CN112453391A - Terbium oxide coated neodymium iron boron permanent magnet material composite powder, preparation method and system device thereof - Google Patents
Terbium oxide coated neodymium iron boron permanent magnet material composite powder, preparation method and system device thereof Download PDFInfo
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- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 136
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 title claims abstract description 127
- 229910003451 terbium oxide Inorganic materials 0.000 title claims abstract description 79
- SCRZPWWVSXWCMC-UHFFFAOYSA-N terbium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Tb+3].[Tb+3] SCRZPWWVSXWCMC-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 239000000843 powder Substances 0.000 title claims abstract description 67
- 239000002131 composite material Substances 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 47
- 239000000463 material Substances 0.000 title claims abstract description 36
- 238000006243 chemical reaction Methods 0.000 claims abstract description 97
- 239000012495 reaction gas Substances 0.000 claims abstract description 78
- 239000002245 particle Substances 0.000 claims abstract description 66
- 229910052771 Terbium Inorganic materials 0.000 claims abstract description 65
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 claims abstract description 65
- 238000002156 mixing Methods 0.000 claims abstract description 48
- 238000000926 separation method Methods 0.000 claims abstract description 16
- 239000007787 solid Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 6
- 238000005243 fluidization Methods 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims description 63
- 239000012159 carrier gas Substances 0.000 claims description 58
- 230000001681 protective effect Effects 0.000 claims description 49
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 28
- 239000000203 mixture Substances 0.000 claims description 15
- 229910052786 argon Inorganic materials 0.000 claims description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 12
- 239000001307 helium Substances 0.000 claims description 11
- 229910052734 helium Inorganic materials 0.000 claims description 11
- 230000005484 gravity Effects 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 7
- 239000000047 product Substances 0.000 claims description 5
- 230000008016 vaporization Effects 0.000 claims description 4
- 238000003860 storage Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- GFISHBQNVWAVFU-UHFFFAOYSA-K terbium(iii) chloride Chemical group Cl[Tb](Cl)Cl GFISHBQNVWAVFU-UHFFFAOYSA-K 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000009827 uniform distribution Methods 0.000 abstract description 4
- 239000000696 magnetic material Substances 0.000 description 36
- -1 neodymium iron boron rare earth Chemical class 0.000 description 9
- 229910052761 rare earth metal Inorganic materials 0.000 description 9
- 239000011259 mixed solution Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 230000001360 synchronised effect Effects 0.000 description 2
- 238000009834 vaporization Methods 0.000 description 2
- MAYVZUQEFSJDHA-UHFFFAOYSA-N 1,5-bis(methylsulfanyl)naphthalene Chemical compound C1=CC=C2C(SC)=CC=CC2=C1SC MAYVZUQEFSJDHA-UHFFFAOYSA-N 0.000 description 1
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 1
- 229910003440 dysprosium oxide Inorganic materials 0.000 description 1
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(iii) oxide Chemical compound O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0572—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes with a protective layer
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Power Engineering (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The invention provides terbium oxide-coated neodymium iron boron permanent magnet material composite powder, a preparation method and a system device thereof, wherein the preparation method comprises the following steps: and mixing the fluidized neodymium iron boron particles with the terbium source and the reaction gas for reaction, and carrying out gas-solid separation on the reaction product to obtain the terbium oxide coated neodymium iron boron permanent magnet material composite powder. The invention adopts a fluidization process, so that the neodymium-iron-boron powder is fully contacted with the terbium source and the reaction gas in the fluidized bed reaction device, a dynamic basis is provided for subsequent full reaction, the uniform distribution of the micro-scale powder is realized, the uniformity of the macro-scale of the permanent magnet is further ensured, and the coercive force and the temperature stability of the neodymium-iron-boron permanent magnet material are effectively improved.
Description
Technical Field
The invention belongs to the technical field of magnetic materials, and relates to terbium oxide-coated neodymium iron boron permanent magnet material composite powder, a preparation method and a system device thereof.
