CN105858625A - Iron nitride nanowire and production method thereof - Google Patents
Iron nitride nanowire and production method thereof Download PDFInfo
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0615—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium
- C01B21/0622—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium with iron, cobalt or nickel
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
The invention relates to an iron nitride nanowire and a production method thereof. The production method includes: preparing in an electrolytic cell, an iron nanowire on an aluminum oxide base plate by means of electrodeposition; removing the iron nanowire, placing in a thermal treatment furnace, introducing O2 at a constant speed, and oxidizing at 300-400 DEG C for 1-10 h to obtain an iron oxide nanowire; introducing hydrogen, reducing at 300-400 DEG C for 4-20 h to re-obtain an iron nanowire; introducing ammonia gas, nitriding at 120-200 DEG C for 1-30 h to obtain the iron nitride nanowire high in Alpha'-Fe16N2 content. Iron nitride is produced herein with nano-scale linear iron powder, and the diametric directional size of the nanowire is very small, thereby facilitating nitriding.
Description
Technical field
The present invention relates to a kind of nitrided iron nano wire and preparation method thereof, belong to field of material preparation.
Background technology
There is wide hysteresis curve, high-coercive force, high remanent magnetism, the material of constant magnetic can be kept once magnetization.Also known as hard magnetic material.In practicality, permanent magnet material work in degree of depth magnetic saturation and magnetize after the second quadrant demagnetization part of hysteresis curve.Permanent magnet material includes the materials such as ferrite permanent-magnet, rare earth permanent magnet (Rare-Earth Cobalt, neodymium iron boron etc.), aluminum nickel cobalt, siderochrome cobalt, ferro-aluminum, and what most common of which, consumption were maximum is ferrite permanent-magnet, Nd-Fe-B rare-earth permanent magnet.What magnetic property was best at present is exactly Nd-Fe-B permanent magnet, has the good reputation of " magnetic king ".But neodymium iron boron itself is the most imperfect, shortcoming is obvious, such as equally: content of rare earth is high, and price is high, corrosion-resistant.Therefore, people are actively finding a new generation's permanent magnet material always.And the appearance of nitrided iron, make everything be possibly realized.
With the change of nitrogen content, nitrided iron has different structures and performance, mainly includes interstitial solid solution (alpha, gamma, ε), compound phase (γ-Fe4N, ε-Fe3N) and be situated between steady phase (alpha martensite and α "-Fe16N2).All nitrided irons are all metastable phase, can resolve into Fe and N2.But below 400 DEG C, its dynamic process decomposed slowly, is limited by dynamic process, and nitrided iron can be with stable existence in room temperature.α "-Fe among these16N2Saturation magnetization value be 2.83 T, far above other materials, cause people's keen interest.
For many years, numerous scientists employ multiple method, such as: nitridation annealing method, eutectrol process, ion implantation, chemical vapour deposition technique, physical vaporous deposition etc..Fail prepares single-phase α "-Fe the most always16N2.One possible reason is: α "-Fe16N2It is metastable phase, is easily decomposed into α+γ-Fe when temperature is more than 200 DEG C4N.And Fe4N, Fe3N is stable phase, during preparing Fe-N thin film by traditional film deposition techniques, has the Fe of relatively low saturation magnetization4N, Fe3N compound is than metastable phase α "-Fe16N2It is more likely formed, so preparing pure single-phase α "-Fe16N2It is relatively difficult.1989, Sugita of FDAC institute et al. used molecular beam epitaxy at In0.2Ga0.8α "-Fe is successfully prepared on As (001) monocrystal chip16N2Monocrystal thin films, and to record its saturation magnetization value with vibrating specimen magnetometer be 2.9T.
