CN105081338B - Method for preparing mono-dispersed NdFeB nano particles - Google Patents
Method for preparing mono-dispersed NdFeB nano particles Download PDFInfo
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Abstract
The invention provides a method for preparing mono-dispersed NdFeB nano particles. The method combines a high-temperature solvent thermal synthesis method with a high-temperature solid-phase reduction method and comprises the steps: firstly forming NdFeO3-Fe3O4-B2O3 polycrystalline oxide particles by utilizing the high-temperature solvent thermal synthesis; mixing the NdFeO3-Fe3O4-B2O3 polycrystalline oxide particles with abundant calcium element precursors and surface active agents to have a high-temperature solvent thermal reaction to obtain CaO-coated NdFeO3-Fe3O4-B2O3 polycrystalline oxide particles; finally mixing the CaO-coated NdFeO3-Fe3O4-B2O3 polycrystalline oxide particles with abundant metallic calcium particles and tabletting the mixture, and performing high-temperature reduction on the tablets to obtain Nd2Fe14B nano particles with core shell structure. Based on experiments, the method for preparing the mono-dispersed NdFeB nano particles can prepare monocrystalline NdFeB nano particles with the uniform size and high dispersity; the size of the monocrystalline NdFeB nano particles ranges within 50-100 nm; therefore, the method for preparing the mono-dispersed NdFeB nano particles has wide application prospect in the technical fields related to magnetofluids, magnetic recording and biomedicine.
Description
Technical field
The invention belongs to magnetic Nano material technical field, and in particular to a kind of preparation of single dispersing Nd-Fe-B nano particle
Method.
Background technology
Neodymium-iron-boron magnetic material is extensively quoted in numerous areas.At present, neodymium is prepared by traditional physical method
Fe-Mn magnetism material early has been achieved with extensive industrialization, but the generally block that prepared using these physical methods or
Person's powder body material, its crystallite dimension is micron or submicron.
Comparatively, chemical method has unique advantage in terms of nano materials, so far, in synthesis metal
The existing numerous studies of oxide, simple substance and alloy aspect and report.However, when nanoparticle when containing rare earth element, due to dilute
Earth elements have high reduction potential, and transition elements obvious difference, therefore the uniform Multi-element nano particle of prepared composition
Difficulty it is very big, for example, the controllable monodispersed Nd of granularity is not also chemically prepared up to now2Fe14B nanoparticles
Son.
The content of the invention
The technical purpose of the present invention is to provide a kind of preparation method of single dispersing Nd-Fe-B nano particle, and the method is simply easy
OK, can be obtained that grain size is uniform, the Nd-Fe-B nano particle of high degree of dispersion.
To realize above-mentioned technical purpose, the present inventor after many experiments exploration, by high-temperature solvent process for thermosynthesizing with
High temperature solid-state method of reducing combines, and Nd of the monodispersed, size in 50～100nm has been obtained2Fe14B nano-particle.
Technical scheme is as follows：A kind of preparation method of single dispersing Nd-Fe-B nano particle, comprises the steps：
(1) under inert gas shielding, ferrum, neodymium, the presoma of boron element, organic complexing agent and organic solvent are uniformly mixed
Close, be heated to 80～160 DEG C, make organic complexing agent that complex reaction occur with metal precursor；
(2) surfactant is added in the product that step (1) is obtained and presoma decomposition temperature is heated to, then
Room temperature is cooled to, NdFeO is obtained3-Fe3O4-B2O3Polycrystalline oxide particle, washs and is scattered in normal hexane, obtains polycrystalline oxygen
Compound particle solution；
(3) under inert gas shielding, calcium constituent presoma, surfactant are uniformly mixed with organic solvent, is heated to
Pre-reaction temperature, makes calcium constituent presoma decompose and reacts and combined with surfactant molecule；It is subsequently adding step (2) to obtain
The polycrystalline oxide particle solution for arriving, is heated to 250～350 DEG C, is subsequently cooled to room temperature, separates solid product and is dried, and obtains
To NdFeBOX@CaO particles, the i.e. NdFeO of CaO claddings3-Fe3O4-B2O3Polycrystalline oxide particle；
Described calcium constituent presoma and NdFeBOXThe mol ratio of polycrystalline oxide particle is more than or equal to 3:1, preferably
More than or equal to 5:1；
(4) under inert gas shielding, by NdFeBOX@CaO particles are compressed to block after mixing with calcium metal granule, so
After be put into heating furnace, 700～1000 DEG C are warming up in reducibility gas atmosphere, room temperature, broken, washing, dry is cooled to afterwards
Nd is obtained after dry2Fe14B@CaO product particles；
Described calcium granule and NdFeBOXThe mol ratio of@CaO particles is more than or equal to 3:1, preferably greater than or equal to 5:
1。
In described step (1), ferrum, neodymium, the presoma of boron element are not limited, such as including the nothing of the ferrum, neodymium or boron element
Machine salt, acid and metal-organic complex.For example, the presoma of ferrum element includes but is not limited to ferric acetyl acetonade, iron chloride, nitre
The inorganic salts such as sour ferrum or metal-organic complex；The presoma of neodymium element includes the inorganic salts such as acetic acid neodymium, neodymium nitrate or has
Organic metal complex；The presoma of boron element includes inorganic salt or the boron-containing compounds such as boric acid, boron oxide.
