CN102436893B - A kind of high-coercivity magnet without the few Dy of Tb and preparation method - Google Patents
A kind of high-coercivity magnet without the few Dy of Tb and preparation method Download PDFInfo
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- CN102436893B CN102436893B CN201110421952.7A CN201110421952A CN102436893B CN 102436893 B CN102436893 B CN 102436893B CN 201110421952 A CN201110421952 A CN 201110421952A CN 102436893 B CN102436893 B CN 102436893B
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- 238000002360 preparation method Methods 0.000 title claims description 17
- 230000005291 magnetic effect Effects 0.000 claims description 43
- 239000000203 mixture Substances 0.000 claims description 24
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 17
- 238000002844 melting Methods 0.000 claims description 16
- 230000008018 melting Effects 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 16
- 238000005245 sintering Methods 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 13
- 229910052691 Erbium Inorganic materials 0.000 claims description 12
- 229910052689 Holmium Inorganic materials 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 238000003801 milling Methods 0.000 claims description 11
- 229910052802 copper Inorganic materials 0.000 claims description 9
- 239000010949 copper Substances 0.000 claims description 9
- 230000003647 oxidation Effects 0.000 claims description 9
- 238000007254 oxidation reaction Methods 0.000 claims description 9
- 229910052733 gallium Inorganic materials 0.000 claims description 7
- 239000000314 lubricant Substances 0.000 claims description 7
- 229910052758 niobium Inorganic materials 0.000 claims description 7
- 238000005266 casting Methods 0.000 claims description 6
- 238000006356 dehydrogenation reaction Methods 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 6
- 229910000521 B alloy Inorganic materials 0.000 claims description 5
- 230000006698 induction Effects 0.000 claims description 5
- 239000011261 inert gas Substances 0.000 claims description 5
- 239000004615 ingredient Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 5
- 238000007493 shaping process Methods 0.000 claims description 5
- 230000005540 biological transmission Effects 0.000 claims description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 3
- 239000000956 alloy Substances 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 229910000831 Steel Inorganic materials 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 239000010959 steel Substances 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- 229910052779 Neodymium Inorganic materials 0.000 claims 1
- 238000013467 fragmentation Methods 0.000 claims 1
- 238000006062 fragmentation reaction Methods 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 239000006247 magnetic powder Substances 0.000 claims 1
- 239000000126 substance Substances 0.000 claims 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 28
- 150000002910 rare earth metals Chemical class 0.000 description 26
- 239000012071 phase Substances 0.000 description 14
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 238000005516 engineering process Methods 0.000 description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 239000006249 magnetic particle Substances 0.000 description 5
- 229910001172 neodymium magnet Inorganic materials 0.000 description 5
- 238000013461 design Methods 0.000 description 4
- 238000005984 hydrogenation reaction Methods 0.000 description 4
- 230000005389 magnetism Effects 0.000 description 4
- 229910052771 Terbium Inorganic materials 0.000 description 3
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000003963 antioxidant agent Substances 0.000 description 3
- 230000003078 antioxidant effect Effects 0.000 description 3
- 125000005456 glyceride group Chemical group 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 150000002885 octadecanoids Chemical class 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920013639 polyalphaolefin Polymers 0.000 description 2
- 230000005303 antiferromagnetism Effects 0.000 description 1
- 150000007514 bases Chemical class 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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Abstract
Without high-coercivity magnet and a preparation method of the few Dy of Tb, belong to technical field of magnetic materials.This magnet composition expression formula is (Nd
100-xhRE
x)
afe
100-a-b-cb
btM
c(wt.%), wherein x, a, b and c represent the mass percent of corresponding element respectively, and 0%≤x≤14%, 29%≤a≤30%, 0.8%≤b≤1.5%, 0.5%≤c≤2%, wherein HR is Dy or Dy
95(Ho, Er)
5, TM is one or more in Ga, Co, Cu, Nb, Al element.Advantage is, uses mishmetal to prepare burden, and decreasing to adopt increases cost through the rare earth be separated further, purify.Under maintenance magnet performance prerequisite, the addition of heavy rare earth can be made to be down to 6% ~ 14% by originally accounted for total amount of rare earth 16% ~ 24%, also to add a certain amount of Ho, Er etc. simultaneously and make the consumption of Dy reduce to 5% ~ 12%; Adopt the present invention only to need melting two kinds of composition quick setting belts, can make serial trade mark magnet, composition is adjustable, greatly reduces production cost, is suitable for industrial mass production.
