CN108597710A - 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 PDFInfo
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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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Abstract
The present invention relates to a kind of preparation method of samarium iron nitrogen magnetic nano-array, which prepares samarium Fe nanowire array under magnetic field using Woelm Alumina as template using square-wave pulse electrodeposition process；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 is consistent with the aperture of porous alumina formwork, and the length of nano wire is 1 ~ 50 μm；Samarium iron nitrogen magnetic nano-array has higher magnetic energy product and excellent magnetic anisotropy.
Description
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 technology
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 in the 60's of 20th century, including first generation rare earth permanent magnet 1：5
Type SmCo alloys, second generation rare earth permanent magnet 2：17 type SmCo alloys；The first generation and second generation rare earth permanent-magnetic material all contain
Have a rare earth element Co, and Co be strategic materials, it is expensive, which greatly limits being widely used for they, in
It is to be developed third generation Nd-Fe-B rare earth permanent-magnetic materials.Compared with the first and second generation rare earth permanent-magnetic material, the magnetic of Nd-Fe-B
It has excellent performance, there is the good reputation of " magnetic king " in rapid rare-earth permanent magnet market.But Nd-Fe-B itself is simultaneously imperfect, and disadvantage is equally bright
It is aobvious, such as Curie temperature is low when content of rare earth height, poor corrosion resistance and high temperature.Therefore people actively seek rare earth permanent magnet of new generation
Material.Sm-Fe-N no matter in terms of the magnetic property, or from production cost for, all probably replace Nd-Fe-
B becomes the forth generation rare earth permanent-magnetic material of people's expectation.
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 compatibility it is integrated require it is higher and higher.The Sm-Fe-N magnets that current process is prepared are difficult to meet high-end
It needs, so being badly in need of Sm-Fe-N magnetic Nano material of the exploitation with high energy product and excellent magnetic anisotropy.
Invention content
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 is consistent with the aperture of porous alumina formwork, receives
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, it is of the invention the specific steps are：
1）, porous alumina formwork prepare：The alumina formwork that aperture is 100nm bilaterals is chosen, in its back side magnetron sputtering one
The copper film that layer thickness is 5 μm is dried after trimethylsilyl cyanide, ethyl alcohol, distilled water are cleaned by ultrasonic with spare successively；
2）, samarium Fe nanowire array preparation：Samarium Fe nanowire array is prepared using square-wave pulse electrodeposition process under magnetic field：With
The first step gets out alumina formwork as working electrode, and mercury electrode is to electrode, and Ag/AgCl electrodes are auxiliary electrode, are added
It deposits and carries out square-wave pulse electro-deposition after liquid at a temperature of 30 ~ 50 DEG C, deposition is completed porous oxidation with the NaOH solution of 2M/L
Aluminum alloy pattern plate dissolves, and is then cleaned to neutrality with ethyl alcohol and distilled water；
The direction in the magnetic field is parallel with nanowire growth direction, and the size in magnetic field is 1 ~ 5 T；
The solute of the deposition liquid is：SmCl3•6H2O、FeCl2•4H2O、Na3C6H5O7•2H2O、 H2C2O4、NaCl、H3BO3
And ascorbic acid, solvent 1:1 water and ethylene glycol solution；
The condition of the square-wave pulse electro-deposition is：Continue 60 s in 0 V, then moment add 30 s of potential duration of -1.3 V
Square-wave pulse electro-deposition certain time；
3）, annealing：Samarium Fe nanowire array is placed in heat-treatment furnace, high-purity argon gas is passed through with constant rate, 500 ~ 700
Anneal 1 ~ 5h at DEG C；
4）, hydrogenation：Be passed through the argon hydrogen gaseous mixture containing 50% hydrogen with constant rate, at 300 ~ 400 DEG C hydrogenate 10 ~ for 24 hours；
5）, nitridation：It is passed through high pure nitrogen with constant rate, 2 ~ 20h is nitrogenized at 400 ~ 500 DEG C, is down to room temperature, takes out sample
Obtain samarium iron nitrogen magnetic nano-array.
Technique effect：The present invention using magnetic field, water and ethylene glycol mixed solvent and square-wave pulse electro-deposition process conditions,
SmFe is set to be co-deposited in Woelm Alumina 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 implementation mode
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 described in conjunction with the specific embodiment, 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 domain 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.
