CN107564648A - A kind of deposition process for preparing high-performance Ne-Fe-B magnetic - Google Patents
A kind of deposition process for preparing high-performance Ne-Fe-B magnetic Download PDFInfo
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- CN107564648A CN107564648A CN201710848593.0A CN201710848593A CN107564648A CN 107564648 A CN107564648 A CN 107564648A CN 201710848593 A CN201710848593 A CN 201710848593A CN 107564648 A CN107564648 A CN 107564648A
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- iron boron
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- 230000005291 magnetic effect Effects 0.000 title claims abstract description 30
- 238000005137 deposition process Methods 0.000 title claims abstract description 15
- 229910001172 neodymium magnet Inorganic materials 0.000 claims abstract description 65
- 238000000034 method Methods 0.000 claims abstract description 64
- 239000000843 powder Substances 0.000 claims abstract description 60
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 claims abstract description 52
- 230000008569 process Effects 0.000 claims abstract description 49
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 48
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 47
- 238000010438 heat treatment Methods 0.000 claims abstract description 31
- 238000002791 soaking Methods 0.000 claims abstract description 10
- 238000012545 processing Methods 0.000 claims description 38
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 239000002184 metal Substances 0.000 claims description 15
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 11
- 229910052750 molybdenum Inorganic materials 0.000 claims description 11
- 239000011733 molybdenum Substances 0.000 claims description 11
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 7
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 5
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 5
- 229910052582 BN Inorganic materials 0.000 claims description 4
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 238000003801 milling Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 4
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 3
- 238000000498 ball milling Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims 1
- 239000010931 gold Substances 0.000 claims 1
- 229910052737 gold Inorganic materials 0.000 claims 1
- 239000000463 material Substances 0.000 description 16
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 12
- 235000016768 molybdenum Nutrition 0.000 description 11
- 238000005245 sintering Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 8
- 239000007789 gas Substances 0.000 description 8
- 239000010410 layer Substances 0.000 description 8
- 229910052692 Dysprosium Inorganic materials 0.000 description 6
- 229910052771 Terbium Inorganic materials 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000000696 magnetic material Substances 0.000 description 5
- PXAWCNYZAWMWIC-UHFFFAOYSA-N [Fe].[Nd] Chemical compound [Fe].[Nd] PXAWCNYZAWMWIC-UHFFFAOYSA-N 0.000 description 4
- 239000006247 magnetic powder Substances 0.000 description 3
- 230000005389 magnetism Effects 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
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- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
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- 239000000126 substance Substances 0.000 description 2
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
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- 230000008878 coupling Effects 0.000 description 1
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- 230000005611 electricity Effects 0.000 description 1
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- 238000007499 fusion processing Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000008676 import Effects 0.000 description 1
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- 239000011812 mixed powder Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052754 neon Inorganic materials 0.000 description 1
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
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- Hard Magnetic Materials (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
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Abstract
The invention discloses a kind of deposition process for preparing high-performance Ne-Fe-B magnetic, and first neodymium iron boron fine powder and heavy rare earth metal Dy blocks are respectively placed in process chamber different in heat-treatment furnace；It will be evacuated inside heat-treatment furnace, the process chamber for being placed with heavy rare earth metal Dy blocks heated again then, the inner treatment chamber temperature is reached 700 ~ 1200 DEG C, and soaking time is 1 ~ 24h, so that heavy rare earth metal Dy blocks form Dy steams；The body of heater of rotary heat treatment furnace while heating, allow Dy steams and neodymium iron boron fine powder fully to contact and be cooled down on neodymium iron boron fine powder top layer and be deposited, finally form one layer of uniform Dy shell on neodymium iron boron fine powder surface.The Sintered NdFeB magnet that the neodymium iron boron powder prepared using the present invention is obtained by following process has the characteristics of high-coercive force, high thermal stability.
Description
Technical field
The present invention relates to a kind of deposition process for preparing high-performance Ne-Fe-B magnetic, belongs to rare earth permanent-magnetic material technology neck
Domain.
