CN101819844A - High-remanence low-coercivity permanent magnetic material and preparation method thereof - Google Patents
High-remanence low-coercivity permanent magnetic material and preparation method thereof Download PDFInfo
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- CN101819844A CN101819844A CN 201010159729 CN201010159729A CN101819844A CN 101819844 A CN101819844 A CN 101819844A CN 201010159729 CN201010159729 CN 201010159729 CN 201010159729 A CN201010159729 A CN 201010159729A CN 101819844 A CN101819844 A CN 101819844A
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- 239000000696 magnetic material Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 72
- 239000010949 copper Substances 0.000 claims abstract description 29
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 19
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 17
- 229910052802 copper Inorganic materials 0.000 claims abstract description 17
- 229910052742 iron Inorganic materials 0.000 claims abstract description 17
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 17
- 229910052796 boron Inorganic materials 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 14
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 5
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052751 metal Inorganic materials 0.000 claims abstract description 4
- 239000002184 metal Substances 0.000 claims abstract description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000010703 silicon Substances 0.000 claims abstract description 3
- 150000002910 rare earth metals Chemical class 0.000 claims description 9
- 238000000137 annealing Methods 0.000 claims description 8
- 238000010791 quenching Methods 0.000 claims description 8
- 230000000171 quenching effect Effects 0.000 claims description 6
- 238000005266 casting Methods 0.000 claims description 4
- 238000003723 Smelting Methods 0.000 claims description 3
- 239000004411 aluminium Substances 0.000 claims description 2
- 238000009950 felting Methods 0.000 claims description 2
- 150000002739 metals Chemical class 0.000 claims description 2
- 239000013081 microcrystal Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000013078 crystal Substances 0.000 abstract description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 9
- 239000001301 oxygen Substances 0.000 description 9
- 229910052760 oxygen Inorganic materials 0.000 description 9
- 238000000034 method Methods 0.000 description 7
- ZDVYABSQRRRIOJ-UHFFFAOYSA-N boron;iron Chemical compound [Fe]#B ZDVYABSQRRRIOJ-UHFFFAOYSA-N 0.000 description 6
- 229910052779 Neodymium Inorganic materials 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 5
- 239000000956 alloy Substances 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 229910000905 alloy phase Inorganic materials 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000004907 flux Effects 0.000 description 3
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 239000011733 molybdenum Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 2
- 229910001172 neodymium magnet Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000000498 cooling water Substances 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
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 239000006249 magnetic particle Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention belongs to the field of magnetic materials, and in particular relates to a high-remanence low-coercivity permanent magnetic material and a preparation method thereof. The material has the atomic components shown as RxFe100-x-y-a-b-cAlaCubSicBy, wherein x is 4 to 4.5; y is 18 to 19.5; a is not zero and is no more than 1.5; b is not zero and is no more than 0.8; c is not zero and no more than 1.4; R is rare-earth element; and Fe, Al, Cu, Si and B respectively refer to iron, aluminum, copper, silicon, boron elements. The material consists of ultra-fine crystals of which the main phase is a mixture of three metal phases, namely R2Fe14B, Fe3B and alpha-Fe, wherein iron atoms are substituted by Al, Cu and Si atoms compositely. The permanent magnetic material prepared by the invention has more outstanding characteristics of high remanence and low coercivity.
Description
(1) technical field
The invention belongs to field of magnetic material, particularly a kind of high-remanence low-coercivity permanent magnetic material and preparation method thereof.
(2) background technology
Magnaglo possesses the very high degree of freedom, can be made into arbitrary shape, is therefore extensively used when making abnormity and special shape bonded permanent magnet.