The present invention the specific steps are：
1）, porous alumina formwork prepare：The alumina formwork that aperture is 100nm bilaterals is chosen, in its back side magnetron sputtering one
The copper film that layer thickness is 5 μm is dried after trimethylsilyl cyanide, ethyl alcohol, distilled water are cleaned by ultrasonic with spare successively；
2）, samarium Fe nanowire array preparation：Samarium Fe nanowire array is prepared using square-wave pulse electrodeposition process under magnetic field：With
The first step gets out alumina formwork as working electrode, and mercury electrode is to electrode, and Ag/AgCl electrodes are auxiliary electrode, are added
It deposits and carries out square-wave pulse electro-deposition after liquid at a temperature of 30 ~ 50 DEG C, deposition is completed porous oxidation with the NaOH solution of 2M/L
Aluminum alloy pattern plate dissolves, and is then cleaned to neutrality with ethyl alcohol and distilled water；
The direction in the magnetic field is parallel with nanowire growth direction, and the size in magnetic field is 1 ~ 5 T；
The solute of the deposition liquid is：SmCl3•6H2O、FeCl2•4H2O、Na3C6H5O7•2H2O、 H2C2O4、NaCl、H3BO3
And ascorbic acid, solvent 1:1 water and ethylene glycol solution；
The condition of the square-wave pulse electro-deposition is：Continue 60 s in 0 V, then moment add 30 s of potential duration of -1.3 V
Square-wave pulse electro-deposition certain time；
3）, annealing：Samarium Fe nanowire array is placed in heat-treatment furnace, high-purity argon gas is passed through with constant rate, 500 ~ 700
Anneal 1 ~ 5h at DEG C；
4）, hydrogenation：Be passed through the argon hydrogen gaseous mixture containing 50% hydrogen with constant rate, at 300 ~ 400 DEG C hydrogenate 10 ~ for 24 hours；
5）, nitridation：It is passed through high pure nitrogen with constant rate, 2 ~ 20h is nitrogenized at 400 ~ 500 DEG C, is down to room temperature, takes out sample
Obtain samarium iron nitrogen magnetic nano-array.
Embodiment 1：
Step is：
1）, porous alumina formwork prepare：The alumina formwork that aperture is 100nm bilaterals is chosen, in its back side magnetron sputtering one
The copper film that layer thickness is 5 μm is dried after trimethylsilyl cyanide, ethyl alcohol, distilled water are cleaned by ultrasonic with spare successively；
2）, samarium Fe nanowire array preparation：Prepare deposition liquid, formula is：0.05 mol/L FeCl2•4H2O、0.3
mol/L SmCl3•6H2O、0.5 mol/L Na3C6H5O7•2H2O、 0.5 mol/L H2C2O4、0.03 mol/L NaCl、0.3
mol/L H3BO3It is dissolved in 1 with 0.3mol/L ascorbic acid:1 water and ethylene glycol solution is prepared under the magnetic field of 1T with the first step
Good alumina formwork is as working electrode, and mercury electrode is to electrode, and Ag/AgCl electrodes are auxiliary electrode, and it is 30 DEG C that temperature, which is added,
Continue 60 s in square wave for 0 V after deposition liquid, -1.3 V continue to carry out 50 cycles of pulse electrodeposition under 30 s, and deposition is completed
Porous alumina formwork is dissolved with the NaOH solution of 2M/L, is then cleaned to neutrality with ethyl alcohol and distilled water；
3）, annealing：Samarium Fe nanowire array is placed in heat-treatment furnace, high-purity argon gas is passed through with constant rate, at 500 DEG C
Anneal 5h；
4）, hydrogenation：It is passed through the argon hydrogen gaseous mixture containing 50% hydrogen with constant rate, is hydrogenated for 24 hours at 300 DEG C；
5）, nitridation：It is passed through high pure nitrogen with constant rate, 20h is nitrogenized at 400 DEG C, is down to room temperature, sample is taken out and obtains
Samarium iron nitrogen magnetic nano-array.
XRD and TEM characterizations are carried out to the sample prepared by embodiment 1, detect samarium iron nitrogen object phase, the pattern of samarium iron nitrogen
For ordered nano linear array structure；VSM tests are carried out to samarium iron nitrogen magnetic nanowires array, find its with higher magnetic energy product and
Excellent magnetic anisotropy.