Background
The neodymium iron boron rare earth permanent magnet material is widely applied to the fields of extra-high voltage direct current power supply systems, quick charging systems, electric automobile motors and the like due to the optimal magnetic energy product performance, and is the permanent magnet material which is most widely applied at present. One of the main applications of the neodymium iron boron rare earth permanent magnet material is to prepare a permanent magnet motor, compared with an alternating current asynchronous motor, the permanent magnet motor provides excitation by a permanent magnet, and the motor has a simple structure and good operation reliability; meanwhile, no exciting current and excitation loss exist, and the power density of the motor is high. At present, most of motors such as automobile starting motors, wind driven generators and the like adopt permanent magnet motors. In particular, in recent years, new energy vehicles such as electric vehicles have been developed in order to protect the environment and save resources. In new energy vehicles, including driving motors, generators, etc., neodymium iron boron rare earth permanent magnet materials are required. The neodymium iron boron permanent magnet is small in size and high in performance, can well reduce the quality of a motor, improves the efficiency of the motor, and is more suitable for miniaturization and light weight of an automobile. At present, in the motor installation vehicle of the new energy automobile in China, the installation proportion of the neodymium iron boron rare earth permanent magnet synchronous motor is up to 91.4%, and the neodymium iron boron rare earth permanent magnet synchronous motor occupies the largest share in the domestic market.
However, the neodymium iron boron rare earth permanent magnet material has poor thermal stability, so that the application of the neodymium iron boron rare earth permanent magnet material in the high-temperature field is severely limited. In recent years, with the rapid development of industries such as electric vehicles and wind power generation, how to improve the thermal stability of the neodymium iron boron rare earth permanent magnet material becomes a main problem in the field of industrial research.
At present, an effective method for improving the high-temperature magnetic performance of a magnet is to greatly improve the coercive force of the magnet, and improve the anisotropy of a magnetic field by doping terbium oxide in a neodymium iron boron rare earth permanent magnet material, so that the coercive force and the temperature stability of the magnet can be effectively improved.
CN104164646A discloses a dysprosium penetration method on the surface of neodymium iron boron, which comprises the following steps in sequence: A. removing black skin and oil on the surface of the neodymium iron boron, cleaning and drying; B. mixing dysprosium oxide, dysprosium chloride and alcohol according to the proportion of 4-6 g to 0.01-0.03 g to 450-550 ml to form a mixed solution; C. putting the mixed solution formed in the step B into a water bath at the temperature of 30-100 ℃; b, placing the neodymium iron boron treated in the step A into the mixed solution, taking out the neodymium iron boron after 4-6 minutes, and drying the neodymium iron boron under the protection of nitrogen; D. c, wrapping the neodymium iron boron treated in the step C with an iron sheet, and carrying out vacuum aging treatment for 4-8 hours at 850-950 ℃; and then carrying out vacuum aging treatment for 4-8 hours at the temperature of 400-600 ℃.
Therefore, how to design and prepare the high-quality terbium oxide-coated neodymium iron boron permanent magnet material composite powder ensures that components on a microscale are uniformly distributed, and becomes a problem to be solved urgently for improving the coercive force and the temperature stability of the neodymium iron boron permanent magnet material.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide terbium oxide-coated neodymium-iron-boron permanent magnet material composite powder, a preparation method and a system device thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a preparation method of terbium oxide-coated neodymium iron boron permanent magnet material composite powder, which comprises the following steps:
and mixing the fluidized neodymium iron boron particles with the terbium source and the reaction gas for reaction, and carrying out gas-solid separation on the reaction product to obtain the terbium oxide coated neodymium iron boron permanent magnet material composite powder.
The invention adopts a fluidization process, so that the neodymium-iron-boron powder is fully contacted with the terbium source and the reaction gas in the fluidized bed reaction device, a dynamic basis is provided for subsequent full reaction, the uniform distribution of the micro-scale powder is realized, the uniformity of the macro-scale of the permanent magnet is further ensured, and the coercive force and the temperature stability of the neodymium-iron-boron permanent magnet material are effectively improved.
As a preferred technical solution of the present invention, the neodymium iron boron particles are fluidized in a protective atmosphere to obtain fluidized neodymium iron boron particles.
Preferably, the protective gas used in the protective atmosphere comprises at least one of nitrogen, argon or helium or a combination of two groups thereof.
The invention can keep the neodymium iron boron particles in a fluidized state and isolate oxygen in the environment by reacting in a protective atmosphere, thereby facilitating the subsequent controllable coating of terbium oxide.
Preferably, the particle size of the neodymium iron boron particles is 0.5-100 μm, for example, 0.5 μm, 1 μm, 10 μm, 20 μm, 30 μm, 40 μm, 50 μm, 60 μm, 70 μm, 80 μm, 90 μm or 100 μm, but is not limited to the values listed, and other values not listed in the range of the values are also applicable.
As a preferred technical solution of the present invention, the mixing manner is: the terbium source and the reaction gas are respectively and independently introduced into the protective atmosphere in which the neodymium iron boron particles in the fluidized state are positioned.
