CN108389676A - A kind of temperature tolerance permanent-magnet material and preparation method thereof - Google Patents
A kind of temperature tolerance permanent-magnet material and preparation method thereof Download PDFInfo
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- CN108389676A CN108389676A CN201810271970.3A CN201810271970A CN108389676A CN 108389676 A CN108389676 A CN 108389676A CN 201810271970 A CN201810271970 A CN 201810271970A CN 108389676 A CN108389676 A CN 108389676A
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- 239000000463 material Substances 0.000 title claims abstract description 71
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000956 alloy Substances 0.000 claims abstract description 101
- 229910010272 inorganic material Inorganic materials 0.000 claims abstract description 28
- 239000011147 inorganic material Substances 0.000 claims abstract description 28
- 238000005245 sintering Methods 0.000 claims abstract description 19
- 239000004615 ingredient Substances 0.000 claims description 37
- 229910052779 Neodymium Inorganic materials 0.000 claims description 36
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 34
- 229910052715 tantalum Inorganic materials 0.000 claims description 34
- 229910052710 silicon Inorganic materials 0.000 claims description 23
- 229910052717 sulfur Inorganic materials 0.000 claims description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- 229910052782 aluminium Inorganic materials 0.000 claims description 13
- 229910052745 lead Inorganic materials 0.000 claims description 10
- 229910052698 phosphorus Inorganic materials 0.000 claims description 10
- 229910052748 manganese Inorganic materials 0.000 claims description 9
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims description 8
- 229910052681 coesite Inorganic materials 0.000 claims description 8
- 229910052906 cristobalite Inorganic materials 0.000 claims description 8
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 claims description 8
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 claims description 8
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- 229910052682 stishovite Inorganic materials 0.000 claims description 8
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 8
- 229910052905 tridymite Inorganic materials 0.000 claims description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 229910052593 corundum Inorganic materials 0.000 claims description 7
- 239000011812 mixed powder Substances 0.000 claims description 7
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 5
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 claims description 5
- 238000005496 tempering Methods 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 14
- 238000000034 method Methods 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 229910045601 alloy Inorganic materials 0.000 description 18
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 18
- 239000000843 powder Substances 0.000 description 15
- 239000007788 liquid Substances 0.000 description 10
- 239000010949 copper Substances 0.000 description 9
- 230000005389 magnetism Effects 0.000 description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 8
- 229910000838 Al alloy Inorganic materials 0.000 description 7
- 229910001172 neodymium magnet Inorganic materials 0.000 description 7
- 229910052761 rare earth metal Inorganic materials 0.000 description 7
- 150000002910 rare earth metals Chemical class 0.000 description 7
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 6
- 238000002844 melting Methods 0.000 description 6
- 238000013461 design Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 229910017493 Nd 2 O 3 Inorganic materials 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 230000006698 induction Effects 0.000 description 3
- 229910000714 At alloy Inorganic materials 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 description 2
- 238000000889 atomisation Methods 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000002513 implantation Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 229910001338 liquidmetal Inorganic materials 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 230000008520 organization Effects 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- ADOYQDMYXWMVDP-UHFFFAOYSA-N [Nd].[B].[Fe].[Nd] Chemical compound [Nd].[B].[Fe].[Nd] ADOYQDMYXWMVDP-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- 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
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The invention discloses a kind of temperature tolerance permanent-magnet material and preparation method thereof, the temperature tolerance permanent-magnet material, which is made of alloy material A, alloy material B, alloy material C and inorganic material D mixed sinterings.Temperature tolerance permanent-magnet material preparation process is easy, prepares that raw materials used cost is relatively low, and process is simple, and temperature tolerance permanent-magnet material is with good performance, is convenient for industrialized production.Temperature tolerance permanent-magnet material prepared by the present invention is suitable for electrical apparatus industry.
Description
Technical field
The present invention relates to functional composite material technical field, specifically a kind of temperature tolerance permanent-magnet material and its preparation side
Method.