In described step (1), organic complexing agent can occur complex reaction with the presoma of ferrum, neodymium, boron element, and this has
Machine chelating agent is not limited, for example, can be long chain organic molecules, including long chain acid, amine, fat, ester and nitrile compounds etc., specifically
It can be one or more the mixing in oleyl amine, Oleic acid etc..
In described step (1), organic solvent is not limited, including long-chain Organic substance, the hydrocarbon of organic long-chain, alcohol, acid, amine, ether
And esters etc..
Preferably, in described step (1), the presoma of neodymium element is acetic acid neodymium, and organic complexing agent is oleyl amine；Ferrum unit
The presoma of element is ferric acetyl acetonade, and organic complexing agent is Oleic acid.
Preferably, in described step (1), Nd elements and the mol ratio of Fe elements are 0.6 in metal precursor：1.2,
Most preferably 0.88.
Preferably, in described step (1), heating-up temperature is 100～150 DEG C, most preferably 120 DEG C.
Preferably, in described step (1), the response time is no less than 2 hours.
In described step (2), surfactant is used to prevent nanoparticle from reuniting, and the surfactant is not limited, including
Cationic surfactant, anion surfactant and nonionic surfactant etc., such as cetyl trimethyl bromination
Ammonium, sodium lauryl sulphate etc..
Preferably, in described step (2), heating-up temperature is 250～350 DEG C, most preferably 300 DEG C.
Preferably, in described step (2), the response time is 0.5～1.5 hour.
In described step (3), the presoma of calcium constituent includes but is not limited to the inorganic salt of calcium constituent, sour and organic
Metal complex etc..The inorganic salt of described calcium constituent includes but is not limited to any one in calcium acetate, calcium chloride, calcium nitrate etc.
Compound.
Preferably, in described step (3), pre-reaction temperature is 100～200 DEG C, more preferably 160 DEG C, during reaction
Between be 0.5 hour～1.5 hours.
In described step (4), reducibility gas atmosphere is not limited, including hydrogen etc..Preferably, described reproducibility gas
Body atmosphere includes noble gases.For example, described reducibility gas atmosphere by 85%～95% noble gases and 5%～
15% hydrogen composition.
Preferably, in described step (4), being warming up to temperature and being not less than 800 DEG C, the reduction reaction time is more than or equal to
2 hours.
