CN108538532A - A kind of composite magnetic and preparation method thereof - Google Patents

A kind of composite magnetic and preparation method thereof Download PDF

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Publication number
CN108538532A
CN108538532A CN201810268326.0A CN201810268326A CN108538532A CN 108538532 A CN108538532 A CN 108538532A CN 201810268326 A CN201810268326 A CN 201810268326A CN 108538532 A CN108538532 A CN 108538532A
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alloy
powder
temperature
liquid
surplus
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王玲
李庆芳
董英华
赵浩峰
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Nanjing University of Information Science and Technology
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Nanjing University of Information Science and Technology
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/09—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials mixtures of metallic and non-metallic particles; metallic particles having oxide skin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/02—Making ferrous alloys by powder metallurgy
    • C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
    • C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H01F41/0266—Moulding; Pressing

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Soft Magnetic Materials (AREA)

Abstract

The invention discloses a kind of composite magnetic and preparation method thereof, which is made of material first, material second, material third and material fourth, and the weight ratio of material first, material second, material third and material fourth is (0.06 0.09):(0.03‑0.08):(0.01‑0.04):1；The weight percentage of each ingredient is in material first：Al2O323 25%, ZrO20.5 0.8%, ZnO 4 9%, BaO 5 8%, MnO 4 8%, Li2O 1 4%, Fe2O30.7 1.3%, GeO20.1 0.4%,Nd2O30.001 0.003%, Lu2O30.001 0.003%, K2O 1 4%, B2O31 2.5%, surplus SiO2；Material second is fine copper, copper content 99.99%.

Description

A kind of composite magnetic and preparation method thereof
Technical field
The invention belongs to field of inorganic materials, it is related to a kind of composite magnetic and preparation method thereof.
Background technology
CN201610136736.0 discloses high magnetic rare earth permanent-magnetic material of a kind of high temperature resistant type and preparation method thereof, material Contain R, Fe, B, M in material, wherein R is by light rare earth elements Pr, Nd according to 1:The alloy of 3 ratio composition, Fe is ferro element, B is boron element, and M is molybdenum element.Using Pr-Nd alloys, Fe-B alloys and metal Mo as raw material, under the protection of inert gas, Vacuum metling is carried out in vacuum melting furnace, obtains the uniform alloy pig of ingredient, then obtained above-mentioned alloy pig is subjected to fast quenching speed Solidifying process, was crushed sieve, and make annealing treatment after obtaining metal sheet band.But the material comprehensive performance is not high.
Invention content
The purpose of the present invention provides a kind of composite magnetic aiming at above-mentioned technological deficiency, which subtracts in high temperature Magnetic rate is small, and has good magnetic property；It is a further object of the present invention to provide a kind of composite magnetic preparation method, the systems Preparation Method is simple for process, and production cost is low, is suitable for industrialized production.
The above-mentioned purpose of the present invention is achieved by following technical solution：
A kind of composite magnetic is made of material first, material second, material third and material fourth, material first, material second, material The weight ratio of material third and material fourth is (0.06-0.09):(0.03-0.08):(0.01-0.04):1；
The weight percentage of each ingredient is in material first：Al2O323-25%, ZrO20.5-0.8%, ZnO 4-9%, BaO 5-8%, MnO 4-8%, Li2O 1-4%, Fe2O30.7-1.3%, GeO20.1-0.4%, Nd2O30.001-0.003%, Lu2O30.001-0.003%, K2O 1-4%, B2O31-2.5%, surplus SiO2；
Material second is fine copper, copper content 99.99%；
The weight percentage of each ingredient is in material third：C 0.28-0.38%；Mn 0.50-0.80%；Si 0.30- 0.5%；S0.02-0.05%, P 0.02-0.045%, Nd 0.4-0.8%, Au 0.03-0.08%, Ge 0.03-0.09%, Lu 0.03-0.08%, Zr 0.02-0.05%, surplus Fe；
The weight percentage of each ingredient is in material fourth：B 3-5.5%, Nd 24-28%, Au 0.3-0.6%, Ge 0.8-1.3%, Lu 0.05-0.09%, S 0.8-1.2%, Zr 0.8-1.4%, surplus Fe.