Background technology
Chinese patent literature CN101719405A proposes pair of low energy consumption corrosion resistant aluminum alloy and neodymium iron boron type rare earth permanent magnet
Phase material, preparation process：By neodymium iron boron type rare earth permanent magnet material and aluminium alloy powder processed respectively, neodymium iron boron type rare earth permanent magnet material
Size distribution is 3-10 μm, and the size distribution of Al alloy powder is 0.05-3 μm, and the above two powder prepared is uniformly mixed,
Wherein the volume fraction of Al alloy powder is 2-25%, and mixed powder, the compression moulding in magnetic field, burns in vacuum sintering furnace
Magnet processed, sintering temperature are less than 660 DEG C.It is pair that aluminium alloy and neodymium iron boron type rare earth permanent magnet material are prepared using powder metallurgic method
The method of phase material.This material has many advantages, such as the high remanent magnetism of neodymium iron boron type rare earth permanent magnet material and high-coercive force, improves list
The mechanical property and corrosion resistance of pure powder metallurgy neodymium iron boron neodymium type rare earth permanent-magnetic material, machinability are good.Sintering temperature is less than
660 DEG C, energy consumption is far below pure neodymium iron boron type rare earth permanent magnet material.But the maximum magnetic energy product of the material is not high enough.
Invention content
The purpose of the present invention is the deficiencies in for the above-mentioned prior art, provide a kind of temperature tolerance permanent-magnet material.
It is a further object of the present invention to provide the preparation methods of temperature tolerance permanent-magnet material.
The purpose of the present invention is what is be achieved through the following technical solutions：
A kind of temperature tolerance permanent-magnet material, the temperature tolerance permanent-magnet material is by alloy material A, alloy material B, alloy material C and inorganic
Material D mixed sinterings are made, wherein：
The weight percentage of each ingredient is in alloy material A：B 1.5~4.5%, Nd 23~28%, Pb 3~5%, Ta
0.05~0.09%, Gd 0.1~0.5%, S 0.8~1.2%, remaining Fe,
The weight percentage of each ingredient is in alloy material B：C 0.06~0.12%, Mn 0.25~0.50%, Si 0.2-
0.35%, S 0.03-0.050%, P 0.03-0.045%, Nd 2~5%, Gd 0.1~0.5%, Ta 0.05~
0.09%, remaining Fe,
The weight percentage of each ingredient is in alloy material C：Ni 12-16 %, Al 2-5%, Si 2-5%, Nd 0.002
~0.005%, Gd 0.001~0.005%, Ta 0.001~0.004%, remaining Cu,
The weight percentage of each ingredient is in inorganic material D：Al2O313-18%, ZnO 3-5%, BaO 3-5%, MnO
2-4%, Li2O 4-6%, Fe2O30.1-0.3%, TiO20.1-0.4%, K2O 1-4%, B2O31-2.5%,
Ta2O50.001-0.003%, Nd2O3 0.001-0.003%, Gd2O3 0.001-0.003%, remaining SiO2。
In the further design scheme of the present invention, alloy material A, alloy material B, alloy material C and inorganic material D weight
Than being 1：（0.12-0.15）：（0.012-0.016）：（0.001-0.005）.
A kind of preparation method of temperature tolerance permanent-magnet material, includes the following steps：
Step 1 prepares alloy material A, alloy material B, alloy material C and inorganic material D respectively.
Step 2, by alloy material A, alloy material B, alloy material C and inorganic material D weight ratios be 0.05：（1-1.3）：
（0.003-0.008）：（0.05-0.09）Dispensing is carried out, is added in mixing machine and is uniformly mixed, obtain mixed powder.
Mixed powder is orientated by step 3 in Magnetic field press, is molded using isostatic pressed mode, is obtained molded blank.
Molded blank is put into sintering furnace and is sintered by step 4 under protection of argon gas, is first warming up to 600-750 DEG C, heat preservation
3-4h then heats to 990-1090 DEG C of sintering 3-4h.
Step 5 after being cooled to room temperature, carries out double tempering processing, i.e., respectively at 690-710 DEG C and 540-570 DEG C of heat
Reason tempering 1-2h, finally heated 210-250 DEG C of heat preservation obtain temperature tolerance permanent-magnet material product in 10-12 hours after postcooling.
