CN103714928A - Ferro-cerium-based rapid quenching permanent magnet powder and preparation method of ferro-cerium-based rapid quenching permanent magnet powder - Google Patents
Ferro-cerium-based rapid quenching permanent magnet powder and preparation method of ferro-cerium-based rapid quenching permanent magnet powder Download PDFInfo
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Abstract
The invention relates to ferro-cerium-based rapid quenching permanent magnet powder and a preparation method of the ferro-cerium-based rapid quenching permanent magnet powder. The alloy composition chemical formula of the ferro-cerium-based rapid quenching permanent magnet powder is [Ce100-x, Rex]aFe100-a-b-cBbTMc, wherein the x is the mass percent of the rare earth gross, the a, the b and the c show the mass percents of corresponding elements respectively, 0<=x<=50%, 27.5%<=a<=32%, 0.8%<=b<=1.5%, 0.5%<=c<=5%, the Re is one or more of Nd, Pr, Dy and Tb, and the TM is one or more of Ga, Co, Cu, Nb and Al. According to the preparation method, the ferro-cerium-based rapid quenching permanent magnet powder and Re'-Fe-B without Ce can be prepared with a water-cooling electromagnetic roller (a copper alloy roller or a molybdenum roller), and a ferro-cerium-based hot-pressing magnet with double hard magnetic principal phases or multiple hard magnetic principal phases can be prepared with the two kinds of magnetic powder. The ferro-cerium-based rapid quenching permanent magnet powder fills up blanks of middle-grade magnet powder and lower-grade magnet powder on the market at present, the product performance cost ratio is high, and the ferro-cerium-based rapid quenching permanent magnet powder and the preparation method are suitable for engineering production.
Description
Technical field
The invention belongs to rare-earth permanent-magnet material technical field, relate in particular to a kind of cerium iron-base quick-quenching permanent magnetism powder and preparation method.
Background technology
Fast quenching permanent magnetism powder is the core material that hot pressing/hot-fluid becomes permanent magnet, determining the performance of magnet, hot pressing/hot-fluid exchanges work that skill has simply, low temperature, in short-term, can near-net forming etc. feature, particularly at radially oriented and multipole oriental magnetic ring and nanometer two-phase built-up magnet, there is distinctive feature aspect preparing.Current hot pressing/hot-fluid becomes neodymium metal Nd in neodymium iron boron magnetic body and accounts for the more than 90% of the cost of raw material.Along with the continuous increase of Global Rare-earth Permanent Magnet body output in recent years, the use that neodymium metal is a large amount of, make the application of rare earth element extremely uneven, novel hot pressing ferrocerium base fast quenching permanent magnetism powder of the present invention and technology of preparing are to realize the important breakthrough of rare earth element balance application, are of great immediate significance.
In natural rare earth resources, except Nd, also have reserves to enrich and cheap metallic cerium Ce.Yet due to Ce
2fe
14the magnetic moment Js of B and anisotropy field H
afar below Nd
2fe
14b, adopts product prepared by traditional preparation method cannot meet the requirement of user to performance.In the prior art, Chinese patent application CN101694797A, discloses Ce content and has surpassed the 40wt% of total amount of rare earth, production be quick setting belt, final permanent magnetic material product is the magnetic of mainly doing bonded permanent magnet.In CN102220538A, principal phase (Re
2fe
14b) in alloy, do not contain La, Ce; In auxiliary phase alloy (being called again liquid phase alloy or rich rare-earth phase alloy), the maximum that Ce accounts for auxiliary phase alloy total weight is that the maximum that 30wt%, La account for auxiliary phase alloy total weight is 25wt%, in embodiment, main-phase alloy and auxiliary phase alloy mix by high mixture ratio 88:12, the Ce in final magnet, La total amount are no more than the 12wt% of magnet middle rare earth total amount, and above-mentioned prior art for be that (weightlessness is unexpectedly up to 2mg/cm for so-called low weightless magnet
2).In CN102360657A, total amount of rare earth accounts for the 35wt% of " N35 lanthanum cerium magnet " total weight, and La-Ce only accounts for the 20wt% of total amount, and the embodiment of this application do not provide respectively the percentage that La and Ce account for total amount of rare earth, obviously, La, Ce proportion difference, the magnetic property of final magnet is also different, can not occur unique result that embodiment provides, Be=12kOe, Hcj=12.6kOe, (BH) max=34.2MGOe.