The preparation method of above-mentioned composite magnetic, includes the following steps：Material first, material second, material third and material fourth Weight ratio is (0.06-0.09):(0.03-0.08):(0.01-0.04):After 1 dispensing, it is added in three-dimensional mixer and mixes It is even, obtain mixed powder；Then mixed powder is orientated in Magnetic field press, is molded using isostatic pressed mode；Molded blank is existed Argon gas protection down enters sintering furnace and is sintered, and is first warming up to 660-700 DEG C, keeps the temperature 3-4h, then heats to 1000-1090 DEG C It is sintered 3-4h, after being cooled to room temperature, carries out double tempering processing, i.e., respectively in 650-690 DEG C and 560-590 DEG C of tempering heat treatment 1-2h；Most product is obtained through 200-230 DEG C of ageing treatment afterwards.
Further, it is Al according to weight percent when the preparation of material first2O323-25%, ZrO20.5-0.8%, ZnO 4- 9%, BaO 5-8%, MnO 4-8%, Li2O 1-4%, Fe2O30.7-1.3%, GeO20.1-0.4%, Nd2O30.001- 0.003%, Lu2O30.001-0.003%, K2O 1-4%, B2O31-2.5%, surplus SiO2Carry out dispensing, each material purity It is all higher than 99.9%；Each raw material is subjected to mixing and breaking up in sand mill, then dries powder at 130-140 DEG C, is dried Re-sieving after dry, sieve are 200-220 mesh, are then placed in sintering furnace and are sintered, and sintering temperature is 1190-1210 DEG C, finally Diameter of particle is set to reach 7-10 microns in grinder sintered product.
Further, when prepared by material second, using fine copper, copper content 99.99%；Raw material is put into induction furnace in melting Melting, smelting temperature are 1260-1290 DEG C, obtain alloy liquid；Alloy liquid injection is located to the centre on atomizer In packet, aluminium alloy is flowed out by tundish bottom leakage eye, and meeting with high-speed flow when passing through nozzle is atomized as fine drop, atomization Drop is rapidly solidificated into alloy powder in closed atomizing cup, and alloy powder average particle size is 8-10 μm, atomization gas pressure Power is 8-10MPa, and liquid metal fluid flow is 3-5kg/min, and alloy liquid implantation temperature is 1230-1260 DEG C, atomizing angle 32 degree.
Further, when prepared by material third, first 275 steel scraps is put into carbonic acid soda lye and are handled 1-2 hours, sodium carbonate is molten Liquid concentration is 2-4%, 60-70 DEG C of alkali liquid temperature；It is dried after being rinsed 3 times with clear water again after base extraction is complete, induction can be put into Melting in stove, then places into the substance for the respective element that Nd, Au, Ge, Lu, Zr and 275 steel scraps are related to, and smelting temperature is 1580-1610 DEG C, obtain alloy liquid；The ingredient of alloy liquid is C 0.28-0.38%；Mn 0.50-0.80%；Si0.30- 0.5%；S 0.02-0.05%, P 0.02-0.045%, Nd 0.4-0.8%, Au 0.03-0.08%, Ge 0.03- 0.09%, Lu 0.03-0.08%, Zr 0.02-0.05%, surplus Fe；Alloy liquid injection is located on atomizer Tundish in, aluminium alloy is flowed out by tundish bottom leakage eye, is met and is atomized as tiny liquid with high-speed flow when passing through nozzle Drop, atomized drop are rapidly solidificated into alloy powder in closed atomizing cup, and alloy powder average particle size is 8-11 μm, atomization Gas pressure is 2-4MPa, and liquid metal fluid flow is 2-4kg/min, and alloy liquid implantation temperature is 1560-1590 DEG C, mist Change 34 degree of angle.