Description
Technical field
The invention belongs to technical field of magnetic materials, particularly relate to a kind of high-coercivity magnet without the few Dy of Tb and preparation method.
Background technology
As third generation rare earth permanent-magnetic material, neodymium iron boron has abundant raw materials, cheap and high remanent magnetism Br and high energy product (BH)
mfeature, important constituent element has been become in many technical fields, as computer technology, information technology, aeronautical and space technology, communications and transportation (automobile) technology etc., especially the demand of various motors to neodymium iron boron of hybrid vehicle (HEV), electric automobile (EV) is larger.But the coercive force H of ternary system sintered NdFeB
cjon the low side, the shortcoming of temperature stability difference limits its application.Current enterprise extensively adopts and effective method directly adds heavy rare earth Dy or Tb Substitute For Partial Nd to improve the magnetocrystalline anisotropy field H of magnet
aimprove magnet coercive force.Because the atomic magnetic moment of heavy rare earth element and the atomic magnetic moment of iron are that antiferromagnetism is coupled, while coercivity heavy rare earth addition increases and improves, the remanent magnetism of magnet also can sharply reduce.On the other hand, heavy rare earth Dy's or Tb is expensive, therefore prepares and not only has high-coercive force but also do not become problem demanding prompt solution containing the neodymium iron boron magnetic body of Dy less containing Tb.
For addressing this problem, people have carried out research extensively and profoundly.The coercive force of NdFeB magnet belongs to Nucleation Mechanism, and magnetic reversal farmland is generally easy at grain boundary area forming core, therefore improves coercitive focusing on and improves Grain-Boundary Phase Structure and Properties.The dual-phase process of immediate development is exactly the Composition and property changing Grain-Boundary Phase by directly adding liquid phase.The method prepares the auxiliary phase of rich heavy rare earth and the principal phase of High Energy Product respectively, and two kinds of alloy powders are mixed aftershaping according to proportioning.But the magnet homogeneity adopting this technique to prepare is poor, reason is that the Nd-rich phase containing heavy rare earth uses as liquid phase, and two kinds of powder are difficult to the admixture reaching desired homogeneous.The people such as the DSLi of Japan in 2009 adopt reduction-diffusion method by Dy
2o
3or DyF
3with CaH
2mixed-powder is coated in the surface of magnet, then by magnet heating in vacuum to 1073 ~ 1273K, and insulation 0.5 ~ 3h.Result allows Dy diffuse to Grain-Boundary Phase, when not reducing remanent magnetism, improves coercive force 40%.But the magnet size that the method is suitable for only has 3.0 × 3.0 × 2.8mm
3, industrial production demand cannot be met.The people such as Yue Ming propose to add the nanometer powder of heavy rare earth dysprosium and terbium or nano level hydride particle technology and the sintered ndfeb permanent magnet body (200810227680.5 and 200610089124.7) prepared with high-coercive force and high remanent magnetism.The heavy rare earth element powder of nanometer scale is very easily oxidized and complicated process of preparation.Someone adopts the method for the magnetic surface electrical depositing nano level coat of metal to improve the coercive force of magnet, but too increases production cost and difficulty.
Summary of the invention
The object of the present invention is to provide a kind of high-coercivity magnet without the few Dy of Tb and preparation method, by main phase grain top layer and Grain-Boundary Phase restructuring, improve its Structure and Properties.Test result shows, compared with the equal performance sintered ndfeb permanent magnet body prepared with conventional art, the magnet adopting the technology of the present invention to prepare can make the addition of heavy rare earth be down to 6% ~ 14% by originally accounted for total amount of rare earth 16% ~ 24%, also add a certain amount of Ho, Er etc. makes the consumption of Dy reduce to 5% ~ 12% simultaneously, improves the utilance of rare earth resources and the cost performance of magnet.