In a word, above-mentioned patent applications/patents relates to the rare earth permanent-magnetic material of Ce element, and its Ce content is all less than 40% of (or equaling) total amount of rare earth, and prepares permanent magnetism quick setting belt and be used for manufacturing isotropism bonding magnetic.Rapid-hardening flake (band) and fast quenching sheet (band) are two different concepts, roller speed (linear resonance surface velocity) while preparing fast quenching sheet (band) is in 15～50m/s scope, rapid tempering belt is amorphous ribbon or microstructure, conventionally isotropism magnetic be can only be prepared into, bonded permanent magnet or single principal phase hot-pressed magnets are used for making.Quick setting belt is a kind of crystallization slab (band), and the roller speed (linear resonance surface velocity) while preparing quick setting belt, in 1～7m scope, mainly waits the thin crystalline substance of axle to form by sheet (band) the shape crystalline substance and the trace that vertically paste the growth of roll surface direction, is mainly used to prepare sintered magnet.In the prior art, for high Ce, for cerium iron-base quick-quenching permanent magnetism powder, have not been reported so far.
Summary of the invention
The object of the present invention is to provide a kind of cerium iron-base quick-quenching permanent magnetism powder and preparation method thereof, this fast quenching permanent magnetism powder can be used for preparing ferrocerium base hot pressing/hot-fluid and becomes magnet; Or mixes with a certain amount of Re '-Fe-B (Re ' for not comprising the rare earth element of Ce) magnetic proportioning, can prepare ferrocerium base hot-pressed magnets and the conventional Ce neodymium iron boron hot-pressed magnets that contains of novel two (Hard Magnetic) principal phases.
The object of the invention is to be achieved through the following technical solutions:
A cerium iron-base quick-quenching permanent magnetism powder, the alloying component chemical formula of fast quenching permanent magnetism powder is: [Ce
100-x, Re
x]
afe
100-a-b-cb
btM
c, wherein, x is the mass percent of Re in total amount of rare earth, a, and b and c represent respectively the mass percent of corresponding element, 0≤x≤50%, 27.5%≤a≤32%; 0.8%≤b≤1.5%; 0.5%≤c≤5%; Re is Nd, Pr, and Dy, one or more in Tb element, TM is Ga, Co, Cu, Nb, one or more in Al element; Wherein, the Ce content in this fast quenching permanent magnetism powder is greater than 50% of total amount of rare earth, and when Re is Nd, Nd content is less than or equal to 50% of total amount of rare earth.
Described iron-base quick-quenching permanent magnetism powder, by the following method preparation:
First adopt the electromagnetism roller of rapid quenching technique to prepare cerium iron-base quick-quenching permanent magnetism band, the microstructure of rapid tempering belt is crystallite, amorphous or equiax crystal, and there will not be the column crystal in quick setting belt prepared by strip casting;
With the cerium iron-base quick-quenching permanent magnetism band obtaining, prepare cerium iron-base permanent-magnet powder and do not contain two kinds of magnetics of Re '-Fe-B of Ce, utilizing above-mentioned two kinds of magnetics to mix, can prepare the ferrocerium base hot-pressed magnets of two Hard Magnetic principal phases or many Hard Magnetics principal phase.
