CN105321699A - Manufacturing method of neodymium-iron-boron series sintered magnet and magnet thereof - Google Patents
Manufacturing method of neodymium-iron-boron series sintered magnet and magnet thereof Download PDFInfo
- Publication number
- CN105321699A CN105321699A CN201410318913.8A CN201410318913A CN105321699A CN 105321699 A CN105321699 A CN 105321699A CN 201410318913 A CN201410318913 A CN 201410318913A CN 105321699 A CN105321699 A CN 105321699A
- Authority
- CN
- China
- Prior art keywords
- iron boron
- neodymium iron
- additive
- sintered magnet
- manufacture method
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical class [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- 239000000654 additive Substances 0.000 claims abstract description 38
- 230000000996 additive effect Effects 0.000 claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 28
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 27
- 239000010937 tungsten Substances 0.000 claims abstract description 27
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000002156 mixing Methods 0.000 claims abstract description 9
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910001172 neodymium magnet Inorganic materials 0.000 claims description 104
- 239000000843 powder Substances 0.000 claims description 33
- 238000005245 sintering Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 239000005543 nano-size silicon particle Substances 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 238000012545 processing Methods 0.000 claims description 8
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 6
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 6
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 4
- 238000010348 incorporation Methods 0.000 claims description 3
- 229910052733 gallium Inorganic materials 0.000 claims description 2
- 229910052758 niobium Inorganic materials 0.000 claims description 2
- 230000005389 magnetism Effects 0.000 abstract description 5
- -1 tungsten nitride Chemical class 0.000 abstract 2
- 239000006185 dispersion Substances 0.000 abstract 1
- 239000002994 raw material Substances 0.000 description 12
- 238000012360 testing method Methods 0.000 description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 239000013078 crystal Substances 0.000 description 8
- 229910010271 silicon carbide Inorganic materials 0.000 description 8
- 238000002844 melting Methods 0.000 description 7
- 230000008018 melting Effects 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 6
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 229910052779 Neodymium Inorganic materials 0.000 description 4
- 230000002159 abnormal effect Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 239000000314 lubricant Substances 0.000 description 4
- 235000012054 meals Nutrition 0.000 description 4
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical group [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 229910000521 B alloy Inorganic materials 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OLBVUFHMDRJKTK-UHFFFAOYSA-N [N].[O] Chemical compound [N].[O] OLBVUFHMDRJKTK-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 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
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000004453 electron probe microanalysis Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000005381 magnetic domain Effects 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
Abstract
The invention provides a manufacturing method of a neodymium-iron-boron series sintered magnet. The manufacturing method is characterized by including the procedure of additive mixing, wherein additives are nanometer tungsten or nanometer tungsten carbide or nanometer tungsten nitride or a combination of nanometer tungsten, nanometer tungsten carbide and nanometer tungsten nitride, and the mean dispersion grain diameter of the additives ranges from 10 nm to 200 nm. By means of the manufacturing method, the grain extraordinary growth (AGG) phenomenon can be effectively restrained, the coercivity of the neodymium-iron-boron series sintered magnet is improved accordingly, the principal phase can be reserved to a larger degree, and therefore the neodymium-iron-boron series sintered magnet has excellent residual magnetism.
Description
Technical field
The invention belongs to the field of Nd-Fe-B series sintered magnet, particularly a kind of manufacture method and magnet thereof being mixed into additive.
Background technology
Nd-Fe-B series sintered magnet is widely used in wind power generation, field of hybrid electric vehicles.Because operational environment is complicated, require that the Nd-Fe-B series sintered magnet used has excellent coercive force performance.Nd-Fe-B series sintered magnet is produced for the single alloy technique of employing, generally improves the coercive force of magnet by heavy rare earth element in interpolation, when especially producing the magnet of SH, UH and more than the EH trade mark, often excessive interpolation especially.But middle heavy rare earth resource is valuable, in recent years, the raw material market price of heavy rare earth rises steadily, and therefore, the coercive force improving magnet in the mode of heavy rare earth element in adding is faced with heavy cost pressure.