In the further design scheme of the present invention, in step 1, the weight percentage of each ingredient is in alloy material A：B
1.5~4.5%, Nd 23~28%, Pb 3~5%, Ta 0.05~0.09%, Gd 0.1~0.5%, S 0.8~1.2%,
Remaining Fe.
Alloy material A primarily forms magnetic main phase Nd2Fe14B and time main phase Gd2Fe14B enhances magnetic coupling interaction, makes
The existing high coercivity of magnet in turn avoids remanent magnetism and declines to a great extent, to obtain higher comprehensive magnetic energy.In sintering process,
High-melting point alloy element Ta is added, can make that cenotype is precipitated in magnet tissue, eliminates the phenomenon that being in direct contact between main phase grain,
Effectively inhibit growing up for main phase grain, be conducive to obtain relatively fine uniform grain structure, while the heat that can improve main phase magnet is steady
It is qualitative.
In the further design scheme of the present invention, in step 1, the weight percentage of each ingredient is in alloy material B： C
0.06~0.12%, Mn 0.25~0.50%, Si 0.2-0.35%, S 0.03-0.050%, P 0.03-0.045%, Nd 2
~5%, Gd 0.1~0.5%, Ta 0.05~0.09%, remaining Fe.Alloy material B, which improves the reason of intrinsic coercivity, is,
Secondary phase Fe-riched phase between the main phase grain of formation, it is suppressed that crystal grain intersection particle is grown up, and has refined main phase grain, therefore just press down
The enhancing of their ambient stray fields has been made, and then has improved intrinsic coercivity.Nd, Gd, Ta and A material in B material is corresponding,
Prevent diffusion transfer of the key element in sintering in A materials.
In the further design scheme of the present invention, in step 1, the weight percentage of each ingredient is in alloy material C：Ni
12-16 %, Al 2-5%, Si 2-5%, Nd 0.002~0.005%, Gd 0.001~0.005%, Ta 0.001~
0.004%, remaining Cu.Alloy material C fusing points are low, reduce rich-Nd phase and the angle of wetting of main phase, inhibit growing up for main phase, make master
Boundary defect concentration is reduced, and magnetic reversal farmland is in interface forming core difficulty.In addition it can be distributed in around main phase grain to disperse, energy
It is enough effectively improved the institutional framework of Grain-Boundary Phase, crystal boundary modified, reinforcing Grain-Boundary Phase is carried out to magnet.Therefore the surplus of material is improved
Magnetic.Nd, Gd, Ta and A material in C-material is corresponding, it is therefore prevented that diffusion transfer of the key element in sintering in A materials.
In the further design scheme of the present invention, in step 1, the weight percentage of each ingredient is in inorganic material D：Ni
12-16 %, Al 2-5%, Si 2-5%, Nd 0.002~0.005%, Gd 0.001~0.005%, Ta 0.001~
0.004%, remaining Cu.Inorganic material D, that is, metal oxide bulk melting point is low, can be evenly distributed in main phase crystal boundary and play pinning work
With coercivity is improved.
The present invention has advantageous effect following prominent：
Temperature tolerance permanent-magnet material of the present invention has excellent magnetic energy.In addition it prepared alloy in kind and passes through proper treatment, ensure that
The uniformity of alloying component, tissue and performance ensure that the quality of alloy.Temperature tolerance permanent-magnet material preparation process is easy, system
Standby raw materials used cost is relatively low, and process is simple, and temperature tolerance permanent-magnet material is with good performance, is convenient for industrialized production.This hair
The temperature tolerance permanent-magnet material of bright preparation is suitable for electrical apparatus industry.
Description of the drawings
Fig. 1 is temperature tolerance permanent-magnet material organization chart in embodiment 1.
