CN109859922A - A kind of preparation method of the R-Fe-B magnet of low heavy rare earth content - Google Patents
A kind of preparation method of the R-Fe-B magnet of low heavy rare earth content Download PDFInfo
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Abstract
The present invention provides a kind of preparation methods of R-Fe-B magnet, comprising the following steps: A) R1-Fe-B-M1 sample is mixed with RH-M2-Q1 sample after hydrogen it is broken, obtain coarse powder；B the coarse powder) is diffused processing, it is broken that the coarse powder obtained after DIFFUSION TREATMENT is carried out hydrogen；C) coarse powder for obtaining step B) carries out airflow milling, and obtained fine powder is formed；D) magnet after molding is sintered, obtains R-Fe-B magnet.During preparing R-Fe-B magnet, by the above method magnet of preparation is had under the premise of keeping the remanent magnetism and maximum magnetic energy product of sintered magnet substantially, significantly improve magnet coercivity using minute quantity heavy rare earth Dy or Tb.
Description
Technical field
The present invention relates to magnet material technical field more particularly to a kind of systems of the R-Fe-B magnet of low heavy rare earth content
Preparation Method.
Background technique
It is institute it is well known that being permanent magnet by the R-Fe-B rare-earth sintered magnet of main phase of Nd2Fe14B type compound
The highest magnet of performance in magnetic material, it is widely used for voice coil motor (VCM), the servo motor, change of hard drive
Frequency air conditioner motor, hybrid electric vehicle are carried with motor, new-energy automobile driving motor etc..R-Fe-B rare-earth sintered magnet exists
During above-mentioned various motor applications, in order to adapt to use environment temperature, guarantee that motor does not demagnetize in hot operation, it is desirable that its
Excellent heat resistance, coercivity with higher.
The coercitive conventional method of R-Fe-B rare-earth sintered magnet is improved mainly using heavy rare earth element RH as original
Expect and the processes such as alloy breaks down, compacting, the sintering of passing through melting are made into magnet.This method characteristic is that light rare earth elements RL makees
Rare earth element for the R2Fe14B phase of rare-earth element R is replaced by heavy rare earth element RH, therefore, the crystallization magnetic of R2Fe14B phase respectively to
Anisotropic (physical quantity for determining coercitive essence) improves.But the magnetic moment specific gravity of the light rare earth elements RL in Nd2Fe14B phase
The magnetic moment of rare-earth element R H wants high, therefore, replaces light rare earth elements RL with heavy rare earth element RH, more will lead to residual flux
Density Br decline.On the other hand, since heavy rare earth element RH is scarce resource, so reducing its usage amount is very important.
Therefore, the method for replacing whole light rare earth elements RL with heavy rare earth element RH by traditional technique is not satisfactory.In addition, due to
The fast development of new-energy automobile, magnet required for new-energy automobile are also required to higher magnetic while needing high-coercive force
Energy product, so how to produce the research hotspot that high performance magnet is Nd-Fe-B permanent magnet material from now under conditions of low heavy rare earth.
In response to the above problems, main at this stage to be solved by two ways: one is effect mechanisms, and one is grain boundary decisions
Technology, but above two mode in the usage amount for reducing heavy rare earth and improves in magnet coercivity effect, the effect of crystal grain refinement
Fruit is than relatively limited, and equipment requirement is high, and process management and control is difficult, high production cost.
Grain boundary decision technology mainly uses the modes such as coating, deposition, plating, sputtering at present, makes containing Dy/Tb metal or change
The powder for closing object (such as Dy203, DyF3, TbF3, DyH3, TbH3) is first attached to magnet outer surface as diffusion source, a certain
It is diffused heat treatment in temperature range, makes rare earth element grain boundary diffusion to main phase grain surface layer, replaces Grain Surface
Nd2Fe14Nd in B forms (Nd, Dy/Tb) 2Fe14B shell structurre, improves grain surface anisotropy field, while improving crystal boundary
Microscopic structure, to improve a kind of coercitive technique of magnet.
And coat diffusion technique and generally pass through two procedures, the first procedure is diffusion source obtained first, and heavy rare earth is expanded
Scattered source is coated in the surface of sintered magnet, is then dried；The second step is that the product placement coated is being sintered magazine, with laggard
Vacuum sintering furnace carries out high-temperature heat treatment, grain boundary decision technology can by add less amount of heavy rare earth element RH hydride or
Fluoride or alloy reach and greatly improve the coercitive effect of magnet, while also ensuring that magnet remanence is unlikely to very big
It reduces, but the production process of this technique is more complicated, the dimensions of product is restricted, and generally within 8 millimeters, magnet is thick
Spend thicker, the effect of diffusion is poorer, and it is longer in addition to increase the multiple working procedure production cycle, and equipment frock investment is big, production process
Complexity, production cost are also relatively high etc..