In the metallic iron melt of low rare earth, high boron, contain a large amount of α-Fe phase and Fe
3B phase and product R
2Fe
14The B phase is because α-Fe phase and Fe
3A large amount of existence of B phase make metallic bond and covalent bond strengthen greatly, externally show than strong hardness, therefore adopt the broken alloy pig of conventional physical to become very difficult.In addition, the prescription of traditional preparation process technology is partial to make high-coercive force, high energy product magnetic more, but making the specific (special) requirements magnet, requires residual magnetic flux density very high, is easy to again magnetize, and just necessary coercive force is lower; For this situation, conventional method is to adjust with high-coercive force, high remanent magnetism magnetic, but the magnetic of adjusting can not guarantee that each magnetic-particle all has the characteristic of big magnet.Describe two-phase rare earth neodymium, iron-boron material among the Chinese patent ZL95102821.9, adopted oxygen uptake, method of dehydrogenating to prepare Magnaglo.A kind of rare earth neodymium has been described in the U.S. Pat 4802931, iron-boron is injected on the metal runner of high speed rotating, make the melt quench cooled form the strip that thickness is no more than 50 μ m, material after the quench cooled contains the crystal grain present situation of noncrystalline phase, form the crystallite that uniform size is no more than 50 μ m after the crystallization of proper temperature is handled, X ray shows that this crystallite is the R of tetragonal
2Fe
14The B phase, when the percentage by volume of crystalline phase in material was no less than 80%, material had the coercive force that is no less than 10000Oe.Chinese patent CN1033018A has described a kind of rare earth iron-boron melt oxygen uptake-put method that oxygen twin crystal method prepares rare earth iron-boron Magnaglo of utilizing, basic step is at first to prepare rare earth iron-boron material, in oxygen atmosphere, remain on then under 500 ℃ to the 1000 ℃ temperature, hydrogen is retained in the metal material, subsequently, with metal material dehydrogenation under 500 ℃ to 1000 ℃ temperature, drop to up to hydrogen pressure and to be not more than 1 * 10
-1Pa, cooling then, the granularity of crystal grain again that this method keeps is that 0.1um is between the 1um, powder has the coercive force greater than 5000Oe, and method is simple, the better performances of powder magnetic, in addition, prepare rare earth iron-boron Magnaglo in this way and generally possess anisotropy.Chinese patent CN1066146A has described a kind of neodymium-iron boron that utilizes and has produced the lattice transformation from the low temperature oxygen uptake, and then the transition process of high temperature oxygen uptake generation crystallization prepares neodymium-iron-boron, carry out oxygen uptake in 200 ℃ to 500 ℃ then, subsequently, again in 600 ℃ to 1000 ℃ oxygen uptakes, carry out to a certain degree in the material crystallization again taking place when oxygen uptake, when crystal was controlled at 0.1-1um, the coercive force of powder was not less than 50000e.But the coercive force of the permanent magnetic material of above method preparation is still than higher, therefore develops high-remanence low-coercivity material and preparation method thereof and is always those skilled in the art and endeavour the problem studying and solve.
(3) summary of the invention
The object of the present invention is to provide a kind of high-remanence low-coercivity permanent magnetic material and preparation method thereof.
The technical solution used in the present invention is as follows:
A kind of high-remanence low-coercivity permanent magnetic material, described material atom consists of: R
xFe
100-x-y-a-b-cAl
aCu
bSi
cB
y, x value 4-4.5 wherein, the y value is 18-19.5, and a value is non-vanishing and be not more than 1.5, and the b value is non-vanishing and be not more than 0.8, and the c value is non-vanishing and be not more than 1.4; R is a rare earth element, and Fe, Al, Cu, Si, B represent iron, aluminium, copper, silicon, boron element respectively; Described material is by R
2Fe
14B, Fe
3Three kinds of metals of B and α-Fe mixture mutually is that the micro crystal of principal phase constitutes, and wherein iron atom is mixed alternative by Al, Cu, Si atom.
Described R element is preferably Nd.
The present invention also provides a kind of preparation method of described high-remanence low-coercivity permanent magnetic material, and step is as follows:
With pure rare earth metal element, pure Fe, B-Fe, Cu, Al, Si is raw material, and the atomic percent of B example is 18-20% among the described B-Fe, and smelting composition according to the ratio of each element is R
xFe
100-x-y-a-b-cAl
aCu
bSi
cB
yIngot casting, then ingot casting is broken into the ingot bar that granularity is 1-15mm, be not more than 5 * 10 in vacuum degree
-2Fast quenching becomes thickness to be not more than the even strip of 0.1mm under the vacuum state of Pa, anneals down in vacuum state then.
When being even strip, fast quenching quenches speed control built in 22-23m/s.
In vacuum degree is 4 * 10
-2-5 * 10
-2The vacuum state of Pa is annealing down, and annealing temperature is controlled at 650-660 ℃, constant temperature 25min-26min.
Handle the R that can make in the crystal with this understanding
2Fe
14B, Fe
3B, α-Fe distributes more even.
R
xFe
100-x-y-a-b-cAl
aCu
bSi
cB
yProportioning is R preferably
4.2Fe
73.4Al
1.5Cu
0.8Si
1.4B
18.7, R
4.2Fe
74Al
1.3Cu
0.6Si
1.2B
18.7Or R
4.2Fe
74.6Al
1.1Cu
0.4Si
1.0B
18.7
The present invention is by adding less Al, Cu and the Si atom of atomic radius, make the α-Fe in the alloy pig after the melting reduce mutually, internal stress increases, fragility increases, be easy to fragmentation, realized the improvement of production technology, and, realized the purpose of the high remanent magnetism of material, low-coercivity by the speed and the change of annealing temperature that melt is quenched.Permanent magnetic material residual magnetic flux density (Br) scope that makes is at 10200-11000Gs, and coercive force (Hcj) scope is at 4280-4400Oe.At 6000-8500Gs, coercive force (Hcj) scope is at 7000-11000Oe compared to traditional fast quenching magnetic residual magnetic flux density (Br) scope, and the characteristics of its high-remanence low-coercivity are more outstanding.
