CN109065348A - A kind of preparation method of the body of high-performance rare-earth permanent-magnetic containing cerium - Google Patents
A kind of preparation method of the body of high-performance rare-earth permanent-magnetic containing cerium Download PDFInfo
- Publication number
- CN109065348A CN109065348A CN201810754049.4A CN201810754049A CN109065348A CN 109065348 A CN109065348 A CN 109065348A CN 201810754049 A CN201810754049 A CN 201810754049A CN 109065348 A CN109065348 A CN 109065348A
- Authority
- CN
- China
- Prior art keywords
- containing cerium
- weight
- added
- slab
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0293—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The invention discloses a kind of preparation method of body of high-performance rare-earth permanent-magnetic containing cerium, main phase of the invention is mainly provided by master alloy, and the surface layer of main phase remains as the shell structurre containing Nd.Intermetallic compound containing cerium is added as auxiliary phase, increase the volume fraction of Nd-rich phase, promote Nd-rich phase removes magnetic coupling exchange interaction, Ce elements fail to significantly change the main phase shell structurre of master alloy again simultaneously, therefore coercitive reduction is fewer, to realize the preparation of the high performance Nd-Fe-B rare-earth permanent magnet containing cerium.
Description
Technical field
The invention belongs to magnetic fields, and in particular to a kind of preparation method of the body of high-performance rare-earth permanent-magnetic containing cerium.
Background technique
Due to its excellent magnetic property, Nd-Fe-B rare-earth permanent magnet is more and more widely used.Due to rare earth metal
Belong to rare metal, price occupies height, and especially some heavy rare earth element such as Dy, Tb are even more particularly expensive.In rare earth element,
Since Ce elements content is rich, and application is less, so price is relatively low.Come this year in industry to substitute Nd- using cerium part
Rare earth element in Fe-B reduces the price of product with this.
Using cerium part for the rare earth element in Nd-Fe-B, Ce2Fe14B, and the Nd-rich phase containing cerium are formed.
The anisotropy field of Ce2Fe14B is much lower compared with Nd2Fe14B, while the Nd-rich phase containing cerium is in main phase surface layer, is also easy anti-
Magnetization, so the substitution of cerium can reduce the coercivity of magnet.At present plus the product of cerium is largely N trade mark series.
Addition for cerium can be directly added into from formula, then what is directly resulted in is coercitive be greatly reduced.Separately
A kind of application method is the method for dual alloy, be distributed in cerium more in main phase, reduces cerium in the influence of crystal boundary, is changed with this
Kind coercivity.In comparison, the method for dual alloy has certain validity, but can not completely inhibit cerium to coercitive
It reduces.Therefore the high-performance Ne-Fe-B rare-earth permanent magnet of preparation plus cerium is relatively difficult.
Summary of the invention
The purpose of the present invention is designing a kind of intermetallic compound containing cerium, master alloy is without cerium at being grouped as.It is main
It is mutually mainly provided by master alloy, the surface layer of main phase remains as the shell structurre containing Nd.Intermetallic compound containing cerium is as auxiliary phase
It is added, increases the volume fraction of Nd-rich phase, promote Nd-rich phase removes magnetic coupling exchange interaction, while Ce elements are again not
The main phase shell structurre of master alloy can be significantly changed, therefore coercitive reduction is fewer, to realize the high performance Nd-containing cerium
The preparation of Fe-B rare-earth permanent magnet.