Technical background
The novel metal functional material to be come out as nineteen sixties, rare earth permanent-magnetic material have been widely used for
The numerous areas such as electromechanics trade, medicine equipment, wind-power electricity generation, electric automobile, Aero-Space.With the continuous hair of modern industry
Exhibition, permanent-magnet material is more widely applied, and its average usage amount in domestic. applications turns into weighs modern people living standard
Standard.With modern science and technology and the integrated of information industry, miniaturization, intelligentized development, 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 substance basis of social progress, provide material base for new industry.
As third generation rare earth permanent-magnetic material, sintered NdFeB is referred to as " magnetic king " because of its high magnetic property.It is
Nineteen eighty-three is found by Sagawa et al., and one is pressed by rare earth elements RE (Nd, Pr etc.), transition metal TM (Fe, Co etc.) and B element
Fixed component ratio it is smelting after composition alloy, it is then compressing using the method for powder metallurgy, it is sintered obtain one
Kind high performance magnetic material.Sintered Nd-Fe-B permanent magnetic material comprehensive magnetic can get well and cost performance is higher, is advantageously implemented product
Miniaturization, using very extensive in many high-end products.
More and more extensive with the application of sintered neodymium iron boron material, the particularly application of the high-temperature field such as electric motor of automobile is right
The performance requirement more and more higher of NdFeB material.However, because the Curie temperature of 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 method for being sintered the wide variety of lifting magnet high-temperature magnetic energy of neodymium iron boron manufacturing industry is big
Width improves its coercivity.Main method has two kinds：One kind is to improve preparation technology.Oxygen is strictly controlled in neodymium iron boron manufacturing process
Content, neodymium iron boron powder is refined 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：Added in fusion process and Dy or Tb, crystalline substance are added in metal, the pulverizing processes such as Dy or Tb
Boundary's diffusion technique introduces heavy metal Dy or Tb in magnet surface.But due to Dy or Tb and Fe anti-ferromagnetic coupling interactions, melting
The method of the metals such as Dy or Tb is 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, the problem of mixing is uneven be present so that heavy rare earth metal distribution is not inside magnet after sintering
Uniformly, magnet performance is influenceed.
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 operated using magnetron sputtering technique more multiple
It is miscellaneous, it is higher to equipment requirement and be not easy to realize industrialization.
The content of the invention
It is an object of the invention to provide a kind of deposition process for preparing high-performance Ne-Fe-B magnetic.
A kind of deposition process for preparing high-performance Ne-Fe-B magnetic, first neodymium iron boron fine powder and heavy rare earth metal Dy blocks are distinguished
It is placed in process chamber different in heat-treatment furnace；It will be evacuated again inside heat-treatment furnace, then to being placed with heavy rare earth metal
The process chamber of Dy blocks is heated, and the inner treatment chamber temperature is reached 700~1200 DEG C, and soaking time is 1~24h, from
And heavy rare earth metal Dy blocks are made to form Dy steams；The body of heater of rotary heat treatment furnace while heating, make Dy steams and neodymium iron boron thin
Powder is fully contacted and cooled down on neodymium iron boron fine powder top layer and deposited, and finally forms one layer of uniform Dy shell on neodymium iron boron fine powder surface
Layer.
Further scheme, described neodymium iron boron fine powder are prepared by airflow milling method or ball-milling method, its particle mean size
It is 50~1000ppm for 2~8 μm, oxygen content.
Further scheme, the heavy rare earth metal Dy blocks are after surface cleaning is handled, and its size is 0.5~30mm.
Further scheme, the heat-treatment furnace include the body of heater rotated along axle center, the inner chamber of the body of heater along its axle center according to
It is secondary to be provided with three process chambers, the metal molybdenum net that aperture is less than 1 μm is installed between adjacent process chamber；The heavy rare earth metal Dy blocks
The first process chamber and the 3rd process chamber positioned at both ends are respectively placed in, neodymium iron boron fine powder is placed on the second processing room of centre；
The periphery of body of heater on the outside of the first process chamber, the 3rd 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 rotary speed of the body of heater is 5~30 revs/min.
Further scheme, also include helping mixing 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, carborundum, boron nitride etc., and its particle diameter is less than
5mm。
Further scheme, the heat-treatment furnace are connected with glove box, and the glove box is interior filled with inert gas, enters raw material
Go out heat-treatment furnace to be operated by glove box.