Specific implementation mode
The invention will be further described with reference to the accompanying drawings and embodiments:
Embodiment 1
A kind of temperature tolerance permanent-magnet material, by alloy material A, alloy material B, alloy material C and inorganic material D mixed sintering systems
At alloy material A, alloy material B, alloy material C and inorganic material D weight ratios are 1:0.12:0.012:0.001, wherein：
The weight percentage of each ingredient is in alloy material A：B 1.5%, Nd 23%, Pb 3%, Ta 0.05%, Gd
0.1%, S 0.8%, remaining Fe.
The weight percentage of each ingredient is in alloy material B：C 0.12%, Mn 0.50%, Si 0.2%, S
0.03%, P 0.03%, Nd 2%, Gd 0.1%, Ta 0.05%, remaining Fe.
The weight percentage of each ingredient is in alloy material C：Ni 12%, Al 2%, Si 2%, Nd 0.002%, Gd
0.001%, Ta 0.001%, remaining Cu.
The weight percentage of each ingredient is in inorganic material D：Al2O313%, ZnO 3%, BaO3%, MnO 2%,
Li2O 4%, Fe2O30.1%, TiO20.1%, K2O 1%, B2O31%, Ta2O50.001%, Nd2O30.001%,
Gd2O3 0.001%, remaining SiO2。
A kind of preparation method of temperature tolerance permanent-magnet material, includes the following steps：
Step 1 prepares alloy material A, alloy material B, alloy material C and inorganic material D respectively, wherein：
The preparation of alloy material A is B 1.5%, Nd 23%, Pb 3%, Ta 0.05%, Gd according to weight percentage
0.1%, S 0.8%, remaining Fe carry out dispensing.Nd, Pb, Ta, Gd, Fe are pure material（Constituent content is more than 99.9%）.B with
The form of ferro-boron intermediate alloy is added, and the amount containing B of ferro-boron intermediate alloy is 24-26%.S is added in the form of sulphur iron intermediate alloy,
The amount containing B of sulphur iron intermediate alloy is 40-50%.The first melting in induction furnace by raw material, smelting temperature are 1570~1590 DEG C, are obtained
To master alloy liquid, melting master alloy liquid is poured under nitrogen protection on forming furnace turntable, forms slab, turntable pour point
Linear velocity is 14~18m/s.Slab thickness is 1~3 millimeter, and long width is 5~8 millimeters.Be then placed in one it is salable
Reaction kettle, reaction kettle is passed through H2After S gases, 80 ~ 130 DEG C are heated, time 2-3h then takes out air-cooled.Again by treated
Slab is put into vacuum degree as 0.06~0.1Pa, and the hydrogen crushing furnace progress hydrogen that air pressure is 0.8~1.3atm in stove is broken, and temperature is heated to
280~305 DEG C, hydrogen obtains coarse powder in broken 450~50 minutes, and it is fine powder that then coarse powder, which is put into coarse powder mill in airflow milling, is made
Average particle size is 2~5 μm, 6~7atm of airflow milling powder pressure.
When prepared by alloy material B, first Q195 steel waste materials are put into sodium hydroxide lye and are handled 1-2 hours, sodium hydroxide
Solution concentration is 2-2.5%, 60-70 DEG C of alkali liquid temperature.It dries, can be put into after being rinsed 3 times with clear water again after base extraction is complete
Melting in induction furnace is then placed in Nd, Gd and Ta, and smelting temperature is 1610~1630 DEG C, obtains alloy liquid, alloy liquid
Ingredient is C 0.12%, Mn 0.50%, Si 0.2%, S 0.03%, P 0.03%, Nd 2%, Gd 0.1%, Ta
0.05%, remaining Fe.Alloy liquid injection is located in the tundish on atomizer.Aluminium alloy leaks eye by tundish bottom
Outflow is met with high-speed flow when passing through nozzle and is atomized as fine drop, atomized drop fast rapid hardening in closed atomizing cup
Gu at alloy powder.Alloy powder average particle size is 8~12 μm.Atomization pressure is 4.5-6.0MPa.Flow of liquid metal
Body flow is 3-5kg/min.Alloy liquid implantation temperature is 1590~1610 DEG C.Atomizing angle is 30 degree.
