CN108597710B - A kind of preparation method of samarium iron nitrogen magnetic nano-array - Google Patents

A kind of preparation method of samarium iron nitrogen magnetic nano-array Download PDF

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CN108597710B
CN108597710B CN201810329637.3A CN201810329637A CN108597710B CN 108597710 B CN108597710 B CN 108597710B CN 201810329637 A CN201810329637 A CN 201810329637A CN 108597710 B CN108597710 B CN 108597710B
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徐靖才
王攀峰
王新庆
洪波
金红晓
金顶峰
彭晓领
葛洪良
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DONGYANG DINGFENG MAGNETISM MATERIAL Co.,Ltd.
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    • 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
    • H01F1/059—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and Va elements, e.g. Sm2Fe17N2
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    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets

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Abstract

The present invention relates to a kind of preparation method of samarium iron nitrogen magnetic nano-array, which prepares samarium Fe nanowire array using square-wave pulse electrodeposition process under magnetic field using porous aluminas as template；Samarium Fe nanowire array is placed in heat-treatment furnace, high-purity argon gas is passed through with constant rate, anneal 1 ~ 5h at 500 ~ 700 DEG C；The argon hydrogen gaseous mixture containing 50% hydrogen is passed through with constant rate again, at 300 ~ 400 DEG C hydrogenate 10 ~ for 24 hours；Then high pure nitrogen is passed through with constant rate, 2 ~ 20h is nitrogenized at 400 ~ 500 DEG C, be down to room temperature, taken out sample and obtain samarium iron nitrogen magnetic nano-array.The samarium iron nitrogen magnetic nano-array that this method obtains is high-sequential nano-wire array, and the diameter of nano wire and the aperture of porous alumina formwork are consistent, and the length of nano wire is 1 ~ 50 μm；Samarium iron nitrogen magnetic nano-array magnetic energy product with higher and excellent magnetic anisotropy.