Preferably, the mixing temperature is 650 to 850 ℃, for example, 650 ℃, 660 ℃, 670 ℃, 680 ℃, 690 ℃, 700 ℃, 710 ℃, 720 ℃, 730 ℃, 740 ℃, 750 ℃, 760 ℃, 770 ℃, 780 ℃, 790 ℃, 800 ℃, 810 ℃, 820 ℃, 830 ℃, 840 ℃ or 850 ℃, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the mixing time is 1min or more, for example 1min, 2min, 3min, 4min, 5min, 6min, 7min, 8min, 9min or 10min, but is not limited to the values listed, and other values not listed within the range of values are equally applicable.
As a preferred technical scheme of the invention, the terbium source is TbCl3。
Preferably, the terbium source is preheated and then mixed for reaction.
Preferably, the terbium source is preheated to 200-800 deg.C, such as 200 deg.C, 250 deg.C, 300 deg.C, 350 deg.C, 400 deg.C, 450 deg.C, 500 deg.C, 550 deg.C, 600 deg.C, 650 deg.C, 700 deg.C, 750 deg.C or 800 deg.C, but not limited to the values listed, and other values not listed in this range are also applicable.
Preferably, the terbium source is fed into the reaction device by a carrier gas to carry out a mixing reaction.
Preferably, the gas flow rate of the terbium source mixed with the carrier gas is 100-800 mL/min, such as 100mL/min, 150mL/min, 200mL/min, 250mL/min, 300mL/min, 350mL/min, 400mL/min, 450mL/min, 500mL/min, 550mL/min, 600mL/min, 650mL/min, 700mL/min, 750mL/min, or 800mL/min, but is not limited to the values listed, and other values not listed in this range are equally applicable.
In a preferred embodiment of the present invention, the reaction gas is steam.
Preferably, the reaction gas is preheated and then mixed for reaction.
Preferably, the reaction gas is preheated to 0 to 100 ℃, for example, 0 ℃, 10 ℃, 20 ℃, 30 ℃, 40 ℃, 50 ℃, 60 ℃, 70 ℃, 80 ℃, 90 ℃ or 100 ℃, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the reaction gas is fed into the reaction device through a carrier gas to carry out mixing reaction.
Preferably, the reaction gas and carrier gas are mixed at a gas flow rate of 75 to 1500mL/min, such as 75mL/min, 100mL/min, 200mL/min, 300mL/min, 400mL/min, 500mL/min, 600mL/min, 700mL/min, 800mL/min, 900mL/min, 1000mL/min, 1100mL/min, 1200mL/min, 1300mL/min, 1400mL/min, or 1500mL/min, but not limited to the values listed, and other values not listed in this range are equally applicable.
The preparation method provided by the invention limits the mixing time and the mixing temperature, and the gas speed of the terbium source and the reaction gas introduced into the fluidized bed reaction device, and realizes the purpose of uniformly depositing the terbium oxide on the surface of the neodymium iron boron permanent magnet material and the regulation and control of the content of the terbium oxide by adjusting the process parameters.
As a preferable technical scheme of the invention, the gas-solid separation method comprises gravity settling, centrifugal settling or filtering.
As a preferred technical solution of the present invention, the preparation method comprises:
carrying out fluidization treatment on neodymium iron boron particles with the particle size of 0.5-100 microns in a protective atmosphere to obtain neodymium iron boron particles in a fluidized state, wherein the protective atmosphere adopts protective gas comprising at least one of nitrogen, argon or helium or a combination of two groups of nitrogen, argon or helium;
(II) preheating the terbium source to 200-800 ℃, mixing the preheated terbium source with carrier gas, and introducing the mixture into a protective atmosphere in which the neodymium iron boron particles in a fluidized state are located at a gas speed of 100-800 mL/min; meanwhile, preheating the reaction gas to 0-100 ℃, mixing the preheated reaction gas with a carrier gas, and introducing the mixture into a protective atmosphere containing the neodymium-iron-boron particles in the fluidized state at a gas speed of 75-1500 mL/min, wherein the mixing temperature of the neodymium-iron-boron particles in the fluidized state, the terbium source and the reaction gas is 650-850 ℃, and the mixing time is more than or equal to 1 min;
and (III) after the reaction is finished, obtaining the terbium oxide-coated neodymium iron boron permanent magnet material composite powder by performing gravity settling, centrifugal settling or filtering on the obtained reaction product.