When prepared by alloy material C, by Ni 12%, Al 2%, Si 2%, Nd 0.002%, Gd 0.001%, Ta
0.001%, remaining Cu carry out dispensing, and Ni, Al, Si, Nd, Gd, Ta, Cu raw material are pure material.Raw material is put into induction furnace
Melting, smelting temperature are 1230~1290 DEG C, obtain copper alloy liquid, during alloy liquid injection is located on atomizer
Between packet in.Aluminium alloy is met with high-speed flow when passing through nozzle and is atomized as fine drop, mist by tundish bottom leakage eye outflow
Change drop and is rapidly solidificated into alloy powder in closed atomizing cup.Alloy powder average particle size is 3~8 μm.Atomization gas
Pressure is 4.5-6.0MPa.Liquid metal fluid flow is 3-5kg/min.Alloy liquid implantation temperature is 1200~1230 DEG C.
Atomizing angle is 30 degree.
Inorganic material D is Al according to weight percent2O313%, ZnO 3%, BaO3%, MnO 2%, Li2O 4%,
Fe2O30.1%, TiO20.1%, K2O 1%, B2O31%, Ta2O50.001%, Nd2O30.001%, Gd2O3
0.001%, remaining SiO2Dispensing is carried out, each material purity is all higher than 99.9%, each raw material is mixed and broken in sand mill
It is broken, then powder is dried at 120-130 DEG C, re-sieving after drying, sieve be 200-220 mesh, be then placed in sintering furnace into
Row sintering.Sintering temperature is 1230-1290 DEG C, finally so that diameter of particle is reached 8-12 microns in grinder sintered product.
Step 2, by alloy material A, alloy material B, alloy material C and inorganic material D weight ratios be 1:0.12:0.012:
0.001 carries out dispensing, is added in three-dimensional mixer and is uniformly mixed, obtains mixed powder,
Mixed powder is orientated by step 3 in Magnetic field press, is molded using isostatic pressed mode, is obtained molded blank.
Molded blank is put into sintering furnace and is sintered by step 4 under protection of argon gas, is first warming up to 600-750 DEG C, heat preservation
3-4h then heats to 990-1090 DEG C of sintering 3-4h.
Step 5 after being cooled to room temperature, carries out double tempering processing, i.e., respectively at 690-710 DEG C and 540-570 DEG C of heat
Reason tempering 1-2h, most obtains temperature tolerance permanent-magnet material product through 210-250 DEG C of ageing treatment afterwards.
With micro- sem observation temperature tolerance permanent-magnet material product, the organization chart of temperature tolerance permanent-magnet material product is by attached drawing 1, it is seen that
Even tissue is fine and close.It analyzes after testing, the maximum magnetic energy product of temperature tolerance permanent-magnet material is 46 (BH) max/MGOe, and coercivity is
23.5Hcj/ KOe, remanent magnetism are 14.1Br/ KGs.Weightless 0.4mg/cm2, it is superior in Chinese patent literature CN101719405A
The performance of material.
Embodiment 2
In the present embodiment, other than the raw material proportioning of alloy material A, alloy material B, alloy material C and inorganic material D are different,
Remaining and preparation method are same as Example 1.
In the present embodiment, the raw material proportioning of temperature tolerance permanent-magnet material is：1:0.13:0.014:0.003.
The weight percentage of each ingredient is in alloy material A：B2.5%, Nd26%, Pb4%, Ta0.07%,
Gd0.3%, S9%, remaining Fe.
The weight percentage of each ingredient is in alloy material B：C 0.09%, Mn 0.3%, Si 0.25%, S
0.04%, P 0.04%, Nd 3%, Gd 0.3%, Ta 0.07%, remaining Fe.
The weight percentage of each ingredient is in alloy material C：Ni 14 %, Al 3%, Si 4%, Nd 0.003%,
Gd 0.003%, Ta 0.002%, remaining Cu.