Description

A kind of preparation method of samarium iron nitrogen magnetic nano-array
Technical field
The present invention relates to a kind of preparation methods of samarium iron nitrogen magnetic nano-array, belong to field of material preparation.
Background technique
Permanent-magnet material is that have larger remanent magnetism, coercivity, magnetic energy product and can keep constant magnetic material once magnetization. Permanent-magnet material experienced carbon steel-aluminum nickel cobalt-ferrite-SmCo5-Sm2Co17-Nd2Fe14The several main developing stage of B.Wherein Rare earth permanent-magnetic material is the novel permanent magnetic material to grow up the 1960s, including first generation rare earth permanent magnet 1:5 type SmCo Alloy, second generation rare earth permanent magnet 2:17 type SmCo alloy；The first generation and second generation rare earth permanent-magnetic material all contain rare earth element Co, And Co be strategic materials, it is expensive, which greatly limits being widely used for they, are then developed third For Nd-Fe-B rare earth permanent-magnetic material.Compared with the first and second generation rare earth permanent-magnetic material, the magnetic property of Nd-Fe-B is excellent, dilute rapidly There is the good reputation of " magnetic king " in native permanent magnet market.But Nd-Fe-B itself is simultaneously imperfect, and disadvantage is equally obvious, such as content of rare earth Curie temperature is low etc. when high, poor corrosion resistance and high temperature.Therefore people actively seek rare earth permanent-magnetic material of new generation.Sm-Fe-N For in terms of the magnetic property, or from production cost for, all probably replace Nd-Fe-B, become people and expect Forth generation rare earth permanent-magnetic material.
Currently, the preparation method of Sm-Fe-N mainly has melt-quenching method (RQ), mechanical alloying method (MA), powder metallurgy Method (PM), hydrogenation-disproportionation-dehydrogenation-chemical combination method (HDDR) again.But with the high-tech development of modern humans society, electronic device Micromation, function it is compatible it is integrated require it is higher and higher.The Sm-Fe-N magnet that current process is prepared is difficult to meet high-end It needs, so being badly in need of the Sm-Fe-N magnetic Nano material that exploitation has high energy product and excellent magnetic anisotropy.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of samarium iron nitrogen magnetic nano-array, the samarium which obtains Iron nitrogen magnetic nano-array is high-sequential nano-wire array, and the diameter of nano wire and the aperture of porous alumina formwork are consistent, receive The length of rice noodles is 1~50 μm；Samarium iron nitrogen magnetic nano-array has high energy product and excellent magnetic anisotropy.
In order to achieve the above-mentioned object of the invention, specific steps of the invention are as follows:
1), porous alumina formwork prepares: choosing the alumina formwork that aperture is 100nm bilateral, magnetic control splashes at its back side The copper film that a layer thickness is 5 μm is penetrated, is successively dried after trimethylsilyl cyanide, ethyl alcohol, distilled water ultrasonic cleaning with spare；
2) samarium Fe nanowire battle array, the preparation of samarium Fe nanowire array: is prepared using square-wave pulse electrodeposition process under magnetic field Column: getting out alumina formwork as working electrode using the first step, and mercury electrode is to electrode, and Ag/AgCl electrode is auxiliary electrode, Square-wave pulse electro-deposition is carried out at a temperature of 30~50 DEG C after deposition liquid is added, deposition is completed will be more with the NaOH solution of 2mol/L The dissolution of porous aluminum oxide template, is then cleaned with ethyl alcohol and distilled water to neutrality；
The direction in the magnetic field is parallel with nanowire growth direction, and the size in magnetic field is 1~5T；
The solute of the deposition liquid are as follows: SmCl3·6H2O、FeCl2·4H2O、Na3C6H5O7·2H2O、H2C2O4、NaCl、 H3BO3And ascorbic acid, solvent are the water and ethylene glycol solution of 1:1；
The condition of the square-wave pulse electro-deposition are as follows: continue 60s in 0V, then moment adds the potential duration 30s of -1.3V Square-wave pulse electro-deposition certain time；
3) it, anneals: samarium Fe nanowire array being placed in heat-treatment furnace, high-purity argon gas is passed through with constant rate, 500 Anneal 1~5h at~700 DEG C；
4), hydrogenate: the argon hydrogen gaseous mixture containing 50% hydrogen is passed through with constant rate, at 300~400 DEG C hydrogenate 10~ 24h；
5) it, nitrogenizes: high pure nitrogen is passed through with constant rate, 2~20h is nitrogenized at 400~500 DEG C, room temperature is down to, takes Sample obtains samarium iron nitrogen magnetic nano-array out.
Technical effect: the present invention utilizes the process conditions in magnetic field, water and ethylene glycol mixed solvent and square-wave pulse electro-deposition, SmFe is set to be co-deposited in porous aluminas duct；The samarium Fe nanowire of nano-scale of the present invention is hydrogenated by annealing, is Nitridation provides advantage, obtains the higher samarium iron nitrogen magnetic nano-array of nitrogen content.
Specific embodiment