To achieve the above object, the invention adopts the following technical scheme:
A kind of preparation method of the body of high-performance rare-earth permanent-magnetic containing cerium, comprising the following steps:
(1) intermetallic compound containing cerium mischmetal is taken, in vacuum induction slab furnace, is melted and is prepared into slab；Described contains
The ingredient of cerium mischmetal intermetallic compound is R1aCebT1cM1d, wherein R1 is selected from least one of rare earth element, and Ce is rare earth
Elemental cerium, T1 are one or both of Fe and Co, and M1 is in Al, Si, C, P, Ti, Nb, Zr, Cr, Cu, Ga
At least one, indicates a of weight percent, b, c, d in the following range: 30≤a≤50,1≤b≤20,0≤d≤2,
Remaining is c, and a+b+c+d=100；
(2) silane sol solution is prepared:
The silane coupling agent kh550 for taking 10-14 parts by weight, is added in the dehydrated alcohol of 20-30 times of its weight, stirs evenly,
The zinc stearate of 4-7 parts by weight is added, it is 3-5 minutes ultrasonic, obtain silanol solution；
The ethyl orthosilicate for taking 30-40 parts by weight is added in the deionized water of 36-40 times of its weight, and 1-2 parts by weight are added
Lauric acid amide of ethanol is stirred to react 4-5 hours, and above-mentioned silanol solution is added, and increasing temperature is 65-70 DEG C, and heat preservation is stirred
Mix 100-120 minutes to get；
(3) above-mentioned intermetallic compound containing cerium mischmetal is taken, is added in above-mentioned silane sol solution, 10-20 minutes ultrasonic, mistake
Filter, must precipitate；
(4) above-mentioned precipitating is placed in vacuum induction slab furnace, is melted and is prepared into slab；
(5) slab is subjected to coarse crushing through hydrogen is broken, the fine powder of 0.5 ~ 20um of average particle size is then ground into through airflow milling；
(6) fine powder is taken to be mixed according to a certain percentage with master alloy, the ingredient of the master alloy is R2aT2bM2cBd, wherein
R2 is selected from rare earth element Pr, Nd, Gd, Tb, Dy, at least one of Ho；T2 is one or both of Fe and Co, and M2 is
Selected from Al, Si, C, P, Ti, Nb, Zr, Cr, Cu, at least one of Ga, B are boron element, indicate a of weight percent,
B, c, d be in the following range: 29≤a≤33,0≤c≤2,0.9≤d≤1.1, remaining is b, and a+b+c+d=100；
(7) under nitrogen protection by mixed powder, magnetic field orientating form, then put the green body into sintering furnace be sintered and
Timeliness to get.
The weight ratio of fine powder described in step (6) and master alloy is 1-50:100.
Pass through the further finely divided detailed process of airflow milling described in step (5) are as follows:
By in the slab powder and petroleum ether importing rotary mill after coarse crushing, sealing pours nitrogen for the sky in ball grinder
Gas discharge, ball milling 1-4 hours to get.
Sintering temperature described in step (7) is between 1100-1200 DEG C, and sintering time is 100-140 minutes.
Beneficial effects of the present invention:
The present invention is mixed by master alloy with the intermetallic compound containing cerium, and the Nd-Fe-B rare-earth permanent magnet containing cerium is prepared,
Since cerium is distributed mainly in neodymium-rich phase at grain boundary, magnetic coupling exchange interaction is played, while failing to significantly change the shell of main phase
Structure, thus to it is coercitive reduction be it is limited, the high performance Nd-Fe-B rare-earth permanent magnet containing cerium can be prepared, more often
The low performance product that the method for rule can only largely prepare N series has biggish progress；The present invention uses silane sol solution
Intermetallic compound containing cerium mischmetal is coated, the oxidation of magnetic powder during the preparation process can be prevented, while being conducive to improve
The magnetic property of magnet, and stearate wherein adulterated etc. can improve between intermetallic compound containing cerium mischmetal and master alloy
Dispersing uniformity, keep the Mass Distribution of finished product magnet uniform, to further increase finished product magnet quality.
Specific embodiment
Embodiment 1
A kind of preparation method of the body of high-performance rare-earth permanent-magnetic containing cerium, comprising the following steps:
(1) intermetallic compound containing cerium mischmetal is taken, in vacuum induction slab furnace, is melted and is prepared into slab；Described contains
The ingredient of cerium mischmetal intermetallic compound is R1aCebT1cM1d, wherein R1 is lanthanum, and Ce is rare-earth element cerium, and T1 Fe, M1 are
Selected from Al, indicate that a of weight percent, b, c, d, a are equal to 50, b and are equal to 20, c equal to 28, d equal to 2；
(2) silane sol solution is prepared:
The silane coupling agent kh550 for taking 10 parts by weight is added in the dehydrated alcohol of 20 times of its weight, stirs evenly, and 4 weights are added
The zinc stearate of part is measured, ultrasound 3 minutes obtains silanol solution；
The ethyl orthosilicate for taking 30 parts by weight is added in the deionized water of 36 times of its weight, and the coconut oil two of 1 parts by weight is added
Glycollic amide is stirred to react 4 hours, is added above-mentioned silanol solution, and increasing temperature is 65 DEG C, and insulated and stirred 100 minutes, i.e.,
?；
(3) above-mentioned intermetallic compound containing cerium mischmetal is taken, is added in above-mentioned silane sol solution, ultrasound 10 minutes, filtering obtains
Precipitating；
(4) above-mentioned precipitating is placed in vacuum induction slab furnace, is melted and is prepared into slab；
(5) slab is subjected to coarse crushing through hydrogen is broken, the fine powder of average particle size 0.5-20um is then ground into through airflow milling；
(6) fine powder is taken to be mixed according to a certain percentage with master alloy, the ingredient of the master alloy is R2aT2bM2cBd, wherein
R2 is selected from rare earth element P；T2 is Fe, and it is boron element that M2, which is selected from Al, B, indicates that a of weight percent, b, c, d, a are equal to 33, c
It is equal to 1.1, b equal to 2, d and is equal to 36.9；
(7) under nitrogen protection by mixed powder, magnetic field orientating form, then put the green body into sintering furnace be sintered and
Timeliness to get.