In recent years, use Nano-sized Ferric Oxide Powder, use H2Reduction, NH3Nitridation preparation is also by extensive concern.But one shortcoming of this method is H2The iron powder activity obtained after reduction is big, mutually reunites serious, hinders nitridation process.In order to overcome the reunion of nano-particle, many scientist Nano-sized Ferric Oxide Powder outer cladding aluminium oxidies or the method for silicon oxide, and achieve certain effect.But new problem occurs in that, aluminium oxide and silicon oxide are non magnetic constituent element, reduce the intensity of magnetization of system.
It practice, the material of same volume, the surface area that circular shape is obtained is minimum, will be much smaller than the shape such as cylinder, thin slice.And nitriding result directly depends on surface area.Therefore, if using the iron powder of wire to prepare iron nitride material, efficiency of nitridation should be good many.It is known that electrodeposition process is one of common method preparing Fe nanowire.Therefore, it is an object of the invention to aluminium oxide as template, using electrodeposition process to prepare in diametric(al) is the Fe nanowire of nano-scale, provides advantage for nitridation, and then by aoxidizing, reduce, nitrogenizing, it is thus achieved that α "-Fe16N2Phase, improves the magnetic of iron nitride material.
Summary of the invention
It is an object of the invention to provide a kind of high α "-Fe16N2The nitrided iron nano wire of content, provides that a kind of to use electrodeposition process to prepare in diametric(al) be the Fe nanowire of nano-scale simultaneously, so by oxidation, reduce and nitrogenize, it is thus achieved that the preparation method of nitrided iron nano wire.
The present invention concretely comprises the following steps:
The first step: prepared by Fe nanowire
Electrodeposition process is used to prepare Fe nanowire in a cell: electrode is alumina formwork, and another side electrode is steel disc, after adding deposition liquid, logical 10V alternating voltage, deposit about 20 minutes, after having deposited, use saturated SnCl2Solution dissolves removes aluminum base, discharges nano wire, be then washed till neutrality with distilled water after being dissolved by alumina formwork by NaOH solution；
Described deposition liquid composition is: FeSO4·7H2O、HBO3、(NH4)2SO4And vitamin C；
In this deposition formula of liquid, HBO3As the pH value of buffer agent stably depositing liquid, add (NH4)2SO4Being to make metal ion be easier to deposit in the nano pore of aluminium oxide, adding vitamin C in deposition liquid is to prevent Fe2+Oxidized；
Second step: aoxidize, reduce
Fe nanowire is taken out, is placed in heat-treatment furnace, is passed through O with constant speed2, aoxidize 1-10h at 300 ~ 400 DEG C, to obtain iron oxide nano-wire；
It is passed through hydrogen, at 300 ~ 400 DEG C of reduction 4-20h, to regain Fe nanowire；
3rd step: nitridation
It is passed through ammonia, nitrogenizes 1 ~ 30h at 120 ~ 200 DEG C；Cooling, cools to room temperature with the furnace, takes out sample, can obtain nitrided iron nano wire, and its phase composition is mainly α "-Fe16N2, and comprise part α-Fe phase.
It is an advantage of the current invention that: preparing nitrided iron by the wire iron powder of nanoscale, it is the least in diametric(al) size, be conducive to nitridation.
Detailed description of the invention
Describe the present invention below in conjunction with embodiment, in order to be more fully understood that the purpose of the present invention, feature and advantage.Although the present invention is to combine this specific embodiment to be described, but is not intended that the invention be limited to described specific embodiment.On the contrary, replacement that the embodiment can being included in the protection domain defined in the claims in the present invention is carried out, the embodiment improving and being equal to, broadly fall into protection scope of the present invention.For the technological parameter not marked especially, can technology carry out routinely.