Here is that the present invention will be described in detail in conjunction with the embodiments, to more fully understand the purpose of the present invention, feature And advantage.Although the present invention is that the specific embodiment is combined to be described, it is not intended that the invention be limited to described tool Body embodiment.On the contrary, to may include in the claims in the present invention defined by embodiment in protection scope replace Generation, improvement and equivalent embodiment, belong to protection scope of the present invention.It can be by normal for the technological parameter not marked especially Rule technology carries out.
Specific steps of the invention are as follows:
1), porous alumina formwork prepares: choosing the alumina formwork that aperture is 100nm bilateral, magnetic control splashes at its back side The copper film that a layer thickness is 5 μm is penetrated, is successively dried after trimethylsilyl cyanide, ethyl alcohol, distilled water ultrasonic cleaning with spare；
2) samarium Fe nanowire battle array, the preparation of samarium Fe nanowire array: is prepared using square-wave pulse electrodeposition process under magnetic field Column: getting out alumina formwork as working electrode using the first step, and mercury electrode is to electrode, and Ag/AgCl electrode is auxiliary electrode, Square-wave pulse electro-deposition is carried out at a temperature of 30~50 DEG C after deposition liquid is added, deposition is completed will be more with the NaOH solution of 2mol/L The dissolution of porous aluminum oxide template, is then cleaned with ethyl alcohol and distilled water to neutrality；
The direction in the magnetic field is parallel with nanowire growth direction, and the size in magnetic field is 1~5T；
The solute of the deposition liquid are as follows: SmCl3·6H2O、FeCl2·4H2O、Na3C6H5O7·2H2O、H2C2O4、NaCl、 H3BO3And ascorbic acid, solvent are the water and ethylene glycol solution of 1:1；
The condition of the square-wave pulse electro-deposition are as follows: continue 60s in 0V, then moment adds the potential duration 30s of -1.3V Square-wave pulse electro-deposition certain time；
3) it, anneals: samarium Fe nanowire array being placed in heat-treatment furnace, high-purity argon gas is passed through with constant rate, 500 Anneal 1~5h at~700 DEG C；
4), hydrogenate: the argon hydrogen gaseous mixture containing 50% hydrogen is passed through with constant rate, at 300~400 DEG C hydrogenate 10~ 24h；
5) it, nitrogenizes: high pure nitrogen is passed through with constant rate, 2~20h is nitrogenized at 400~500 DEG C, room temperature is down to, takes Sample obtains samarium iron nitrogen magnetic nano-array out.
Embodiment 1:
Step are as follows:
1), porous alumina formwork prepares: choosing the alumina formwork that aperture is 100nm bilateral, magnetic control splashes at its back side The copper film that a layer thickness is 5 μm is penetrated, is successively dried after trimethylsilyl cyanide, ethyl alcohol, distilled water ultrasonic cleaning with spare；
2), the preparation of samarium Fe nanowire array: prepare deposition liquid, formula are as follows: 0.05mol/L FeCl2·4H2O、 0.3mol/L SmCl3·6H2O、0.5mol/L Na3C6H5O7·2H2O、0.5mol/L H2C2O4、0.03mol/L NaCl、 0.3mol/L H3BO3The water and ethylene glycol solution of 1:1 are dissolved in 0.3mol/L ascorbic acid, under the magnetic field of 1T, with the first step Alumina formwork is got out as working electrode, mercury electrode is to electrode, and Ag/AgCl electrode is auxiliary electrode, and temperature is added and is Continue 60s in square wave after 30 DEG C of deposition liquid for 0V, -1.3V continues to carry out pulse electrodeposition 50 circulations under 30s, and deposition completes use The NaOH solution of 2mol/L dissolves porous alumina formwork, is then cleaned with ethyl alcohol and distilled water to neutrality；
3) it, anneals: samarium Fe nanowire array being placed in heat-treatment furnace, high-purity argon gas is passed through with constant rate, 500 Anneal 5h at DEG C；
4) it, hydrogenates: the argon hydrogen gaseous mixture containing 50% hydrogen being passed through with constant rate, is hydrogenated for 24 hours at 300 DEG C；
5) it, nitrogenizes: high pure nitrogen being passed through with constant rate, nitrogenizes 20h at 400 DEG C, be down to room temperature, taking out sample is Obtain samarium iron nitrogen magnetic nano-array.
XRD and TEM characterization is carried out to sample prepared by embodiment 1, detects samarium iron nitrogen object phase, the pattern of samarium iron nitrogen For ordered nano linear array structure；To samarium iron nitrogen magnetic nanowires array carry out VSM test, find its magnetic energy product with higher and Excellent magnetic anisotropy.
Embodiment 2:
Step are as follows:
1), porous alumina formwork prepares: choosing the alumina formwork that aperture is 100nm bilateral, magnetic control splashes at its back side The copper film that a layer thickness is 5 μm is penetrated, is successively dried after trimethylsilyl cyanide, ethyl alcohol, distilled water ultrasonic cleaning with spare；