In a second aspect, the invention provides terbium oxide-coated neodymium iron boron permanent magnet material composite powder prepared by the preparation method in the first aspect, wherein the mass fraction of terbium oxide in the terbium oxide-coated neodymium iron boron permanent magnet material composite powder is 0.1-3.0 wt.%.
The terbium oxide-coated neodymium iron boron permanent magnet material composite powder provided by the invention is characterized in that a terbium oxide shell is uniformly coated on the surface of neodymium iron boron particles by combining a chemical vapor deposition principle and a fluidized bed process technology, and the uniform distribution of the microscale ensures the uniformity of the macroscale, so that the aim of improving the coercive force and the temperature stability of the neodymium iron boron permanent magnet material and ensuring the component uniformity of a macroscopic permanent magnet motor is fulfilled.
In a third aspect, the invention provides a system device for preparing the terbium oxide-coated neodymium iron boron permanent magnet material composite powder, which comprises a fluidized bed reaction device, wherein the bottom of the fluidized bed reaction device is externally connected with a protective gas inlet pipe, the lower part of the reaction device is respectively and independently externally connected with a terbium source generating device and a reaction gas inlet pipe, and the upper part of the fluidized bed reaction device is externally connected with a storage bin.
As a preferable technical scheme, the top of the fluidized bed reaction device is externally connected with a tail gas treatment device.
Preferably, a vaporizing device is arranged on the reaction gas inlet pipe.
Preferably, the fluidized bed reaction device is externally connected with a product collecting device.
The system refers to an equipment system, a system device or a production device.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention adopts a fluidization process, so that the neodymium-iron-boron powder is fully contacted with the terbium source and the reaction gas in the fluidized bed reaction device, a dynamic basis is provided for subsequent full reaction, the uniform distribution of the micro-scale powder is realized, the uniformity of the macro-scale of the permanent magnet is further ensured, and the coercive force and the temperature stability of the neodymium-iron-boron permanent magnet material are effectively improved;
(2) the method for preparing the terbium oxide-coated neodymium iron boron composite powder is simple, uniform in coating layer, controllable in thickness, low in cost and easy for large-scale batch production.
Drawings
Fig. 1 is a schematic structural diagram of a system device for preparing terbium oxide-coated neodymium iron boron magnetic material composite powder according to an embodiment of the present invention;
wherein, 1-a storage bin; 2-a fluidized bed reaction device; 3-a terbium source generating device; 4-a vaporization device; 5-a product collection device; 6-tail gas treatment device;
fig. 2 is an SEM image of terbium oxide-coated neodymium iron boron composite powder prepared in example 1 of the present invention.
Detailed Description
It is to be understood that in the description of the present invention, the terms "center", "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., indicate orientations or positional relationships based on those shown in the drawings, and are used only for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be taken as limiting the present invention. Furthermore, the terms "first", "second", etc. are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first," "second," etc. may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless otherwise specified.
It should be noted that, in the description of the present invention, unless otherwise explicitly specified or limited, the terms "disposed," "connected" and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art through specific situations.
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.
In one embodiment, the present invention provides a system device for preparing terbium oxide-coated neodymium iron boron permanent magnet composite powder, which comprises a fluidized bed reaction device 2 as shown in fig. 1, wherein a protective gas inlet pipe is externally connected to the bottom of the fluidized bed reaction device 2, the lower part of the reaction device is respectively and independently externally connected with a terbium source generation device 3 and a reaction gas inlet pipe, and a vaporization device 4 is arranged on the reaction gas inlet pipe. The external feed bin 1 in upper portion of fluidized bed reaction unit 2, the external tail gas processing apparatus 6 in top of fluidized bed reaction unit 2, the external product collection device 5 of fluidized bed reaction unit 2.
In another embodiment, the invention provides a preparation method of terbium oxide-coated neodymium iron boron permanent magnet material composite powder, which comprises the following steps:
(1) carrying out fluidization treatment on neodymium iron boron particles with the particle size of 0.5-100 microns in a protective atmosphere to obtain neodymium iron boron particles in a fluidized state, wherein the protective atmosphere adopts protective gas comprising at least one of nitrogen, argon or helium or a combination of two groups of nitrogen, argon or helium;
(2) the terbium source is preheated to 200-800 ℃, and the preheated terbium source and carrier gas are mixed and then introduced into the protective atmosphere in which the neodymium iron boron particles in the fluidized state are positioned at the gas speed of 100-800 mL/min; meanwhile, preheating the reaction gas to 0-100 ℃, mixing the preheated reaction gas with a carrier gas, and introducing the mixture into a protective atmosphere containing the neodymium-iron-boron particles in the fluidized state at a gas speed of 75-1500 mL/min, wherein the mixing temperature of the neodymium-iron-boron particles in the fluidized state, the terbium source and the reaction gas is 650-850 ℃, and the mixing time is more than or equal to 1 min;
(3) and after the reaction is finished, obtaining the terbium oxide-coated neodymium iron boron permanent magnet material composite powder by performing gravity settling, centrifugal settling or filtering on the obtained reaction product.