The composition expression formula of magnet of the present invention is (Nd
100-xhRE
x)
afe
100-a-b-cb
btM
c(wt.%), wherein x, a, b and c represent the mass percent of corresponding element respectively, and 0%≤x≤14%, 29%≤a≤30%, 0.8%≤b≤1.5%, 0.5%≤c≤2%, wherein HRE is Dy or Dy
95(Ho, Er)
5, TM is one or more in Ga, Co, Cu, Nb, A1 element.
The present invention comprises following processing step without the preparation method of the high-coercivity magnet of the few Dy of Tb:
Step 1: according to the ingredient formula (Nd of Nd Fe B alloys mass percent
100-xhRE
x)
afe
100-a-b-cb
btM
cand Nd (wt.%)
afe
100-a-b-cb
btM
c(wt.%) difference preparation raw material, wherein 0%≤x≤24%, 29%≤a≤30%, 0.8%≤b≤1.5%, 0.5%≤c≤2%, required rare earths material directly can adopt the mishmetal containing Ho, Er, Dy ratio-dependent, TM is Ga, Co, Cu, one or more in Nb, Al element;
Step 2: the raw material that step 1 is prepared melting respectively.First raw material are put into Medium frequency induction melting rapid hardening furnace crucible, reach 10 in vacuum degree
-2power transmission preheating during more than Pa, treats that vacuum degree reaches 10 again
-2stop after more than Pa vacuumizing and being filled with high-purity Ar, after making Ar air pressure in stove reach-0.04 ~-0.08Mpa, carry out melting.Subsequently molten steel is poured on water-cooled copper roller that linear velocity is 1.5 ~ 3m/s, obtains the rapid casting of average thickness range at 0.15 ~ 0.5mm;
Step 3: obtained rapid casting is respectively charged in hydrogenation furnace and carries out coarse crushing.Under protective atmosphere, oxidation lubricant is mixed with the ratio of coarse crushing magnetic according to 3 ~ 7ml/kg, prevent fine powder in airflow milling process subsequently from reuniting and oxidation.Wherein in oxidation lubricant, alcohol gasoline accounts for 85%-96%, and basic artificial oil accounts for 4%-15%.The alcohol adopted can be methyl alcohol or ethanol, adopt the Viscosity Index of basic compound oil to be greater than 90, as Poly alpha Olefins (PAO) or Esters oil etc.The rotary speed of airflow milling selection by winnowing wheel controls at 3000r/min ~ 4000r/min, and composition is Nd
afe
100-a-b-cb
btM
c(wt.%) granularity of magnet powder controls at 3 ~ 5 μm, and composition is (Nd
100-xhRE
x)
afe
100-a-b-cb
btM
c(wt.%) granularity of magnet powder controls at 0.07 ~ 2.5 μm;
Step 4: according to alloy designs composition, takes the magnetic of step 3 preparation in varing proportions respectively and is fully mixed by magnetic in batch mixer.
Step 5: under inert gas shielding atmosphere, is oriented moulding in the magnetic field of 1.5 ~ 2T in magnetic field intensity by mixing magnetic, then carries out isostatic cool pressing, make blank;
Step 6: the sintering furnace that high vacuum put into by the blank after shaping is sintered, within 0.5 ~ 10 hour, dehydrogenation is carried out 400 DEG C ~ 800 DEG C insulations in sintering process, water-cooled or air cooling after sintering temperature 1020 DEG C ~ 1080 DEG C is incubated 1 ~ 4 hour, then carry out the temper of 1 ~ 4 hour respectively 750 DEG C ~ 950 DEG C and 450 DEG C ~ 600 DEG C.
The present invention adopts mishmetal (Dy, Ho, Er) to carry out composition proportion, decreases that rare earth is separated further, increased cost of purifying; The present invention only needs the quick setting belt of two kinds of compositions to prepare magnetic, in the oxidation lubricant that airflow milling process interpolation alcohol and basic artificial oil compound are joined; In the magnet of preparation in Dy, Ho, Er major part skin of being distributed in main phase grain and Grain-Boundary Phase.