Summary of the invention
Present invention solves the technical problem that being to provide a kind of preparation method of R-Fe-B magnet, the class of the application preparation
Magnet can be remarkably improved magnet coercivity under the premise of keeping the remanent magnetism and maximum magnetic energy product of magnet substantially.
In view of this, this application provides a kind of preparation methods of R-Fe-B magnet, comprising the following steps:
A hydrogen is broken after) mixing R1-Fe-B-M1 sample with RH-M2-Q1 sample, obtains coarse powder；
R1 be selected from one of rare earth element nd, Pr, Tb, Dy, Gd, La, Ho and Ce or a variety of, M1 be selected from Ti, V, Cr,
The content of one of Co, Ga, Cu, Mn, Si, Al, Zr, W and Mo or a variety of, R1 are 26wt%~33wt%, and the content of B is
The content of 0.8wt%~1.2wt%, M1 are 0~4wt%, surplus Fe；
RH be selected from least one of Dy and Tb, M2 be selected from Fe, Al, Cu, Zn, Ga, Ge, Nb, Ti or Zr, Q1 be selected from Zn,
Sn, V, W, Ni, Ta, Mn, Cd or Mo, the content of RH are 70wt%~100wt%, and the content of M2 is 0~30wt%, the content of Q1
For 0~10wt%, the total content of RH, M2 and Q1 are 100wt%；
B the coarse powder) is diffused processing, it is broken that the coarse powder obtained after DIFFUSION TREATMENT is carried out hydrogen；
C) coarse powder for obtaining step B) carries out airflow milling, and obtained fine powder is formed；
D) magnet after molding is sintered, obtains R-Fe-B magnet.
Preferably, the RH-M2-Q1 sample is 0.1wt%~10wt% of the R1-Fe-B-M1 sample.
Preferably, the DIFFUSION TREATMENT carries out in a vacuum or inert atmosphere, and the temperature of the DIFFUSION TREATMENT is 750~
1000 DEG C, the time is 1~50h.
Preferably, when the DIFFUSION TREATMENT carries out under vacuum, the vacuum degree is 1*10-5~9*10-1Pa；The expansion
When scattered processing carries out under an inert atmosphere, the inert gas is argon gas, and pressure is 500Pa~80KPa.
Preferably, the step B) and the step C) carried out under stringent sealing and protective atmosphere, and oxygenation amount is less than
1000ppm。
Preferably, the content of the RH is 80wt%~98wt%, and the content of the M2 is 1wt%~18wt%, described
The content of Q1 is 0.5wt%~6wt%.
Preferably, the content of the R1 is 28wt%~30wt%, and the content of the B is 0.9wt%~1.1wt%, institute
The content for stating M1 is 0.5wt%~3wt%.
Preferably, described to be molded over oriented moulding in the magnetic field 1.2T~2.5T.
Preferably, the sintering specifically:
By magnet after molding in 950 DEG C~1100 DEG C 4~25h of heat preservation, ageing treatment is carried out after maximum temperature heat preservation,
The level-one aging temp of the ageing treatment is 850~920 DEG C, and secondary aging temperature is 450~580 DEG C, the level-one timeliness
Time with secondary time effect is 4~6h.
This application provides a kind of preparation methods of R-Fe-B magnet, utilize R1-Fe-B-M1 sample and RH-M2-Q1
Successively pass through the broken processing-airflow milling-molding-sintering of the broken processing-DIFFUSION TREATMENT-hydrogen of hydrogen after sample mixing, results in R-Fe-
B class magnet；In the above preparation method, mixture is carried out the broken processing of hydrogen first by the application, the thin coarse grain of thickness is formed, with benefit
It is handled in being diffused, and DIFFUSION TREATMENT infiltrates into heavy rare earth element RH preferably in R1-Fe-B-M1 alloy, it is right
Main phase grain carries out one and preferably wraps up；Simultaneously because two kinds of samples form coarse powder, diffuser efficiency is high, and consistency is good, most
Make eventually by sintered magnet while guaranteeing that the less remanent magnetism of magnet is reduced, greatly improves the coercivity of magnet.