Further, it is B 3-5.5%, Nd 24-28%, Au according to weight percentage when the preparation of material fourth 0.3-0.6%, Ge 0.8-1.3%, Lu 0.05-0.09%, S 0.8-1.2%, Zr 0.8-1.4%, surplus are that Fe is matched Material；Nd, Au, Ge, Lu, Zr, Fe are the pure material that constituent content is more than 99.9%；B is added in the form of ferro-boron intermediate alloy, boron The amount containing B of iron intermediate alloy is 24-26%；First by melting in raw material induction furnace, smelting temperature is 1610-1640 DEG C, obtains mother Alloy liquid；Melting master alloy liquid is poured under nitrogen protection on forming furnace turntable, forms slab；The rotational line of turntable pour point Speed is 21-25m/s, and slab thickness is 2-4 millimeters, and long width is 5-8 millimeters, is then placed in a sealable reaction kettle, Reaction kettle is passed through H2After S gases, heat 1100-1300 DEG C, time 2-3h, then take out it is air-cooled, then will treated that slab is put Enter vacuum degree for 0.15-0.18Pa, the hydrogen crushing furnace progress hydrogen that air pressure is 1.0-1.4atm in stove is broken, and temperature is heated to 300-315 DEG C, broken 35-40 minutes of hydrogen obtains coarse powder；Then it is fine powder coarse powder to be put into coarse powder mill in airflow milling, and it is equal that average particle size is made It is 6-9 μm, airflow milling powder pressure 6-8atm.
Products obtained therefrom of the present invention has excellent magnetic energy.In addition it prepared alloy in kind and passes through proper treatment, and ensure that material The uniformity of ingredient, tissue and performance is expected, hereby it is ensured that the quality of material.Material first, that is, compound the bulk melting point of metal oxide It is low, main phase crystal boundary can be evenly distributed in and play pinning effect, coercivity is improved.Material second fusing point is low, inhibits material Phase is grown up in fourth, and main phase interface defect density is made to reduce, and magnetic reversal farmland is in interface forming core difficulty.In addition it can be distributed in disperse Around main phase grain, it can be effectively improved the institutional framework of Grain-Boundary Phase, crystal boundary modified, reinforcing Grain-Boundary Phase is carried out to magnet.Cause This improves the remanent magnetism of material.Secondary phase Fe-riched phase, inhibits the length of crystal grain intersection particle between the main phase grain that material third is formed Greatly, main phase grain has been refined, therefore may refrain from the enhancing of their ambient stray fields, and then has improved intrinsic coercivity.Material Nd, Au, Ge, Lu, Zr and material fourth in third is corresponding, it is therefore prevented that diffusion transfer of the key element in sintering in material fourth. Material fourth primarily forms magnetic main phase Nd2Fe14B and time main phase Lu2Fe14B enhances magnetic coupling interaction, makes the existing height of magnet Coercivity in turn avoid remanent magnetism and decline to a great extent, to obtain higher comprehensive magnetic energy.In sintering process, high-melting-point is added Alloy element Zr can make that cenotype is precipitated in magnet tissue, eliminate the phenomenon that being in direct contact between main phase grain, effectively inhibit master Phase crystal grain is grown up, and is conducive to obtain relatively fine uniform grain structure, while can improve the thermal stability of main phase magnet.The material Preparation process is easy, prepares that raw materials used cost is relatively low, and process is simple, and the alloy of production is with good performance, convenient for industry Metaplasia is produced.Permanent-magnet material prepared by the present invention is suitable for electrical apparatus industry.
Description of the drawings
Fig. 1 is a kind of tissue of composite magnetic, it can be seen that even tissue is fine and close.
Specific implementation mode
It is specific with reference to the accompanying drawings and examples to introduce essentiality content of the present invention, but the guarantor of the present invention is not limited with this Protect range.
Embodiment 1：
It is made of material first, material second, material third and material fourth, material first, material second, the weight of material third and material fourth Than being 0.06:0.03:0.01:1；
The weight percentage of each ingredient is in material first：Al2O323%, ZrO20.5%, ZnO 4%, BaO 5%, MnO 4%, Li2O 1%, Fe2O30.7%, GeO20.1%, Nd2O30.001%, Lu2O30.001%, K2O 1%, B2O31%, surplus For SiO2；
Material second is fine copper, copper content 99.99%；
The weight percentage of each ingredient is in material third：C 0.28%；Mn 0.50%；Si 0.30%；S 0.02%, P 0.02%, Nd 0.4%, Au 0.03%, Ge 0.03%, Lu 0.03%, Zr 0.02%, surplus Fe；
The weight percentage of each ingredient is in material fourth：B 3%, Nd 24%, Au 0.3%, Ge 0.8%, Lu 0.05%, S 0.8%, Zr 0.8%, surplus Fe.