Embodiment 2：
Step is：
1）, porous alumina formwork prepare：The alumina formwork that aperture is 100nm bilaterals is chosen, in its back side magnetron sputtering one
The copper film that layer thickness is 5 μm is dried after trimethylsilyl cyanide, ethyl alcohol, distilled water are cleaned by ultrasonic with spare successively；
2）, samarium Fe nanowire array preparation：Prepare deposition liquid, formula is：0.1 mol/L FeCl2•4H2O、0.6 mol/
L SmCl3•6H2O、0.1 mol/L Na3C6H5O7•2H2O、 0.1 mol/L H2C2O4、0.06 mol/L NaCl、0.6 mol/
L H3BO3It is dissolved in 1 with 0.6mol/L ascorbic acid:1 water and ethylene glycol solution is prepared aerobic under the magnetic field of 5T with the first step
Change aluminum alloy pattern plate as working electrode, mercury electrode is to electrode, and Ag/AgCl electrodes are auxiliary electrode, and it is 30 DEG C of depositions that temperature, which is added,
Continue 60 s in square wave for 0 V after liquid, -1.3 V continue to carry out 100 cycles of pulse electrodeposition under 30 s, and deposition completes use
The NaOH solution of 2M/L dissolves porous alumina formwork, is then cleaned to neutrality with ethyl alcohol and distilled water；
3）, annealing：Samarium Fe nanowire array is placed in heat-treatment furnace, high-purity argon gas is passed through with constant rate, at 700 DEG C
Anneal 7h；
4）, hydrogenation：It is passed through the argon hydrogen gaseous mixture containing 50% hydrogen with constant rate, 10h is hydrogenated at 400 DEG C；
5）, nitridation：It is passed through high pure nitrogen with constant rate, 2h is nitrogenized at 500 DEG C, is down to room temperature, sample is taken out and obtains
Samarium iron nitrogen magnetic nano-array.
XRD and TEM characterizations are carried out to the sample prepared by embodiment 2, detect samarium iron nitrogen object phase, the pattern of samarium iron nitrogen
For ordered nano linear array structure；VSM tests are carried out to samarium iron nitrogen magnetic nanowires array, find its with higher magnetic energy product and
Excellent magnetic anisotropy.
Embodiment 3：
Step is：
1）, porous alumina formwork prepare：The alumina formwork that aperture is 100nm bilaterals is chosen, in its back side magnetron sputtering one
The copper film that layer thickness is 5 μm is dried after trimethylsilyl cyanide, ethyl alcohol, distilled water are cleaned by ultrasonic with spare successively；
2）, samarium Fe nanowire array preparation：Prepare deposition liquid, formula is：0.1 mol/L FeCl2•4H2O、0.6 mol/
L SmCl3•6H2O、0.1 mol/L Na3C6H5O7•2H2O、 0.1 mol/L H2C2O4、0.06 mol/L NaCl、0.6 mol/
L H3BO3It is dissolved in 1 with 0.6mol/L ascorbic acid:1 water and ethylene glycol solution is prepared aerobic under the magnetic field of 2T with the first step
Change aluminum alloy pattern plate as working electrode, mercury electrode is to electrode, and Ag/AgCl electrodes are auxiliary electrode, and it is 50 DEG C of depositions that temperature, which is added,
Continue 60 s in square wave for 0 V after liquid, -1.3 V continue to carry out 200 cycles of pulse electrodeposition under 30 s, and deposition completes use
The NaOH solution of 2M/L dissolves porous alumina formwork, is then cleaned to neutrality with ethyl alcohol and distilled water；
3）, annealing：Samarium Fe nanowire array is placed in heat-treatment furnace, high-purity argon gas is passed through with constant rate, at 600 DEG C
Anneal 3h；
4）, hydrogenation：It is passed through the argon hydrogen gaseous mixture containing 50% hydrogen with constant rate, 18h is hydrogenated at 350 DEG C；
5）, nitridation：It is passed through high pure nitrogen with constant rate, 10h is nitrogenized at 450 DEG C, is down to room temperature, sample is taken out and obtains
Samarium iron nitrogen magnetic nano-array.
XRD and TEM characterizations are carried out to the sample prepared by embodiment 3, detect samarium iron nitrogen object phase, the pattern of samarium iron nitrogen
For ordered nano linear array structure；VSM tests are carried out to samarium iron nitrogen magnetic nanowires array, find its with higher magnetic energy product and
Excellent magnetic anisotropy.
