CN103714928B - A kind of cerium iron-base quick-quenching permanent magnetism powder and preparation method thereof - Google Patents
A kind of cerium iron-base quick-quenching permanent magnetism powder and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of cerium iron-base quick-quenching permanent magnetism powder and technology of preparing, the alloying component chemical formula of the cerium iron-base quick-quenching permanent magnetism powder is：[Ce100‑x,Rex]aFe100‑a‑b‑cBbTMc, wherein, x is the mass percent of total amount of rare earth, and a, b and c represent the mass percent of corresponding element, 0≤x≤50%, 27.5%≤a≤32% respectively；0.8%≤b≤1.5%；0.5%≤c≤5%；Re is Nd, Pr, Dy, the one or more in Tb elements, the one or more in TM Ga, Co, Cu, Nb, Al elements；The present invention can prepare ferrocerium base permanent magnetism powder and two kinds of magnetics of Re ' Fe B without Ce using water-cooled electromagnetic roller (copper alloy roller or molybdenum roller), and the ferrocerium base hot-pressed magnets of double Hard Magnetic principal phases or more Hard Magnetic principal phases can be prepared using above two magnetic.The invention filled up in the market in, the blank of low-grade magnetic, product cost is high, is produced suitable for engineering.
Description
Technical field
The invention belongs to rare-earth permanent-magnet material technical field, more particularly to a kind of cerium iron-base quick-quenching permanent magnetism powder and preparation side
Method.
Background technology
Fast quenching permanent magnetism powder is the core material that hot pressing/hot-fluid becomes permanent magnet, decides the performance of magnet, and hot pressing/hot-fluid becomes
Technique have the characteristics that simple, low temperature, in short-term, can near-net forming, particularly in radially oriented and multipole oriental magnetic ring and nanometer
There is distinctive feature in terms of the preparation of two-phase built-up magnet.Current hot pressing/hot-fluid becomes neodymium metal Nd in neodymium iron boron magnetic body and accounts for former material
Expect more than the 90% of cost.With being continuously increased for Global Rare-earth Permanent Magnet body yield in recent years, neodymium metal largely uses, and makes dilute
The application of earth elements is extremely uneven, and new hot pressing cerium iron-base quick-quenching permanent magnetism powder and technology of preparing of the invention are to realize rare earth element
The important breakthrough of application is balanced, is of great immediate significance.
In natural rare earth resources, there are rich reserves and cheap metallic cerium Ce in addition to Nd.Yet with
Ce2Fe14B magnetic moment Js and anisotropy field HAFar below Nd2Fe14B, the product prepared using traditional preparation method can not expire
Requirement of the sufficient user to performance.In the prior art, Chinese patent application CN101694797A, Ce contents is disclosed and are not above
The 40wt% of total amount of rare earth, production is quick setting belt, and final permanent-magnet material product is the magnetic for mainly doing bonded permanent magnet.
In CN102220538A, principal phase（Re2Fe14B）La, Ce are free of in alloy；In auxiliary phase alloy（Also known as liquid phase alloy or rich rare earth
Phase alloy）In, the maximum that Ce accounts for auxiliary phase alloy gross weight is that the maximum that 30wt%, La account for auxiliary phase alloy gross weight is
25wt%, in embodiment, main-phase alloy is with auxiliary phase alloy by highest proportioning 88：12 mix, then Ce, La total amount in final magnet
No more than the 12wt% of magnet middle rare earth total amount, and above-mentioned prior art is directed to so-called low weightless magnet（Weightlessness is up to unexpectedly
2mg/cm2）.In CN102360657A, total amount of rare earth accounts for the 35wt% of " N35 lanthanum ceriums magnet " gross weight, and La-Ce is only accounted for always
The 20wt% of amount, and the embodiment of this application does not provide the percentage that La and Ce accounts for total amount of rare earth respectively, it is clear that La, Ce institute
Accounting example is different, and the magnetic property of final magnet is also different, it is impossible to goes out the unique consequence that current embodiment provides, Be=12kOe, Hcj
=12.6kOe, (BH) max=34.2MGOe.