The weight percentage of each ingredient is in inorganic material D：Al2O315%, ZnO4%, BaO4%, MnO 3%,
Li2O 3%, Fe2O30.2%, TiO20.3%, K2O 3%, B2O32%, Ta2O50.002%,Nd 2 O 30.002%,Gd2O3
0.002%, remaining SiO2。
It analyzes after testing, the maximum magnetic energy product of temperature tolerance permanent-magnet material is 47 (BH) max/MGOe, and coercivity is
24.9Hcj/ KOe, remanent magnetism are 15.6Br/ KGs, weightless 0.2mg/cm2.It is superior in Chinese patent literature CN107424703A
The performance of material.
Embodiment 3
In the present embodiment, other than the raw material proportioning of alloy material A, alloy material B, alloy material C and inorganic material D are different,
Remaining and preparation method are same as Example 1.
In the present embodiment, the raw material proportioning of temperature tolerance permanent-magnet material is：1: 0.15: 0.016: 0.005.
The weight percentage of each ingredient is in alloy material A：B 4.5%, Nd 28%, Pb 5%, Ta 0.09%,
Gd 0.5%, S%, remaining Fe.
The weight percentage of each ingredient is in alloy material B：C 0.12%, Mn 0.50%, Si 0.35%, S
0.050%, P 0.045%, Nd 5%, Gd 0.5%, Ta 0.09%, remaining Fe.
The weight percentage of each ingredient is in alloy material C：Ni 16%, Al 5%, Si 5%, Nd 0.005%, Gd
0.005%, Ta 0.004%, remaining Cu.
The weight percentage of each ingredient is in inorganic material D：Al2O318%, ZnO 5%, BaO 5%, MnO 4%,
Li2O 6%, Fe2O30.3%, TiO20.4%, K2O 4%, B2O32.5%, Ta2O50.003%,Nd 2 O 30.003%,
Gd2O30.003%, remaining SiO2。
It analyzes after testing, the maximum magnetic energy product of temperature tolerance permanent-magnet material is 45 (BH) max/MGOe, and coercivity is
22.8Hcj/ KOe, remanent magnetism 15.1Br/KGs, weightless 0.3mg/cm2.It is superior in Chinese patent literature CN107424703A
The performance of material.
Embodiment 4
In the present embodiment, other than the raw material proportioning of alloy material A, alloy material B, alloy material C and inorganic material D are different,
Remaining and preparation method are same as Example 1.
In the present embodiment, the raw material proportioning of temperature tolerance permanent-magnet material is：1:0.1 :0.01 :0.0005.
The weight percentage of each ingredient is in alloy material A：B 1%, Nd 21%, Pb 2%, Ta 0.03%, Gd
0.05%, S 0.5%, remaining Fe,
The weight percentage of each ingredient is in alloy material B：C 0.04%, Mn0.2%, Si 0.1%, S 0.02%, P
0.02%, Nd 1%, Gd 0.05%, Ta 0.03%, remaining Fe,
The weight percentage of each ingredient is in alloy material C：Ni 10%, Al 1%, Si 1%, Nd 0.001%, Gd
0.0005%, Ta 0.0004%, remaining Cu,
The weight percentage of each ingredient is in inorganic material D：Al2O312%, ZnO 2%, BaO 2%, MnO 1%, Li2O
3%, Fe2O30.03%, TiO20.04%, K2O 0.8%, B2O30.8%, Ta2O50.0008%, Nd2O3 0.0007%,
Gd2O30.0006%, remaining SiO2。
It analyzes after testing, the maximum magnetic energy product of temperature tolerance permanent-magnet material is 43 (BH) max/MGOe, and coercivity is
21.3Hcj/ KOe, remanent magnetism are 13.2Br/ KGs, weightless 0.5mg/cm2.It is found that the temperature tolerance permanent magnetism material that the embodiment obtains
The performance of temperature tolerance permanent-magnet material of the sexuality of material less than embodiment 1-3.
Embodiment 5
In the present embodiment, other than the raw material proportioning of alloy material A, alloy material B, alloy material C and inorganic material D are different,
Remaining and preparation method are same as Example 1.