Embodiment 2：
It is made of material first, material second, material third and material fourth, material first, material second, the weight of material third and material fourth Than for 0.0.8:0.05:0.02:1；
The weight percentage of each ingredient is in material first：Al2O324%, ZrO20.6%, ZnO 7%, BaO 6%, MnO 6%, Li2O 3%, Fe2O30.9%, GeO20.3%, Nd2O30.002%, Lu2O30.002%, K2O 3%, B2O32%, surplus For SiO2；
Material second is fine copper, copper content 99.99%；
The weight percentage of each ingredient is in material third：C 0.32%；Mn 0.60%；Si 0.4%；S 0.04%, P 0.03%, Nd 0.6%, Au 0.05%, Ge 0.07%, Lu 0.06%, Zr 0.04%, surplus Fe；
The weight percentage of each ingredient is in material fourth：B 4%, Nd 26%, Au 0.4%, Ge 1%, Lu 0.07%, S 1%, Zr 1%, surplus Fe.
Embodiment 3：
It is made of material first, material second, material third and material fourth, material first, material second, the weight of material third and material fourth Than being 0.09:0.08:0.04:1；
The weight percentage of each ingredient is in material first：Al2O325%, ZrO20.8%, ZnO 9%, BaO 8%, MnO 8%, Li2O 4%, Fe2O31.3%, GeO20.4%, Nd2O30.003%, Lu2O30.003%, K2O 4%, B2O32.5%, it is remaining Amount is SiO2；
Material second is fine copper, copper content 99.99%；
The weight percentage of each ingredient is in material third：C 0.38%；Mn 0.80%；Si 0.5%；S 0.05%, P 0.045%, Nd 0.8%, Au 0.08%, Ge 0.09%, Lu 0.08%, Zr 0.05%, surplus Fe；
The weight percentage of each ingredient is in material fourth：B 5.5%, Nd 28%, Au 0.6%, Ge 1.3%, Lu 0.09%, S 1.2%, Zr 1.4%, surplus Fe.
Embodiment 4：
It is made of material first, material second, material third and material fourth, material first, material second, the weight of material third and material fourth Than being 0.04:0.02:0.006:1；
The weight percentage of each ingredient is in material first：Al2O322%, ZrO20.4%, ZnO 3%, BaO 4%, MnO 3%, Li2O 0.8%, Fe2O30.5%, GeO20.07%, Nd2O30.0008%, Lu2O30.0008%, K2O 0.6%, B2O30.8%, surplus SiO2；
Material second is fine copper, copper content 99.99%；
The weight percentage of each ingredient is in material third：C 0.2%；Mn 0.4%；Si 0.2%；S 0.01%, P 0.01%, Nd 0.3%, Au 0.02%, Ge 0.02%, Lu 0.02%, Zr 0.01%, surplus Fe；
The weight percentage of each ingredient is in material fourth：B 2%, Nd 21%, Au 0.2%, Ge 0.5%, Lu 0.03%, S 0.7%, Zr 0.7%, surplus Fe.
Embodiment 5：
It is made of material first, material second, material third and material fourth, material first, material second, the weight of material third and material fourth Than being 0.1:0.1:0.05:1；
The weight percentage of each ingredient is in material first：Al2O327%, ZrO20.9%, ZnO 11%, BaO 9%, MnO 9%, Li2O 5%, Fe2O32%, GeO20.5%, Nd2O30.004%, Lu2O30.004%, K2O 5%, B2O33%, it is remaining Amount is SiO2；
Material second is fine copper, copper content 99.99%；
The weight percentage of each ingredient is in material third：C 0.4%；Mn 0.9%；Si 0.6%；S 0.07%, P 0.06%, Nd 0.9%, Au 0.09%, Ge 0.11%, Lu 0.09%, Zr 0.06%, surplus Fe；
The weight percentage of each ingredient is in material fourth：B 7%, Nd 30%, Au 0.7%, Ge 2%, Lu 0.1%, S 1.4%, Zr 1.5%, surplus Fe.