The preparation method of described iron-base quick-quenching permanent magnetism powder,
First adopt electromagnetism roller to prepare cerium iron-base quick-quenching permanent magnetism band, with the cerium iron-base quick-quenching permanent magnetism band obtaining, prepare cerium iron-base permanent-magnet powder and do not contain Re '-Fe-B magnetic of Ce, utilize above-mentioned two kinds of magnetics, the ferrocerium base hot-pressed magnets that can prepare two Hard Magnetic principal phases or many Hard Magnetics principal phase, specifically comprises the steps:
Step 1: the composition chemical formula according to following mass percent is prepared burden: [Ce
100-x, Re
x]
afe
100-a-b-cb
btM
c, wherein x is the mass percent of Re in total amount of rare earth, a, and b and c represent respectively the mass percent of corresponding element, 0≤x≤50%, 27.5%≤a≤32%; 0.8%≤b≤1.5%; 0.5%≤c≤5%; Re is Nd, Pr, and Dy, one or more in Tb element, TM is Ga, Co, Cu, Nb, one or more in Al element;
Step 2: the raw material preparing packs in fast quenching equipment, then low smelting heat and carry out electromagnetic agitation refining under Ar gas protection, according to roller speed and alloying component, the frequency of adjusting water-cooled electromagnetic roller is between zero or 2000Hz～9000Hz, then being cast in linear velocity is that 15～45m/s has arranged on the water-cooled electromagnetic roller roller superficial layer 4 of electromagnetic frequency, and making average thickness is fast quenching sheet or the rapid tempering belt 3 of 0.01～0.06mm;
Step 3: fast quenching sheet or rapid tempering belt 3 are carried out to fragmentation, obtain particle size range at fast quenching sheet or the rapid tempering belt of 0.056～0.28mm.
In described step 2: first raw material are put into the material containing device 1 of the equipment of Medium frequency induction melting, reached 10 in vacuum degree
-2when Pa is above, use heater coil 2 to feed electric preheating, treat that vacuum degree reaches 10 again
-2after Pa is above, stop vacuumizing and being filled with high-purity Ar, make in stove after Ar air pressure reaches-0.04～-0.08MPa to carry out melting; Until raw material, all after fusing, impose electromagnetic agitation refining, carry out subsequently molten steel cast.
In step 3, according to the different demands to fast quenching sheet or rapid tempering belt 3, adopt stirring mill or sand milling to carry out powder process, be met the magnetic of requirement, prepare forerunner's magnetic of magnet.
In order to obtain the magnetic of uniform particle diameter, select respectively the vibrating screen of 45 order～260 order different meshes, magnetic is poured in vibrating screen and looked over so as to check, by category filter, obtain the magnetic of required particle diameter.
Described roller superficial layer 4 is copper alloy roll surface or molybdenum roll surface.
The rapidly quenched magnetic powder that novel hot pressing ferrocerium base permanent magnet of the present invention is used has Nd
2fe
14the crystal structure of B, but its Ce content is more than or equal to 50% of total amount of rare earth, and Nd content is less than or equal to 50% of total amount of rare earth.This Ce-Fe base rapidly quenched magnetic powder is mixed with a certain amount of NdFeB magnetic powder proportioning, through hot pressing/hot-fluid skill of exchanging work, not only can prepare the conventional neodymium iron boron hot-pressed magnets containing Ce, also can prepare the ferrocerium base hot-pressed magnets of novel pair of Hard Magnetic phase or many Hard Magnetics phase.
Beneficial effect of the present invention is:
Compared with prior art, the present invention has the following advantages:
1, be first fast quenching sheet (band) and the anisotropic magnet powder of high cerium content, its cerium content is generally more than or equal to 50% of total amount of rare earth; Contrast iron boron magnetic quick setting belt, smelting temperature and the time of cerium iron-base quick-quenching sheet (band) obviously reduce, and can save production time and energy resource consumption;
2, the antioxygenic property of cerium iron-base quick-quenching sheet (band) and anisotropic magnet powder is obviously better than metallic cerium, has solved and has deposited merely the oxidizable problem of metallic cerium;
3, the present invention adopts the water-cooled electromagnetic roller (copper alloy roll surface or molybdenum alloy roll surface) of brand-new design, and the rapid tempering belt of preparing is substantially all crystallite, amorphous or equiax crystal structure, and there will not be thick column crystal in quick setting belt prepared by strip casting.