(4) description of drawings
Fig. 1 obtains the performance curve that permanent magnetic material detects acquisition to embodiment 1 under 22 ℃ of conditions;
Fig. 2 obtains the performance curve that permanent magnetic material detects acquisition to embodiment 2 under 22 ℃ of conditions;
Fig. 3 obtains the performance curve that permanent magnetic material detects acquisition to embodiment 3 under 22 ℃ of conditions.
(5) embodiment:
Below with specific embodiment technical scheme of the present invention is described, but protection scope of the present invention is not limited thereto:
Embodiment 1-3
Get pure Nd, pure Fe, B-Fe (wherein the atomic percent of B is 19%), Cu, Al and Si according to following ratio respectively:
1、4.2at％Nd??73.4at％Fe???18.7at％B???0.8at％Cu???1.5at％Al???1.4at％Si；
2、4.2at％Nd??74at％Fe?????18.7at％B???0.6at％Cu???1.3at％Al???1.2at％Si；
3、4.2at％Nd??74.6at％Fe???18.7at％B???0.4at％Cu???1.1at％Al???1.0at％Si；
Select the melting of induction type smelting furnace for use, melting vacuum degree is 5 * 10
-2Pa, and to charge into Ar gas vacuum degree to the stove be that 0.06Mpa is as protective gas, to prevent the alloy pig oxidation.Be cast in after the melting and be connected with the watering on the injection molding of cold water, be controlled at pouring time 2-3 minute, wherein embodiment 1,2 is 2.5 minutes, and embodiment 3 is 3 minutes.Cool off and normally come out of the stove after 1 hour, main phase structure is Nd in the alloy pig at this moment
2Fe
14The B phase, α-Fe phase and Fe
3The B phase, because the control of the adding of Cu, Al, Si, the alloy pig phase content in three components of embodiment 1-3 changes to some extent, below is the percent by volume of three kinds of alloy phases:
1、Nd
2Fe
14B??10.6％??Fe
3B??73％??α-Fe??16.4％
2、Nd
2Fe
14B??11.3％??Fe
3B??71％??α-Fe??17.7％
3、Nd
2Fe
14B??12％????Fe
3B??69％??α-Fe??19％
Become the ingot bar of 1-15mm with medium-sized crusher in crushing, carry out second melting in the vacuum quick quenching furnace of packing into, and get rid of into the strip of wide 5mm, thick 0.1mm by the molybdenum wheel of high speed rotating, and logical cooling water in the molybdenum wheel (hydraulic pressure＞0.2MPa), molybdenum wheel speed 22.5m/s.After testing, variation has taken place in strip alloy phase structure, and α-Fe increases mutually, Nd
2Fe
14B reduces mutually, and three kinds of alloy phase percents by volume of detection are as follows:
1、Nd
2Fe
14B??7.9％??Fe
3B??64％??α-Fe??28.1％
2、Nd
2Fe
14B??8.7％??Fe
3B??62％??α-Fe??29.3％
3、Nd
2Fe
14B??9.1％??Fe
3B??59％??α-Fe??31.9％
And increased rich Nd mutually with rich B two kinds of unstable phase structures mutually, but Nd
2Fe
14B phase and Fe
3B phase number significantly improves, and crystal size diminishes.
Above strip is pressed into＜powder of 0.8mm with the 5MPa press, and (vacuum degree is 5 * 10 in 650 ℃ of vacuum annealing furnaces
-2Pa) annealing is 26 minutes, and it is as follows to detect three kinds of properties of product:
1、Br：11000Gs??Hcj：4400Oe??(BH)max：9.8MGOe
2、Br：10800Gs??Hcj：4320Oe??(BH)max：9.3MGOe
3、Br：10200Gs??Hcj：4280Oe??(BH)max：9.0MGOe
Reduce Nd mutually by the magnetic α-Fe after the annealing
2Fe
14B grows up mutually and increases, Fe
3B improves mutually, and rich Nd disappears mutually with rich B mutually, and three kinds of alloy phase percents by volume are as follows after testing:
1、Nd
2Fe
14B??13.7％????Fe
3B??70.6％????α-Fe??15.7％
2、Nd
2Fe
14B??14.1％????Fe
3B??72.8％????α-Fe??13.1％
3、Nd
2Fe
14B??14.8％????Fe
3B??74.2％????α-Fe??11％。
The permanent magnetic material of embodiment 1-3 adopts NIM-2000HB bonded permanent magnet magnetic measurement systems to measure its performance, and its detection curve is referring to Fig. 1-3.