The problem of mixed powder is uneven when what the present invention solved is and heavy rare earth metal fine powder is introduced in powder processed be present, by adding
Heat arrives certain temperature, and block heavy rare earth metal Dy blocks distillation becomes Dy steams, and Dy steams run into the neodymium iron boron fine powder of lower temperature
And cool down and be 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.Sintered NdFeB magnet prepared by the neodymium iron boron powder prepared using the present invention has high-coercive force, high thermal stability
The characteristics of.
The present invention is sublimed into steam at a certain temperature using heavy rare earth metal Dy, and then cooling is deposited on powder surface
Method, powder surface wrap up one layer of heavy rare earth metal shell, have it is simple to operate, energy expenditure is low and is easily achieved industry
The advantage of change.
The rotation of body of heater and the addition of stirring body is helped neodymium iron boron fine powder is fully contacted with heavy rare earth metal Dy steams.
Brief description of the drawings
Fig. 1 is the pattern schematic diagram of high-performance Ne-Fe-B magnetic prepared by the present invention,
Fig. 2 is the structural representation of the heat-treatment furnace of the present invention.
In figure：1- bodies of heater, the process chambers of 1.1- first, 1.2- second processings room, the process chambers of 1.3- the 3rd, 1.4- metal molybdenums
Net；2- heavy rare earth metal Dy blocks, 3-, which is helped, mixes agent, 4- neodymium iron boron fine powders, 5- calandrias, 6-Dy shells.
Embodiment
The present invention is described in further details below, those skilled in the art is engaged in reference to specification word energy to allow
It is enough to implement.
The pattern schematic diagram of high-performance Ne-Fe-B magnetic prepared by the present invention as shown in figure 1, heavy rare earth metal Dy certain
At a temperature of distil formation steam run into lower temperature neodymium iron boron fine powder 4 and cool down be deposited on its top layer, make its surface wrap
One layer of heavy rare earth metal Dy shell 6 is wrapped up in, so as to obtain high performance sintered NdFeB magnetic.
The structure of heat-treatment furnace of the present invention is as shown in Figure 2.The heat-treatment furnace includes the stove rotated along axle center
Body 1, the inner chamber of the body of heater 1 are sequentially provided with 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 blocks 2 are respectively placed in positioned at first process chamber 1.1 at both ends and the 3rd process chamber
1.3, neodymium iron boron fine powder 4 is placed on the second processing room 1.2 of centre；Outside the first process chamber 1.1, the 3rd process chamber 1.3
The periphery of the body of heater 1 of side is arranged with a calandria 5 respectively.
It is connected respectively with moveable glove box at the import and export of body of heater 1, inert gas, such as nitrogen is filled with 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 stove
In second processing room 1.2 in body 1；Heavy rare earth metal Dy blocks 2 are placed in by the first process chamber 1.1 and the 3rd processing by glove box
In room 1.3.Metal molybdenum net 1.4 between adjacent process chamber is in order to ensure heavy rare earth metal Dy blocks 2 and neodymium iron boron powder 4 be not straight
Contact.＜ 1 × 10 will be evacuated to inside body of heater 1-2After Pa, calandria 5 works, and makes the first process chamber 1.1, the 3rd process chamber
Temperature rises to 700~1200 DEG C in 1.3, and soaking time is 1~24h；And second processing room 1.2 is not heated.That heats is same
When body of heater 1 is rotated along its axle center, rotary speed be 5~30 revs/min.With the rise of temperature, heavy rare earth metal Dy
The distillation of block 2 be Dy steams, during body of heater rotates, Dy steams by molybdenum net into second processing room 1.2, and with neodymium iron
Boron fine powder 4 contacts, and runs into the neodymium iron boron fine powder 4 of lower temperature and cools down and be deposited on its top layer, with the rise of vapour pressure, Dy steams
The gap that gas constantly enters between neodymium iron boron fine powder, and cool down and be deposited on neodymium iron boron fine powder surface, its surface is wrapped up one layer of weight
Rare earth metal Dy shells 6.
Described neodymium iron boron fine powder is prepared by airflow milling method or ball-milling method, and its particle mean size is 2~8 μm, oxygen
Content is 50~1000ppm.