Embodiment 4：
Step is：
1）, porous alumina formwork prepare：The alumina formwork that aperture is 100nm bilaterals is chosen, in its back side magnetron sputtering one
The copper film that layer thickness is 5 μm is dried after trimethylsilyl cyanide, ethyl alcohol, distilled water are cleaned by ultrasonic with spare successively；
2）, samarium Fe nanowire array preparation：Prepare deposition liquid, formula is：0.05 mol/L FeCl2•4H2O、0.3
mol/L SmCl3•6H2O、0.5 mol/L Na3C6H5O7•2H2O、 0.5 mol/L H2C2O4、0.03 mol/L NaCl、0.3
mol/L H3BO3It is dissolved in 1 with 0.3mol/L ascorbic acid:1 water and ethylene glycol solution is prepared under the magnetic field of 3T with the first step
Good alumina formwork is as working electrode, and mercury electrode is to electrode, and Ag/AgCl electrodes are auxiliary electrode, and it is 40 DEG C that temperature, which is added,
Continue 60 s in square wave for 0 V after deposition liquid, -1.3 V continue to carry out 200 cycles of pulse electrodeposition under 30 s, and deposition is completed
Porous alumina formwork is dissolved with the NaOH solution of 2M/L, is then cleaned to neutrality with ethyl alcohol and distilled water；
3）, annealing：Samarium Fe nanowire array is placed in heat-treatment furnace, high-purity argon gas is passed through with constant rate, at 650 DEG C
Anneal 2h；
4）, hydrogenation：It is passed through the argon hydrogen gaseous mixture containing 50% hydrogen with constant rate, 20h is hydrogenated at 400 DEG C；
5）, nitridation：It is passed through high pure nitrogen with constant rate, 17h is nitrogenized at 450 DEG C, is down to room temperature, sample is taken out and obtains
Samarium iron nitrogen magnetic nano-array.
XRD and TEM characterizations are carried out to the sample prepared by embodiment 4, detect samarium iron nitrogen object phase, the pattern of samarium iron nitrogen
For ordered nano linear array structure；VSM tests are carried out to samarium iron nitrogen magnetic nanowires array, find its with higher magnetic energy product 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 prepare：The alumina formwork that aperture is 100nm bilaterals is chosen, in its back side magnetron sputtering one
The copper film that layer thickness is 5 μm is dried after trimethylsilyl cyanide, ethyl alcohol, distilled water are cleaned by ultrasonic with spare successively；
2）, samarium Fe nanowire array preparation：Samarium Fe nanowire array is prepared using square-wave pulse electrodeposition process under magnetic field：With
The first step gets out alumina formwork as working electrode, and mercury electrode is to electrode, and Ag/AgCl electrodes are auxiliary electrode, are added
It deposits and carries out square-wave pulse electro-deposition after liquid at a temperature of 30 ~ 50 DEG C, deposition is completed porous oxidation with the NaOH solution of 2M/L
Aluminum alloy pattern plate dissolves, and is then cleaned to neutrality with ethyl alcohol and distilled water；
The direction in the magnetic field is parallel with nanowire growth direction, and the size in magnetic field is 1 ~ 5 T；
The solute of the deposition liquid is：SmCl3•6H2O、FeCl2•4H2O、Na3C6H5O7•2H2O、 H2C2O4、NaCl、H3BO3With
Ascorbic acid, solvent 1:1 water and ethylene glycol solution；
The condition of the square-wave pulse electro-deposition is：Continue 60 s in 0 V, then moment add 30 s of potential duration of -1.3 V
Square-wave pulse electro-deposition certain time；
3）, annealing：Samarium Fe nanowire array is placed in heat-treatment furnace, high-purity argon gas is passed through with constant rate, 500 ~ 700
Anneal 1 ~ 5h at DEG C；
4）, hydrogenation：Be passed through the argon hydrogen gaseous mixture containing 50% hydrogen with constant rate, at 300 ~ 400 DEG C hydrogenate 10 ~ for 24 hours；
5）, nitridation：It is passed through high pure nitrogen with constant rate, 2 ~ 20h is nitrogenized at 400 ~ 500 DEG C, is down to room temperature, takes out sample
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 is consistent with the aperture of porous alumina formwork, 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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| CN110246685A (en) * | 2019-07-17 | 2019-09-17 | 徐靖才 | A kind of preparation method of samarium ferromagnetic phase |
| CN110277211A (en) * | 2019-07-17 | 2019-09-24 | 徐靖才 | A kind of preparation method of samarium iron nitrogen magnetic nanotube |
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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 |
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