CN107564648B - A kind of deposition method preparing high-performance Ne-Fe-B magnetic powder - Google Patents
A kind of deposition method preparing high-performance Ne-Fe-B magnetic powder Download PDFInfo
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- CN107564648B CN107564648B CN201710848593.0A CN201710848593A CN107564648B CN 107564648 B CN107564648 B CN 107564648B CN 201710848593 A CN201710848593 A CN 201710848593A CN 107564648 B CN107564648 B CN 107564648B
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Abstract
The invention discloses a kind of deposition methods for preparing high-performance Ne-Fe-B magnetic powder, and first neodymium iron boron fine powder and heavy rare earth metal Dy block are respectively placed in process chamber different in heat-treatment furnace;To be evacuated inside heat-treatment furnace, the process chamber for being placed with heavy rare earth metal Dy block heated again then, the inner treatment chamber temperature is made to reach 700 ~ 1200 DEG C, and soaking time be 1 ~ for 24 hours, so that heavy rare earth metal Dy block be made to form Dy steam;The furnace body of rotary heat treatment furnace while heating allows Dy steam and neodymium iron boron fine powder to come into full contact with and cooling deposits on neodymium iron boron fine powder surface layer, finally forms one layer of uniform Dy shell on neodymium iron boron fine powder surface.Have the characteristics that high-coercive force, high thermal stability by the Sintered NdFeB magnet that following process obtains using neodymium iron boron powder prepared by the present invention.
Description
Technical field
The present invention relates to a kind of deposition methods for preparing high-performance Ne-Fe-B magnetic powder, belong to rare earth permanent-magnetic material technology neck
Domain.
Technical background
As the novel metal functional material that nineteen sixties come out, rare earth permanent-magnetic material is had been widely used for
The numerous areas such as electromechanics trade, medical instrument, wind-power electricity generation, electric car, aerospace.With the continuous hair of modern industry
Exhibition, permanent-magnet material is more widely applied, its average usage amount in domestic applications, which has become, measures modern people living standard
Standard.With integrated, the micromation, intelligentized development of modern science and technology and information industry, have superelevation comprehensive
The appearance of energy permanent-magnet material, effectively promotes the development of more new industries.Permanent-magnet material has become promotion contemporary science and technology
One of with the important material base of social progress, material base is provided for novel industry.
As third generation rare earth permanent-magnetic material, sintered NdFeB is referred to as " magnetic king " due to its high magnetic property.It is
Nineteen eighty-three is found by Sagawa et al., presses one by rare earth elements RE (Nd, Pr etc.), transition metal TM (Fe, Co etc.) and B element
Then the alloy formed after fixed component ratio is smelting uses the method compression moulding of powder metallurgy, through being sintered obtain one
Kind high performance magnetic material.Sintered Nd-Fe-B permanent magnetic material comprehensive magnetic can well and sexual valence is relatively high, is advantageously implemented product
Micromation, it is very widely used in many high-end products.
It is right as sintered neodymium iron boron material is using more and more extensive, the especially application of the high-temperature fields such as electric motor of automobile
The performance requirement of NdFeB material is higher and higher.However, the Curie temperature due to neodymium iron boron is low, temperature stability is poor, so that neodymium
Iron boron material is very restricted in the application of many high-temperature fields.
For a long time, a kind of widely applied method for promoting magnet high-temperature magnetic energy of neodymium iron boron manufacturing industry that is sintered is big
Width improves its coercivity.There are two types of main methods: one is improve preparation process.The strict control oxygen in neodymium iron boron manufacturing process
Content refines neodymium iron boron powder in pulverizing process.Another method is that the heavy rare earth such as Dy or Tb are introduced into neodymium iron boron magnetic body
Metal.Mainly include following three method: the metals such as Dy or Tb being added in fusion process, Dy or Tb, crystalline substance is added in pulverizing process
Boundary's diffusion technique introduces heavy metal Dy or Tb in magnet surface.But due to Dy or Tb and Fe anti-ferromagnetic coupling interaction, melting
The method that the metals such as Dy or Tb are added in journey makes magnet lose part magnetic energy product because of the decline of remanent magnetism.But in pulverizing process
In be mixed into heavy rare earth metal fine powder, there is the non-uniform problem of mixing, so that heavy rare earth metal distribution is not inside magnet after sintering
Uniformly, magnet performance is influenced.