In sum, the present invention combines high-temperature solvent process for thermosynthesizing and high temperature solid-state method of reducing, has the advantage that：
(1) high-temperature solvent process for thermosynthesizing can synthesize the homogeneous single dispersing oxide nano-particles of size composition.High temperature
Solid-phase reduction process being capable of effective reduced oxide.The present invention combines the two, first by high-temperature solvent thermal synthesis
NdFeO3-Fe3O4-B2O3Polycrystalline oxide particle；Then with enough calcium constituent presoma (calcium constituent presoma and NdFeBOX
The mol ratio of polycrystalline oxide particle is more than or equal to 3:1), the mixing such as surfactant, Jing after high-temperature solvent thermal response, obtains
The NdFeO of CaO claddings3-Fe3O4-B2O3Polycrystalline oxide particle；Finally, the NdFeO for CaO being coated3-Fe3O4-B2O3Polycrystalline oxygen
Compound particle and enough calcium metal granule (calcium granule and NdFeBOXThe mol ratio of@CaO particles is more than or equal to 3:1) mix
Tabletting, Jing high temperature reductions obtain the Nd with nucleocapsid structure2Fe14B nanoparticles, wherein kernel are Nd2Fe14B, CaO or carbon
Sour calcium is coated on kernel outer layer for shell.Or Calcium Carbonate is covered in Nd2Fe14B kernels periphery.
(2) preparation method of the invention design is ingenious, and the NdFeO of cladding CaO is prepared first3-Fe3O4-B2O3Polycrystalline is aoxidized
Thing particle, CaO can be effectively isolated polycrystalline oxide particle in the structure, and oxygen element biography is played during solid phase reduction
The function served as bridge passed, so as to the Nd for finally giving CaO or Calcium Carbonate is shell cladding2Fe14B nanoparticles, aoxidize in the structure
Calcium or Calcium Carbonate can play a part of certain isolation air, protection particle.
(3) as advantageous measure, when in oxide nano-particles synthetic system, it is vinegar to select when the presoma of neodymium element
Sour neodymium, organic complexing agent selects to be oleyl amine that the presoma of ferrum element selects to be ferric acetyl acetonade that organic complexing agent selects to be Oleic acid
When, acetic acid neodymium and oleyl amine are combined and generate oleyl amine neodymium, and ferric acetyl acetonade and Oleic acid are combined and generate iron oleate, anti-so as to significantly improve
The heat stability of thing is answered, reaction rate is reduced, the uniform multiple grain of decomposition reaction forming component can be effectively cooperateed with
Son.
(4) in preparation method of the invention, by adjusting NdFeBOXThe size and composition of polycrystalline oxide particle being capable of essence
The true corresponding size and composition of control final product particle, so as to further for structure Nanocomposite magnet provide it is good forever
Magnetic cell.
It is experimentally confirmed that size uniform can be obtained using the preparation method of the present invention, the monocrystalline neodymium iron boron of high degree of dispersion is received
Rice corpuscles, in 50～100nm, the magnetic nano-particle is in correlation techniques such as magnetic fluid, magnetic recording and bio-medicals for its size
Field is with a wide range of applications.
Description of the drawings
Fig. 1 is the X ray diffracting spectrum of Nd-Fe-B nano particle obtained in the embodiment of the present invention 1；
Fig. 2 a are NdFeBO obtained in the embodiment of the present invention 1XThe transmission electron microscope photo of@CaO particles；
Fig. 2 b are the transmission electron microscope photos of nanoparticle obtained in the embodiment of the present invention 1；
Fig. 3 is the selected diffraction collection of illustrative plates of Nd-Fe-B nano particle obtained in the embodiment of the present invention 1；
Fig. 4 is the hysteresis curve figure at room temperature of Nd-Fe-B nano particle obtained in the embodiment of the present invention 1；
Fig. 5 is the transmission electron microscope photo of Nd-Fe-B nano particle obtained in the embodiment of the present invention 2.
Specific embodiment
Below in conjunction with the accompanying drawings embodiment is described in further detail to the present invention, it should be pointed out that described below is implemented
Example is intended to be easy to the understanding of the present invention, and does not play any restriction effect to it.
Embodiment 1：
(1) 0.8g acetic acid neodymiums, 1.0g ferric acetyl acetonades and 0.3g boric acid are dissolved in into 8mL Oleic acid, 10mL oleyl amines and 25mL ten
Eight alkene, mixed solution is positioned in 250mL four-hole boiling flasks, and is passed through argon as reducing atmosphere, arranges reflux cooling device.