2), the preparation of samarium Fe nanowire array: prepare deposition liquid, formula are as follows: 0.1mol/L FeCl2·4H2O、 0.6mol/L SmCl3·6H2O、0.1mol/L Na3C6H5O7·2H2O、0.1mol/L H2C2O4、0.06mol/L NaCl、 0.6mol/L H3BO3The water and ethylene glycol solution of 1:1 are dissolved in 0.6mol/L ascorbic acid, under the magnetic field of 5T, with the first step Alumina formwork is got out as working electrode, mercury electrode is to electrode, and Ag/AgCl electrode is auxiliary electrode, and temperature is added and is Continue 60s in square wave after 30 DEG C of deposition liquid for 0V, -1.3V continues to carry out pulse electrodeposition 100 circulations under 30s, and deposition is completed Porous alumina formwork is dissolved with the NaOH solution of 2mol/L, is then cleaned with ethyl alcohol and distilled water to neutrality；
3) it, anneals: samarium Fe nanowire array being placed in heat-treatment furnace, high-purity argon gas is passed through with constant rate, 700 Anneal 7h at DEG C；
4) it, hydrogenates: the argon hydrogen gaseous mixture containing 50% hydrogen being passed through with constant rate, hydrogenates 10h at 400 DEG C；
5) it, nitrogenizes: high pure nitrogen being passed through with constant rate, nitrogenizes 2h at 500 DEG C, be down to room temperature, taking out sample is Obtain samarium iron nitrogen magnetic nano-array.
XRD and TEM characterization is carried out to sample prepared by embodiment 2, detects samarium iron nitrogen object phase, the pattern of samarium iron nitrogen For ordered nano linear array structure；To samarium iron nitrogen magnetic nanowires array carry out VSM test, find its magnetic energy product with higher and Excellent magnetic anisotropy.
Embodiment 3:
Step are as follows:
1), porous alumina formwork prepares: choosing the alumina formwork that aperture is 100nm bilateral, magnetic control splashes at its back side The copper film that a layer thickness is 5 μm is penetrated, is successively dried after trimethylsilyl cyanide, ethyl alcohol, distilled water ultrasonic cleaning with spare；
2), the preparation of samarium Fe nanowire array: prepare deposition liquid, formula are as follows: 0.1mol/L FeCl2·4H2O、 0.6mol/L SmCl3·6H2O、0.1mol/L Na3C6H5O7·2H2O、0.1mol/L H2C2O4、0.06mol/L NaCl、 0.6mol/L H3BO3The water and ethylene glycol solution of 1:1 are dissolved in 0.6mol/L ascorbic acid, under the magnetic field of 2T, with the first step Alumina formwork is got out as working electrode, mercury electrode is to electrode, and Ag/AgCl electrode is auxiliary electrode, and temperature is added and is Continue 60s in square wave after 50 DEG C of deposition liquid for 0V, -1.3V continues to carry out pulse electrodeposition 200 circulations under 30s, and deposition is completed Porous alumina formwork is dissolved with the NaOH solution of 2mol/L, is then cleaned with ethyl alcohol and distilled water to neutrality；
3) it, anneals: samarium Fe nanowire array being placed in heat-treatment furnace, high-purity argon gas is passed through with constant rate, 600 Anneal 3h at DEG C；
4) it, hydrogenates: the argon hydrogen gaseous mixture containing 50% hydrogen being passed through with constant rate, hydrogenates 18h at 350 DEG C；
5) it, nitrogenizes: high pure nitrogen being passed through with constant rate, nitrogenizes 10h at 450 DEG C, be down to room temperature, taking out sample is Obtain samarium iron nitrogen magnetic nano-array.
XRD and TEM characterization is carried out to sample prepared by embodiment 3, detects samarium iron nitrogen object phase, the pattern of samarium iron nitrogen For ordered nano linear array structure；To samarium iron nitrogen magnetic nanowires array carry out VSM test, find its magnetic energy product with higher and Excellent magnetic anisotropy.
Embodiment 4:
Step are as follows:
1), porous alumina formwork prepares: choosing the alumina formwork that aperture is 100nm bilateral, magnetic control splashes at its back side The copper film that a layer thickness is 5 μm is penetrated, is successively dried after trimethylsilyl cyanide, ethyl alcohol, distilled water ultrasonic cleaning with spare；
2), the preparation of samarium Fe nanowire array: prepare deposition liquid, formula are as follows: 0.05mol/L FeCl2·4H2O、 0.3mol/L SmCl3·6H2O、0.5mol/L Na3C6H5O7·2H2O、0.5mol/L H2C2O4、0.0 3mol/L NaCl、 0.3mol/LH3BO3The water and ethylene glycol solution of 1:1 are dissolved in 0.3mol/L ascorbic acid, under the magnetic field of 3T, with first step standard Alumina formwork is got ready as working electrode, mercury electrode is to electrode, and Ag/AgCl electrode is auxiliary electrode, and it is 40 that temperature, which is added, It in square wave is that 0V continues 60s after DEG C deposition liquid, -1.3V continues to carry out pulse electrodeposition 200 circulations under 30s, deposition completion use The NaOH solution of 2mol/L dissolves porous alumina formwork, is then cleaned with ethyl alcohol and distilled water to neutrality；
3) it, anneals: samarium Fe nanowire array being placed in heat-treatment furnace, high-purity argon gas is passed through with constant rate, 650 Anneal 2h at DEG C；
4) it, hydrogenates: the argon hydrogen gaseous mixture containing 50% hydrogen being passed through with constant rate, hydrogenates 20h at 400 DEG C；
5) it, nitrogenizes: high pure nitrogen being passed through with constant rate, nitrogenizes 17h at 450 DEG C, be down to room temperature, taking out sample is Obtain samarium iron nitrogen magnetic nano-array.
XRD and TEM characterization is carried out to sample prepared by embodiment 4, detects samarium iron nitrogen object phase, the pattern of samarium iron nitrogen For ordered nano linear array structure；To samarium iron nitrogen magnetic nanowires array carry out VSM test, find its magnetic energy product with higher and Excellent magnetic anisotropy.