Specific embodiment
For a further understanding of the present invention, the preferred embodiment of the invention is described below with reference to embodiment, still
It should be appreciated that these descriptions are only further explanation the features and advantages of the present invention, rather than to the claims in the present invention
Limitation.
Magnet coercivity can be improved for the preparation method of prior art magnet, it is surplus that magnet is but unavoidably greatly lowered
The problem of magnetic, this application provides a kind of preparation method of R-Fe-B magnet, this method preparation with R12Fe14B type chemical combination
R-Fe-B rare-earth sintering magnet based on object is coercitive simultaneously in raising magnet, and it is small that remanent magnetism reduces amplitude.Specifically, this Shen
Please the R-Fe-B magnet preparation method, comprising the following steps:
A hydrogen is broken after) mixing R1-Fe-B-M1 sample with RH-M2-Q1 sample, obtains coarse powder；
R1 be selected from one of rare earth element nd, Pr, Tb, Dy, Gd, La, Ho and Ce or a variety of, M1 be selected from Ti, V, Cr,
The content of one of Co, Ga, Cu, Mn, Si, Al, Zr, W and Mo or a variety of, R1 are 26wt%~33wt%, and the content of B is
The content of 0.8wt%~1.2wt%, M1 are 0~4wt%, surplus Fe；
RH be selected from least one of Dy and Tb, M2 be selected from Fe, Al, Cu, Zn, Ga, Ge, Nb, Ti or Zr, Q1 be selected from Zn,
Sn, V, W, Ni, Ta, Mn, Cd or Mo, the content of RH are 70wt%~100wt%, and the content of M2 is 0~30wt%, the content of Q1
For 0~10wt%, the total content of RH, M2 and Q1 are 100wt%；
B the coarse powder) is diffused processing, it is broken that the coarse powder obtained after DIFFUSION TREATMENT is carried out hydrogen；
C) coarse powder for obtaining step B) carries out airflow milling, and obtained fine powder is formed；
D) magnet after molding is sintered, obtains R-Fe-B magnet.
In the preparation method of above-mentioned R-Fe-B magnet, the application is first by R1-Fe-B-M1 sample and RH-M2-Q1 sample
Product mixing；For above two sample, wherein in R1-Fe-B-M1 sample R1 be selected from rare earth element nd, Pr, Tb, Dy, Gd, La,
One of Ho and Ce or a variety of, M1 are selected from one of Ti, V, Cr, Co, Ga, Cu, Mn, Si, Al, Zr, W and Mo or a variety of,
In a particular embodiment, R1 is selected from Nb, and M1 is selected from Co.The content of R1 is 26wt%~33wt%, the content of B be 0.8wt%~
The content of 1.2wt%, M1 are 0~4wt%, surplus Fe；In a particular embodiment, the content of the R1 be 28wt%~
The content of 30wt%, the B are 0.9wt%~1.1wt%, and the content of the M1 is 0.5wt%~3wt%.
In the RH-M2-Q1 sample, RH be selected from least one of Dy and Tb, M2 be selected from Fe, Al, Cu, Zn, Ga, Ge,
Nb, Ti or Zr, Q1 are selected from Zn, Sn, V, W, Ni, Ta, Mn, Cd or Mo, and in a particular embodiment, RH is selected from Dy, and M2 is selected from copper；RH
Content be 70wt%~100wt%, the content of M2 is 0~30wt%, and the content of Q1 is 0~10wt%, and RH, M2 and Q1's is total
Content is 100wt%, and in a particular embodiment, the content of the RH is 80wt%~98wt%, and the content of the M2 is 1wt%
The content of~18wt%, the Q1 are 0.5wt%~6wt%.In RH-M2-Q1 sample, the content mistake of described RH, M2 and Q1
Low, then the remanent magnetism decline of magnet is more after spreading, and coercivity increases less, the too high levels of described RH, M2 and Q1, then the broken difficulty of hydrogen
Broken complete with hydrogen, the diffusion temperature additionally needed is higher, is easier to enter in main phase, causes the larger reduction of remanent magnetism.