Magnetron sputtering technique is to report the more technology that heavy rare earth and its compound are deposited in powder particle surface at present
(such as patent ZL201110242847.7 and patent ZL201310416673.0).But it is operated using magnetron sputtering technique more multiple
It is miscellaneous, it the high requirements on the equipment and is not easy to realize industrialization.
Summary of the invention
The object of the present invention is to provide a kind of deposition methods for preparing high-performance Ne-Fe-B magnetic powder.
A kind of deposition method preparing high-performance Ne-Fe-B magnetic powder first distinguishes neodymium iron boron fine powder and heavy rare earth metal Dy block
It is placed in process chamber different in heat-treatment furnace;It will be evacuated inside heat-treatment furnace again, then to being placed with heavy rare earth metal
The process chamber of Dy block is heated, and the inner treatment chamber temperature is made to reach 700~1200 DEG C, and soaking time be 1~for 24 hours, from
And heavy rare earth metal Dy block is made to form Dy steam;The furnace body of rotary heat treatment furnace while heating, makes Dy steam and neodymium iron boron thin
Powder comes into full contact with and in the cooling deposition in neodymium iron boron fine powder surface layer, finally forms one layer of uniform Dy shell on neodymium iron boron fine powder surface
Layer.
Further scheme, the neodymium iron boron fine powder are prepared by airflow milling method or ball-milling method, average particle size
It is 50~1000ppm for 2~8 μm, oxygen content.
Further scheme, the heavy rare earth metal Dy block is that treated through surface cleaning, having a size of 0.5~30mm.
Further scheme, the heat-treatment furnace include the furnace body along axle center rotation, the inner cavity of the furnace body along its axle center according to
It is secondary to set there are three process chamber, metal molybdenum net of the aperture less than 1 μm is installed between adjacent process chamber;The heavy rare earth metal Dy block
It is respectively placed in the first process chamber and third process chamber positioned at both ends, neodymium iron boron fine powder is placed on intermediate second processing room;
The periphery of furnace body on the outside of the first process chamber, third process chamber is arranged with a calandria respectively.
Further scheme, its air pressure is less than 1 × 10 after the heat-treatment furnace vacuumizes-2Pa。
Further scheme, the rotation speed of the furnace body are 5~30 revs/min.
Further scheme further includes helping to mix agent in the neodymium iron boron fine powder, the neodymium iron boron fine powder and the matter for helping whipping up agent
Amount is than being 0.5~3.
Further scheme, described help mix agent as spherical zirconium oxide, silicon nitride, silicon carbide, boron nitride etc., and partial size is less than
5mm。
Further scheme, the heat-treatment furnace are connected with glove box, filled with inert gas in the glove box, make raw material into
Heat-treatment furnace is operated by glove box out.
The invention solves there is mixed powder non-uniform problem when introducing heavy rare earth metal fine powder in powder processed, by adding
Heat arrives certain temperature, and blocky heavy rare earth metal Dy block distillation becomes Dy steam, and Dy steam encounters the neodymium iron boron fine powder of lower temperature
And cooling is deposited on powder face, so that one layer of heavy rare earth metal shell is wrapped up on powder surface, obtains high performance sintering neodymium iron
Boron magnetic powder.There is high-coercive force, high thermal stability using Sintered NdFeB magnet prepared by neodymium iron boron powder prepared by the present invention
The characteristics of.
