h, be cooled to room temperature；
D, ageing treatment is carried out after sintered molded blank being carried out double tempering processing, magnetic composite is made；It is described
The temperature of double tempering processing is respectively 890-910 DEG C and 540-570 DEG C of soaking time is respectively 2-4h；The ageing treatment
Temperature is 210-250 DEG C, soaking time 20-40h.
11. the preparation method of magnetic composite as claimed in claim 10, it is characterised in that: pressed described in the step B
Type is made to form using Bidirectional pressure mode, pressure 150KN, pressure maintaining 10-20s.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0396880A1 (en) * | 1989-05-12 | 1990-11-14 | Krupp Widia GmbH | NdFeB magnet and surface passivation process of NdFeB magnets |
| US6019859A (en) * | 1994-09-02 | 2000-02-01 | Sumitomo Special Metals Co., Ltd. | Iron-based permanent magnets and their fabrication as well as iron-based permanent magnet alloy powders for permanent bonded magnets and iron-based bonded magnets |
| JP2003031407A (en) * | 2001-07-16 | 2003-01-31 | Sumitomo Special Metals Co Ltd | Iron base anisotropic permanent magnet and its manufacturing method |
| CN101364465B (en) * | 2008-06-06 | 2013-07-10 | 浙江西子富沃德电机有限公司 | Permanent magnetic RE material and preparation thereof |
| CN104446427A (en) * | 2014-11-18 | 2015-03-25 | 连云港市兆昱新材料实业有限公司 | Rare-earth doped spinel type ferrite magnetic powder prepared based on NdFeB wastes and preparation method thereof |
| CN106448988A (en) * | 2015-08-04 | 2017-02-22 | 青岛金立磁性材料有限公司 | Ferrite-neodymium iron boron composite injection molding granular material and preparation method thereof |
| CN106910585A (en) * | 2015-12-22 | 2017-06-30 | 比亚迪股份有限公司 | A kind of Nd-Fe-B permanent magnet material and preparation method thereof and motor |
| CN106920615A (en) * | 2017-03-08 | 2017-07-04 | 江苏南方永磁科技有限公司 | A kind of sintered neodymium iron boron material and preparation method |
-
2017
- 2017-09-15 CN CN201710844219.3A patent/CN107564653B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0396880A1 (en) * | 1989-05-12 | 1990-11-14 | Krupp Widia GmbH | NdFeB magnet and surface passivation process of NdFeB magnets |
| US6019859A (en) * | 1994-09-02 | 2000-02-01 | Sumitomo Special Metals Co., Ltd. | Iron-based permanent magnets and their fabrication as well as iron-based permanent magnet alloy powders for permanent bonded magnets and iron-based bonded magnets |
| JP2003031407A (en) * | 2001-07-16 | 2003-01-31 | Sumitomo Special Metals Co Ltd | Iron base anisotropic permanent magnet and its manufacturing method |
| CN101364465B (en) * | 2008-06-06 | 2013-07-10 | 浙江西子富沃德电机有限公司 | Permanent magnetic RE material and preparation thereof |
| CN104446427A (en) * | 2014-11-18 | 2015-03-25 | 连云港市兆昱新材料实业有限公司 | Rare-earth doped spinel type ferrite magnetic powder prepared based on NdFeB wastes and preparation method thereof |
| CN106448988A (en) * | 2015-08-04 | 2017-02-22 | 青岛金立磁性材料有限公司 | Ferrite-neodymium iron boron composite injection molding granular material and preparation method thereof |
| CN106910585A (en) * | 2015-12-22 | 2017-06-30 | 比亚迪股份有限公司 | A kind of Nd-Fe-B permanent magnet material and preparation method thereof and motor |
| CN106920615A (en) * | 2017-03-08 | 2017-07-04 | 江苏南方永磁科技有限公司 | A kind of sintered neodymium iron boron material and preparation method |
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Address after: 241100 No.1, Yonghe Road, Wanzhe District, Wuhu City, Anhui Province Patentee after: ANHUI INSTITUTE OF INFORMATION TECHNOLOGY Address before: No. 8, Wen Jin Xi Road, Yijiang District, Wuhu, Anhui Province Patentee before: ANHUI INSTITUTE OF INFORMATION TECHNOLOGY |
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Application publication date: 20180109 Assignee: ANHUI LIANHUA NEW MATERIAL CO.,LTD. Assignor: ANHUI INSTITUTE OF INFORMATION TECHNOLOGY Contract record no.: X2022980017549 Denomination of invention: A magnetic composite material and its preparation method Granted publication date: 20190702 License type: Common License Record date: 20221010 |