Chinese patent CN102237166A discloses a kind of preparation method of Nd-Fe-Bo permanent magnet material; wherein disclose: Nd Fe B alloys is broken, powder process; add nanometer silicon carbide again; then magnetic field orientating, compressing is carried out; finally carry out sintering and temper under vacuum or inert gas shielding, the Nd-Fe-B series sintered magnet with high-coercive force can be prepared.Wherein, the addition of nanometer silicon carbide is 0.02 ~ 3wt% for Nd Fe B alloys weight.The mechanism of action of this technical scheme is: the nano silicon carbide granulate of part is evenly spread in around principal phase in sintering, drawing process, intercept the magnetic coupling interaction of main phase grain, hinder growing up and the merging of adjacent main phase grain of main phase grain, the main phase grain of refinement sintered NdFeB, reaches the effect improving microstructure; And the nano silicon carbide granulate of another part carries out the inside of principal phase crystal, when under outfield and/or high temperature, when magnetic domain deflects, play pinning effect, stop neticdomain wall deflection and/or move, be conducive to improving coercive force; In addition, element silicon itself can substitute ferro element and occupy the brilliant position of K2 in Tetragonal, makes that total exchange interaction strengthens, anisotropy field improves, and is conducive to improving coercive force.But, researcher finds through test, according to the sintering process that the document discloses---sintering temperature is 1050 ~ 1090 DEG C, sintering time is 4 ~ 6h, and carborundum cannot be made evenly to be spread in the surrounding of principal phase or to enter the inside of principal phase, result of the test shows: after the sintering, element silicon mainly concentrates on crystal boundary triradius region, and the phenomenon of abnormal grain growth (AGG) can be detected in Nd-Fe-B series sintered magnet, detect finally by magnetic property, the coercive force of Nd-Fe-B series sintered magnet there is no and significantly improves; And change principal phase structure because element silicon substitutes ferro element, Magnetic Phase is reduced, the remanent magnetism of Nd-Fe-B series sintered magnet can be reduced.
Summary of the invention
The object of the invention is to, propose a kind of manufacture Nd-Fe-B series sintered magnet method being mixed into additive, and obtain the magnet with excellent magnetic energy according to the method.
Technical scheme of the present invention is, the manufacture method of Nd-Fe-B series sintered magnet comprises the operation being mixed into additive, and additive is nanometer tungsten or nanometer tungsten carbide or nano silicon nitride tungsten or its combination, and its average mark shot footpath is 10 ~ 200nm.Especially, when additive is nanometer tungsten, its average mark shot footpath is 40 ~ 100nm; When additive is nanometer tungsten carbide, its average mark shot footpath is 50 ~ 80nm; When additive is nano silicon nitride tungsten, its average mark shot footpath is 25 ~ 40nm.
Additive be mixed into the problem relating to solid solubility.The factor affecting solid solubility comprises: 1) ion size, and when the atomic radius relative difference of solute and host crystal is more than 14 ~ 15%, size factor is unfavorable for that solid solution generates, and the solid solubility between two solids is limited; 2) ioni valence, when two kinds of solid ioni valence summations that are only identical at ioni valence or jack per line ion are identical, just may meet electroneutral requirement and generate continuous solid solution.The essential element of Nd-Fe-B series sintered magnet crystal boundary is neodymium (Nd), it is less that the ionic radius of tungsten (W) and neodymium (Nd) and electronics form difference, therefore, the relative silicon (Si) of tungsten (W) has larger solid solubility in crystal boundary.Under identical sintering temperature, tungsten (W) can to a greater degree from the rich region of crystal boundary triradius to intergranular regional diffusion, thus be evenly distributed in around principal phase, play pinning (Pining) effect, prevent abnormal grain growth (AGG) phenomenon.And the essential element of Nd-Fe-B series sintered magnet principal phase is iron (Fe), the ionic radius of tungsten (W) and iron (Fe) and electronics form and differ greatly, and therefore, tungsten (W) enters in principal phase hardly.Relative interpolation silicon (Si), adding tungsten (W) can retain principal phase structure more, thus makes Nd-Fe-B series sintered magnet have excellent remanent magnetism (Br).In addition, tungsten (W) is mixed into as additive and carries out sintering but not carry out melting as raw material, reason is: one, as shown in Figure 1, tungsten (W) is mixed into raw material carry out melting and with get rid of band method cast time, raw materials melt alloy first forms the chilling crystalline substance (region 1) of tungstenic (W) on copper roller surface, then on chilling crystalline substance, form column crystal (region 2) again, such situation is unfavorable for pulverizing, and therefore will affect the magnetic property of Nd-Fe-B series sintered magnet; They are two years old, smelting temperature is more than 1400 DEG C, tungsten (W) has larger migration kinetic energy, wherein a part will enter the principal phase of Nd-Fe-B series sintered magnet, thus change principal phase structure, sintering temperature is below 1100 DEG C, the migration kinetic energy of tungsten (W) is less, almost be gathered in the Grain-Boundary Phase of Nd-Fe-B series sintered magnet, thus retain principal phase more, by contrast, tungsten (W) is mixed into carry out sintering as additive Nd-Fe-B series sintered magnet can be made to have excellent remanent magnetism (Br).