In the present embodiment, the raw material proportioning of temperature tolerance permanent-magnet material is：1:0.7:0.017:0.008.
The weight percentage of each ingredient is in alloy material A：B 5.5%, Nd 29%, Pb 7%, Ta 0.1%,
Gd0.8%, S2%, remaining Fe,
The weight percentage of each ingredient is in alloy material B：C 0.15%, Mn 0.8%, Si 0. 5%, S 0.06%, P
0.06%, Nd 6%, Gd 0.7%, Ta 0.11%, remaining Fe,
The weight percentage of each ingredient is in alloy material C：Ni 18%, Al 6%, Si 6%, Nd 0.008%, Gd
0.008%, Ta 0.006%, remaining Cu,
The weight percentage of each ingredient is in inorganic material D：Al2O320%, ZnO 7%, BaO 6%, MnO 5%, Li2O
8%, Fe2O30.5%, TiO20.6%, K2O5%, B2O33%, Ta2O50.005%,Nd 2 O 3 0.004%,Gd2O3
0.005%, remaining SiO2。
It analyzes after testing, the maximum magnetic energy product of temperature tolerance permanent-magnet material is 44 (BH) max/MGOe, and coercivity is
22.1Hcj/ KOe, remanent magnetism are 13.9Br/ KGs, weightless 0.6mg/cm2.It is found that the temperature tolerance permanent magnetism material that the embodiment obtains
The performance of temperature tolerance permanent-magnet material of the sexuality of material less than embodiment 1-3.
The above are preferred embodiments of the present invention, all any changes made according to the technical solution of the present invention, and generated function is made
When with range without departing from technical solution of the present invention, all belong to the scope of protection of the present invention.
Claims (7)
1. a kind of temperature tolerance permanent-magnet material, which is characterized in that the temperature tolerance permanent-magnet material is by alloy material A, alloy material B, conjunction
Golden material C and inorganic material D mixed sinterings are made, wherein：
The weight percentage of each ingredient is in alloy material A：B 1.5~4.5%, Nd 23~28%, Pb 3~5%, Ta
0.05~0.09%, Gd 0.1~0.5%, S 0.8~1.2%, remaining Fe；
The weight percentage of each ingredient is in alloy material B：C 0.06~0.12%, Mn 0.25~0.50%, Si 0.2-
0.35%, S 0.03-0.050%, P 0.03-0.045%, Nd 2~5%, Gd 0.1~0.5%, Ta 0.05~
0.09%, remaining Fe；
The weight percentage of each ingredient is in alloy material C：Ni 12-16 %, Al 2-5%, Si 2-5%, Nd 0.002
~0.005%, Gd 0.001~0.005%, Ta 0.001~0.004%, remaining Cu；
The weight percentage of each ingredient is in inorganic material D：Al2O313-18%, ZnO 3-5%, BaO 3-5%, MnO 2-
4%, Li2O 4-6%, Fe2O30.1-0.3%, TiO20.1-0.4%, K2O 1-4%, B2O31-2.5%, Ta2O5
0.001-0.003%, Nd2O3 0.001-0.003%, Gd2O3 0.001-0.003%, remaining SiO2。
2. temperature tolerance permanent-magnet material according to claim 1, which is characterized in that alloy material A, alloy material B, alloy material
Expect that C and inorganic material D weight ratios are 1：（0.12-0.15）：（0.012-0.016）：（0.001-0.005）.
3. a kind of preparation method of temperature tolerance permanent-magnet material, includes the following steps：
Step 1 prepares alloy material A, alloy material B, alloy material C and inorganic material D respectively；
Step 2, by alloy material A, alloy material B, alloy material C and inorganic material D weight ratios be 0.05：（1-1.3）：
（0.003-0.008）：（0.05-0.09）Dispensing is carried out, is added in mixing machine and is uniformly mixed, obtain mixed powder；
Mixed powder is orientated by step 3 in Magnetic field press, is molded using isostatic pressed mode, is obtained molded blank；
Molded blank is put into sintering furnace and is sintered by step 4 under protection of argon gas, is first warming up to 600-750 DEG C, keeps the temperature 3-
4h then heats to 990-1090 DEG C of sintering 3-4h；
Step 5 after being cooled to room temperature, carries out double tempering processing, i.e., is heat-treated back respectively at 690-710 DEG C and 540-570 DEG C
Fiery 1-2h, 10-12 hours postcoolings of finally heated 210-250 DEG C of heat preservation, obtains temperature tolerance permanent-magnet material product.