The preparation method of embodiment 1-5 composite magnetics includes the following steps：Material first, material second, material third and material After expecting fourth by weight dispensing, it is added in three-dimensional mixer and is uniformly mixed, obtain mixed powder；Then by mixed powder in magnetic field It is orientated in press, is molded using isostatic pressed mode；Molded blank is put into sintering furnace under protection of argon gas to be sintered, is first heated up To 680 DEG C, 3.5h is kept the temperature, 1050 DEG C of sintering 3.5h is then heated to, after being cooled to room temperature, carries out double tempering processing, that is, divide Not in 670 DEG C and 575 DEG C of tempering heat treatment 1.5h；Most product is obtained through 215 DEG C of ageing treatments afterwards.According to weight when prepared by material first It measures percentage and carries out dispensing, each material purity is all higher than 99.9%；Each raw material is subjected to mixing and breaking up in sand mill, then Powder is dried at 135 DEG C, re-sieving after drying, sieve is 200-220 mesh, is then placed in sintering furnace and is sintered, and is sintered Temperature is 1200 DEG C, finally so that diameter of particle is reached 7-10 microns in grinder sintered product.When prepared by material second, use Fine copper, copper content 99.99%；Raw material is put into induction furnace melting in melting, smelting temperature is 1275 DEG C, obtains aluminium alloy Body；Alloy liquid injection is located in the tundish on atomizer, aluminium alloy is flowed out by tundish bottom leakage eye, passes through spray It meets and is atomized as fine drop with high-speed flow when mouth, atomized drop is rapidly solidificated into alloyed powder in closed atomizing cup End, alloy powder average particle size are 8-10 μm, atomization pressure 9MPa, and liquid metal fluid flow is 4kg/min, is closed Golden liquid implantation temperature is 1245 DEG C, 32 degree of atomizing angle.When prepared by material third, first 275 steel scraps are put into carbonic acid soda lye Reason 1.5 hours, sodium carbonate liquor concentration is 3%, 65 DEG C of alkali liquid temperature；It is dried after being rinsed 3 times with clear water again after base extraction is complete, It can be put into melting in induction furnace, then place into the substance for the respective element that Nd, Au, Ge, Lu, Zr and 275 steel scraps are related to, melted It is 1595 DEG C to refine temperature, obtains alloy liquid；By alloy liquid injection be located at atomizer on tundish in, aluminium alloy by Tundish bottom leaks eye outflow, and meeting with high-speed flow when passing through nozzle is atomized as fine drop, and atomized drop is closed Alloy powder is rapidly solidificated into atomizing cup, alloy powder average particle size is 8-11 μm, atomization pressure 3MPa, liquid Metal fluid flow is 3kg/min, and alloy liquid implantation temperature is 1575 DEG C, 34 degree of atomizing angle.When the preparation of material fourth, according to Weight percentage carries out dispensing；Nd, Au, Ge, Lu, Zr, Fe are the pure material that constituent content is more than 99.9%；B is in ferro-boron Between the form of alloy be added, the amount containing B of ferro-boron intermediate alloy is 25%；First by melting in raw material induction furnace, smelting temperature is 1625 DEG C, obtain master alloy liquid；Melting master alloy liquid is poured under nitrogen protection on forming furnace turntable, forms slab；Turntable The linear velocity of pour point be 23m/s, slab thickness be 3 millimeters, long width be 6.5 millimeters, be then placed in one it is salable Reaction kettle, reaction kettle is passed through H2After S gases, heat 1200 DEG C, time 2.5h, then take out it is air-cooled, then will treated casting Piece is put into vacuum degree as 0.17Pa, and the hydrogen crushing furnace progress hydrogen that air pressure is 1.2atm in stove is broken, and temperature is heated to 308 DEG C, hydrogen broken 38 Minute obtains coarse powder；Then it is fine powder coarse powder to be put into coarse powder mill in airflow milling, and it is 6-9 μm that average particle size, which is made, air-flow Powder-grinding pressure 7atm.
Embodiment 6：
The magnetic property of embodiment 1-5 materials and CN201610136736.0 materials is measured respectively.Subtracting quantity of magnetism test method is, Be prepared into φ 10*10mm magnet magnetize after, be put into 160 DEG C of baking oven after 8 hours, take out and measure its flux loss and subtract magnetic Rate.