In certain preferred embodiment, the manufacture method of Nd-Fe-B series sintered magnet comprises the following steps: 1) by getting rid of band legal system for neodymium iron boron slab, and its average thickness controls to be 0.2 ~ 0.5mm; 2) neodymium iron boron slab is pulverized obtained neodymium iron boron powder; 3) by compressing for neodymium iron boron powder orientation, obtained neodymium iron boron pressed compact; 4) by obtained for neodymium iron boron pressed compact sintering Nd-Fe-B series sintered magnet; Wherein, in step 1) neodymium iron boron slab or step 2) neodymium iron boron powder in be mixed into additive, and its addition is 0.03 ~ 0.15wt% of neodymium iron boron slab or neodymium iron boron powder quality.
In certain preferred embodiment, step 1) neodymium iron boron slab also through heat treatment, wherein, heat treated temperature is 400 ~ 900 DEG C, and the processing time is 20min ~ 3h.The object that neodymium iron boron slab is heat-treated is: the rich neodymium crystal boundary that hands down fully is spread, reduces and reunite, the rich neodymium in Nd-Fe-B series sintered magnet can be made to have mutually evenly distribution.
In certain preferred embodiment, step 2) the average grain diameter of neodymium iron boron powder controls below 15 μm, Control for Oxygen Content is at below 2500ppm.The average grain diameter of neodymium iron boron powder is less, is more conducive to the flowing of nanometer additive; Oxygen content is lower, is more conducive to avoiding nanometer additive oxidized.
In certain preferred embodiment, step 2) in, neodymium iron boron powder mixes in high speed mixer with additive, and wherein, hybird environment is oxygen-free atmosphere, and batch mixer rotating speed is 300 ~ 2000rpm, and incorporation time is at least 30min.The conical mixer used with routine is compared with three-dimensional material mixer, the nanometer powder of additive is broken up by the blade of High Rotation Speed by high speed mixer, avoid the reunion of nanometer powder, be conducive to the intensity of raising Nd-Fe-B series sintered magnet and suppress abnormal grain growth (AGG) phenomenon.If it should be noted that in step 1) neodymium iron boron slab in be mixed into additive, then additive with neodymium iron boron slab through pulverizing, be blended in neodymium iron boron powder, directly this neodymium iron boron powder be placed in high speed mixer and carry out mixing; If in step 2) in neodymium iron boron powder in be mixed into additive, then neodymium iron boron powder and additive can be placed in high speed mixer simultaneously mix, also the two can be placed in step by step high speed mixer and mix.
In certain preferred embodiment, mixing comprises following steps: 1) additive is placed in high speed mixer mixing 5 ~ 10min; 2) add neodymium iron boron powder again to mix.The particle diameter of additive is less than the particle diameter of neodymium iron boron powder, therefore more easily reunites, and after using high speed mixer first to be broken up by additive, then mixes with neodymium iron boron powder, can improve the uniformity of the two mixing.
Based on the Nd-Fe-B series sintered magnet that said method manufactures, it comprises following material composition:
RaFe100-a-b-c-d-e-fBbCocAldCueMf; Wherein, a, b, c, d, e, f, g are the percentage by weight of each element, 28≤a≤32wt%, 0.9≤b≤1.3wt%, 0.5≤c≤3.0wt%, 0.1≤d≤0.8wt%, 0.05≤e≤0.5wt%, 0.05≤f≤0.4wt%; R is the rare earth element containing Y; M is selected from least one of Ga or Nb.