Claims (2)

1. a kind of preparation method of samarium iron nitrogen magnetic nano-array, which is characterized in that comprise the steps of:
1), porous alumina formwork prepares: the alumina formwork that aperture is 100nm bilateral is chosen, in its back side magnetron sputtering one Layer is successively dried with a thickness of 5 μm of copper film after trimethylsilyl cyanide, ethyl alcohol, distilled water ultrasonic cleaning with spare；
2), the preparation of samarium Fe nanowire array: square-wave pulse electrodeposition process is used to prepare samarium Fe nanowire array under magnetic field: with The first step gets out alumina formwork as working electrode, and mercury electrode is to electrode, and Ag/AgCl electrode is auxiliary electrode, is added Square-wave pulse electro-deposition is carried out at a temperature of 30~50 DEG C after depositing liquid, deposition is completed to use the NaOH solution of 2mol/L by porous oxygen Change aluminum alloy pattern plate dissolution, is then cleaned with ethyl alcohol and distilled water to neutrality；
The direction in the magnetic field is parallel with nanowire growth direction, and the size in magnetic field is 1~5T；
The solute of the deposition liquid are as follows: SmCl3·6H2O、FeCl2·4H2O、Na3C6H5O7·2H2O、H2C2O4、NaCl、H3BO3 And ascorbic acid, solvent are the water and ethylene glycol solution of 1:1；
The condition of the square-wave pulse electro-deposition are as follows: continue 60s in 0V, then moment adds the side of the potential duration 30s of -1.3V Wave impulse electro-deposition certain time；
3) it, anneals: samarium Fe nanowire array being placed in heat-treatment furnace, high-purity argon gas is passed through with constant rate, 500~ Anneal 1~5h at 700 DEG C；
4), hydrogenate: the argon hydrogen gaseous mixture containing 50% hydrogen is passed through with constant rate, at 300~400 DEG C hydrogenate 10~for 24 hours；
5) it, nitrogenizes: high pure nitrogen is passed through with constant rate, 2~20h is nitrogenized at 400~500 DEG C, be down to room temperature, take out sample Product obtain samarium iron nitrogen magnetic nano-array.
2. a kind of preparation method of samarium iron nitrogen magnetic nano-array as described in claim 1, which is characterized in that samarium iron nitrogen magnetic nanometer Array is high-sequential nano-wire array, and the diameter of nano wire and the aperture of porous alumina formwork are consistent, the length of nano wire It is 1~50 μm；Samarium iron nitrogen magnetic nano-array has excellent magnetic property and magnetic anisotropy.
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RU2770919C1 (en) * 2021-06-07 2022-04-25 Федеральное государственное учреждение "Федеральный научно-исследовательский центр "Кристаллография и фотоника" Российской академии наук" Method for producing layered nanowires from ferromagnetic metals with a programmable structure and a device for its implementation
RU2774669C1 (en) * 2021-12-17 2022-06-21 Федеральное государственное бюджетное образовательное учреждение высшего образования "Российский химико-технологический университет имени Д.И. Менделеева" (РХТУ им. Д.И. Менделеева) Method for obtaining multilayer nanowires consisting of alternating layers of copper and nickel-copper alloy

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