Measurement result is as shown in the table.
The effect of above-described embodiment is specifically to introduce the essentiality content of the present invention, but those skilled in the art should know Protection scope of the present invention should not be confined to the specific embodiment by road.

Claims (6)

1. a kind of composite magnetic, which is characterized in that it is made of material first, material second, material third and material fourth, material first, The weight ratio of material second, material third and material fourth is (0.06-0.09):(0.03-0.08):(0.01-0.04):1；
The weight percentage of each ingredient is in material first：Al2O323-25%, ZrO20.5-0.8%, ZnO 4-9%, BaO 5-8%, MnO 4-8%, Li2O 1-4%, Fe2O30.7-1.3%, GeO20.1-0.4%, Nd2O30.001-0.003%, Lu2O30.001-0.003%, K2O 1-4%, B2O31-2.5%, surplus SiO2；
Material second is fine copper, copper content 99.99%；
The weight percentage of each ingredient is in material third：C 0.28-0.38%；Mn 0.50-0.80%；Si 0.30- 0.5%；S 0.02-0.05%, P 0.02-0.045%, Nd 0.4-0.8%, Au 0.03-0.08%, Ge 0.03- 0.09%, Lu 0.03-0.08%, Zr 0.02-0.05%, surplus Fe；
The weight percentage of each ingredient is in material fourth：B 3-5.5%, Nd 24-28%, Au 0.3-0.6%, Ge 0.8- 1.3%, Lu 0.05-0.09%, S 0.8-1.2%, Zr 0.8-1.4%, surplus Fe.
2. the preparation method of composite magnetic described in claim 1, which is characterized in that include the following steps：Material first, material Second, material third and material fourth weight ratio are (0.06-0.09):(0.03-0.08):(0.01-0.04):After 1 dispensing, it is added to three It ties up in mixing machine and is uniformly mixed, obtain mixed powder；Then mixed powder is orientated in Magnetic field press, using isostatic pressed mode at Type；Molded blank is put into sintering furnace under protection of argon gas to be sintered, is first warming up to 660-700 DEG C, 3-4h is kept the temperature, then rises Temperature after being cooled to room temperature, carries out double tempering processing, i.e., respectively in 650-690 DEG C and 560- to 1000-1090 DEG C of sintering 3-4h 590 DEG C of tempering heat treatment 1-2h；Most product is obtained through 200-230 DEG C of ageing treatment afterwards.
3. preparation method according to claim 2, it is characterised in that：Material first prepare when according to weight percent be Al2O3 23-25%, ZrO20.5-0.8%, ZnO 4-9%, BaO 5-8%, MnO 4-8%, Li2O 1-4%, Fe2O3 0.7- 1.3%, GeO20.1-0.4%, Nd2O30.001-0.003%, Lu2O30.001-0.003%, K2O 1-4%, B2O3 1- 2.5%, surplus SiO2Dispensing is carried out, each material purity is all higher than 99.9%；Each raw material is carried out in sand mill mixing and It is broken, then powder is dried at 130-140 DEG C, re-sieving after drying, sieve is 200-220 mesh, is then placed in sintering furnace It is sintered, sintering temperature is 1190-1210 DEG C, finally so that diameter of particle is reached 7-10 in grinder sintered product micro- Rice.
4. preparation method according to claim 2, it is characterised in that：When prepared by material second, the fine copper of use, copper content 99.99%；Raw material is put into induction furnace melting in melting, smelting temperature is 1260-1290 DEG C, obtains alloy liquid；It will close The injection of golden liquid is located in the tundish on atomizer, and aluminium alloy is flowed out by tundish bottom leakage eye, when passing through nozzle with High-speed flow, which meets, to be atomized as fine drop, and atomized drop is rapidly solidificated into alloy powder, alloy in closed atomizing cup Powder mean particle sizes are 8-10 μm, atomization pressure 8-10MPa, and liquid metal fluid flow is 3-5kg/min, alloy Liquid implantation temperature is 1230-1260 DEG C, and atomizing angle is 32 degree.