The particle size distribution of embodiment 1-3 permanent magnetic material is as follows:
| Granularity | ??＞80 | ??80-100 | ??100-200 | ??200-300 | ??300-400 | ??＜400 |
| Embodiment 1 (%) | ??- | ??19 | ??51 | ??23 | ??6 | ??1 |
| Embodiment 2 (%) | ??- | ??19 | ??51 | ??23 | ??6 | ??1 |
| Embodiment 3 (%) | ??- | ??19 | ??51 | ??23 | ??6 | ??1 |
Claims (6)
1. a high-remanence low-coercivity permanent magnetic material is characterized in that, described material atom consists of: R
xFe
100-x-y-a-b-cAl
aCu
bSi
cB
y, x value 4-4.5 wherein, the y value is 18-19.5, and a value is non-vanishing and be not more than 1.5, and the b value is non-vanishing and be not more than 0.8, and the c value is non-vanishing and be not more than 1.4; R is a rare earth element, and Fe, Al, Cu, Si, B represent iron, aluminium, copper, silicon, boron element respectively; Described material is by R
2Fe
14B, Fe
3Three kinds of metals of B and α-Fe mixture mutually is that the micro crystal of principal phase constitutes, and wherein iron atom is mixed alternative by Al, Cu, Si atom.
2. high-remanence low-coercivity permanent magnetic material as claimed in claim 1 is characterized in that, described R element is Nd.
3. the preparation method of the described high-remanence low-coercivity permanent magnetic material of claim 1, it is characterized in that, with pure rare earth metal element, pure Fe, B-Fe, Cu, Al, Si is raw material, and the atomic percent of B example is 18-20% among the described B-Fe, and smelting into composition according to the ratio of each element is R
xFe
100-x-y-a-b-cAl
aCu
bSi
cB
yIngot casting, then ingot casting is broken into the ingot bar that granularity is 1-15mm, be not more than 5 * 10 in vacuum degree
-2Fast quenching becomes thickness to be not more than the even strip of 0.1mm under the vacuum state of Pa, anneals down in vacuum state then.
4. the preparation method of high-remanence low-coercivity permanent magnetic material as claimed in claim 3 is characterized in that, quenches speed control built in 22-23m/s when fast quenching is even strip.
5. as the preparation method of claim 3 or 4 described high-remanence low-coercivity permanent magnetic materials, it is characterized in that, is 4 * 10 in vacuum degree
-2-5 * 10
-2The vacuum state of Pa is annealing down, and annealing temperature is controlled at 650-660 ℃, constant temperature 25-26min.
6. the preparation method of high-remanence low-coercivity permanent magnetic material as claimed in claim 3 is characterized in that, R
xFe
100-x-y-a-b-cAl
aCu
bSi
cB
yComponent content be R
4.2Fe
73.4Al
1.5Cu
0.8Si
1.4B
18.7, R
4.2Fe
74Al
1.3Cu
0.6Si
1.2B
18.7Or R
4.2Fe
74.6Al
1.1Cu
0.4Si
1.0B
18.7
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|---|---|---|---|
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|---|---|---|---|
| CN2010101597295A CN101819844B (en) | 2010-04-29 | 2010-04-29 | High-remanence low-coercivity permanent magnetic material and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1085007A (en) * | 1991-11-11 | 1994-04-06 | 住友特殊金属株式会社 | Alloy powder that rare earth magnet and rare earth magnet are used and manufacture method thereof |
| CN1455937A (en) * | 2001-02-07 | 2003-11-12 | 住友特殊金属株式会社 | Method of making material alloy for iron-based rare earth magnet |
| US7160398B2 (en) * | 2002-08-08 | 2007-01-09 | Neomax Co., Ltd. | Method of making rapidly solidified alloy for magnet |
-
2010
- 2010-04-29 CN CN2010101597295A patent/CN101819844B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1085007A (en) * | 1991-11-11 | 1994-04-06 | 住友特殊金属株式会社 | Alloy powder that rare earth magnet and rare earth magnet are used and manufacture method thereof |
| CN1455937A (en) * | 2001-02-07 | 2003-11-12 | 住友特殊金属株式会社 | Method of making material alloy for iron-based rare earth magnet |
| US7160398B2 (en) * | 2002-08-08 | 2007-01-09 | Neomax Co., Ltd. | Method of making rapidly solidified alloy for magnet |
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| CN101819844B (en) | 2012-11-07 |
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