The present invention is sublimed into steam using heavy rare earth metal Dy at a certain temperature, and then cooling is deposited on powder surface
Method, powder surface wrap up one layer of heavy rare earth metal shell, have it is easy to operate, energy consumption is low and is easily achieved industry
The advantage of change.
The rotation of furnace body and the addition of stirring body is helped to come into full contact with neodymium iron boron fine powder with heavy rare earth metal Dy steam.
Detailed description of the invention
Fig. 1 is the pattern schematic diagram of high-performance Ne-Fe-B magnetic powder prepared by the present invention,
Fig. 2 is the structural schematic diagram of heat-treatment furnace of the invention.
In figure: 1- furnace body, the first process chamber of 1.1-, 1.2- second processing room, 1.3- third process chamber, 1.4- metal molybdenum
Net;2- heavy rare earth metal Dy block, 3-, which is helped, mixes agent, 4- neodymium iron boron fine powder, 5- calandria, 6-Dy shell.
Specific embodiment
The present invention is described in further details below, is engaged in those skilled in the art's refer to the instruction text energy to allow
It is enough to implement.
The pattern schematic diagram of high-performance Ne-Fe-B magnetic powder prepared by the present invention as shown in Figure 1, heavy rare earth metal Dy certain
At a temperature of distil formation steam encounter lower temperature neodymium iron boron fine powder 4 and cooling be deposited on its surface layer, make its surface wrap
One layer of heavy rare earth metal Dy shell 6 is wrapped up in, to obtain high performance sintered NdFeB magnetic powder.
The structure of heat-treatment furnace of the present invention is as shown in Figure 2.The heat-treatment furnace includes the furnace along axle center rotation
The inner cavity of body 1, the furnace body 1 is successively arranged three process chambers along its axle center, and aperture is installed between adjacent process chamber less than 1 μm
Metal molybdenum net 1.4;The heavy rare earth metal Dy block 2 is respectively placed in the first process chamber 1.1 and third process chamber positioned at both ends
1.3, neodymium iron boron fine powder 4 is placed on intermediate second processing room 1.2;Outside the first process chamber 1.1, third process chamber 1.3
The periphery of the furnace body 1 of side is arranged with a calandria 5 respectively.
It is connect respectively with moveable glove box at the import and export of furnace body 1, inert gas, such as nitrogen is filled in the glove box
Gas, neon etc..After glove box transition, by neodymium iron boron fine powder 4 or neodymium iron boron fine powder 4 and the mixture of stirring 3 is helped to be placed in furnace
In second processing room 1.2 in body 1;Heavy rare earth metal Dy block 2 is placed in the first process chamber 1.1 by glove box and third is handled
In room 1.3.Metal molybdenum net 1.4 between adjacent process chamber is in order to ensure heavy rare earth metal Dy block 2 and neodymium iron boron powder 4 be not straight
Contact.< 1 × 10 will be evacuated to inside furnace body 1-2After Pa, calandria 5 works, and makes the first process chamber 1.1, third process chamber
Temperature rises to 700~1200 DEG C in 1.3, and soaking time be 1~for 24 hours;And second processing room 1.2 is not heated.That heats is same
When rotate furnace body 1 along its axle center, rotation speed be 5~30 revs/min.As the temperature rises, heavy rare earth metal Dy
Block 2 distillation be Dy steam, furnace body rotation during, Dy steam is entered in second processing room 1.2 by molybdenum net, and with neodymium iron
The contact of boron fine powder 4, encounters the neodymium iron boron fine powder 4 of lower temperature and cooling is deposited on its surface layer, and with the raising of vapour pressure, Dy steams
Gas constantly enters the gap between neodymium iron boron fine powder, and cooling is deposited on neodymium iron boron fine powder surface, its surface is made to wrap up one layer of weight
Rare earth metal Dy shell 6.
The neodymium iron boron fine powder is prepared by airflow milling method or ball-milling method, and average particle size is 2~8 μm, oxygen
Content is 50~1000ppm.