The present invention compared with prior art advantage is: use mishmetal to prepare burden, and decreasing to adopt increases cost through the rare earth be separated further, purify.Under maintenance magnet performance prerequisite, the addition of heavy rare earth can be made to be down to 6% ~ 14% by originally accounted for total amount of rare earth 16% ~ 24%, also to add a certain amount of Ho, Er etc. simultaneously and make the consumption of Dy reduce to 5% ~ 12%; Secondly adopt the present invention only to need melting two kinds of composition quick setting belts, just can make the magnet of the serial trade mark, there is the adjustable degree of freedom of higher composition, production cost can be reduced greatly, be suitable for industrial mass production.
Accompanying drawing explanation
Fig. 1 is that superfine powder of the present invention adds preparation technology.
Fig. 2 is that magnet prepared by the present invention organizes schematic diagram.Nd in principal phase
2fe
14b still keeps higher volume fraction, and Dy, Ho, Er major part cloth is in the skin and Grain-Boundary Phase of main phase grain.
Embodiment
Below the embodiment under premised on technical solution of the present invention is elaborated, to understand the present invention better.But it should be noted that following examples only for the purpose of illustration, protection scope of the present invention is not limited to following embodiment.
Embodiment 1
By design mix (Nd
97hRE
3)
30fe
bal1b
0.94tM
0.67(TM=Ga, Co, Cu, Nb) (HRE=Dy or Dy
95(Ho, Er)
5), the mass fraction wherein shared by heavy rare earth is about 1%.
Step 1: according to the ingredient formula (Nd of Nd Fe B alloys mass percent
80hRE
20)
afe
100-a-b-cb
btM
cand Nd (wt.%)
afe
100-a-b-cb
btM
c(wt.%) difference preparation raw material;
Step 2: by the raw material melting respectively prepared.First raw material being put into Medium frequency induction melting rapid hardening furnace crucible, is 10 in vacuum degree
-2power transmission preheating during more than Pa, treats that vacuum degree reaches 10 again
-2stop after more than Pa vacuumizing and being filled with high-purity Ar, after making Ar air pressure in stove reach-0.06MPa, carry out melting.Adopt single texture R (rare earth)-Fe-B rapid hardening technology, obtained average thickness is the rapid-hardening flake of 0.3mm;
Step 3: obtained rapid casting is respectively charged in hydrogenation furnace and carries out coarse crushing.Mixed according to the ratio of 5ml/kg with the magnetic after thick breaking respectively by antioxidant under protective atmosphere, wherein in oxidation lubricant, methanol gasoline accounts for 90%, and tristerin (octadecanoid acid fat glyceride) accounts for 10%.Composition is Nd
afe
100-a-b-cb
btM
c(wt.%) during airflow milling, the adjustment of rotational speed of selection by winnowing wheel is 3100r/min, and magnet particle mean size controls at 3 μm; Composition is (Nd
80hRE
20)
afe
100-a-b-cb
btM
c(wt.%) during airflow milling, the adjustment of rotational speed of selection by winnowing wheel is 4000r/min, and magnetic particle mean size controls at 1.5 μm;
Step 4: the two kinds of magnetics getting the preparation of appropriate step 3 mix, and the ratio making the magnetic containing heavy rare earth account for total weight is no more than 15%, is fully mixed by two kinds of magnetics in batch mixer;
Step 5: under inert gas shielding atmosphere, is oriented moulding in the magnetic field of 2T in magnetic field intensity by mixing magnetic, then carries out isostatic cool pressing, make blank;
Step 6: the sintering furnace that high vacuum put into by the blank after shaping is sintered, at 400 DEG C in sintering process, 600 DEG C, 800 DEG C respectively insulation within 1 hour, carry out dehydrogenation, water-cooled after sintering temperature 1050 DEG C is incubated 2 hours, then carries out the temper of 2 hours respectively 900 DEG C and 520 DEG C.
Adopt NIM-2000HF rare earth permanent magnet standard measuring equipment to survey the magnetic property of magnet, performance is as table one.