4, the present invention is not that simple Ce substitutes Nd problem, because cerium content is generally more than or equal to 50% of total amount of rare earth, product is a kind of novel CeFeB permanent magnetism rapid tempering sheet (band) or magnetic, not only can prepare the conventional neodymium iron boron hot-pressed magnets containing Ce, also can prepare the ferrocerium base hot-pressed magnets of novel pair of Hard Magnetic phase or many Hard Magnetics phase.This invention filled up in the market in, the blank of low-grade magnetic, product cost performance is high, is suitable for through engineering approaches and produces.
Reference numeral
1 material containing device
2 heater coils
3 fast quenching sheet or rapid tempering belts
4 roller superficial layers (copper alloy roll surface or molybdenum roll surface)
5 field coils (going out)
6 field coils (entering)
Accompanying drawing explanation
Fig. 1 is rapid quenching technique schematic diagram of the present invention.
Fig. 2 is that composition of the present invention is (Ce
90nd
10)
30fe
balco
4ga
0.4b
0.92the magnetic hysteresis loop of magnetic.
Fig. 3 is that composition of the present invention is (Ce
70nd
30)
30fe
balco
3.9ga
0.4cu
0.1b
0.92the magnetic hysteresis loop of magnetic.
Fig. 4 is that composition of the present invention is (Ce
50nd
50)
30fe
balco
3.9ga
0.4al
0.1b
0.92the magnetic hysteresis loop of magnetic.
Fig. 5 is that composition of the present invention is (Ce
55nd
42)
30fe
balco
3.9ga
0.4b
0.92the magnetic hysteresis loop of magnetic.
Fig. 6 is that composition of the present invention is (Ce
50nd
47d
y1pr
1tb
1)
32fe
balco
4.2ga
0.8b
1.5the magnetic hysteresis loop of magnetic.
Fig. 7 is that composition of the present invention is (Ce
74nd
25d
y1)
27,5fe
balga
0.5b
0.8the magnetic hysteresis loop of magnetic.
Embodiment
Below in conjunction with drawings and Examples, the specific embodiment of the present invention is described in further detail.
Adopt low smelting heat, fast quenching process is prepared magnetic (as shown in Figure 1) on copper alloy roller or molybdenum roller, and processing step is as follows:
Step 1: according to the composition chemical formula of mass percent: [Ce
100-x, Re
x]
afe
100-a-b-cb
btM
cpreparation raw material (as shown in table 1), wherein Re is Nd, Pr, Dy, one or more in Tb element, TM is Ga, Co, Cu, Nb, one or more in Al element.
The different embodiment alloying component of table 1 chemical formula
| ? | Nominal composition |
| Embodiment 1 | (Ce 90Nd 10) 30Fe balCo 4Ga 0.4B 0.92 |
| Embodiment 2 | (Ce 70Nd 30) 30Fe balCo 3.9Ga 0.4Cu 0.1B 0.92 |
| Embodiment 3 | (Ce 50Nd 50) 30Fe balCo 3.9Ga 0.4Al 0.1B 0.92 |
| Embodiment 4 | (Ce 55Nd 45) 30Fe balCo 3.9Ga 0.4B 0.92 |
| Embodiment 5 | (Ce 50Nd 47D y1Pr 1Tb 1) 32Fe balCo 4.2Ga 0.8B 1.5 |
| Embodiment 6 | (Ce 74Nd 25D y1) 27,5Fe balGa 0.5B 0.8 |
Step 2: the raw material preparing melting respectively: as shown in Figure 1, first raw material are put into the material containing device 1 of Medium frequency induction smelting equipment, reached 10 in vacuum degree
-2when Pa is above, use heater coil 2 to feed electric preheating, treat that vacuum degree reaches 10 again
-2after Pa is above, stop vacuumizing and being filled with high-purity Ar, make in stove after Ar air pressure reaches-0.04～-0.08MPa to carry out melting; Treat that temperature reaches 1200 ℃ up and down, raw material all impose electromagnetic agitation refining after fusing, subsequently molten steel being poured into linear velocity is on 15～45m/s and the roller superficial layer 4 that electromagnetic frequency has been set, and making average thickness is the fast quenching sheet 3 (band) of 0.01～0.06mm.