The heavy rare earth metal Dy block is that treated through surface cleaning, having a size of 0.5~30mm.
Described help mixes agent as spherical zirconium oxide, silicon nitride, silicon carbide, boron nitride etc., and partial size is less than 5mm.
Comparative example 1
Choose performance be 45H sintered NdFeB raw material, using melting rapid hardening+hydrogen it is quick-fried+jet milling process obtain neodymium iron boron
Fine powder.The part fine powder is taken out by orientation compression moulding, static pressure is waited, obtains sintered magnet after sintering heat treatment, as a comparison
Example 1.
Embodiment 1
45H neodymium iron boron fine powder prepared by above-mentioned comparative example 1 of learning from else's experience, the second processing in furnace body is placed it in by glove box
In room;Heavy rare earth metal Dy block is respectively placed in the first process chamber and third process chamber again.It is installed between adjacent process chamber
1 μm of aperture < of metal molybdenum net is to ensure that heavy rare earth metal Dy block is not directly contacted with neodymium iron boron fine powder.Furnace interior is taken out true
Sky is to < 1 × 10-2After Pa, second processing room and second processing room are heated to respectively by calandria to keep the temperature 5h after 850 DEG C, and
Rotate furnace body simultaneously, rotation speed is arranged at 5 revs/min.
After to soaking time, argon gas is filled with into furnace body to 85~90kPa, after being cooled to room temperature, in oxygen-free environment
It is lower to take out treated magnetic powder, by being orientated compression moulding, static pressure are waited, obtain sintered magnet after sintering heat treatment.To magnet into
The magnetic property that permanent-magnet material measuring system test comparison example 1 and embodiment 1 are used after row processing, is as a result listed in table 1.
Embodiment 2
45H neodymium iron boron fine powder prepared by the above-mentioned comparative example 1 of learning from else's experience with help that stir zirconium oxide be that 0.5:1 is mixed in mass ratio,
It is placed it in the second processing room in furnace body by glove box;Again by heavy rare earth metal Dy block be respectively placed in the first process chamber and
In third process chamber.1 μm of aperture < of metal molybdenum net is installed between adjacent process chamber to ensure heavy rare earth metal Dy block and neodymium
Iron boron fine powder is not directly contacted with.Furnace interior is evacuated to < 1 × 10-2After Pa, by calandria respectively by second processing room
It is heated to keeping the temperature 10h after 900 DEG C with second processing room, and rotates furnace body simultaneously, rotation speed is arranged at 10 revs/min.
After to soaking time, argon gas is filled with into furnace body to 85~90kPa, after being cooled to room temperature, in oxygen-free environment
It is lower to take out treated magnetic powder, by being orientated compression moulding, static pressure are waited, obtain sintered magnet after sintering heat treatment.To magnet into
The magnetic property that 2 magnet of permanent-magnet material measuring system testing example is used after row processing, is as a result listed in table 1.
Embodiment 3
45H neodymium iron boron fine powder prepared by the above-mentioned comparative example 1 of learning from else's experience with to help stirring zirconium oxide be that 1:1 is mixed in mass ratio, it is logical
It crosses in the second processing room that glove box places it in furnace body;Heavy rare earth metal Dy block is respectively placed in the first process chamber and again
In three process chambers.1 μm of aperture < of metal molybdenum net is installed between adjacent process chamber to ensure heavy rare earth metal Dy block and neodymium iron
Boron fine powder is not directly contacted with.Furnace interior is evacuated to < 1 × 10-2After Pa, by calandria respectively by second processing room and
Second processing room keeps the temperature 15h after being heated to 1000 DEG C, and rotates furnace body simultaneously, and rotation speed is arranged at 15 revs/min.
After to soaking time, argon gas is filled with into furnace body to 85~90kPa, after being cooled to room temperature, in oxygen-free environment
It is lower to take out treated magnetic powder, by being orientated compression moulding, static pressure are waited, obtain sintered magnet after sintering heat treatment.To magnet into
The magnetic property that 3 magnet of permanent-magnet material measuring system testing example is used after row processing, is as a result listed in table 1.