Table 1,
Embodiment 2
By design mix (Nd
91hRE
9)
30fe
balb
0.94tM
0.67(TM=Ga, Co, Cu, Nb) (HRE=Dy or Dy
95(Ho, Er)
5), the mass fraction wherein shared by heavy rare earth is about 2.7%.
Step 1: according to the ingredient formula (Nd of Nd Fe B alloys mass percent
80hRE
20)
afe
100-a-b-cb
btM
cand Nd (wt.%)
afe
100-a-b-cb
btM
c(wt.%) difference preparation raw material;
Step 2: by the raw material melting respectively prepared.First raw material being put into Medium frequency induction melting rapid hardening furnace crucible, is 10 in vacuum degree
-2power transmission preheating during more than Pa, treats that vacuum degree reaches 10 again
-2stop after more than Pa vacuumizing and being filled with high-purity Ar, after making Ar air pressure in stove reach-0.06MPa, carry out melting.Adopt single texture R (rare earth)-Fe-B rapid hardening technology, obtained average thickness is the rapid-hardening flake of 0.3mm;
Step 3: obtained rapid casting is respectively charged in hydrogenation furnace and carries out coarse crushing.Mixed according to the ratio of 5ml/kg with the magnetic after thick breaking respectively by antioxidant under protective atmosphere, wherein in oxidation lubricant, methanol gasoline accounts for 90%, and tristerin (octadecanoid acid fat glyceride) accounts for 10%.Composition is Nd
afe
100-a-b-cb
btM
c(wt.%) during airflow milling, the adjustment of rotational speed of selection by winnowing wheel is 3100r/min, and magnetic particle mean size controls at 3 μm; Composition is (Nd
80hRE
20)
afe
100-a-b-cb
btM
c(wt.%) during airflow milling, the adjustment of rotational speed of selection by winnowing wheel is 4000r/min, and magnetic particle mean size controls at 1.5 μm;
Step 4: the two kinds of magnetics getting the preparation of appropriate step 3 mix, and the ratio making the magnetic containing heavy rare earth account for total weight is no more than 40%, is fully mixed by two kinds of magnetics in batch mixer;
Step 5: under inert gas shielding atmosphere, is oriented moulding in the magnetic field of 2T in magnetic field intensity by mixing magnetic, then carries out isostatic cool pressing, make blank;
Step 6: the sintering furnace that high vacuum put into by the blank after shaping is sintered, at 400 DEG C in sintering process, 600 DEG C, 800 DEG C respectively insulation within 1 hour, carry out dehydrogenation, water-cooled after sintering temperature 1050 DEG C is incubated 2 hours, then carries out the temper of 2 hours respectively 900 DEG C and 520 DEG C.
Adopt NIM-2000HF rare earth permanent magnet standard measuring equipment to survey the magnetic property of magnet, performance is as table two.
Table 2,
Embodiment 3
By design mix (Nd
87hRE
13)
30fe
balb
0.94tM
0.67(TM=Ga, Co, Cu, Nb) (HRE=Dy or Dy
95(Ho, Er)
5), the mass fraction wherein shared by heavy rare earth is about 4%.