This smelting equipment is wound around in the outside of iron core the conductive winding matching with its power, and this alive coil has magnetic as magnet, and it is also called electromagnet.Electromagnet has many advantages: the magnetic of electromagnet has or not can use switching Current Control; How many sizes of magnetic can be controlled by the power of electric current or the number of turn of coil; Also can control magnetic size by changing resistance control size of current; Its magnetic pole can be controlled by changing sense of current, etc.That is: the power of magnetic can change, magnetic have or not can control, the direction of magnetic pole can change, magnetic can disappear because of the disappearance of electric current.
Step 3: according to the different demands to fast quenching sheet 3 (band), adopt and stir forerunner's magnetic that frosted grinds or hydrogen fragmentation is prepared, obtain particle size range at the fast quenching sheet (band) of 0.056～0.28mm.
Step 4: in order to obtain the magnetic of uniform particle diameter, select the vibrating screen of different meshes (45 order～260 order), magnetic is poured in vibrating screen and looked over so as to check, by category filter, obtain the magnetic of required particle diameter.
The concrete technology parameter of different embodiment is referring to table 2.
The different embodiment alloy preparation technology of table 2 parameter
Note: the thickness of fast quenching sheet and the size of average grain diameter are relevant to the rotating speed of running roller and selection by winnowing wheel, when running roller and selection by winnowing wheel speed are larger time, thickness and granularity can be less.
Employing Versalab multifunction vibration sample magnetic strength instrumentation obtains the magnetic property of magnetic, referring to table 3 and accompanying drawing 2,3,4,5,6,7.
The magnetic parameter of the different embodiment alloys of table 3
| ? | B r/kGs | H
cj/ |
| Embodiment | ||
| 1 | 5.765 | 3.508 |
| |
5.474 | 9.793 |
| |
5.305 | 12.500 |
| |
5.891 | 11.367 |
| Embodiment 5 | 6.313 | 11.459 |
| Embodiment 6 | 3.180 | 1.405 |
Claims (7)
1. a cerium iron-base quick-quenching permanent magnetism powder, is characterized in that, the alloying component chemical formula of fast quenching permanent magnetism powder is: [Ce
100-x, Re
x]
afe
100-a-b-cb
btM
c, wherein, x is the mass percent of Re in total amount of rare earth, a, and b and c represent respectively the mass percent of corresponding element, 0≤x≤50%, 27.5%≤a≤32%; 0.8%≤b≤1.5%; 0.5%≤c≤5%; Re is Nd, Pr, and Dy, one or more in Tb element, TM is Ga, Co, Cu, Nb, one or more in Al element; Wherein, the Ce content in this fast quenching permanent magnetism powder is greater than 50% of total amount of rare earth, and when Re is Nd, Nd content is less than or equal to 50% of total amount of rare earth.
2. iron-base quick-quenching permanent magnetism powder as claimed in claim 1, is characterized in that, by the following method preparation:
First adopt the electromagnetism roller of rapid quenching technique to prepare cerium iron-base quick-quenching permanent magnetism band, the microstructure of rapid tempering belt is crystallite, amorphous or equiax crystal, and there will not be the column crystal in quick setting belt prepared by strip casting;
With the cerium iron-base quick-quenching permanent magnetism band obtaining, prepare cerium iron-base permanent-magnet powder and do not contain two kinds of magnetics of Re '-Fe-B of Ce, utilizing above-mentioned two kinds of magnetics to mix, can prepare the ferrocerium base hot-pressed magnets of two Hard Magnetic principal phases or many Hard Magnetics principal phase.