The weight ratio of fine powder described in step (6) and master alloy is 1:100.
Pass through the further finely divided detailed process of airflow milling described in step (5) are as follows:
By in the slab powder and petroleum ether importing rotary mill after coarse crushing, sealing pours nitrogen for the sky in ball grinder
Gas discharge, ball milling 4 hours to get.
Sintering temperature described in step (7) is between 1100 DEG C, and sintering time is 140 minutes.
Embodiment 2
A kind of preparation method of the body of high-performance rare-earth permanent-magnetic containing cerium, comprising the following steps:
(1) intermetallic compound containing cerium mischmetal is taken, in vacuum induction slab furnace, is melted and is prepared into slab；Described contains
The ingredient of cerium mischmetal intermetallic compound is R1aCebT1cM1d, wherein R1 is selected from Pr, and Ce is rare-earth element cerium, T1 Co, M1
Selected from Ga, to indicate a of weight percent, b, c, d in the following range: a is equal to 30, b and is equal to 1, d 0.1, c 68.9；
(2) silane sol solution is prepared:
The silane coupling agent kh550 for taking 14 parts by weight is added in the dehydrated alcohol of 30 times of its weight, stirs evenly, and 7 weights are added
The zinc stearate of part is measured, ultrasound 5 minutes obtains silanol solution；
The ethyl orthosilicate for taking 40 parts by weight is added in the deionized water of 40 times of its weight, and the coconut oil two of 2 parts by weight is added
Glycollic amide is stirred to react 5 hours, is added above-mentioned silanol solution, and increasing temperature is 70 DEG C, and insulated and stirred 120 minutes, i.e.,
?；
(3) above-mentioned intermetallic compound containing cerium mischmetal is taken, is added in above-mentioned silane sol solution, ultrasound 20 minutes, filtering obtains
Precipitating；
(4) above-mentioned precipitating is placed in vacuum induction slab furnace, is melted and is prepared into slab；
(5) slab is subjected to coarse crushing through hydrogen is broken, the fine powder of 0.5 ~ 20um of average particle size is then ground into through airflow milling；
(6) fine powder is taken to be mixed according to a certain percentage with master alloy, the ingredient of the master alloy is R2aT2bM2cBd, wherein
R2 is selected from rare earth element Ho；T2 is Fe, and it is boron element that M2, which is selected from Ga, B, indicates a of weight percent, b, c, d is in following model
In enclosing: a is equal to 29, c and is equal to 1, d equal to 0.9, remaining is 69.1；
(7) under nitrogen protection by mixed powder, magnetic field orientating form, then put the green body into sintering furnace be sintered and
Timeliness to get.
The weight ratio of fine powder described in step (6) and master alloy is 1:2.
Pass through the further finely divided detailed process of airflow milling described in step (5) are as follows:
By in the slab powder and petroleum ether importing rotary mill after coarse crushing, sealing pours nitrogen for the sky in ball grinder
Gas discharge, ball milling 4 hours to get.
Sintering temperature described in step (7) is between 1200 DEG C, and sintering time is 100 minutes.
The magnetic property of the embodiment of the present invention 1:
Br(kGs): 11.77；
(BH) max(MGOe): 43.20；
Hcj(kOe): 23.19.
The magnetic property of the embodiment of the present invention 2:
Br(kGs): 12.26；
(BH) max(MGOe): 44.52；
Hcj(kOe): 24.03.