Magnetic agitation is carried out to mixture, 120 DEG C is heated to and is incubated 1 hour；
(2) add dissolved with 1.0g cetyl trimethylammonium bromide (CTAB) in the product that step (1) is obtained
Methanol solution 15mL simultaneously continues insulation 1 hour.Afterwards, the mixed solution is heated to 300 DEG C, insulation removes thermal source after 1.5 hours
System is set to be cooled to room temperature.Then, add isopropanol, 10000rpm that 10 minutes isolated polycrystalline oxide nanoparticles are centrifuged
Son, is cleaned multiple times after centrifugation with normal hexane, and polycrystalline oxide nanoparticle is dispersed in normal hexane, is obtained polycrystalline oxide and is received
Rice corpuscles solution.
(3) being passed through argon and under conditions of being stirred vigorously, 0.3g calcium acetates, 0.3g cetyl trimethylammonium bromide and
0.2g boric acid is dissolved in 50mL benzyl ether, the polycrystalline oxide nano-particle solution for adding 60mg steps (2) to obtain, after stirring
It is heated to 160 DEG C and is incubated 1 hour, is brought rapidly up afterwards to 300 DEG C.After reaction terminates, remove thermal source, cooling body and be tied to room
Temperature, isopropanol are separated after solid product, and centrifugation is cleaned multiple times with normal hexane, and (centrifugation rate is 10000rpm, during centrifugal treating
Between be 10 minutes), the solid product for obtaining in atmosphere 80 DEG C drying, obtain NdFeBOX@CaO particles.
(4) NdFeBO for obtaining step (3)X@CaO particles in argon glove box with 0.3g calcium granule mixed pressuring plates,
Kept for 5 minutes under 200MPa.It is transferred to after the block for obtaining is put in quartz boat and is connected with reducing atmosphere (reproducibility gas
Atmosphere is made up of 92% argon and 8% hydrogen) tube furnace in, be rapidly heated to 800 DEG C and be incubated 2 hours, it is then natural
It is cooled to room temperature, (wherein, hydrochloric acid solution and the volume ratio of ethanol are 1 with the mixed liquor of 0.5M hydrochloric acid solutions and ethanol：1) wash
Repeatedly, finally it is vacuum dried, obtains nanoparticle powder and be stored in glove box.
Fig. 1 is the X ray diffracting spectrum of nanoparticle obtained above.From figure 1 it appears that the nanoparticle sample
Principal phase be Nd2Fe14B, also including a small amount of CaO and CaCO3, without other impurities.
Fig. 2 a are NdFeBO obtained in above-mentioned steps (3)XThe transmission electron microscope photo of@CaO particles.Fig. 2 b are step (4) systems
Obtain the transmission electron microscope photo of nanoparticle.
NdFeBO obtained in above-mentioned steps (3) is can be seen that from Fig. 2 aXThe size of@CaO polycrystalline oxide nanoparticles exists
80nm or so, and be in agglomeration between particle due to the presence of excessive oxidation calcium particle with typical nucleocapsid structure.
Can be seen that using nano-particles size obtained in said method in 100nm or so from Fig. 2 b, and dispersibility is good
Good, with nucleocapsid structure, its kernel is Nd2Fe14B, outer layer is fine and close calcium oxide or Calcium Carbonate protective layer.
Following table is the elementary analysiss result (EDS) of nanoparticle obtained above.
The nanoparticle that can be seen that the nucleocapsid structure from the table has close 1/7 Nd/Fe atomic ratios, additionally
There is the compositions such as calcium and oxygen, belong to shell composition.
Fig. 3 is the selection diffracting spectrum of nanoparticle obtained above.From figure 3, it can be seen that for individual particle
Diffraction shows that it has typical tetragonal phase, belongs to Nd2Fe14B, and for monocrystalline.
Fig. 4 is Nd obtained above2Fe14B nanoparticles hysteresis curve figure at room temperature.Figure 4, it is seen that should
Nd2Fe14B nanoparticles have obvious ferromagnetic characteristics, and room temperature coercivity is 400Oe, and saturation magnetization is 25emu/g.
Embodiment 2：
The present embodiment is substantially substantially the same manner as Example 1, except that by adjusting surfactant in step (2)
The addition of CTAB, controls the granular size of polycrystalline oxide nanometer example, specially：Reduce CTAB additions, from 1.0g to
0.6g, can cause oxide particle size to increase to 200nm or so, and not affect the ratio of wherein two kinds of elements of neodymium ferrum,
Still remain in 1:7 or so.With calcium oxide parcel and after high temperature reduction annealing, granule is still tied with typical nucleocapsid
Structure, preferable dispersibility and similar magnetic performance.