In a word, above-mentioned patent applications/patents are related to the rare earth permanent-magnetic material of Ce elements, and its Ce content is both less than（Or wait
In）The 40% of total amount of rare earth, and prepare permanent magnetism quick setting belt and be used for manufacturing isotropism bonding magnetic.Rapid-hardening flake (band) with it is fast
Piece (band) of quenching is two different concepts, prepares roller speed during fast quenching piece (band)（Linear resonance surface velocity）In 15~50m/s scopes, soon
Band of quenching is amorphous ribbon or microstructure, is typically only capable to be prepared into isotropism magnetic, for making bonded permanent magnet or single principal phase heat
Press magnet.Quick setting belt is a kind of crystallization slab (band), prepares roller speed during quick setting belt（Linear resonance surface velocity）It is main in 1~7m scopes
To be made up of the brilliant and micro isometric fine grain of piece (band) shape for vertically pasting the growth of roll surface direction, be mainly used to prepare sintered magnet.
In the prior art, it is used for cerium iron-base quick-quenching permanent magnetism powder for high Ce, has not been reported so far.
The content of the invention
It is an object of the invention to provide a kind of cerium iron-base quick-quenching permanent magnetism powder and preparation method thereof, the fast quenching permanent magnetism powder can use
Become magnet in preparing ferrocerium base hot pressing/hot-fluid；Or with a certain amount of Re '-Fe-B (Re ' is not include Ce rare earth element) magnetic
Proportioning mixing, it can prepare new double（Hard Magnetic）The ferrocerium base hot-pressed magnets of principal phase and the conventional hot-pressed magnets of neodymium iron boron containing Ce.
The purpose of the present invention is achieved through the following technical solutions：
A kind of cerium iron-base quick-quenching permanent magnetism powder, the alloying component chemical formula of fast quenching permanent magnetism powder are：[Ce100-x,Rex]aFe100-a-b-cBbTMc, wherein, x is the mass percent of Re in total amount of rare earth, and a, b and c represent the quality hundred of corresponding element respectively
Divide ratio, 0≤x≤50%, 27.5%≤a≤32%；0.8%≤b≤1.5%；0.5%≤c≤5%；Re is Nd, Pr, Dy, in Tb elements
One or more, the one or more in TM Ga, Co, Cu, Nb, Al elements；Wherein, the Ce contents in the fast quenching permanent magnetism powder
More than the 50% of total amount of rare earth, when Re is Nd, Nd contents are less than or equal to the 50% of total amount of rare earth.
Described iron-base quick-quenching permanent magnetism powder, is prepared via a method which：
Cerium iron-base quick-quenching permanent magnetism band is prepared using the electromagnetism roller of rapid quenching technique first, the microstructure of rapid tempering belt be crystallite,
Amorphous or equiax crystal, without the column crystal in the quick setting belt of strip casting preparation；
Ferrocerium base permanent magnetism powder and two kinds of magnetics of Re '-Fe-B without Ce are prepared with obtained cerium iron-base quick-quenching permanent magnetism band,
Mixed using above two magnetic, the ferrocerium base hot-pressed magnets of double Hard Magnetic principal phases or more Hard Magnetic principal phases can be prepared.