Example 1
The embodiment provides a preparation method of terbium oxide-coated neodymium iron boron magnetic material composite powder, the preparation method is performed in a system device shown in fig. 1, and the preparation method comprises the following steps:
(1) introducing nitrogen as a protective gas into the fluidized bed reaction container to enable the neodymium iron boron particles with the particle size of 1-3 mu m to be in a fluidized state in a protective atmosphere;
(2) terbium source TbCl3Preheating to 200 ℃ and then sending the mixture into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the terbium source and the carrier gas is 100 mL/min; preheating the reaction gas to 40 ℃, and then conveying the reaction gas into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the reaction gas and the carrier gas is 90 mL/min; the terbium source and the reaction gas are synchronously introduced into the fluidized bed reaction device 2 and are mixed with the neodymium iron boron particles in a fluidized state, the mixing temperature is 650 ℃, and the mixing time is 60 min;
(3) and after the reaction is finished, performing gravity settling gas-solid separation to obtain the terbium oxide-coated neodymium iron boron magnetic material composite powder, wherein the terbium oxide content of the terbium oxide-coated neodymium iron boron magnetic material composite powder is 0.1 wt.%.
Example 2
The embodiment provides a preparation method of terbium oxide-coated neodymium iron boron magnetic material composite powder, the preparation method is performed in a system device shown in fig. 1, and the preparation method comprises the following steps:
(1) introducing argon gas into the fluidized bed reaction container as a protective gas to enable the neodymium iron boron particles with the particle size of 1-3 mu m to be in a fluidized state in a protective atmosphere;
(2) terbium source TbCl3Preheating to 300 ℃, and then sending the mixture into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the terbium source and the carrier gas is 200 mL/min; preheating the reaction gas to 60 ℃, and then conveying the reaction gas into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the reaction gas and the carrier gas is 120 mL/min; the terbium source and the reaction gas are synchronously introduced into the fluidized bed reaction device 2 and are mixed with the neodymium iron boron particles in a fluidized state, the mixing temperature is 700 ℃, and the mixing time is 60 min;
(3) and after the reaction is finished, performing centrifugal settling gas-solid separation to obtain the terbium oxide-coated neodymium iron boron magnetic material composite powder, wherein the terbium oxide content of the terbium oxide-coated neodymium iron boron magnetic material composite powder is 0.4 wt.%.
Fig. 2 is an SEM image of the terbium oxide-coated neodymium iron boron magnetic material composite powder prepared in this embodiment, and it can be seen from fig. 2 that a layer of terbium oxide film is uniformly coated on the surface of the neodymium iron boron powder.
Example 3
The embodiment provides a preparation method of terbium oxide-coated neodymium iron boron magnetic material composite powder, the preparation method is performed in a system device shown in fig. 1, and the preparation method comprises the following steps:
(1) introducing nitrogen as a protective gas into the fluidized bed reaction container to enable the neodymium iron boron particles with the particle size of 1-3 mu m to be in a fluidized state in a protective atmosphere;
(2) terbium source TbCl3Preheating to 400 ℃, and then sending the mixture into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the terbium source and the carrier gas is 300 mL/min; preheating the reaction gas to 60 ℃, and then conveying the reaction gas into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the reaction gas and the carrier gas is 120 mL/min; the terbium source and the reaction gas are synchronously introduced into the fluidized bed reaction device 2 and are mixed with the neodymium iron boron particles in a fluidized state, the mixing temperature is 800 ℃, and the mixing time is 60 min;
(3) and after the reaction is finished, performing gravity settling gas-solid separation to obtain the terbium oxide-coated neodymium iron boron magnetic material composite powder, wherein the terbium oxide content of the terbium oxide-coated neodymium iron boron magnetic material composite powder is 0.9 wt.%.