Fig. 5 is the transmission electron microscope photo of above-mentioned prepared nanoparticle.It can be seen that obtained nano-particles size is in 200nm
Left and right, and with nucleocapsid structure, its kernel is Nd2Fe14B, outer layer is fine and close calcium oxide or Calcium Carbonate protective layer.
Embodiment described above has been described in detail to technical scheme, it should be understood that the above is only
For the specific embodiment of the present invention, the present invention is not limited to, all any modifications made in the spirit of the present invention,
Supplementary or similar fashion replacement etc., should be included within the scope of the present invention.
Claims (17)
1. a kind of preparation method of single dispersing Nd-Fe-B nano particle, is characterized in that：Comprise the steps：
(1) under inert gas shielding, ferrum, neodymium, the presoma of boron element, organic complexing agent are uniformly mixed with organic solvent, plus
Heat makes organic complexing agent that complex reaction occur with the presoma of ferrum, neodymium, boron element to 80～160 DEG C；
(2) surfactant is added in the product that step (1) is obtained and presoma decomposition temperature is heated to, is then cooled down
To room temperature, NdFeO is obtained3-Fe3O4-B2O3Polycrystalline oxide particle, washs and is scattered in normal hexane, obtains polycrystalline oxide
Particle solution；
(3) under inert gas shielding, calcium constituent presoma, surfactant are uniformly mixed with organic solvent, is first heated to
Pre-reaction temperature, makes calcium constituent presoma decompose and reacts and combined with surfactant molecule；It is subsequently adding step (2) to obtain
The polycrystalline oxide particle solution for arriving, is heated to 250～350 DEG C, is then cooled to room temperature, separates solid product and is dried, and obtains
To NdFeBOX@CaO particles；
Described calcium constituent presoma and NdFeBOXThe mass ratio of polycrystalline oxide particle is more than or equal to 3:1；(4) in indifferent gas
Under body protection, by NdFeBOX@CaO particles are compressed to block after mixing with calcium metal granule, are then placed in heating furnace, in reduction
Property atmosphere in be warming up to 700～1000 DEG C, room temperature, broken, washing are cooled to afterwards, be dried after obtain Nd2Fe14B@CaO
Product particles；
Described calcium granule and NdFeBOXThe mol ratio of@CaO particles is more than or equal to 3:1.
2. the preparation method of single dispersing Nd-Fe-B nano particle as claimed in claim 1, is characterized in that：Before described calcium constituent
Drive body and NdFeBOXThe mass ratio of polycrystalline oxide particle is more than or equal to 5:1.
3. the preparation method of single dispersing Nd-Fe-B nano particle as claimed in claim 1, is characterized in that：Described calcium granule with
NdFeBOXThe mol ratio of@CaO particles is more than or equal to 5:1.
4. the preparation method of single dispersing Nd-Fe-B nano particle as claimed in claim 1, is characterized in that：Described step (1)
In, ferrum, neodymium, the presoma of boron element are inorganic salt, acid and the metal-organic complexs of the ferrum, neodymium or boron element.
5. the preparation method of single dispersing Nd-Fe-B nano particle as claimed in claim 1, is characterized in that：Described step (1)
In, organic complexing agent is long chain acid, amine, fat, ester and nitrile compounds.
6. the preparation method of single dispersing Nd-Fe-B nano particle as claimed in claim 3, is characterized in that：Described step (1)
In, organic complexing agent is one or two the mixing in oleyl amine, Oleic acid.
7. the preparation method of single dispersing Nd-Fe-B nano particle as claimed in claim 1, is characterized in that：Described step (1)
In, the presoma of neodymium element is acetic acid neodymium, and the presoma of ferrum element is ferric acetyl acetonade, and organic complexing agent is Oleic acid and oleyl amine
Mixture.
8. the preparation method of single dispersing Nd-Fe-B nano particle as claimed in claim 1, is characterized in that：Described step (1)
In, the mol ratio of Nd elements and Fe elements is 0.6-1.2 in ferrum, neodymium, the presoma of boron element.