In certain preferred embodiment, in magnet, the volume ratio of rich W phase is 5.0 ~ 11.0%.
Compared with prior art, the manufacture method of Nd-Fe-B series sintered magnet of the present invention effectively can suppress the phenomenon of abnormal grain growth (AGG), thus improves the coercive force of neodymium iron boron magnetic body, and, principal phase can be retained to a greater degree, thus make neodymium iron boron magnetic body have excellent remanent magnetism.
Accompanying drawing explanation
Fig. 1 is the crystallization schematic diagram of raw materials melt alloy after the chilling of copper roller surface.
Embodiment
Embodiment one
The preparation section of Nd-Fe-B series sintered magnet is as follows:
1) by the component preparation raw material of table 1.
The raw material composition table of table 1 embodiment one
2) raw material prepared is put into alumina crucible, be placed in high-frequency vacuum induction melting furnace, be evacuated to 10
-2pa, carries out vacuum melting with the temperature of 1450 DEG C.
3) vacuum melting terminates, and passes into argon gas, make air pressure to 5 × 10 in smelting furnace
4pa, use is got rid of band method and is cast, with 10
2~ 10
4dEG C/cooling rate of s obtains neodymium iron boron slab, controls the average thickness of neodymium iron boron slab at 0.3mm.Neodymium iron boron slab is placed in heat-treatment furnace, carries out the heat treatment of 2h with the temperature of 600 DEG C.
4) neodymium iron boron slab is put into hydrogen broken furnace, vacuumize, then pass into the hydrogen that purity is 99.99%, reach 0.1MPa to air pressure, maintain 2h, back vacuumize limit heat up, at the temperature of 500 DEG C, vacuumize 2h, naturally cool afterwards, obtain neodymium iron boron meal.
5) in neodymium iron boron meal, add the antioxidant of 0.05 ~ 0.20wt% (with neodymium iron boron meal weight for benchmark), air-flow grinding machine is put into after stirring, the pressure of pulverizing chamber is 0.4MPa, carries out air-flow crushing to neodymium iron boron meal, obtains the neodymium iron boron powder that granularity is less.To neodymium iron boron dust sampling, detect with MS2000 laser particle size analyzer, average grain diameter (D50) is 4.3 μm; Use oxygen-nitrogen analyzer to detect in an inert atmosphere, oxygen content is 2420ppm.
6) in neodymium iron boron powder, add additive and lubricant, mixed by high speed mixer, wherein, the content of lubricant is 0.05 ~ 0.10wt% of neodymium iron boron powder weight.Vacuumize in high speed mixer, batch mixer rotating speed is 2000rpm, and the processing time is 30min.Afterwards mixed-powder is packed into mould, then mould is put into right angle orientation type pressing under magnetic field machine, with the magnetic field intensity of 1.6 ~ 2.0T, 1.0 ~ 1.8T/cm
2briquetting pressure suppress, the demoulding afterwards obtains neodymium iron boron pressed compact, and its oxygen content is 1450ppm.
7) neodymium iron boron pressed compact is put into sintering furnace, be evacuated to 10
-3pa, with the temperature of 1040 DEG C sintering 4h, then logical argon gas is to 0.08MPa, is cooled to room temperature, obtains the Nd-Fe-B series sintered magnet that oxygen content is below 2500ppm.
8) by neodymium iron boron magnetic body in argon gas atmosphere, 1.5h heat treatment is carried out with the temperature of 600 DEG C, use NIM-10000H type magnetic property detector to detect the magnetic property of magnet afterwards, and use FE-EPMA (Jeol Ltd.) to observe magnet sample.
According to the preparation section of above Nd-Fe-B series sintered magnet, change operation 6) additive carry out contrast test, and detect the magnetic property of prepared magnet.As shown in table 2, be additive comparative test result.Wherein, SiC represents nanometer silicon carbide, and W represents nano-tungsten powder, and WC represents nanometer tungsten carbide, and WN represents nano silicon nitride tungsten.