Example 4
The embodiment provides a preparation method of terbium oxide-coated neodymium iron boron magnetic material composite powder, the preparation method is performed in a system device shown in fig. 1, and the preparation method comprises the following steps:
(1) introducing nitrogen as a protective gas into the fluidized bed reaction container to enable the neodymium iron boron particles with the particle size of 1-3 mu m to be in a fluidized state in a protective atmosphere;
(2) terbium source TbCl3Preheating to 600 ℃, and then sending the mixture into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the terbium source and the carrier gas is 400 mL/min; preheating the reaction gas to 80 ℃, and then conveying the reaction gas into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the reaction gas and the carrier gas is 200 mL/min; the terbium source and the reaction gas are synchronously introduced into the fluidized bed reaction device 2 to be mixed with the neodymium iron boron particles in a fluidized stateThe temperature is 880 ℃, and the mixing time is 90 min;
(3) and after the reaction is finished, performing gravity settling gas-solid separation to obtain the terbium oxide-coated neodymium iron boron magnetic material composite powder, wherein the terbium oxide content of the terbium oxide-coated neodymium iron boron magnetic material composite powder is 2.4 wt.%.
Example 5
The embodiment provides a preparation method of terbium oxide-coated neodymium iron boron magnetic material composite powder, the preparation method is performed in a system device shown in fig. 1, and the preparation method comprises the following steps:
(1) introducing argon gas into the fluidized bed reaction container as a protective gas to enable the neodymium iron boron particles with the particle size of 1-3 mu m to be in a fluidized state in a protective atmosphere;
(2) terbium source TbCl3Preheating to 300 ℃, and then sending the mixture into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the terbium source and the carrier gas is 300 mL/min; preheating the reaction gas to 80 ℃, and then conveying the reaction gas into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the reaction gas and the carrier gas is 200 mL/min; the terbium source and the reaction gas are synchronously introduced into the fluidized bed reaction device 2 and are mixed with the neodymium iron boron particles in a fluidized state, the mixing temperature is 730 ℃, and the mixing time is 120 min;
(3) and after the reaction is finished, performing centrifugal settling gas-solid separation to obtain the terbium oxide-coated neodymium iron boron magnetic material composite powder, wherein the terbium oxide content of the terbium oxide-coated neodymium iron boron magnetic material composite powder is 1.9 wt.%.
Example 6
The embodiment provides a preparation method of terbium oxide-coated neodymium iron boron magnetic material composite powder, the preparation method is performed in a system device shown in fig. 1, and the preparation method comprises the following steps:
(1) introducing helium gas serving as protective gas into the fluidized bed reaction container to enable the neodymium iron boron particles with the particle size of 1-3 mu m to be in a fluidized state in protective atmosphere;
(2) terbium source TbCl3Preheating to 700 deg.C, and feeding into fluidized bed reactor 2 with carrier gas, wherein the mixed gas speed of terbium source and carrier gas is 500 mL/min; preheating the reaction gas to 80 ℃, and then conveying the reaction gas into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the reaction gas and the carrier gas is 500 mL/min; the terbium source and the reaction gas are synchronously introduced into the fluidized bed reaction device 2 and are mixed with the neodymium iron boron particles in a fluidized state, the mixing temperature is 830 ℃, and the mixing time is 60 min;
(3) and after the reaction is finished, filtering and carrying out gas-solid separation to obtain the terbium oxide-coated neodymium iron boron magnetic material composite powder, wherein the terbium oxide content of the terbium oxide-coated neodymium iron boron magnetic material composite powder is 1.6 wt.%.
Example 7
The embodiment provides a preparation method of terbium oxide-coated neodymium iron boron magnetic material composite powder, the preparation method is performed in a system device shown in fig. 1, and the preparation method comprises the following steps:
(1) introducing nitrogen as a protective gas into the fluidized bed reaction container to enable the neodymium iron boron particles with the particle size of 1-3 mu m to be in a fluidized state in a protective atmosphere;
(2) terbium source TbCl3Preheating to 300 ℃, and then sending the mixture into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the terbium source and the carrier gas is 600 mL/min; preheating the reaction gas to 60 ℃, and then conveying the reaction gas into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the reaction gas and the carrier gas is 300 mL/min; the terbium source and the reaction gas are synchronously introduced into the fluidized bed reaction device 2 and are mixed with the neodymium iron boron particles in a fluidized state, the mixing temperature is 700 ℃, and the mixing time is 50 min;
(3) and after the reaction is finished, performing gravity settling gas-solid separation to obtain the terbium oxide-coated neodymium iron boron magnetic material composite powder, wherein the terbium oxide content of the terbium oxide-coated neodymium iron boron magnetic material composite powder is 1.4 wt.%.