4. the preparation method of temperature tolerance permanent-magnet material according to claim 3, which is characterized in that in step 1, alloy material
The weight percentage of each ingredient is in A：B 1.5~4.5%, Nd 23~28%, Pb 3~5%, Ta 0.05~0.09%,
Gd 0.1~0.5%, S 0.8~1.2%, remaining Fe.
5. the preparation method of temperature tolerance permanent-magnet material according to claim 3, which is characterized in that in step 1, alloy material
The weight percentage of each ingredient is in B：C 0.06~0.12%, Mn 0.25~0.50%, Si 0.2-0.35%, S
0.03-0.050%, P 0.03-0.045%, Nd 2~5%, Gd 0.1~0.5%, Ta 0.05~0.09%, remaining Fe.
6. the preparation method of temperature tolerance permanent-magnet material according to claim 3, which is characterized in that in step 1, alloy material
The weight percentage of each ingredient is in C：Ni 12-16 %, Al 2-5%, Si 2-5%, Nd 0.002~0.005%, Gd
0.001~0.005%, Ta 0.001~0.004%, remaining Cu.
7. the preparation method of temperature tolerance permanent-magnet material according to claim 3, which is characterized in that in step 1, inorganic material
The weight percentage of each ingredient is in D：Ni 12-16 %, Al 2-5%, Si 2-5%, Nd 0.002~0.005%, Gd
0.001~0.005%, Ta 0.001~0.004%, remaining Cu.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108922720A (en) * | 2018-08-16 | 2018-11-30 | 安徽信息工程学院 | The preparation method of magnetic core composite material |
| CN108922712A (en) * | 2018-08-16 | 2018-11-30 | 安徽信息工程学院 | Magnetic composite and preparation method thereof |
| CN108922711A (en) * | 2018-08-16 | 2018-11-30 | 安徽信息工程学院 | Rare earth modified material and preparation method thereof |
| CN108922719A (en) * | 2018-08-16 | 2018-11-30 | 安徽信息工程学院 | The preparation method of inorganic functional composite material |
| CN109087770A (en) * | 2018-08-16 | 2018-12-25 | 安徽信息工程学院 | magnetic function material |
| CN109102980A (en) * | 2018-08-16 | 2018-12-28 | 安徽信息工程学院 | The preparation method of Ferrite Material |
| CN109166685A (en) * | 2018-08-16 | 2019-01-08 | 安徽信息工程学院 | magnetic core composite material |
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| 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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| JPS6181603A (en) * | 1984-09-04 | 1986-04-25 | Tohoku Metal Ind Ltd | Preparation of rare earth magnet |
| 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 |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108922720A (en) * | 2018-08-16 | 2018-11-30 | 安徽信息工程学院 | The preparation method of magnetic core composite material |
| CN108922712A (en) * | 2018-08-16 | 2018-11-30 | 安徽信息工程学院 | Magnetic composite and preparation method thereof |
| CN108922711A (en) * | 2018-08-16 | 2018-11-30 | 安徽信息工程学院 | Rare earth modified material and preparation method thereof |
| CN108922719A (en) * | 2018-08-16 | 2018-11-30 | 安徽信息工程学院 | The preparation method of inorganic functional composite material |
| CN109087770A (en) * | 2018-08-16 | 2018-12-25 | 安徽信息工程学院 | magnetic function material |
| CN109102980A (en) * | 2018-08-16 | 2018-12-28 | 安徽信息工程学院 | The preparation method of Ferrite Material |
| CN109166685A (en) * | 2018-08-16 | 2019-01-08 | 安徽信息工程学院 | magnetic core composite material |
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