The present invention concretely comprises the following steps:
The first step: prepared by Fe nanowire
Electrodeposition process is used to prepare Fe nanowire in a cell: electrode is alumina formwork, and another side electrode is steel disc, after adding deposition liquid, logical 10V alternating voltage, deposit about 20 minutes, after having deposited, use saturated SnCl2Solution dissolves removes aluminum base, discharges nano wire, be then washed till neutrality with distilled water after being dissolved by alumina formwork by NaOH solution；
Described deposition liquid composition is: FeSO4·7H2O、HBO3、(NH4)2SO4And vitamin C；
In this deposition formula of liquid, HBO3As the pH value of buffer agent stably depositing liquid, add (NH4)2SO4Being to make metal ion be easier to deposit in the nano pore of aluminium oxide, adding vitamin C in deposition liquid is to prevent Fe2+Oxidized；
Second step: aoxidize, reduce
Fe nanowire is taken out, is placed in heat-treatment furnace, is passed through O with constant speed2, aoxidize 1-10h at 300 ~ 400 DEG C, to obtain iron oxide nano-wire；
It is passed through hydrogen, at 300 ~ 400 DEG C of reduction 4-20h, to regain Fe nanowire；
3rd step: nitridation
It is passed through ammonia, nitrogenizes 1 ~ 30h at 120 ~ 200 DEG C；Cooling, cools to room temperature with the furnace, takes out sample.
α "-Fe can be prepared by the present invention16N2The nitrided iron nano wire that content is high.
Embodiment 1:
Step is:
The first step: prepared by Fe nanowire
Electrodeposition process is used to prepare Fe nanowire in a cell: preparing electrodeposit liquid, its formula is: FeSO4·7H2O、HBO3、(NH4)2SO4And vitamin C；Electrode is alumina formwork on one side, and another side electrode is steel disc, after adding deposition liquid, and logical 10V alternating voltage, deposit about 20 minutes, after having deposited, use saturated SnCl2Solution dissolves removes aluminum base, discharges nano wire, be then washed till neutrality with distilled water after being dissolved by alumina formwork by NaOH solution；
Second step: aoxidize, reduce
Fe nanowire is taken out, is placed in heat-treatment furnace, is passed through O with constant speed2, aoxidize 10h at 300 DEG C, to obtain iron oxide nano-wire；
It is passed through hydrogen, at 300 DEG C of reductase 12 0h, to regain Fe nanowire；
3rd step: nitridation
It is passed through ammonia, nitrogenizes 30h at 120 DEG C；Cooling, cools to room temperature with the furnace, takes out sample.
Sample prepared by embodiment 1 carries out XRD and SEM characterize, detect α "-Fe16N2Phase, and find that nitrided iron pattern is nano wire.
Embodiment 2:
Step is:
The first step: prepared by Fe nanowire
Electrodeposition process is used to prepare Fe nanowire in a cell: preparing electrodeposit liquid, its formula is: FeSO4·7H2O、HBO3、(NH4)2SO4And vitamin C；Electrode is alumina formwork on one side, and another side electrode is steel disc, after adding deposition liquid, and logical 10V alternating voltage, deposit about 20 minutes, after having deposited, use saturated SnCl2Solution dissolves removes aluminum base, discharges nano wire, be then washed till neutrality with distilled water after being dissolved by alumina formwork by NaOH solution；
Second step: aoxidize, reduce
Fe nanowire is taken out, is placed in heat-treatment furnace, is passed through O with constant speed2, aoxidize 8h at 320 DEG C, to obtain iron oxide nano-wire；
It is passed through hydrogen, at 320 DEG C of reduction 16h, to regain Fe nanowire；
3rd step: nitridation
It is passed through ammonia, nitrogenizes 16h at 140 DEG C；Cooling, cools to room temperature with the furnace, takes out sample.
Sample prepared by embodiment 2 carries out XRD and SEM characterize, detect α "-Fe16N2Phase, and find that nitrided iron pattern is nano wire.