The heavy rare earth metal Dy blocks are after surface cleaning is handled, and its size is 0.5~30mm.
Described help mixes agent as spherical zirconium oxide, silicon nitride, carborundum, boron nitride etc., and its particle diameter is less than 5mm.
Comparative example 1
Choose performance be 45H sintered NdFeB raw material, using melting rapid hardening+hydrogen it is quick-fried+air-flow grinding process obtain neodymium iron boron
Fine powder.The part fine powder is taken out by being orientated compressing, isostatic pressed, obtains sintered magnet after sintering heat treatment, as a comparison
Example 1.
Embodiment 1
45H neodymium iron boron fine powders prepared by the above-mentioned comparative example 1 of learning from else's experience, the second processing being placed on by glove box in body of heater
In room；Heavy rare earth metal Dy blocks are respectively placed in the first process chamber and the 3rd process chamber again.It is installed between adjacent process chamber
1 μm of aperture ＜ metal molybdenum net is to ensure that heavy rare earth metal Dy blocks are not directly contacted with neodymium iron boron fine powder.Furnace interior is taken out very
It is empty to ＜ 1 × 10-2After Pa, second processing room and second processing room are heated to respectively by calandria to be incubated 5h after 850 DEG C, and
Rotate body of heater simultaneously, rotary speed is arranged on 5 revs/min.
After soaking time terminates, argon gas is filled with into body of heater to 85~90kPa, after being cooled to room temperature, in oxygen-free environment
Magnetic after lower taking-up processing, by being orientated compressing, isostatic pressed, sintered magnet is obtained after sintering heat treatment.Magnet is entered
Using the magnetic property of permanent-magnet material measuring system test comparison example 1 and embodiment 1 after row processing, table 1 is as a result listed in.
Embodiment 2
45H neodymium iron borons fine powder prepared by above-mentioned comparative example 1 of learning from else's experience is 0.5 in mass ratio with helping stirring zirconium oxide:1 mixing,
It is placed on by glove box in the second processing room in body of heater；Again by heavy rare earth metal Dy blocks be respectively placed in the first process chamber and
In 3rd process chamber.1 μm of aperture ＜ metal molybdenum net is installed between adjacent process chamber to ensure heavy rare earth metal Dy blocks 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 being incubated 10h after 900 DEG C with second processing room, and rotates body of heater simultaneously, rotary speed is arranged on 10 revs/min.
After soaking time terminates, argon gas is filled with into body of heater to 85~90kPa, after being cooled to room temperature, in oxygen-free environment
Magnetic after lower taking-up processing, by being orientated compressing, isostatic pressed, sintered magnet is obtained after sintering heat treatment.Magnet is entered
The magnetic property of the magnet of permanent-magnet material measuring system testing example 2 is used after row processing, is as a result listed in table 1.
Embodiment 3
45H neodymium iron borons fine powder prepared by above-mentioned comparative example 1 of learning from else's experience is 1 in mass ratio with helping stirring zirconium oxide:1 mixing, leads to
Cross in the second processing room that glove box is placed in body of heater；Heavy rare earth metal Dy blocks are respectively placed in the first process chamber and again
In three process chambers.1 μm of aperture ＜ metal molybdenum net is installed between adjacent process chamber to ensure heavy rare earth metal Dy blocks 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 incubated 15h after being heated to 1000 DEG C, and rotates body of heater simultaneously, and rotary speed is arranged on 15 revs/min.
After soaking time terminates, argon gas is filled with into body of heater to 85~90kPa, after being cooled to room temperature, in oxygen-free environment
Magnetic after lower taking-up processing, by being orientated compressing, isostatic pressed, sintered magnet is obtained after sintering heat treatment.Magnet is entered
The magnetic property of the magnet of permanent-magnet material measuring system testing example 3 is used after row processing, is as a result listed in table 1.
Table 1：45H Nd-Fe-B permanent magnet materials are heat-treated front and rear performance comparison through different condition
As seen from Table 1, the NdFeB magnetic powder prepared using the present invention, the magnetic prepared after subsequent technique
The coercivity of body is greatly improved, and remanent magnetism reduction is smaller.By optimize the parameters such as temperature, time can obtain it is more excellent
Magnetic property.