In above two sample, the RH-M2-Q1 sample be the R1-Fe-B-M1 sample 0.1wt%~
10wt%；More specifically, the RH-M2-Q1 sample is 0.5wt%~5wt% of the R1-Fe-B-M1 sample；The RH-
The additive amount of M2-Q1 sample is less than 0.1wt%, then heavy rare earth additive amount is less, is difficult to play the effect of diffusion, can not be to coarse powder
In main phase grain form cladding, when the additive amount of RH-M2-Q1 sample is greater than 10wt%, since additive amount is larger, magnet is surplus
Magnetic reduction is more, in addition, heavy rare earth element is easier to enter in crystal grain since heavy rare-earth element content is higher, further decreases
Magnet magnetic property.
The concrete form of herein described RH-M2-Q1 sample and the R1-Fe-B-M1 sample is those skilled in the art
Well known form is specifically as follows bulk form or slab form, and more specifically, the RH-M2-Q1 sample is slab or maximum
The bulk of size < 20mm；The size of the RH-M2-Q1 sample is smaller, then granularity is smaller after hydrogen is broken, is easy to make in diffusion process
At waste, powder activity is big, and easy to oxidize, alloy is oversized, cannot be crushed completely after hydrogen is broken, be not easy to spread.
Obtained mixture is then subjected to the broken processing of hydrogen after the mixing of above two raw material, to obtain initial coarse powder；Institute
Stating the broken processing of hydrogen is the broken processing of hydrogen well known to those skilled in the art, to its specific embodiment the application without particularly limiting
System.The partial size of the initial coarse powder is 45~355 μm, is largely 100~150 μm, in favor of the DIFFUSION TREATMENT in later period；Initially
The excessive diffusion for being unfavorable for the later period of the partial size of coarse powder, the too small then activity of partial size is too high, is easy to happen oxidation.
According to the present invention, the initial coarse powder after hydrogen is broken is diffused processing, and the DIFFUSION TREATMENT is so that RH-M2-Q1 coarse powder
It diffuses in R1-Fe-B-M1 main phase, a preferably package is carried out to main phase grain.The DIFFUSION TREATMENT is in vacuum or inertia
It is carried out under gas shield, when the DIFFUSION TREATMENT carries out under vacuum, the vacuum degree is 1*10-5~9*10-1Pa；The expansion
When scattered processing carries out under an inert atmosphere, the inert gas is argon gas, and pressure is 500Pa~80kPa, in specific embodiment
In, the pressure is 15kPa~60kPa.The temperature of the DIFFUSION TREATMENT is 750~1000 DEG C, and the time is 1~50h；Specific
In embodiment, the temperature of the DIFFUSION TREATMENT is 820~950 DEG C, and the time is 3~15h；The temperature of the DIFFUSION TREATMENT is lower than
At 750 DEG C, since driving force reduces, heavy rare earth element diffusion is difficult, to be difficult to coat main phase grain；Work as temperature
When degree is higher than 1000 DEG C, heavy rare earth element is easier to enter in crystal grain, reduces magnet magnetic property；Soaking time is shorter, diffusion effect
Fruit is poor, and consistency is poor, can not preferably form the cladding to main phase grain, in addition soaking time is longer, heavy rare earth element
It is easier to enter in main phase, remanent magnetism is caused to be substantially reduced, magnetic property is deteriorated.
Then coarse powder Jing Guo DIFFUSION TREATMENT is carried out the broken processing of hydrogen by the application again, the broken processing of hydrogen is this field skill
Technological means known to art personnel, to its concrete operations mode the application without particularly limiting.In the broken processing of above-mentioned hydrogen
Afterwards, then the coarse powder by hydrogen after broken carries out airflow milling, to obtain fine powder；The airflow milling is technology well known to those skilled in the art
Mode, to its concrete operations means the application without particularly limiting.The application finally successively carries out into obtained fine powder
Type, sintering, to obtain R-Fe-B magnet.During above-mentioned molding, the oriented moulding preferably in the magnetic field 1.2T~2.5T.Institute
The temperature for stating sintering is 950~1100 DEG C, and the time is 4~25h.After being sintered maximum temperature heat preservation, magnet is carried out
Ageing treatment, during ageing treatment, the temperature of level-one timeliness is 850~920 DEG C, the temperature of secondary time effect is 450~
580 DEG C, the time of the level-one timeliness and secondary time effect is 4~6h.
The broken processing of herein described hydrogen, DIFFUSION TREATMENT, airflow milling and molding be under stringent sealing and protective atmosphere into
Capable, and control oxygenation amount and be less than 1000ppm, to avoid the oxidation of product after processing.