Table 2 additive comparative test result
Can observe from the data of upper table, adopt technique of the present invention, add the main magnetic property of nanometer tungsten or nanometer tungsten carbide or nano silicon nitride tungsten or its Sintered NdFeB magnet combined apparently higher than the Sintered NdFeB magnet without additive and interpolation carborundum.
Embodiment two
Preparation raw material is carried out by the component of table 3.
The raw material composition table of table 3 embodiment two
Manufacturing process is substantially with embodiment one, and local process parameter adjustment is as follows:
Operation 2) in, carry out vacuum melting with the temperature of 1470 DEG C;
Operation 3) in, the average thickness of neodymium iron boron slab is controlled at 0.5mm, is placed in heat-treatment furnace afterwards, regulate treatment temperature and processing time to carry out contrast test;
Operation 5) in, the average grain diameter (D50) of neodymium iron boron powder is 7.6 μm, and oxygen content is 2390ppm;
Operation 6) in, be first 40nm by average mark shot footpath, addition is that the nanometer tungsten of the 0.07wt% of neodymium iron boron powder quality is placed in high speed mixer mixing 10min, again neodymium iron boron powder and lubricant are placed in high speed mixer to mix, vacuumize in high speed mixer, batch mixer rotating speed is 1800rpm, and the processing time is 40min;
Operation 8) in, by neodymium iron boron magnetic body in argon gas atmosphere, carry out 1h heat treatment with the temperature of 650 DEG C.
As shown in table 4, be regulate operation 3) treatment temperature and the result of the test in processing time:
Table 4 neodymium iron boron slab heat treatment comparative test result
Can observe from the data of upper table, in technique of the present invention, after heat treatment, the magnetic property of manufactured neodymium iron boron magnetic body is apparently higher than not carrying out processing for neodymium iron boron slab.
Embodiment three
Preparation raw material is carried out by the component of table 5.
The raw material composition table of table 5 embodiment three
Manufacturing process is substantially with embodiment one, and local process parameter adjustment is as follows:
Operation 2) in, carry out vacuum melting with the temperature of 1450 DEG C;
Operation 3) in, control at 0.2mm by the average thickness of neodymium iron boron slab, be placed in heat-treatment furnace afterwards, treatment temperature is 800 DEG C, and the processing time is 2h/3;
Operation 5) in, the average grain diameter (D50) of neodymium iron boron powder is 8.9 μm, and oxygen content is 2370ppm;
Operation 6) in, be first 80nm by average mark shot footpath, addition is that the nanometer tungsten carbide of the 0.11wt% of neodymium iron boron powder quality is placed in high speed mixer mixing 5min, again neodymium iron boron powder and lubricant are placed in high speed mixer to mix, in addition, the technological parameter of high speed mixer is regulated to carry out contrast test;
Operation 8) in, by neodymium iron boron magnetic body in argon gas atmosphere, carry out 2h heat treatment with the temperature of 550 DEG C.
As shown in table 6, for regulating the result of the test of the technological parameter of high speed mixer:
Table 6 high speed mixer technological parameter comparative test result
Can observe from the data of upper table, in technique of the present invention, be 1000 ~ 2000rpm by the speed setting of high speed mixer, incorporation time is set as at least 30min, and the performance of the neodymium iron boron magnetic body obtained is comparatively excellent.
Specific embodiment described herein is only to the explanation for example of the present invention's spirit.Those skilled in the art can make various amendment or supplement or adopt similar mode substitute but can't depart from spirit of the present invention or surmount appended claims limited range to described specific embodiment.
Claims (9)
1. a manufacture method for Nd-Fe-B series sintered magnet, is characterized in that: comprise the operation being mixed into additive, and described additive is nanometer tungsten or nanometer tungsten carbide or nano silicon nitride tungsten or its combination, and its average mark shot footpath is 10 ~ 200nm.
2. manufacture method as claimed in claim 1, it is characterized in that: when described additive is nanometer tungsten, its average mark shot footpath is 40 ~ 100nm; When described additive is nanometer tungsten carbide, its average mark shot footpath is 50 ~ 80nm; When described additive is nano silicon nitride tungsten, its average mark shot footpath is 25 ~ 40nm.