3. a preparation method for iron-base quick-quenching permanent magnetism powder as claimed in claim 1, is characterized in that,
First adopt electromagnetism roller to prepare cerium iron-base quick-quenching permanent magnetism band, with the cerium iron-base quick-quenching permanent magnetism band obtaining, prepare cerium iron-base permanent-magnet powder and do not contain Re '-Fe-B magnetic of Ce, utilize above-mentioned two kinds of magnetics, the ferrocerium base hot-pressed magnets that can prepare two Hard Magnetic principal phases or many Hard Magnetics principal phase, specifically comprises the steps:
Step 1: the composition chemical formula according to following mass percent is prepared burden: [Ce
100-x, Re
x]
afe
100-a-b-cb
btM
c, wherein x is the mass percent of Re in total amount of rare earth, a, and b and c represent respectively the mass percent of corresponding element, 0≤x≤50%, 27.5%≤a≤32%; 0.8%≤b≤1.5%; 0.5%≤c≤5%; Re is Nd, Pr, and Dy, one or more in Tb element, TM is Ga, Co, Cu, Nb, one or more in Al element;
Step 2: the raw material preparing packs in fast quenching equipment, then low smelting heat and carry out electromagnetic agitation refining under Ar gas protection, according to roller speed and alloying component, the frequency of adjusting water-cooled electromagnetic roller is between zero or 2000Hz～9000Hz, then being cast in linear velocity is that 15～45m/s has arranged on the water-cooled electromagnetic roller roller superficial layer (4) of electromagnetic frequency, and making average thickness is fast quenching sheet or the rapid tempering belt (3) of 0.01～0.06mm;
Step 3: fast quenching sheet or rapid tempering belt (3) are carried out to fragmentation, obtain particle size range at fast quenching sheet or the rapid tempering belt of 0.056～0.28mm.
4. preparation method as claimed in claim 3, is characterized in that, in described step 2: first raw material are put into the material containing device (1) of the equipment of Medium frequency induction melting, reached 10 in vacuum degree
-2when Pa is above, use heater coil (2) to feed electric preheating, treat that vacuum degree reaches 10 again
-2after Pa is above, stop vacuumizing and being filled with high-purity Ar, make in stove after Ar air pressure reaches-0.04～-0.08MPa to carry out melting; Until raw material, all after fusing, impose electromagnetic agitation refining, carry out subsequently molten steel cast.
5. preparation method as claimed in claim 3, is characterized in that, in step 3, according to the different demands to fast quenching sheet or rapid tempering belt (3), adopts stirring mill or sand milling to carry out powder process, is met the magnetic of requirement, prepares forerunner's magnetic of magnet.
6. preparation method as claimed in claim 5, is characterized in that, in order to obtain the magnetic of uniform particle diameter, selects respectively the vibrating screen of 45 order～260 order different meshes, and magnetic is poured in vibrating screen and looked over so as to check, and by category filter, obtains the magnetic of required particle diameter.
7. preparation method as claimed in claim 3, is characterized in that, described roller superficial layer (4) is copper alloy roll surface or molybdenum roll surface.
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| CN106799479A (en) * | 2017-03-17 | 2017-06-06 | 山东三尺企业管理咨询有限公司 | D.C. magnetic field changes amorphous method and device of the spray with magnetic domain orientation |
| CN113035559A (en) * | 2021-04-01 | 2021-06-25 | 包头市科锐微磁新材料有限责任公司 | Preparation method of high-performance neodymium iron boron isotropic magnetic powder |
| CN113782290A (en) * | 2021-09-07 | 2021-12-10 | 钢铁研究总院 | high-Ce-content double-main-phase high-magnetic-energy product magnet and preparation method thereof |
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