Comparative example 2
Choose performance be 48M sintered NdFeB raw material, using melting rapid hardening+hydrogen it is quick-fried+air-flow grinding process obtain neodymium iron boron
Fine powder.The part fine powder is taken out by being orientated compressing, isostatic pressed, obtains sintered magnet after sintering heat treatment, as a comparison
Example 2.
Embodiment 4
48M neodymium iron boron fine powders prepared by the above-mentioned comparative example 2 of learning from else's experience, the second processing being placed on by glove box in body of heater
In room；Heavy rare earth metal Dy blocks are respectively placed in the first process chamber and the 3rd process chamber again.It is installed between adjacent process chamber
1 μm of aperture ＜ metal molybdenum net is to ensure that heavy rare earth metal Dy blocks are not directly contacted with neodymium iron boron fine powder.Furnace interior is taken out very
It is empty to ＜ 1 × 10-2After Pa, 10h is incubated after second processing room and second processing room are heated into 900 DEG C respectively by calandria,
And rotating body of heater simultaneously, rotary speed is arranged on 10 revs/min.
After soaking time terminates, argon gas is filled with into body of heater to 85~90kPa, after being cooled to room temperature, in oxygen-free environment
Magnetic after lower taking-up processing, by being orientated compressing, isostatic pressed, sintered magnet is obtained after sintering heat treatment.Magnet is entered
The magnetic property of the magnet of permanent-magnet material measuring system testing example 4 is used after row processing, is as a result listed in table 2.
Embodiment 5
48M neodymium iron borons fine powder prepared by above-mentioned comparative example 2 of learning from else's experience is 2 in mass ratio with helping stirring carborundum:1 mixing, leads to
Cross in the second processing room that glove box is placed in body of heater；Heavy rare earth metal Dy blocks are respectively placed in the first process chamber and again
In three process chambers.1 μm of aperture ＜ metal molybdenum net is installed between adjacent process chamber to ensure heavy rare earth metal Dy blocks 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 incubated 1h after being heated to 1200 DEG C, and rotates body of heater simultaneously, and rotary speed is arranged on 30 revs/min.
After soaking time terminates, argon gas is filled with into body of heater to 85~90kPa, after being cooled to room temperature, in oxygen-free environment
Magnetic after lower taking-up processing, by being orientated compressing, isostatic pressed, sintered magnet is obtained after sintering heat treatment.Magnet is entered
The magnetic property of the magnet of permanent-magnet material measuring system testing example 5 is used after row processing, is as a result listed in table 2.
Embodiment 6
48M neodymium iron borons fine powder prepared by above-mentioned comparative example 2 of learning from else's experience is 3 in mass ratio with helping stirring boron nitride:1 mixing, leads to
Cross in the second processing room that glove box is placed in body of heater；Heavy rare earth metal Dy blocks are respectively placed in the first process chamber and again
In three process chambers.1 μm of aperture ＜ metal molybdenum net is installed between adjacent process chamber to ensure heavy rare earth metal Dy blocks 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 incubated 24h after being heated to 700 DEG C, and rotates body of heater simultaneously, and rotary speed is arranged on 20 revs/min.
After soaking time terminates, argon gas is filled with into body of heater to 85~90kPa, after being cooled to room temperature, in oxygen-free environment
Magnetic after lower taking-up processing, by being orientated compressing, isostatic pressed, sintered magnet is obtained after sintering heat treatment.Magnet is entered
The magnetic property of the magnet of permanent-magnet material measuring system testing example 6 is used after row processing, is as a result listed in table 2.
Table 2：48M Nd-Fe-B permanent magnet materials are heat-treated front and rear performance comparison through different condition
As seen from Table 2, compared with traditional milling method, using the NdFeB magnetic powder for preparing of the present invention,
The coercivity of the magnet prepared after subsequent technique is greatly improved, and remanent magnetism reduction is smaller.
With reference to table 1, table 2 as can be seen that the present invention is applied to prepare the magnet of different trade mark performances.
Above content is the explanation done in conjunction with specific embodiments to the present invention.But protection scope of the present invention bag
Include but should not be limited only to embodiment of above.The modification of all any parameters within claims of the present invention, made, replace
Deng should all belong within protection scope of the present invention.