Table 1:45H Nd-Fe-B permanent magnet material is heat-treated front and back performance comparison through different condition
As seen from Table 1, using NdFeB magnetic powder prepared by the present invention, the magnetic that is prepared after subsequent technique
The coercivity of body is greatly improved, and remanent magnetism reduction is smaller.It can be obtained more preferably by parameters such as optimization temperature, times
Magnetic property.
Comparative example 2
Choose performance be 48M sintered NdFeB raw material, using melting rapid hardening+hydrogen it is quick-fried+jet milling process obtain neodymium iron boron
Fine powder.The part fine powder is taken out by orientation compression moulding, static pressure is waited, obtains sintered magnet after sintering heat treatment, as a comparison
Example 2.
Embodiment 4
48M neodymium iron boron fine powder prepared by above-mentioned comparative example 2 of learning from else's experience, the second processing in furnace body is placed it in by glove box
In room;Heavy rare earth metal Dy block is respectively placed in the first process chamber and third process chamber again.It is installed between adjacent process chamber
1 μm of aperture < of metal molybdenum net is to ensure that heavy rare earth metal Dy block is not directly contacted with neodymium iron boron fine powder.Furnace interior is taken out true
Sky is to < 1 × 10-2After Pa, 10h is kept the temperature after second processing room and second processing room are heated to 900 DEG C respectively by calandria,
And rotating furnace body simultaneously, rotation speed is arranged at 10 revs/min.
After to soaking time, argon gas is filled with into furnace body to 85~90kPa, after being cooled to room temperature, in oxygen-free environment
It is lower to take out treated magnetic powder, by being orientated compression moulding, static pressure are waited, obtain sintered magnet after sintering heat treatment.To magnet into
The magnetic property that 4 magnet of permanent-magnet material measuring system testing example is used after row processing, is as a result listed in table 2.
Embodiment 5
48M neodymium iron boron fine powder prepared by the above-mentioned comparative example 2 of learning from else's experience with to help stirring silicon carbide be that 2:1 is mixed in mass ratio, it is logical
It crosses in the second processing room that glove box places it in furnace body;Heavy rare earth metal Dy block is respectively placed in the first process chamber and again
In three process chambers.1 μm of aperture < of metal molybdenum net is installed between adjacent process chamber to ensure heavy rare earth metal Dy block and neodymium iron
Boron fine powder is not directly contacted with.Furnace interior is evacuated to < 1 × 10-2After Pa, by calandria respectively by second processing room and
Second processing room keeps the temperature 1h after being heated to 1200 DEG C, and rotates furnace body simultaneously, and rotation speed is arranged at 30 revs/min.
After to soaking time, argon gas is filled with into furnace body to 85~90kPa, after being cooled to room temperature, in oxygen-free environment
It is lower to take out treated magnetic powder, by being orientated compression moulding, static pressure are waited, obtain sintered magnet after sintering heat treatment.To magnet into
The magnetic property that 5 magnet of permanent-magnet material measuring system testing example is used after row processing, is as a result listed in table 2.
Embodiment 6
48M neodymium iron boron fine powder prepared by the above-mentioned comparative example 2 of learning from else's experience with to help stirring boron nitride be that 3:1 is mixed in mass ratio, it is logical
It crosses in the second processing room that glove box places it in furnace body;Heavy rare earth metal Dy block is respectively placed in the first process chamber and again
In three process chambers.1 μm of aperture < of metal molybdenum net is installed between adjacent process chamber to ensure heavy rare earth metal Dy block and neodymium iron
Boron fine powder is not directly contacted with.Furnace interior is evacuated to < 1 × 10-2After Pa, by calandria respectively by second processing room and
Second processing room is kept the temperature for 24 hours after being heated to 700 DEG C, and rotates furnace body simultaneously, and rotation speed is arranged at 20 revs/min.