Step 1: according to the ingredient formula (Nd of Nd Fe B alloys mass percent
80hRE
20)
afe
100-a-b-cb
btM
cand Nd (wt.%)
afe
100-a-b-cb
btM
c(wt.%) difference preparation raw material;
Step 2: by the raw material melting respectively prepared.First raw material being put into Medium frequency induction melting rapid hardening furnace crucible, is 10 in vacuum degree
-2to small-power preheating during more than Pa, treat that vacuum degree reaches 10 again
-2stop after more than Pa vacuumizing and being filled with high-purity Ar, after making Ar air pressure in stove reach-0.06MPa, carry out melting.Adopt single texture R (rare earth)-Fe-B rapid hardening technology, obtained average thickness is the rapid-hardening flake of 0.3mm;
Step 3: obtained rapid casting is respectively charged in hydrogenation furnace and carries out coarse crushing.Mixed according to the ratio of 5ml/kg with the magnetic after thick breaking respectively by antioxidant under protective atmosphere, wherein in oxidation lubricant, methanol gasoline accounts for 90%, and tristerin (octadecanoid acid fat glyceride) accounts for 10%.Composition is Nd
afe
100-a-b-cb
btM
c(wt.%) during airflow milling, the adjustment of rotational speed of selection by winnowing wheel is 3100r/min, and magnetic particle mean size controls at 3 μm.Composition is (Nd
80hRE
20)
afe
100-a-b-cb
btM
c(wt.%) during airflow milling, the adjustment of rotational speed of selection by winnowing wheel is 4000r/min, and magnetic particle mean size controls at 1.5 μm;
Step 4: the two kinds of magnetics getting the preparation of appropriate step 3 mix, is wherein no more than 65% containing the ratio that the magnetic of heavy rare earth accounts for total weight, is fully mixed by two kinds of magnetics in batch mixer;
Step 5: under inert gas shielding atmosphere, is oriented moulding in the magnetic field of 2T in magnetic field intensity by mixing magnetic, then carries out isostatic cool pressing, make blank;
Step 6: the sintering furnace that high vacuum put into by the blank after shaping is sintered, at 400 DEG C in sintering process, 600 DEG C, 800 DEG C respectively insulation within 1 hour, carry out dehydrogenation, water-cooled after sintering temperature 1050 DEG C is incubated 2 hours, then carries out the temper of 2 hours respectively 900 DEG C and 520 DEG C.
Adopt NIM-2000HF rare earth permanent magnet standard measuring equipment to survey the magnetic property of magnet, performance is as table three.
Table 3,
Claims (2)
1., without a high-coercivity magnet of the few Dy of Tb, it is characterized in that, by (the Nd of two kinds of heterogeneities
0.76hRE
0.24)
afe
100-a-b-cb
btM
cand Nd (wt%)
afe
100-a-b-cb
btM
c(wt%) permanent magnetic powder is composited, wherein, and Nd
afe
100-a-b-cb
btM
cgranularity of magnet powder control at 3 ~ 5 μm, composition is (Nd
76hRE
24)
afe
100-a-b-cb
btM
cgranularity of magnet powder control at 0.07 ~ 2.5 μm; The equivalent chemical formulas of whole magnet is expressed as: (Nd
1-xhRE
x)
afe
100-a-b-cb
btM
c(wt%), wherein 0≤x≤0.14,29≤a≤30,0.8≤b≤1.5,0.5≤c≤2, wherein HRE is Dy or Dy
0.95(Ho, Er)
0.05, TM is one or more in Ga, Co, Cu, Nb, Al element.
2. a preparation method for the high-coercivity magnet without the few Dy of Tb according to claim 1, it is characterized in that, processing step is as follows:
(1) by the ingredient formula (Nd of Nd Fe B alloys mass percent
0.76hRE
0.24)
afe
100-a-b-cb
btM
cand Nd
afe
100-a-b-cb
btM
c, use Nd, Dy or mishmetal Dy
0.95(Ho, Er)
0.05, prepare two kinds of alloy raw materials, wherein 29≤a≤30 respectively, 0.8≤b≤1.5,0.5≤c≤2, TM is one or more in Ga, Co, Cu, Nb, Al element;
(2) raw material step (1) prepared melting respectively: first raw material are put into Medium frequency induction melting rapid hardening furnace crucible, reach 10 in vacuum degree
-2power transmission preheating during more than Pa, treats that vacuum degree reaches 10 again
-2stop after more than Pa vacuumizing and being filled with high-purity Ar, after making Ar air pressure in stove reach-0.04 ~-0.08Mpa, carry out melting; Subsequently molten steel is poured on water-cooled copper roller that linear velocity is 1.5 ~ 3m/s, obtains the rapid casting of average thickness range at 0.15 ~ 0.5mm;