The preparation method of described iron-base quick-quenching permanent magnetism powder,
Cerium iron-base quick-quenching permanent magnetism band is prepared using electromagnetism roller first, ferrocerium is prepared with obtained cerium iron-base quick-quenching permanent magnetism band
Base permanent magnetism powder and the Re '-Fe-B magnetics without Ce, using above two magnetic, can prepare double Hard Magnetic principal phases or more Hard Magnetic masters
The ferrocerium base hot-pressed magnets of phase, specifically comprise the following steps：
Step 1：Dispensing is carried out according to the Components Chemical formula of following mass percent：[Ce100-x,Rex]aFe100-a-b- cBbTMc, wherein x is the mass percent of Re in total amount of rare earth, and a, b and c represent the mass percent of corresponding element, 0≤x respectively
≤50%,27.5%≤a≤32%；0.8%≤b≤1.5%；0.5%≤c≤5%；Re is Nd, Pr, Dy, one kind or several in Tb elements
Kind, the one or more in TM Ga, Co, Cu, Nb, Al elements；
Step 2：The raw material prepared is fitted into fast quenching equipment, then low smelting heat and progress electromagnetic agitation under Ar gas shieldeds
Refining, according to roller speed and alloying component, the frequency of adjustment water-cooled electromagnetic roller is between zero or 2000Hz~9000Hz, is then poured into a mould
On-line velocity be 15~45m/s set on the water-cooled electromagnetic roller roller surface layer 4 of electromagnetic frequency, be made average thickness be 0.01~
0.06mm fast quenching piece or rapid tempering belt 3；
Step 3：Fast quenching piece or rapid tempering belt 3 are crushed, obtain particle size range in 0.056~0.28mm fast quenching piece or
Rapid tempering belt.
In the step 2：Raw material are put into the material containing device 1 of the equipment of Medium frequency induction melting first, reached in vacuum
To 10-2Electric preheating is fed using heating coil 2 during more than Pa, treats that vacuum reaches 10 again-2Stop vacuumizing simultaneously after more than Pa
High-purity Ar is filled with, Ar air pressure in stove is carried out melting after reaching -0.04~-0.08MPa；Electricity is imposed after raw material all fusing
Magnetic stirring refining, then carries out molten steel cast.
In step 3, according to the different demands to fast quenching piece or rapid tempering belt 3, powder processed is carried out using Ball-stirring mill or sand milling, obtained
The magnetic required to satisfaction, prepare forerunner's magnetic of magnet.
In order to obtain the magnetic of uniform particle diameter, the vibratory sieve of the mesh different meshes of 45 mesh~260 is selected respectively, magnetic is fallen
Enter in vibratory sieve and look over so as to check, by category filter, the magnetic of particle diameter needed for acquisition.
The roller surface layer 4 is copper alloy roll surface or molybdenum roll surface.
The rapidly quenched magnetic powder of the new hot pressing ferrocerium base permanent magnet of the present invention has Nd2Fe14B crystal structure, but its Ce
Content is more than or equal to the 50% of total amount of rare earth, and Nd contents are less than or equal to the 50% of total amount of rare earth.By this Ce-Fe bases fast quenching
Magnetic mixes with a certain amount of NdFeB magnetic powder proportioning, becomes technique by hot pressing/hot-fluid, can not only prepare the routine containing Ce
Neodymium iron boron hot-pressed magnets, it can also prepare the ferrocerium base hot-pressed magnets of new double Hard Magnetic phases or more Hard Magnetic phases.
The beneficial effects of the present invention are：
Compared with prior art, the present invention has advantages below：
1st, it is that the fast quenching piece (band) of high cerium content and anisotropic magnet powder, its cerium content are typically greater than or equal to rare earth first
The 50% of total amount；Iron boron magnetic quick setting belt is contrasted, the smelting temperature of cerium iron-base quick-quenching piece (band) and time substantially reduce, can saved
Production time and energy resource consumption；
2nd, the antioxygenic property of cerium iron-base quick-quenching piece (band) and anisotropic magnet powder is substantially better than metallic cerium, solves simple
Deposit the problem of metallic cerium is oxidizable；
3rd, the present invention uses the water-cooled electromagnetic roller of brand-new design（Copper alloy roll surface or molybdenum alloy roll surface）, the fast quenching prepared
Band is substantially crystallite, amorphous or isometric crystal structure, thick column crystal in the quick setting belt prepared without strip casting.