After to soaking time, argon gas is filled with into furnace body to 85~90kPa, after being cooled to room temperature, in oxygen-free environment
It is lower to take out treated magnetic powder, by being orientated compression moulding, static pressure are waited, obtain sintered magnet after sintering heat treatment.To magnet into
The magnetic property that 6 magnet of permanent-magnet material measuring system testing example is used after row processing, is as a result listed in table 2.
Table 2:48M Nd-Fe-B permanent magnet material is heat-treated front and back performance comparison through different condition
As seen from Table 2, compared with traditional milling method, using NdFeB magnetic powder prepared by the present invention,
The coercivity of the magnet prepared after subsequent technique is greatly improved, and remanent magnetism reduction is smaller.
In conjunction with table 1, table 2 as can be seen that the present invention is suitable for preparing the magnet of different trade mark performances.
The above content is the explanations done in conjunction with specific embodiments to the present invention.But protection scope of the present invention packet
It includes but should not be limited only to embodiment of above.Modification, the replacement of all any parameters within claims of the present invention, made
Deng all should belong within protection scope of the present invention.
Claims (8)
1. a kind of deposition method for preparing high-performance Ne-Fe-B magnetic powder, it is characterised in that: first by neodymium iron boron fine powder and heavy rare earth gold
Belong to Dy block to be respectively placed in process chamber different in heat-treatment furnace;It will be evacuated inside heat-treatment furnace again, then to being placed with
The process chamber of heavy rare earth metal Dy block is heated, and so that the inner treatment chamber temperature is reached 700 ~ 1200 DEG C, and soaking time is 1
~ for 24 hours, so that heavy rare earth metal Dy block be made to form Dy steam;The furnace body of rotary heat treatment furnace while heating, allows Dy steam and neodymium
Iron boron fine powder comes into full contact with and in the cooling deposition in neodymium iron boron fine powder surface layer, finally forms one layer uniformly on neodymium iron boron fine powder surface
Dy shell;
The heat-treatment furnace includes the furnace body (1) along axle center rotation, and the inner cavity of the furnace body (1) is successively arranged three along its axle center
Process chamber is installed with metal molybdenum net (1.4) of the aperture less than 1 μm between adjacent process chamber;The heavy rare earth metal Dy block difference
It is placed on first process chamber (1.1) and third process chamber (1.3) at both ends, neodymium iron boron fine powder is placed at intermediate second
It manages room (1.2);The periphery of furnace body (1) on the outside of the first process chamber (1.1), third process chamber (1.3) is arranged with one respectively
Calandria (5).
2. deposition method according to claim 1, it is characterised in that: the neodymium iron boron fine powder be by airflow milling method or
Ball-milling method is prepared, and average particle size is 2 ~ 8 μm, oxygen content is 50 ~ 1000ppm.
3. deposition method according to claim 1, it is characterised in that: the heavy rare earth metal Dy block is through at surface cleaning
After reason, having a size of 0.5 ~ 30mm.
4. deposition method according to claim 1, it is characterised in that: its air pressure is less than 1 after the heat-treatment furnace vacuumizes
×10-2Pa。
5. deposition method according to claim 1, it is characterised in that: the rotation speed of the furnace body is 5 ~ 30 revs/min.
6. deposition method according to claim 1, it is characterised in that: it further include helping to mix agent in the neodymium iron boron fine powder, institute
Stating neodymium iron boron fine powder and helping the mass ratio for mixing agent is 0.5 ~ 3.
7. deposition method according to claim 6, it is characterised in that: it is described help mix agent be spherical zirconium oxide, silicon nitride,
Silicon carbide, boron nitride, partial size are less than 5mm.
8. deposition method according to claim 1, it is characterised in that: the heat-treatment furnace is connected with glove box, the hand
Filled with inert gas in casing, making raw material disengaging heat-treatment furnace is operated by glove box.
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