Example 8
The embodiment provides a preparation method of terbium oxide-coated neodymium iron boron magnetic material composite powder, the preparation method is performed in a system device shown in fig. 1, and the preparation method comprises the following steps:
(1) introducing argon gas into the fluidized bed reaction container as a protective gas to enable the neodymium iron boron particles with the particle size of 1-3 mu m to be in a fluidized state in a protective atmosphere;
(2) terbium source TbCl3Preheating to 600 ℃, and then sending the mixture into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the terbium source and the carrier gas is 200 mL/min; preheating the reaction gas to 30 ℃, and then conveying the reaction gas into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the reaction gas and the carrier gas is 150 mL/min; the terbium source and the reaction gas are synchronously introduced into the fluidized bed reaction device 2 and are mixed with the neodymium iron boron particles in a fluidized state, the mixing temperature is 680 ℃, and the mixing time is 30 min;
(3) and after the reaction is finished, performing centrifugal settling gas-solid separation to obtain the terbium oxide-coated neodymium iron boron magnetic material composite powder, wherein the terbium oxide content of the terbium oxide-coated neodymium iron boron magnetic material composite powder is 0.4 wt.%.
Example 9
The embodiment provides a preparation method of terbium oxide-coated neodymium iron boron magnetic material composite powder, the preparation method is performed in a system device shown in fig. 1, and the preparation method comprises the following steps:
(1) introducing helium gas serving as protective gas into the fluidized bed reaction container to enable the neodymium iron boron particles with the particle size of 1-3 mu m to be in a fluidized state in protective atmosphere;
(2) terbium source TbCl3Preheating to 800 ℃, and then sending the mixture into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the terbium source and the carrier gas is 200 mL/min; preheating the reaction gas to 80 ℃, and then conveying the reaction gas into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the reaction gas and the carrier gas is 200 mL/min; the terbium source and the reaction gas are synchronously introduced into the fluidized bed reaction device 2 and are mixed with the neodymium iron boron particles in a fluidized state, the mixing temperature is 790 ℃, and the mixing time is 60 min;
(3) and after the reaction is finished, filtering and carrying out gas-solid separation to obtain the terbium oxide-coated neodymium iron boron magnetic material composite powder, wherein the terbium oxide content of the terbium oxide-coated neodymium iron boron magnetic material composite powder is 2.1 wt.%.
Example 10
The embodiment provides a preparation method of terbium oxide-coated neodymium iron boron magnetic material composite powder, the preparation method is performed in a system device shown in fig. 1, and the preparation method comprises the following steps:
(1) introducing argon gas into the fluidized bed reaction container as a protective gas to enable the neodymium iron boron particles with the particle size of 1-3 mu m to be in a fluidized state in a protective atmosphere;
(2) terbium source TbCl3Preheating to 200 ℃ and then sending the mixture into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the terbium source and the carrier gas is 100 mL/min; preheating the reaction gas to 10 ℃, and then conveying the reaction gas into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the reaction gas and the carrier gas is 75 mL/min; the terbium source and the reaction gas are synchronously introduced into the fluidized bed reaction device 2 and are mixed with the neodymium iron boron particles in a fluidized state, the mixing temperature is 650 ℃, and the mixing time is 60 min;
(3) and after the reaction is finished, performing centrifugal settling gas-solid separation to obtain the terbium oxide-coated neodymium iron boron magnetic material composite powder, wherein the terbium oxide content of the terbium oxide-coated neodymium iron boron magnetic material composite powder is 0.1 wt.%.
Example 11
The embodiment provides a preparation method of terbium oxide-coated neodymium iron boron magnetic material composite powder, the preparation method is performed in a system device shown in fig. 1, and the preparation method comprises the following steps:
(1) introducing argon gas into the fluidized bed reaction container as a protective gas to enable the neodymium iron boron particles with the particle size of 1-3 mu m to be in a fluidized state in a protective atmosphere;
(2) terbium source TbCl3Preheating to 800 ℃, and then sending the mixture into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the terbium source and the carrier gas is 800 mL/min; preheating the reaction gas to 100 ℃, and then conveying the reaction gas into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the reaction gas and the carrier gas is 1500 mL/min; the terbium source and the reaction gas are synchronously introduced into the fluidized bed reaction device 2 and are mixed with the neodymium iron boron particles in a fluidized state, the mixing temperature is 850 ℃, and the mixing time is 1 min;
(3) and after the reaction is finished, performing centrifugal settling gas-solid separation to obtain the terbium oxide-coated neodymium iron boron magnetic material composite powder, wherein the terbium oxide content of the terbium oxide-coated neodymium iron boron magnetic material composite powder is 0.2 wt.%.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.