9. the preparation method of single dispersing Nd-Fe-B nano particle as claimed in claim 8, is characterized in that：Ferrum, neodymium, boron element
Nd elements and the mol ratio of Fe elements are 0.88 in presoma.
10. the preparation method of the single dispersing Nd-Fe-B nano particle as described in any claim in claim 1 to 9, it is special
Levying is：In described step (1), heating-up temperature is 100～150 DEG C.
The preparation method of 11. single dispersing Nd-Fe-B nano particles as claimed in claim 10, is characterized in that：Described step
(1) in, heating-up temperature is 120 DEG C.
The preparation method of the single dispersing Nd-Fe-B nano particle in 12. such as claim 1 to 9 as described in any claim, it is special
Levying is：In described step (2), heating-up temperature is 250～350 DEG C.
The preparation method of 13. single dispersing Nd-Fe-B nano particles as claimed in claim 12, is characterized in that：Described step
(2) in, heating-up temperature is 300 DEG C.
The preparation method of the single dispersing Nd-Fe-B nano particle in 14. such as claim 1 to 9 as described in any claim, it is special
Levying is：In described step (3), pre-reaction temperature is 100～200 DEG C, and the response time is 0.5 hour～1.5 hours.
The preparation method of 15. single dispersing Nd-Fe-B nano particles as claimed in claim 14, is characterized in that：Described step
(3) in, pre-reaction temperature is 160 DEG C.
The preparation method of the single dispersing Nd-Fe-B nano particle in 16. such as claim 1 to 9 as described in any claim, it is special
Levying is：In described step (4), reducibility gas atmosphere is hydrogen.
The preparation method of 17. single dispersing Nd-Fe-B nano particles as claimed in claim 16, is characterized in that：Described step
(4) in, reducibility gas atmosphere includes noble gases.
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| CN106782981B (en) * | 2017-02-21 | 2018-12-21 | 济南大学 | A kind of composite magnetic particle and preparation method thereof based on neodymium iron boron |
| KR102092327B1 (en) | 2017-11-28 | 2020-03-23 | 주식회사 엘지화학 | Manufacturing method of magnetic powder and magnetic powder |
| CN108806960B (en) * | 2018-04-24 | 2020-07-17 | 沈阳工业大学 | Liquid phase combination method for preparing neodymium iron boron permanent magnetic nano particles |
| CN110146357B (en) * | 2019-05-23 | 2020-04-14 | 东北大学 | Preparation method of vanadium slag/calcium oxide diffusion couple |
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| CN1174104A (en) * | 1997-05-22 | 1998-02-25 | 南开大学 | Co-precipitation reduction diffusion process for preparing neodymium-boron permanent-magnet alloy |
| CN103106991A (en) * | 2013-01-30 | 2013-05-15 | 浙江大学 | High-coercivity and high-stability neodymium iron boron magnet and preparation method based on crystal boundary reconstruction |
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| JP3247839B2 (en) * | 1996-09-18 | 2002-01-21 | 信越化学工業株式会社 | Manufacturing method of rare earth permanent magnet |
| KR100374706B1 (en) * | 2000-05-26 | 2003-03-04 | 한국기계연구원 | Production method of Fine powder of Nd-Fe-B Alloy |
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| CN1174104A (en) * | 1997-05-22 | 1998-02-25 | 南开大学 | Co-precipitation reduction diffusion process for preparing neodymium-boron permanent-magnet alloy |
| CN103106991A (en) * | 2013-01-30 | 2013-05-15 | 浙江大学 | High-coercivity and high-stability neodymium iron boron magnet and preparation method based on crystal boundary reconstruction |
| CN103317142A (en) * | 2013-07-09 | 2013-09-25 | 中国石油大学(华东) | Method for preparing nanometer double-phase neodymium-iron-boron magnetic powder according to sol-gel method |
| CN103774036A (en) * | 2014-01-13 | 2014-05-07 | 宁波金科磁业有限公司 | Method for preparing NdFeB (Neodymium Iron Boron) via nano diffusion-reduction method |
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