The present invention provides a kind of R-Fe-B sintered magnet preparation methods, by R1-Fe-B-M1 sample and RH-M2-Q1
The broken processing of hydrogen is carried out after sample mixing together, the coarse powder after hydrogen is broken is transferred in rotation diffusion furnace and is diffused processing, on the one hand exists
Processing is diffused in coarse powder, heavy rare earth can be penetrated into preferably in alloy, carry out a preferably packet to main phase grain
It wraps up in, since slab thickness is thin, diffuser efficiency is high, and consistency is good, and is permeated during coarse powder, does not influence subsequent work
Sequence, high production efficiency.Therefore, the class magnet of the application preparation is before remanent magnetism and the maximum magnetic energy product for keeping sintered magnet substantially
It puts, has used minimal amount of heavy rare earth and significantly improved the coercivity of magnet.
For a further understanding of the present invention, below with reference to embodiment to the preparation side of R-Fe-B magnet provided by the invention
Method is described in detail, and protection scope of the present invention is not limited by the following examples.
Embodiment 1
Configured former material is carried out under inert gas protection using vacuum melting furnace according to the composition proportion of Tables 1 and 2
Melting, melting R1-Fe-B-M1 alloy casting piece and RH-M2-Q1 alloy casting piece, form the slab of 0.1~1mm of thickness respectively, according to
The 1wt% of R1-Fe-B-M1 weight adds RH-M2-Q1 alloy casting piece；Two kinds of alloy casting pieces are transferred to rotation diffusion after hydrogen is broken
Furnace is diffused processing according to 870 DEG C/5h under 20~40kPa pressure under inert atmosphere, turns to carry out in hydrogen crushing furnace after diffusion
Secondary hydrogen is broken, and airflow milling is crushed its SMD to 3.2 μm；Using the magnetic field orientating compression moulding of 15KOe, green compact, green density is made
For 3.95g/cm3；Green compact carries out vacuum-sintering, 1045 DEG C first sintering 500min in sintering furnace, then carries out ageing treatment, in
890 DEG C of timeliness 180min obtain green compact in 490 DEG C of timeliness 240min.Diameter 10mm sample column is taken to test magnetic property M1.
The composition proportion table of the R1-Fe-B-M1 of the R-Fe-B of 1 embodiment 1 of table preparation
| Group | Nd | B | Co | Small powder | Fe |
| Content wt% | 30.6 | 0.92 | 0.5 | 0.3 | It is remaining |
The RH-M2-Q1 composition proportion table of the R-Fe-B of 2 embodiment 1 of table preparation
The performance data table of the R-Fe-B magnet of 3 embodiment 1 of table preparation
Embodiment 2
According to the composition proportion of table 4 and table 5 using vacuum melting furnace under inert gas protection to configured raw material into
Row melting, melting R1-Fe-B-M1 alloy casting piece and RH-M2-Q1 alloy casting piece, form the slab of 0.1~1mm of thickness, press respectively
RH-M2-Q1 alloy casting piece is added according to the 1wt% of R1-Fe-B-M1 weight；Two kinds of alloy casting pieces are transferred to rotation and expand after hydrogen is broken
Furnace is dissipated, processing is diffused according to 870 DEG C/10h under 20~40kPa pressure under inert atmosphere, turns in hydrogen crushing furnace after diffusion
It is broken to carry out secondary hydrogen, airflow milling is crushed its SMD to 3.2 μm；Using the magnetic field orientating compression moulding of 15KOe, green compact, green compact is made
Density is 3.95g/cm3；Green compact carries out vacuum-sintering, 1045 DEG C first sintering 500min in sintering furnace, then carries out at timeliness
Reason, in 890 DEG C of timeliness 180min, obtains green compact in 490 DEG C of timeliness 240min.Diameter 10mm sample column is taken to test magnetic property M2.
The composition proportion table of the R1-Fe-B-M1 of the R-Fe-B of 4 embodiment 4 of table preparation
| Group | Nd | B | Co | Small powder | Fe |
| Content wt% | 30.6 | 0.92 | 0.5 | 0.3 | It is remaining |
The RH-M2-Q1 composition proportion table of the R-Fe-B of 5 embodiment 2 of table preparation
| Group | Dy | Cu | Mn |
| Content wt% | 92 | 7 | 1 |
The performance data table of the R-Fe-B magnet of 6 embodiment 2 of table preparation
As shown in Table 6, M2 coercivity illustrates that diffusion time is longer, magnetic compared with M1 high 0.66kOe, remanent magnetism 0.05kGs low compared with M1
The coercivity of body is higher, and remanent magnetism is lower.