3. manufacture method as claimed in claim 1, is characterized in that: comprise the following steps,
1) by getting rid of band legal system for neodymium iron boron slab, and the average thickness of described neodymium iron boron slab controls to be 0.2 ~ 0.5mm;
2) described neodymium iron boron slab is pulverized obtained neodymium iron boron powder;
3) by compressing for described neodymium iron boron powder orientation, obtained neodymium iron boron pressed compact;
4) by the obtained neodymium iron boron magnetic body of described neodymium iron boron pressed compact sintering;
Wherein, in step 1) described neodymium iron boron slab or step 2) described neodymium iron boron powder in be mixed into described additive, and its addition is 0.03 ~ 0.15wt% of described neodymium iron boron slab or described neodymium iron boron powder quality.
4. manufacture method as claimed in claim 3, is characterized in that: step 1) described neodymium iron boron slab also through heat treatment, wherein, described heat treated temperature is 400 ~ 900 DEG C, and the processing time is 20min ~ 3h.
5. manufacture method as claimed in claim 3, is characterized in that: step 2) the average grain diameter of described neodymium iron boron powder to control be less than 15 μm, Control for Oxygen Content is below 2500ppm.
6. manufacture method as claimed in claim 3, it is characterized in that: step 2) described neodymium iron boron powder mix in high speed mixer with described additive, wherein, hybird environment is oxygen-free atmosphere, batch mixer rotating speed is 1000 ~ 2000rpm, and incorporation time is at least 30min.
7. manufacture method as claimed in claim 6, is characterized in that: described mixing comprises the following steps: 1) described additive is placed in described high speed mixer mixing 5 ~ 10min; 2) add described neodymium iron boron powder again to mix.
8. based on the Nd-Fe-B series sintered magnet that the method for claim 1 manufactures, it is characterized in that, comprise following material composition:
RaFe100-a-b-c-d-e-fBbCocAldCueMf; Wherein, a, b, c, d, e, f, g are the percentage by weight of each element, 28≤a≤32wt%, 0.9≤b≤1.3wt%, 0.5≤c≤3.0wt%, 0.1≤d≤0.8wt%, 0.05≤e≤0.5wt%, 0.05≤f≤0.4wt%; R is the rare earth element containing Y; M is selected from least one of Ga or Nb.
9. Nd-Fe-B series sintered magnet as claimed in claim 8, is characterized in that: in described magnet, the volume ratio of rich W phase is 5.0 ~ 11.0%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410318913.8A CN105321699B (en) | 2014-07-07 | 2014-07-07 | A kind of manufacture method and its magnet of Nd-Fe-B series sintered magnet |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410318913.8A CN105321699B (en) | 2014-07-07 | 2014-07-07 | A kind of manufacture method and its magnet of Nd-Fe-B series sintered magnet |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105321699A true CN105321699A (en) | 2016-02-10 |
| CN105321699B CN105321699B (en) | 2017-11-24 |
Family
ID=55248878
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410318913.8A Active CN105321699B (en) | 2014-07-07 | 2014-07-07 | A kind of manufacture method and its magnet of Nd-Fe-B series sintered magnet |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105321699B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105903950A (en) * | 2016-05-23 | 2016-08-31 | 苏州思创源博电子科技有限公司 | Preparation method of nanometer neodymium iron boron magnetic material |
| CN112919896A (en) * | 2020-12-28 | 2021-06-08 | 横店集团东磁股份有限公司 | Preparation method of high-density permanent magnetic ferrite material |
| CN114724837A (en) * | 2022-03-28 | 2022-07-08 | 江西理工大学 | Method for preparing neodymium iron boron magnet by utilizing material defects |