Embodiment 3:
Step is:
The first step: prepared by Fe nanowire
Electrodeposition process is used to prepare Fe nanowire in a cell: preparing electrodeposit liquid, its formula is: FeSO4·7H2O、HBO3、(NH4)2SO4And vitamin C；Electrode is alumina formwork on one side, and another side electrode is steel disc, after adding deposition liquid, and logical 10V alternating voltage, deposit about 20 minutes, after having deposited, use saturated SnCl2Solution dissolves removes aluminum base, discharges nano wire, be then washed till neutrality with distilled water after being dissolved by alumina formwork by NaOH solution；
Second step: aoxidize, reduce
Fe nanowire is taken out, is placed in heat-treatment furnace, is passed through O with constant speed2, aoxidize 6h at 340 DEG C, to obtain iron oxide nano-wire；
It is passed through hydrogen, at 340 DEG C of reduction 12h, to regain Fe nanowire；
3rd step: nitridation
It is passed through ammonia, nitrogenizes 8h at 160 DEG C；Cooling, cools to room temperature with the furnace, takes out sample.
Sample prepared by embodiment 3 carries out XRD and SEM characterize, detect α "-Fe16N2Phase, and find that nitrided iron pattern is nano wire.
Embodiment 4:
Step is:
The first step: prepared by Fe nanowire
Electrodeposition process is used to prepare Fe nanowire in a cell: preparing electrodeposit liquid, its formula is: FeSO4·7H2O、HBO3、(NH4)2SO4And vitamin C；Electrode is alumina formwork on one side, and another side electrode is steel disc, after adding deposition liquid, and logical 10V alternating voltage, deposit about 20 minutes, after having deposited, use saturated SnCl2Solution dissolves removes aluminum base, discharges nano wire, be then washed till neutrality with distilled water after being dissolved by alumina formwork by NaOH solution；
Second step: aoxidize, reduce
Fe nanowire is taken out, is placed in heat-treatment furnace, is passed through O with constant speed2, aoxidize 4h at 360 DEG C, to obtain iron oxide nano-wire；
It is passed through hydrogen, at 360 DEG C of reduction 8h, to regain Fe nanowire；
3rd step: nitridation
It is passed through ammonia, nitrogenizes 4h at 170 DEG C；Cooling, cools to room temperature with the furnace, takes out sample.
Sample prepared by embodiment 4 carries out XRD and SEM characterize, detect α "-Fe16N2Phase, and find that nitrided iron pattern is nano wire.
Embodiment 5:
Step is:
The first step: prepared by Fe nanowire
Electrodeposition process is used to prepare Fe nanowire in a cell: preparing electrodeposit liquid, its formula is: FeSO4·7H2O、HBO3、(NH4)2SO4And vitamin C；Electrode is alumina formwork on one side, and another side electrode is steel disc, after adding deposition liquid, and logical 10V alternating voltage, deposit about 20 minutes, after having deposited, use saturated SnCl2Solution dissolves removes aluminum base, discharges nano wire, be then washed till neutrality with distilled water after being dissolved by alumina formwork by NaOH solution；
Second step: aoxidize, reduce
Fe nanowire is taken out, is placed in heat-treatment furnace, is passed through O with constant speed2, aoxidize 2h at 380 DEG C, to obtain iron oxide nano-wire；
It is passed through hydrogen, at 380 DEG C of reduction 6h, to regain Fe nanowire；
3rd step: nitridation
It is passed through ammonia, nitrogenizes 2h at 180 DEG C；Cooling, cools to room temperature with the furnace, takes out sample.
Sample prepared by embodiment 5 carries out XRD and SEM characterize, detect α "-Fe16N2Phase, and find that nitrided iron pattern is nano wire.
Embodiment 6:
Step is:
The first step: prepared by Fe nanowire
Electrodeposition process is used to prepare Fe nanowire in a cell: preparing electrodeposit liquid, its formula is: FeSO4·7H2O、HBO3、(NH4)2SO4And vitamin C；Electrode is alumina formwork on one side, and another side electrode is steel disc, after adding deposition liquid, and logical 10V alternating voltage, deposit about 20 minutes, after having deposited, use saturated SnCl2Solution dissolves removes aluminum base, discharges nano wire, be then washed till neutrality with distilled water after being dissolved by alumina formwork by NaOH solution；
Second step: aoxidize, reduce
Fe nanowire is taken out, is placed in heat-treatment furnace, is passed through O with constant speed2, aoxidize 1h at 400 DEG C, to obtain iron oxide nano-wire；
It is passed through hydrogen, at 400 DEG C of reduction 4h, to regain Fe nanowire；
3rd step: nitridation
It is passed through ammonia, nitrogenizes 1h at 200 DEG C；Cooling, cools to room temperature with the furnace, takes out sample.