Embodiment 3
According to the composition proportion of table 7 and table 8 using vacuum melting furnace under inert gas protection to configured raw material into
Row melting, melting R1-Fe-B-M1 alloy casting piece and RH-M2-Q1 alloy casting piece, form the slab of 0.1~1mm of thickness, press respectively
RH-M2-Q1 alloy casting piece is added according to the 1wt% of R1-Fe-B-M1 weight；Two kinds of alloy casting pieces are transferred to rotation diffusion after hydrogen is broken
Furnace is diffused processing according to 910 DEG C/5h under 15~35kPa pressure under inert atmosphere, turns to carry out in hydrogen crushing furnace after diffusion
Secondary hydrogen is broken, and airflow milling is crushed its SMD to 3.2 μm；Using the magnetic field orientating compression moulding of 15KOe, green compact, green density is made
For 3.95g/cm3；Green compact carries out vacuum-sintering, 1045 DEG C first sintering 500min in sintering furnace, then carries out ageing treatment, in
890 DEG C of timeliness 180min obtain green compact in 490 DEG C of timeliness 240min.Diameter 10mm sample column is taken to test magnetic property M3.
The composition proportion table of the R1-Fe-B-M1 of the R-Fe-B of 7 embodiment 3 of table preparation
| Group | Nd | B | Co | Small powder | Fe |
| Content wt% | 30.6 | 0.92 | 0.5 | 0.3 | It is remaining |
The RH-M2-Q1 composition proportion table of the R-Fe-B of 8 embodiment 3 of table preparation
| Group | Dy | Cu | Mn |
| Content wt% | 92 | 7 | 1 |
The performance data table of the R-Fe-B magnet of 9 embodiment 3 of table preparation
As shown in Table 9, M3 coercivity illustrates that diffusion temperature is higher, magnetic compared with M1 high 0.57kOe, remanent magnetism 0.07kGs low compared with M1
The coercivity of body is higher, and remanent magnetism is lower.
Embodiment 4
According to table 10 and 11 composition proportion of table using vacuum melting furnace under inert gas protection to configured raw material into
Row melting, melting R1-Fe-B-M1 and RH-M2-Q1 alloy casting piece, forms the slab of 0.1~1mm of thickness, according to R1-Fe- respectively
The 1wt% of B-M1 weight adds RH-M2-Q1 alloy casting piece；Two kinds of alloy casting pieces are transferred to rotation diffusion furnace, in lazy after hydrogen is broken
It is diffused processing according to 870 DEG C/5h under 30~50kPa pressure under property atmosphere, turns to carry out secondary hydrogen in hydrogen crushing furnace after diffusion
Broken, airflow milling is crushed its SMD to 3.2 μm；Using the magnetic field orientating compression moulding of 15KOe, green compact is made, green density is
3.95g/cm3；Green compact carries out vacuum-sintering, 1045 DEG C first sintering 500min in sintering furnace, then carries out ageing treatment, in
890 DEG C of timeliness 180min obtain green compact in 490 DEG C of timeliness 240min.Diameter 10mm sample column is taken to test magnetic property M4.
The composition proportion table of the R1-Fe-B-M1 of the R-Fe-B of 10 embodiment 4 of table preparation
| Group | Nd | B | Co | Small powder | Fe |
| Content wt% | 30.6 | 0.92 | 0.5 | 0.3 | It is remaining |
The RH-M2-Q1 composition proportion table of the R-Fe-B of 11 embodiment 4 of table preparation
| Group | Dy | Cu | Mn |
| Content wt% | 85 | 12 | 3 |
The performance data table of the R-Fe-B magnet of 12 embodiment 4 of table preparation
As shown in Table 12, M4 coercivity 0.8kOe low compared with M1, remanent magnetism 0.11kGs low compared with M1, illustrates with heavy rare earth content
It reduces, metal M2 content increases, and coercivity, the remanent magnetism of magnet reduce.