Claims (9)
- A kind of 1. deposition process for preparing high-performance Ne-Fe-B magnetic, it is characterised in that：First by neodymium iron boron fine powder and heavy rare earth gold Category Dy blocks are respectively placed in process chamber different in heat-treatment furnace；It will be evacuated again inside heat-treatment furnace, then to being placed with The process chamber of heavy rare earth metal Dy blocks is heated, and the inner treatment chamber temperature is reached 700 ~ 1200 DEG C, and soaking time is 1 ~ 24h, so that heavy rare earth metal Dy blocks form Dy steams；The body of heater of rotary heat treatment furnace while heating, allows Dy steams and neodymium Iron boron fine powder is fully contacted and cooled down on neodymium iron boron fine powder top layer and deposited, and one layer is finally formed on neodymium iron boron fine powder surface uniformly Dy shells.
- 2. deposition process according to claim 1, it is characterised in that：Described neodymium iron boron fine powder be by airflow milling method or Ball-milling method is prepared, and its particle mean size is 2 ~ 8 μm, oxygen content is 50 ~ 1000ppm.
- 3. deposition process according to claim 1, it is characterised in that：The heavy rare earth metal Dy blocks are through at surface cleaning After reason, its size is 0.5 ~ 30mm.
- 4. deposition process according to claim 1, it is characterised in that：The heat-treatment furnace includes the body of heater rotated along axle center （1）, the body of heater（1）Inner chamber be sequentially provided with three process chambers along its axle center, aperture is installed between adjacent process chamber less than 1 μm metal molybdenum net（1.4）；The heavy rare earth metal Dy blocks are respectively placed in the first process chamber positioned at both ends（1.1）At the 3rd Manage room（1.3）, neodymium iron boron fine powder be placed on centre second processing room（1.2）；Positioned at the first process chamber（1.1）, at the 3rd Manage room（1.3）The body of heater in outside（1）Periphery be arranged with a calandria respectively（5）.
- 5. deposition process according to claim 1, it is characterised in that：Its air pressure is less than 1 after the heat-treatment furnace vacuumizes ×10-2Pa。
- 6. deposition process according to claim 1, it is characterised in that：The rotary speed of the body of heater is 5 ~ 30 revs/min.
- 7. deposition process according to claim 1, it is characterised in that：Agent also is mixed including helping in the neodymium iron boron fine powder, institute It is 0.5 ~ 3 that neodymium iron boron fine powder, which is stated, with helping the mass ratio of whipping up agent.
- 8. deposition process according to claim 7, it is characterised in that：It is described help mix agent for spherical zirconium oxide, silicon nitride, Carborundum, boron nitride etc., its particle diameter are less than 5mm.
- 9. deposition process 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, raw material disengaging heat-treatment furnace is set to be operated by glove box.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108766753A (en) * | 2018-05-11 | 2018-11-06 | 包头稀土研究院 | The preparation method of high energy product high-coercive force Sintered NdFeB magnet |
| CN116741485A (en) * | 2022-10-21 | 2023-09-12 | 宁波众海磁业有限公司 | A silicon carbide/rare earth NdFeB composite magnetic material and its preparation method |
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| US20150132174A1 (en) * | 2009-09-04 | 2015-05-14 | Electron Energy Corporation | Rare Earth Composite Magnets with Increased Resistivity |
| CN104907572A (en) * | 2015-07-16 | 2015-09-16 | 浙江中杭新材料股份有限公司 | Preparation method of NdFeB magnetic material |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150132174A1 (en) * | 2009-09-04 | 2015-05-14 | Electron Energy Corporation | Rare Earth Composite Magnets with Increased Resistivity |
| CN104907572A (en) * | 2015-07-16 | 2015-09-16 | 浙江中杭新材料股份有限公司 | Preparation method of NdFeB magnetic material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108766753A (en) * | 2018-05-11 | 2018-11-06 | 包头稀土研究院 | The preparation method of high energy product high-coercive force Sintered NdFeB magnet |
| CN116741485A (en) * | 2022-10-21 | 2023-09-12 | 宁波众海磁业有限公司 | A silicon carbide/rare earth NdFeB composite magnetic material and its preparation method |
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