| JP2022109870A (en) * | 2021-01-15 | 2022-07-28 | 煙台東星磁性材料株式有限公司 | METHOD OF PRODUCING Nd-Fe-B BASED SINTERED MAGNETIC BODY |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02201903A (en) * | 1989-01-30 | 1990-08-10 | Tdk Corp | Permanent magnet powder |
| CN1303109A (en) * | 1999-12-27 | 2001-07-11 | 住友特殊金属株式会社 | Manufacturing method of ferrous magnetic material alloy powder |
| CN102299000A (en) * | 2010-06-26 | 2011-12-28 | 比亚迪股份有限公司 | NdFeB (neodymium iron boron) permanent magnet material and preparation method thereof |
| CN103093912A (en) * | 2013-01-30 | 2013-05-08 | 浙江大学 | Rare earth permanent magnet produced by using abundant rare earth La and preparation method thereof |
| CN103106991A (en) * | 2013-01-30 | 2013-05-15 | 浙江大学 | High-coercivity and high-stability neodymium iron boron magnet and preparation method based on crystal boundary reconstruction |
| CN103212710A (en) * | 2013-05-05 | 2013-07-24 | 沈阳中北真空磁电科技有限公司 | Manufacturing method of NdFeB rare earth permanent magnetic material |
| CN103668178A (en) * | 2013-12-03 | 2014-03-26 | 江苏大学 | Method for improving corrosion resistance of sintered neodymium iron boron magnet |
| CN103890868A (en) * | 2011-10-28 | 2014-06-25 | Tdk株式会社 | R-t-b sintered magnet |
-
2014
- 2014-07-07 CN CN201410318913.8A patent/CN105321699B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02201903A (en) * | 1989-01-30 | 1990-08-10 | Tdk Corp | Permanent magnet powder |
| CN1303109A (en) * | 1999-12-27 | 2001-07-11 | 住友特殊金属株式会社 | Manufacturing method of ferrous magnetic material alloy powder |
| CN102299000A (en) * | 2010-06-26 | 2011-12-28 | 比亚迪股份有限公司 | NdFeB (neodymium iron boron) permanent magnet material and preparation method thereof |
| CN103890868A (en) * | 2011-10-28 | 2014-06-25 | Tdk株式会社 | R-t-b sintered magnet |
| CN103093912A (en) * | 2013-01-30 | 2013-05-08 | 浙江大学 | Rare earth permanent magnet produced by using abundant rare earth La and preparation method thereof |
| CN103106991A (en) * | 2013-01-30 | 2013-05-15 | 浙江大学 | High-coercivity and high-stability neodymium iron boron magnet and preparation method based on crystal boundary reconstruction |
| CN103212710A (en) * | 2013-05-05 | 2013-07-24 | 沈阳中北真空磁电科技有限公司 | Manufacturing method of NdFeB rare earth permanent magnetic material |
| CN103668178A (en) * | 2013-12-03 | 2014-03-26 | 江苏大学 | Method for improving corrosion resistance of sintered neodymium iron boron magnet |
Non-Patent Citations (1)
| Title |
|---|
| ARU YAN ET AL: "Magnetic and microstructural properties of sintered FeNdB-based magnets with W, Mo and Nb additions", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105903950A (en) * | 2016-05-23 | 2016-08-31 | 苏州思创源博电子科技有限公司 | Preparation method of nanometer neodymium iron boron magnetic material |
| CN112919896A (en) * | 2020-12-28 | 2021-06-08 | 横店集团东磁股份有限公司 | Preparation method of high-density permanent magnetic ferrite material |
| CN112919896B (en) * | 2020-12-28 | 2022-01-18 | 横店集团东磁股份有限公司 | Preparation method of high-density permanent magnetic ferrite material |
| JP2022109870A (en) * | 2021-01-15 | 2022-07-28 | 煙台東星磁性材料株式有限公司 | METHOD OF PRODUCING Nd-Fe-B BASED SINTERED MAGNETIC BODY |
| EP4044202A1 (en) | 2021-01-15 | 2022-08-17 | Yantai Shougang Magnetic Materials Inc. | Method of preparing a high-coercivity sintered ndfeb magnet |
| JP7211691B2 (en) | 2021-01-15 | 2023-01-24 | 煙台東星磁性材料株式有限公司 | Method for producing Nd--Fe--B based sintered magnetic material |
| CN114724837A (en) * | 2022-03-28 | 2022-07-08 | 江西理工大学 | Method for preparing neodymium iron boron magnet by utilizing material defects |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105321699B (en) | 2017-11-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106920617B (en) | High-performance Ne-Fe-B rare earth permanent-magnetic material and preparation method thereof | |
| CN105513737A (en) | Preparation method of sintered neodymium-iron-boron magnet without containing heavy rare earth elements | |