Claims (4)
1. a kind of preparation method of the body of high-performance rare-earth permanent-magnetic containing cerium, which comprises the following steps:
(1) intermetallic compound containing cerium mischmetal is taken, in vacuum induction slab furnace, is melted and is prepared into slab；Described contains
The ingredient of cerium mischmetal intermetallic compound is R1aCebT1cM1d, wherein R1 is selected from least one of rare earth element, and Ce is rare earth
Elemental cerium, T1 are one or both of Fe and Co, and M1 is in Al, Si, C, P, Ti, Nb, Zr, Cr, Cu, Ga
At least one, indicates a of weight percent, b, c, d in the following range: 30≤a≤50,1≤b≤20,0≤d≤2,
Remaining is c, and a+b+c+d=100；
(2) silane sol solution is prepared:
The silane coupling agent kh550 for taking 10-14 parts by weight, is added in the dehydrated alcohol of 20-30 times of its weight, stirs evenly,
The zinc stearate of 4-7 parts by weight is added, it is 3-5 minutes ultrasonic, obtain silanol solution；
The ethyl orthosilicate for taking 30-40 parts by weight is added in the deionized water of 36-40 times of its weight, and 1-2 parts by weight are added
Lauric acid amide of ethanol is stirred to react 4-5 hours, and above-mentioned silanol solution is added, and increasing temperature is 65-70 DEG C, and heat preservation is stirred
Mix 100-120 minutes to get；
(3) above-mentioned intermetallic compound containing cerium mischmetal is taken, is added in above-mentioned silane sol solution, 10-20 minutes ultrasonic, mistake
Filter, must precipitate；
(4) above-mentioned precipitating is placed in vacuum induction slab furnace, is melted and is prepared into slab；
(5) slab is subjected to coarse crushing through hydrogen is broken, the fine powder of 0.5 ~ 20um of average particle size is then ground into through airflow milling；
(6) fine powder is taken to be mixed according to a certain percentage with master alloy, the ingredient of the master alloy is R2aT2bM2cBd, wherein
R2 is selected from rare earth element Pr, Nd, Gd, Tb, Dy, at least one of Ho；T2 is one or both of Fe and Co, and M2 is
Selected from Al, Si, C, P, Ti, Nb, Zr, Cr, Cu, at least one of Ga, B are boron element, indicate a of weight percent,
B, c, d be in the following range: 29≤a≤33,0≤c≤2,0.9≤d≤1.1, remaining is b, and a+b+c+d=100；
(7) under nitrogen protection by mixed powder, magnetic field orientating form, then put the green body into sintering furnace be sintered and
Timeliness to get.
2. a kind of preparation method of body of high-performance rare-earth permanent-magnetic containing cerium according to claim 1, which is characterized in that step
(6) weight ratio of fine powder described in and master alloy is 1-50:100.
3. a kind of preparation method of body of high-performance rare-earth permanent-magnetic containing cerium according to claim 1, which is characterized in that step
(5) pass through the further finely divided detailed process of airflow milling described in are as follows:
By in the slab powder and petroleum ether importing rotary mill after coarse crushing, sealing pours nitrogen for the sky in ball grinder
Gas discharge, ball milling 1-4 hours to get.