Claims (10)
1. A preparation method of terbium oxide-coated neodymium iron boron permanent magnet material composite powder is characterized by comprising the following steps:
and mixing the fluidized neodymium iron boron particles with the terbium source and the reaction gas for reaction, and carrying out gas-solid separation on the reaction product to obtain the terbium oxide coated neodymium iron boron permanent magnet material composite powder.
2. The preparation method according to claim 1, wherein the neodymium iron boron particles are subjected to fluidization treatment in a protective atmosphere to obtain the neodymium iron boron particles in a fluidized state;
preferably, the protective gas used in the protective atmosphere comprises at least one of nitrogen, argon or helium or a combination of two groups of nitrogen, argon or helium;
preferably, the particle size of the neodymium iron boron particles is 0.5-100 μm.
3. The method according to claim 1 or 2, wherein the mixing is performed by: respectively and independently introducing a terbium source and a reaction gas into a protective atmosphere in which the neodymium iron boron particles in a fluidized state are positioned;
preferably, the mixing temperature is 650-850 ℃;
preferably, the mixing time is more than or equal to 1 min.
4. The method of any one of claims 1-3, wherein the terbium source is TbCl3；
Preferably, the terbium source is preheated and then mixed for reaction;
preferably, the terbium source is preheated to 200-800 ℃;
preferably, the terbium source is sent into the reaction device by a carrier gas to carry out mixing reaction;
preferably, the gas velocity after the terbium source and the carrier gas are mixed is 100-800 mL/min.
5. The production method according to any one of claims 1 to 4, wherein the reaction gas is water vapor;
preferably, the reaction gas is preheated and then is mixed for reaction;
preferably, the reaction gas is preheated to 0-100 ℃;
preferably, the reaction gas is sent into the reaction device through a carrier gas to carry out mixing reaction;
preferably, the gas velocity after the reaction gas and the carrier gas are mixed is 75-1500 mL/min.
6. The process according to any one of claims 1 to 5, wherein the gas-solid separation comprises gravity settling, centrifugal settling or filtration.
7. The method according to any one of claims 1 to 6, wherein the method comprises:
the method comprises the following steps of (I) fluidizing neodymium iron boron particles with the particle size of 0.5-100 mu m in a protective atmosphere to obtain the neodymium iron boron particles in a fluidized state, wherein the protective atmosphere adopts protective gas comprising at least one of nitrogen, argon or helium or a combination of two groups of nitrogen, argon or helium;
(II) preheating the terbium source to 200-800 ℃, mixing the preheated terbium source with carrier gas, and introducing the mixture into a protective atmosphere in which the neodymium iron boron particles in a fluidized state are located at a gas speed of 100-800 mL/min; meanwhile, preheating the reaction gas to 0-100 ℃, mixing the preheated reaction gas with a carrier gas, and introducing the mixture into a protective atmosphere containing the neodymium-iron-boron particles in the fluidized state at a gas speed of 75-1500 mL/min, wherein the mixing temperature of the neodymium-iron-boron particles in the fluidized state, the terbium source and the reaction gas is 650-850 ℃, and the mixing time is more than or equal to 1 min;
and (III) after the reaction is finished, obtaining the terbium oxide-coated neodymium iron boron permanent magnet material composite powder by performing gravity settling, centrifugal settling or filtering on the obtained reaction product.
8. The terbium oxide-coated neodymium-iron-boron permanent magnet material composite powder prepared by the preparation method of any one of claims 1 to 7 is characterized in that the mass fraction of terbium oxide in the terbium oxide-coated neodymium-iron-boron permanent magnet material composite powder is 0.1 to 3.0 wt.%.
9. The system device for preparing terbium oxide-coated neodymium iron boron permanent magnet material composite powder according to claim 8, wherein the system device comprises a fluidized bed reaction device, the bottom of the fluidized bed reaction device is externally connected with a protective gas inlet pipe, the lower part of the reaction device is respectively and independently externally connected with a terbium source generating device and a reaction gas inlet pipe, and the upper part of the fluidized bed reaction device is externally connected with a storage bin.
10. The system device according to claim 9, wherein the top of the fluidized bed reactor is externally connected with a tail gas treatment device;
preferably, a vaporizing device is arranged on the reaction gas inlet pipe;
preferably, the fluidized bed reaction device is externally connected with a product collecting device.
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