| CN102568807B (en) | Method for preparing high-coercivity SmCoFeCuZr (samarium-cobalt-ferrum-copper-zirconium) high-temperature permanent magnet by doping nano-Cu powder | |
| CN106128677B (en) | A kind of multistage sintering method of neodymium iron boron magnetic body | |
| TW202111735A (en) | Rare earth permanent magnet material, raw material composition, preparation method, application, motor | |
| CN103280290A (en) | Cerium-containing low-melting-point rare-earth permanent magnet liquid phase alloy and production method of permanent magnet comprising same | |
| CN106448986A (en) | Anisotropic nanocrystalline rare earth permanent magnet and preparation method therefor | |
| WO2015149685A1 (en) | W-containing r-fe-b-cu sintered magnet and quenching alloy | |
| JP7253071B2 (en) | RTB Permanent Magnet Material, Manufacturing Method, and Application | |
| KR102631761B1 (en) | Neodymium iron boron magnetic material, raw material composition, manufacturing method and application | |
| CN109585113A (en) | A kind of preparation method of Sintered NdFeB magnet | |
| CN105321699B (en) | A kind of manufacture method and its magnet of Nd-Fe-B series sintered magnet | |
| CN103545079A (en) | Double-principal-phase yttrium-contained permanent magnet and preparing method of double-principal-phase yttrium-contained permanent magnet | |
| CN104332264A (en) | Method for enhancing properties of sintered neodymium-iron-boron magnets | |
| CN107316727A (en) | A kind of sintered NdFeB preparation method | |
| CN103258634A (en) | Method for preparing high-performance R-Fe-B system sintering magnetic body | |
| CN110957089A (en) | Preparation method of samarium cobalt permanent magnet material | |
| CN112435820A (en) | High-performance sintered neodymium-iron-boron magnet and preparation method thereof | |
| CN104464997B (en) | A kind of preparation method of high-coercivity neodymium-iron-boronpermanent-magnet permanent-magnet material | |
| JP2020505754A (en) | Method for producing neodymium-iron-boron permanent magnet material | |
| CN106328331B (en) | Sintered NdFeB magnet assistant alloy slab and preparation method thereof | |
| CN107799256A (en) | A kind of permanent-magnetic composite materials and preparation method | |
| CN111210960A (en) | High-squareness-degree high-magnetic-energy-product samarium cobalt permanent magnet material and preparation method thereof | |
| CN106783123A (en) | The low-temperature melt producing method of NdFeB material | |
| CN103343250B (en) | Method for improving coercive force of Sm5Co19 alloy through step-by-step doping |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20190711 Address after: No. 1005 Anling Road, Huli District, Xiamen City, Fujian Province, 361000 Co-patentee after: FUJIAN CHANGTING GOLDEN DRAGON RARE-EARTH Co.,Ltd. Patentee after: XIAMEN TUNGSTEN Co.,Ltd. Address before: 361015 No. 1005 Anling Road, Huli District, Xiamen City, Fujian Province Patentee before: XIAMEN TUNGSTEN Co.,Ltd. |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20220707 Address after: 366300 new industrial zone, Changting Economic Development Zone, Longyan City, Fujian Province Patentee after: FUJIAN CHANGTING GOLDEN DRAGON RARE-EARTH Co.,Ltd. Address before: No. 1005 Anling Road, Huli District, Xiamen City, Fujian Province, 361000 Patentee before: XIAMEN TUNGSTEN Co.,Ltd. Patentee before: FUJIAN CHANGTING GOLDEN DRAGON RARE-EARTH Co.,Ltd. |
|
| TR01 | Transfer of patent right | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 366300 new industrial zone, Changting Economic Development Zone, Longyan City, Fujian Province Patentee after: Fujian Jinlong Rare Earth Co.,Ltd. Address before: 366300 new industrial zone, Changting Economic Development Zone, Longyan City, Fujian Province Patentee before: FUJIAN CHANGTING GOLDEN DRAGON RARE-EARTH Co.,Ltd. |
|
| CP01 | Change in the name or title of a patent holder |