4th, the present invention is not that simple Ce substitutes Nd problems, because cerium content is typically greater than or equal to total amount of rare earth
50%, product is a kind of new CeFeB permanent magnetism rapid temperings piece (band) or magnetic, can not only prepare the conventional neodymium iron boron containing Ce
Hot-pressed magnets, it can also prepare the ferrocerium base hot-pressed magnets of new double Hard Magnetic phases or more Hard Magnetic phases.Current city has been filled up in the invention
In on field, the blank of low-grade magnetic, product cost is high, and is produced suitable for engineering
Reference
1 material containing device
2 heating coils
3 fast quenching pieces or rapid tempering belt
4 roller surface layers（Copper alloy roll surface or molybdenum roll surface）
5 field coils（Go out）
6 field coils（Enter）
Brief description of the drawings
Fig. 1 is rapid quenching technique schematic diagram of the present invention.
Fig. 2 is that present component is (Ce90Nd10)30FebalCo4Ga0.4B0.92The hysteresis curve of magnetic.
Fig. 3 is that present component is (Ce70Nd30)30FebalCo3.9Ga0.4Cu0.1B0.92The hysteresis curve of magnetic.
Fig. 4 is that present component is (Ce50Nd50)30FebalCo3.9Ga0.4Al0.1B0.92The hysteresis curve of magnetic.
Fig. 5 is that present component is (Ce55Nd42)30FebalCo3.9Ga0.4B0.92The hysteresis curve of magnetic.
Fig. 6 is that present component is (Ce50Nd47Dy1Pr1Tb1)32FebalCo4.2Ga0.8B1.5The hysteresis curve of magnetic.
Fig. 7 is that present component is (Ce74Nd25Dy1)27,5FebalGa0.5B0.8The hysteresis curve of magnetic.
Embodiment
With reference to the accompanying drawings and examples, the embodiment of the present invention is described in further detail.
Using low smelting heat, fast quenching process prepares magnetic on copper alloy roller or molybdenum roller（As shown in Figure 1）, processing step is such as
Under：
Step 1：According to the Components Chemical formula of mass percent：[Ce100-x,Rex]aFe100-a-b-cBbTMcPreparation raw material（Such as
Shown in table 1）, wherein Re is Nd, Pr, Dy, the one or more in Tb elements, one kind in TM Ga, Co, Cu, Nb, Al elements
It is or several.
The different embodiment alloying component chemical formulas of table 1
| Nominal composition | |
| Embodiment 1 | (Ce90Nd10)30FebalCo4Ga0.4B0.92 |
| Embodiment 2 | (Ce70Nd30)30FebalCo3.9Ga0.4Cu0.1B0.92 |
| Embodiment 3 | (Ce50Nd50)30FebalCo3.9Ga0.4Al0.1B0.92 |
| Embodiment 4 | (Ce55Nd45)30FebalCo3.9Ga0.4B0.92 |
| Embodiment 5 | (Ce50Nd47Dy1Pr1Tb1)32FebalCo4.2Ga0.8B1.5 |
| Embodiment 6 | (Ce74Nd25Dy1)27,5FebalGa0.5B0.8 |
Step 2：The raw material difference melting prepared：As shown in figure 1, raw material are put into Medium frequency induction smelting equipment first
In material containing device 1, reach 10 in vacuum-2Electric preheating is fed using heating coil 2 during more than Pa, treats that vacuum reaches again
10-2Stop vacuumizing and being filled with high-purity Ar after more than Pa, Ar air pressure in stove is carried out melting after reaching -0.04~-0.08MPa；
Treat that temperature reaches about 1200 DEG C, raw material impose electromagnetic agitation refining after all melting, molten steel then is poured into linear velocity
For 15~45m/s and set on the roller surface layer 4 of electromagnetic frequency, the fast quenching piece 3 that average thickness is 0.01~0.06mm is made
(band).