Comparative example 1
Configured former material is carried out under inert gas protection using vacuum melting furnace according to the composition proportion of Tables 1 and 2
Melting, melting R1-Fe-B-M1 alloy casting piece and RH-M2-Q1 alloy casting piece, form the slab of 0.1~1mm of thickness respectively, according to
The 1wt% of R1-Fe-B-M1 weight adds RH-M2-Q1 alloy casting piece；It is coarse powder that it is broken, which to turn hydrogen crushing furnace hydrogen, and airflow milling is crushed its SMD
To 3.2 μm；Using the magnetic field orientating compression moulding of 15KOe, green compact, green density 4.05g/cm3 is made；Green compact is in sintering furnace
Middle carry out vacuum-sintering, 1045 DEG C first sintering 500min.Ageing treatment is carried out again, in 890 DEG C of timeliness 180min, in 490 DEG C
Timeliness 240min obtains green compact.Diameter 10mm sample column is taken to test magnetic property D1.
The performance data table of the R-Fe-B magnet of 13 comparative example of table preparation
The above description of the embodiment is only used to help understand the method for the present invention and its core ideas.It should be pointed out that pair
For those skilled in the art, without departing from the principle of the present invention, the present invention can also be carried out
Some improvements and modifications, these improvements and modifications also fall within the scope of protection of the claims of the present invention.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest scope of cause.
Claims (9)
1. a kind of preparation method of R-Fe-B magnet, which comprises the following steps:
A hydrogen is broken after) mixing R1-Fe-B-M1 sample with RH-M2-Q1 sample, obtains coarse powder；
R1 be selected from one of rare earth element nd, Pr, Tb, Dy, Gd, La, Ho and Ce or a variety of, M1 be selected from Ti, V, Cr, Co, Ga,
One of Cu, Mn, Si, Al, Zr, W and Mo or a variety of, the content of R1 are 26wt%~33wt%, and the content of B is 0.8wt%
The content of~1.2wt%, M1 are 0~4wt%, surplus Fe；
RH be selected from least one of Dy and Tb, M2 be selected from Fe, Al, Cu, Zn, Ga, Ge, Nb, Ti or Zr, Q1 be selected from Zn, Sn, V,
W, Ni, Ta, Mn, Cd or Mo, the content of RH are 70wt%~100wt%, and the content of M2 is 0~30wt%, the content of Q1 is 0~
The total content of 10wt%, RH, M2 and Q1 are 100wt%；
B the coarse powder) is diffused processing, it is broken that the coarse powder obtained after DIFFUSION TREATMENT is carried out hydrogen；
C) coarse powder for obtaining step B) carries out airflow milling, and obtained fine powder is formed；
D) magnet after molding is sintered, obtains R-Fe-B magnet.
2. preparation method according to claim 1, which is characterized in that the RH-M2-Q1 sample is the R1-Fe-B-M1
0.1wt%~10wt% of sample.
3. preparation method according to claim 1, which is characterized in that the DIFFUSION TREATMENT in a vacuum or inert atmosphere into
Row, the temperature of the DIFFUSION TREATMENT are 750~1000 DEG C, and the time is 1~50h.
4. preparation method according to claim 3, which is characterized in that described when the DIFFUSION TREATMENT carries out under vacuum
Vacuum degree is 1*10-5~9*10-1Pa；When the DIFFUSION TREATMENT carries out under an inert atmosphere, the inert gas is argon gas, pressure
Power is 500Pa~80KPa.
5. preparation method according to claim 1, which is characterized in that the step B) and the step C) strictly sealing
It is carried out under protective atmosphere, and oxygenation amount is less than 1000ppm.
6. preparation method according to claim 1, which is characterized in that the content of the RH is 80wt%~98wt%, institute
The content for stating M2 is 1wt%~18wt%, and the content of the Q1 is 0.5wt%~6wt%.
7. preparation method according to claim 1, which is characterized in that the content of the R1 is 28wt%~30wt%, institute
The content for stating B is 0.9wt%~1.1wt%, and the content of the M1 is 0.5wt%~3wt%.
8. preparation method according to claim 1, which is characterized in that described be molded in the magnetic field 1.2T~2.5T is orientated to
Type.
9. preparation method according to claim 1, which is characterized in that the sintering specifically:
By magnet after molding in 950 DEG C~1100 DEG C 4~25h of heat preservation, ageing treatment is carried out after maximum temperature heat preservation, it is described
The level-one aging temp of ageing treatment is 850~920 DEG C, and secondary aging temperature is 450~580 DEG C, the level-one timeliness and two
The time of grade timeliness is 4~6h.
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| CN113643892B (en) * | 2021-08-19 | 2024-03-22 | 太原开元智能装备有限公司 | Preparation method of RFeB sintered magnet |
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