4. a kind of preparation method of body of high-performance rare-earth permanent-magnetic containing cerium according to claim 1, which is characterized in that step
(7) sintering temperature described in is between 1100-1200 DEG C, and sintering time is 100-140 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810754049.4A CN109065348A (en) | 2018-07-11 | 2018-07-11 | A kind of preparation method of the body of high-performance rare-earth permanent-magnetic containing cerium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810754049.4A CN109065348A (en) | 2018-07-11 | 2018-07-11 | A kind of preparation method of the body of high-performance rare-earth permanent-magnetic containing cerium |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109065348A true CN109065348A (en) | 2018-12-21 |
Family
ID=64815816
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810754049.4A Pending CN109065348A (en) | 2018-07-11 | 2018-07-11 | A kind of preparation method of the body of high-performance rare-earth permanent-magnetic containing cerium |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109065348A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103996475A (en) * | 2014-05-11 | 2014-08-20 | 沈阳中北通磁科技股份有限公司 | High-performance neodymium-iron-boron rare earth permanent magnet with composite main phase and manufacturing method |
| CN103996523A (en) * | 2014-05-11 | 2014-08-20 | 沈阳中北通磁科技股份有限公司 | Method for manufacturing La-contained high-performance neodymium iron boron rare earth permanent magnet |
| CN105489336A (en) * | 2016-01-22 | 2016-04-13 | 宁波松科磁材有限公司 | Method for dysprosium infiltration of NdFeB magnets |
| CN105575577A (en) * | 2016-03-04 | 2016-05-11 | 四川大学 | Sintered cerium-rich rare earth permanent magnetic material and preparation method thereof |
-
2018
- 2018-07-11 CN CN201810754049.4A patent/CN109065348A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103996475A (en) * | 2014-05-11 | 2014-08-20 | 沈阳中北通磁科技股份有限公司 | High-performance neodymium-iron-boron rare earth permanent magnet with composite main phase and manufacturing method |
| CN103996523A (en) * | 2014-05-11 | 2014-08-20 | 沈阳中北通磁科技股份有限公司 | Method for manufacturing La-contained high-performance neodymium iron boron rare earth permanent magnet |
| CN105489336A (en) * | 2016-01-22 | 2016-04-13 | 宁波松科磁材有限公司 | Method for dysprosium infiltration of NdFeB magnets |
| CN105575577A (en) * | 2016-03-04 | 2016-05-11 | 四川大学 | Sintered cerium-rich rare earth permanent magnetic material and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102956336B (en) | A kind of method preparing the sintered Nd-Fe-B permanent magnetic material of compound interpolation gadolinium, holmium and yttrium | |
| US10340064B2 (en) | Rare earth permanent magnetic material and method of preparing the same | |
| CN103280290B (en) | Containing cerium low melting point rare earth permanent magnetic liquid phase alloy and permanent magnet preparation method thereof | |
| EP3327734B1 (en) | Method for producing a rare earth-cobalt-based composite magnetic material | |
| WO2014101247A1 (en) | Method for preparing sintered neodymium-iron-boron magnet | |
| CN103426624B (en) | The preparation method of Nd-Fe-B permanent magnet | |
| CN103903824B (en) | A kind of rare earth permanent-magnetic material and preparation method thereof | |
| CN101266855A (en) | Rare earth permanent magnetism material and its making method | |
| US20110074530A1 (en) | Mixed rare-earth permanent magnet and method of fabrication | |
| EP2415541A1 (en) | Alloy material for r-t-b-type rare-earth permanent magnet, process for production of r-t-b-type rare-earth permanent magnet, and motor | |
| CN108281246B (en) | High-performance sintered neodymium-iron-boron magnet and preparation method thereof | |
| CN101266857A (en) | Method for improving sintered neodymium-iron-boron coercive force and working temperature based on nano Ti powder modification | |
| JP4951703B2 (en) | Alloy material for RTB-based rare earth permanent magnet, method for manufacturing RTB-based rare earth permanent magnet, and motor | |
| KR100204256B1 (en) | Rare-earth-element-fe-b permanent magnet powder excellent in magnetic anisotropy and corrosion resistivity and bonded magnet therefrom | |
| CN103137314A (en) | Method for preparing rare earth-iron-boron permanent magnet | |
| CN105761925A (en) | Method for preparing high-performance NdFeB magnets through holmium ferrite and gallium eutectic adulteration | |
| CN108364739B (en) | Neodymium-iron-boron magnet and preparation method thereof | |
| EP2612940A1 (en) | Alloy material for r-t-b-based rare earth permanent magnet, production method for r-t-b-based rare earth permanent magnet, and motor | |
| JP2023081336A (en) | Rare earth sintered neodymium-iron-boron magnet, method of manufacturing the same, and use of hydrogenated praseodymium | |
| CN109065348A (en) | A kind of preparation method of the body of high-performance rare-earth permanent-magnetic containing cerium | |
| CN104575897A (en) | High-performance rare-earth permanent magnetic material and preparation method thereof | |
| CN109637768B (en) | Yttrium-containing rare earth permanent magnetic material and preparation method thereof | |
| JP2007250605A (en) | Method for manufacturing r-t-b-based rare-earth permanent magnet | |
| CN104934175B (en) | It is a kind of based on the crystal boundary modified low dysprosium of high-coercive force/terbium neodymium iron boron magnetic body | |
| CN110379578A (en) | It is a kind of inexpensive without rareearth magnetic material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20181221 |