The conductive winding that the smelting equipment matches in the outside winding of iron core with its power, this coil to alive
There is magnetic as magnet, it is also referred to as electromagnet.Electromagnet has many advantages：The magnetic of electromagnet whether there is can use it is logical,
Power off flow control；How much the size of magnetic can be controlled with the power of electric current or the number of turn of coil；Also can be by changing resistance
Control electric current size controls magnetic size；Its magnetic pole can be controlled, etc. by change sense of current.I.e.：Magnetic
Power can change, the presence or absence of magnetic can control, the direction of magnetic pole can change, and magnetic can disappear because of the disappearance of electric current.
Step 3：According to the different demands to fast quenching piece 3 (band), crushed using stirring frosted mill or hydrogen before being prepared
Magnetic is driven, obtains fast quenching piece (band) of the particle size range in 0.056~0.28mm.
Step 4：In order to obtain the magnetic of uniform particle diameter, different meshes are selected（The mesh of 45 mesh~260）Vibratory sieve, by magnetic
Powder is poured into vibratory sieve and looked over so as to check, by category filter, the magnetic of particle diameter needed for acquisition.
The specific process parameter of different embodiments is referring to table 2.
The different embodiment alloy preparation technology parameters of table 2
Note：The thickness of fast quenching piece and the size of average grain diameter, the rotating speed to disk roller and selection by winnowing wheel are related, work as disk roller
With selection by winnowing wheel speed it is bigger when, thickness and granularity can be smaller.
The magnetic property of magnetic is measured using Versalab multifunction vibration sample magnetometers, referring to table 3 and accompanying drawing 2,3,4,
5、6、7。
The magnetic parameter of the different embodiment alloys of table 3
| Br/kGs | Hcj/kOe | |
| Embodiment 1 | 5.765 | 3.508 |
| Embodiment 2 | 5.474 | 9.793 |
| Embodiment 3 | 5.305 | 12.500 |
| Embodiment 4 | 5.891 | 11.367 |
| Embodiment 5 | 6.313 | 11.459 |
| Embodiment 6 | 3.180 | 1.405 |
Claims (4)
1. a kind of cerium iron-base quick-quenching permanent magnetism powder, it is characterised in that the alloying component chemical formula of fast quenching permanent magnetism powder is：[Ce100-x,
Rex]aFe100-a-b-cBbTMc, wherein, x is the mass percent of Re in total amount of rare earth, and a, b and c represent the matter of corresponding element respectively
Measure percentage, 0≤x≤50,27.5≤a≤32；0.8≤b≤1.5；0.5≤c≤5；Re is Nd, Pr, Dy, one in Tb elements
Kind or several, the one or more in TM Ga, Co, Cu, Nb, Al elements；Wherein, the Ce contents in the fast quenching permanent magnetism powder are more than
The 50% of total amount of rare earth, when Re is Nd, Nd contents are less than or equal to the 50% of total amount of rare earth；
The microstructure of the fast quenching permanent magnetism powder is crystallite, amorphous or equiax crystal, without the quick setting belt of strip casting preparation
In column crystal；
In rapid quenching technique, the frequency of adjustment water-cooled electromagnetic roller is between zero or 2000Hz~9000Hz.