5. preparation method according to claim 2, it is characterised in that：When prepared by material third, 275 steel scraps are first put into carbonic acid It is handled 1-2 hours in soda lye, sodium carbonate liquor concentration is 2-4%, 60-70 DEG C of alkali liquid temperature；It is used again after base extraction is complete clear Water is dried after rinsing 3 times, can be put into melting in induction furnace, then places into Nd, Au, Ge, Lu, Zr and 275 steel scraps are related to The substance of respective element, smelting temperature are 1580-1610 DEG C, obtain alloy liquid；The ingredient of alloy liquid is C 0.28- 0.38%；Mn 0.50-0.80%；Si 0.30-0.5%；S 0.02-0.05%, P 0.02-0.045%, Nd 0.4- 0.8%, Au 0.03-0.08%, Ge 0.03-0.09%, Lu 0.03-0.08%, Zr 0.02-0.05%, surplus Fe；It will Alloy liquid injection is located in the tundish on atomizer, and aluminium alloy is flowed out by tundish bottom leakage eye, when passing through nozzle It meets and is atomized as fine drop with high-speed flow, atomized drop is rapidly solidificated into alloy powder in closed atomizing cup, closes Golden powder mean particle sizes are 8-11 μm, atomization pressure 2-4MPa, and liquid metal fluid flow is 2-4kg/min, is closed Golden liquid implantation temperature is 1560-1590 DEG C, and atomizing angle is 34 degree.
6. preparation method according to claim 2, it is characterised in that：When the preparation of material fourth, according to weight percentage For B 3-5.5%, Nd 24-28%, Au 0.3-0.6%, Ge 0.8-1.3%, Lu 0.05-0.09%, S 0.8-1.2%, Zr 0.8-1.4%, surplus are that Fe carries out dispensing；Nd, Au, Ge, Lu, Zr, Fe are the pure material that constituent content is more than 99.9%；B It is added in the form of ferro-boron intermediate alloy, the amount containing B of ferro-boron intermediate alloy is 24-26%；First by melting in raw material induction furnace, melt It is 1610-1640 DEG C to refine temperature, obtains master alloy liquid；Melting master alloy liquid is poured under nitrogen protection on forming furnace turntable, Form slab；The linear velocity of turntable pour point is 21-25m/s, and slab thickness is 2-4 millimeters, and long width is 5-8 millimeters, It is then placed in a sealable reaction kettle, reaction kettle is passed through H2After S gases, 1100-1300 DEG C, time 2-3h is heated, then Take out it is air-cooled, then will treated slab is put into vacuum degree is 0.15-0.18Pa, the hydrogen crushing furnace that air pressure is 1.0-1.4atm in stove Progress hydrogen is broken, and temperature is heated to 300-315 DEG C, and broken 35-40 minutes of hydrogen obtains coarse powder；Then coarse powder is put into airflow milling will be thick Grinding is fine powder, and it is 6-9 μm that average particle size, which is made, airflow milling powder pressure 6-8atm.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111347054A (en) * 2018-12-21 2020-06-30 财团法人金属工业研究发展中心 Magnetic powder composite material and preparation method thereof
CN114539723A (en) * 2022-04-21 2022-05-27 空间液态金属科技发展(江苏)有限公司 High-performance thermal interface material with anisotropy and preparation method thereof

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JP2012212782A (en) * 2011-03-31 2012-11-01 Tdk Corp Rare earth magnet, method of manufacturing the same, and rotary machine
CN107321998A (en) * 2017-07-24 2017-11-07 清远先导材料有限公司 The preparation method of copper gallium alloy powder
CN107564651A (en) * 2017-08-11 2018-01-09 南京信息工程大学 A kind of high remanent magnetism material and preparation method thereof

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JP2012212782A (en) * 2011-03-31 2012-11-01 Tdk Corp Rare earth magnet, method of manufacturing the same, and rotary machine
CN107321998A (en) * 2017-07-24 2017-11-07 清远先导材料有限公司 The preparation method of copper gallium alloy powder
CN107564651A (en) * 2017-08-11 2018-01-09 南京信息工程大学 A kind of high remanent magnetism material and preparation method thereof

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CN111347054A (en) * 2018-12-21 2020-06-30 财团法人金属工业研究发展中心 Magnetic powder composite material and preparation method thereof
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Application publication date: 20180914