(3) rapid-hardening flake obtained by step (2) is carried out hydrogen fragmentation, after dehydrogenation, obtain coarse crushing magnetic; Under protective atmosphere, oxidation lubricant is mixed with the ratio of coarse crushing magnetic according to 3 ~ 7ml/kg, prevent fine powder in airflow milling process subsequently from reuniting and oxidation; The rotary speed of airflow milling selection by winnowing wheel controls at 3000r/min ~ 4000r/min, and composition is Nd
afe
100-a-b-cb
btM
cgranularity of magnet powder control at 3 ~ 5 μm, composition is (Nd
0.76hRE
0.24)
afe
100-a-b-cb
btM
cgranularity of magnet powder control at 0.07 ~ 2.5 μm;
(4) according to the component requirements of different trade mark magnet, take magnetic prepared by step (3) in varing proportions respectively, and in batch mixer, magnetic is mixed;
(5) under inert gas shielding atmosphere, be oriented moulding in the magnetic field of 1.5 ~ 2T in magnetic field intensity by mixing magnetic, then carry out isostatic cool pressing, make blank;
(6) sintering furnace blank after shaping being put into high vacuum sinters, within 0.5 ~ 10 hour, dehydrogenation is carried out 400 DEG C ~ 800 DEG C insulations in sintering process, water-cooled or air cooling after sintering temperature 1020 DEG C ~ 1080 DEG C is incubated 1 ~ 4 hour, then carry out the temper of 1 ~ 4 hour respectively 750 DEG C ~ 950 DEG C and 450 DEG C ~ 600 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110421952.7A CN102436893B (en) | 2011-12-15 | 2011-12-15 | A kind of high-coercivity magnet without the few Dy of Tb and preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110421952.7A CN102436893B (en) | 2011-12-15 | 2011-12-15 | A kind of high-coercivity magnet without the few Dy of Tb and preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102436893A CN102436893A (en) | 2012-05-02 |
| CN102436893B true CN102436893B (en) | 2016-04-27 |
Family
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| EP2722855A1 (en) * | 2012-10-19 | 2014-04-23 | Siemens Aktiengesellschaft | Nd-Fe-B permanent magnet without Dysprosium, rotor assembly, electromechanical transducer, wind turbine |
| CN103280288B (en) * | 2013-06-25 | 2016-03-02 | 新昌县辰逸服饰有限公司 | A kind of preparation method of high-coercive force SmCo based permanent magnetic material |
| CN103506626B (en) * | 2013-10-22 | 2015-07-08 | 宁波科田磁业有限公司 | A manufacturing method for improving the coercive force of sintered NdFeB magnets |
| CN104348264B (en) * | 2014-10-30 | 2017-02-22 | 浙江鑫盛永磁科技有限公司 | Special magnetic steel for hybrid electric vehicle driving motor and preparation method thereof |
| CN104393691A (en) * | 2014-10-30 | 2015-03-04 | 浙江鑫盛永磁科技有限公司 | Magnetic steel specialized for pure electric automobile drive motor and preparation method thereof |
| CN106067358A (en) * | 2016-05-20 | 2016-11-02 | 江苏普隆磁电有限公司 | A kind of magnetic powder particle and preparation method thereof |
| CN114203380A (en) * | 2021-12-17 | 2022-03-18 | 沈阳中北通磁科技股份有限公司 | High-performance rare earth permanent magnet |
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| CN1092899A (en) * | 1993-01-29 | 1994-09-28 | 日立金属株式会社 | Neodymium-iron-Nd-Fe-B permanent magnet |
| CN101615459A (en) * | 2009-04-28 | 2009-12-30 | 中国科学院宁波材料技术与工程研究所 | Method for Improving the Performance of Sintered NdFeB Permanent Magnets |
| CN101981634A (en) * | 2008-03-31 | 2011-02-23 | 日立金属株式会社 | R-T-B system sintered magnet and its manufacturing method |
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| US7199690B2 (en) * | 2003-03-27 | 2007-04-03 | Tdk Corporation | R-T-B system rare earth permanent magnet |
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| CN1092899A (en) * | 1993-01-29 | 1994-09-28 | 日立金属株式会社 | Neodymium-iron-Nd-Fe-B permanent magnet |
| CN101981634A (en) * | 2008-03-31 | 2011-02-23 | 日立金属株式会社 | R-T-B system sintered magnet and its manufacturing method |
| CN101615459A (en) * | 2009-04-28 | 2009-12-30 | 中国科学院宁波材料技术与工程研究所 | Method for Improving the Performance of Sintered NdFeB Permanent Magnets |
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