A kind of 2. preparation method of iron-base quick-quenching permanent magnetism powder as claimed in claim 1, it is characterised in that
Cerium iron-base quick-quenching permanent magnetism band is prepared using electromagnetism roller first, ferrocerium base is prepared forever with obtained cerium iron-base quick-quenching permanent magnetism band
Magnetic and the Re '-Fe-B magnetics without Ce, using above two magnetic, double Hard Magnetic principal phases or more Hard Magnetic principal phases can be prepared
Ferrocerium base hot-pressed magnets, specifically comprise the following steps：
Step 1：Dispensing is carried out according to the Components Chemical formula of following mass percent：[Ce100-x,Rex]aFe100-a-b-cBbTMc, its
Middle x is the mass percent of Re in total amount of rare earth, and a, b and c represent the mass percent of corresponding element respectively, 0≤x≤50,
27.5≤a≤32；0.8≤b≤1.5；0.5≤c≤5；Re is Nd, Pr, Dy, the one or more in Tb elements, TM Ga,
One or more in Co, Cu, Nb, Al element；
Step 2：The raw material prepared is fitted into fast quenching equipment, then low smelting heat and progress electromagnetic agitation essence under Ar gas shieldeds
Refining, according to roller speed and alloying component, the frequency of adjustment water-cooled electromagnetic roller is between zero or 2000Hz~9000Hz, is then cast in
Linear velocity be 15~45m/s set on the water-cooled electromagnetic roller roller surface layer (4) of electromagnetic frequency, be made average thickness be 0.01~
0.06mm fast quenching piece or rapid tempering belt (3)；
The microstructure of the rapid tempering belt is crystallite, amorphous or equiax crystal, in the quick setting belt prepared without strip casting
Column crystal；
Step 3：Fast quenching piece or rapid tempering belt (3) are crushed, according to the different demands to fast quenching piece or rapid tempering belt (3), used
Ball-stirring mill or sand milling carry out powder processed；
Step 4：In order to obtain the magnetic of uniform particle diameter, the vibratory sieve of the mesh different meshes of 45 mesh~260 is selected respectively, by magnetic
Pour into vibratory sieve and look over so as to check, by category filter, the magnetic of particle diameter needed for acquisition, 0.056~0.28mm of particle size range.
3. preparation method as claimed in claim 2, it is characterised in that in the step 2：Raw material are put into intermediate frequency sense first
The material containing device (1) of the equipment of melting is answered, reaches 10 in vacuum-2Using heating coil (2) feeding electric preheating during more than Pa, treat
Vacuum reaches 10 again-2Stop after more than Pa vacuumizing and being filled with high-purity Ar, make in stove Ar air pressure reach -0.04~-
Melting is carried out after 0.08MPa；Electromagnetic agitation refining is imposed after raw material all fusing, then carries out molten steel cast.
4. preparation method as claimed in claim 2, it is characterised in that the roller surface layer (4) is copper alloy roll surface or molybdenum roller
Face.
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| JP6409867B2 (en) * | 2014-04-15 | 2018-10-24 | Tdk株式会社 | Rare earth permanent magnet |
| CN104599802B (en) * | 2014-12-03 | 2017-07-04 | 中国科学院宁波材料技术与工程研究所 | Rare earth permanent-magnetic material and preparation method thereof |
| CN105225781B (en) * | 2015-10-27 | 2017-09-29 | 钢铁研究总院 | A kind of many Hard Magnetic principal phase Ce permanent magnets of high corrosion-resistant and preparation method thereof |
| CN106128670B (en) * | 2016-06-12 | 2018-12-11 | 钢铁研究总院 | A kind of low-cost rare earth iron boron permanent magnet and preparation method thereof |
| 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 |
| CN113035559B (en) * | 2021-04-01 | 2022-07-08 | 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 |
| CN113782290B (en) * | 2021-09-07 | 2023-06-02 | 钢铁研究总院 | Double-main-phase high-magnetic energy product magnet with high Ce content and preparation method thereof |
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| CN102699294B (en) * | 2012-06-12 | 2013-12-25 | 钢铁研究总院 | Electromagnetic solidification Nd-Fe-B permanent magnet rapid-solidification sheet and preparation method thereof |
| CN102693799B (en) * | 2012-06-12 | 2015-03-25 | 钢铁研究总院 | Electromagnetically-solidified and hot-pressed nanocrystalline magnet of permanent magnet rapidly-quenched ribbon and preparation method of electromagnetically-solidified and hot-pressed nanocrystalline magnet |
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