Sample prepared by embodiment 6 carries out XRD and SEM characterize, detect α "-Fe16N2Phase, and find that nitrided iron pattern is nano wire.
Claims (2)
1. a nitrided iron nano wire, it is characterised in that: the main phase of nitrided iron is α "-Fe16N2, and comprise part α-Fe phase；Nitrided iron pattern is wire, a diameter of nanoscale.
2. a kind of nitrided iron nano wire as claimed in claim 1, it is characterised in that preparation process is:
The first step: prepared by Fe nanowire
Electrodeposition process is used to prepare Fe nanowire in a cell: electrode is alumina formwork, and another side electrode is steel disc, after adding deposition liquid, logical 10V alternating voltage, deposit about 20 minutes, after having deposited, use saturated SnCl2Solution dissolves removes aluminum base, discharges nano wire, be then washed till neutrality with distilled water after being dissolved by alumina formwork by NaOH solution；
Described deposition liquid composition is: FeSO4·7H2O、HBO3、(NH4)2SO4And vitamin C；
Second step: aoxidize, reduce
Fe nanowire is taken out, is placed in heat-treatment furnace, is passed through O with constant speed2, aoxidize 1-10h at 300 ~ 400 DEG C, to obtain iron oxide nano-wire；
It is passed through hydrogen, at 300 ~ 400 DEG C of reduction 4-20h, to regain Fe nanowire；
3rd step: nitridation
It is passed through ammonia, nitrogenizes 1 ~ 30h at 120 ~ 200 DEG C；Cooling, cools to room temperature with the furnace, takes out sample, can obtain nitrided iron nano wire.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108483505A (en) * | 2018-06-11 | 2018-09-04 | 彭晓领 | A kind of preparation method of nano magnetic material |
| CN116081582A (en) * | 2022-11-25 | 2023-05-09 | 四川大学 | Method for preparing transition metal nitride nanocrystals |
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| JP2000272909A (en) * | 1999-03-24 | 2000-10-03 | Nobuyuki Hiratsuka | Production of iron nitride and iron |
| CN101628712A (en) * | 2009-08-21 | 2010-01-20 | 东北大学 | Method for preparing single phase nanometer epsilon-Fe3N or gamma'-Fe4N powder and device thereof |
| CN101886283A (en) * | 2010-06-24 | 2010-11-17 | 浙江大学 | Preparation method and application of magnetically encoded nano-wire |
| CN103349993A (en) * | 2013-07-17 | 2013-10-16 | 北京航空航天大学 | Method for synthesizing magnetically separable iron nitride-based magnetic nanophotocatalyst |
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- 2016-06-26 CN CN201610469980.9A patent/CN105858625B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2000272909A (en) * | 1999-03-24 | 2000-10-03 | Nobuyuki Hiratsuka | Production of iron nitride and iron |
| CN101628712A (en) * | 2009-08-21 | 2010-01-20 | 东北大学 | Method for preparing single phase nanometer epsilon-Fe3N or gamma'-Fe4N powder and device thereof |
| CN101886283A (en) * | 2010-06-24 | 2010-11-17 | 浙江大学 | Preparation method and application of magnetically encoded nano-wire |
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Non-Patent Citations (1)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108483505A (en) * | 2018-06-11 | 2018-09-04 | 彭晓领 | A kind of preparation method of nano magnetic material |
| CN116081582A (en) * | 2022-11-25 | 2023-05-09 | 四川大学 | Method for preparing transition metal nitride nanocrystals |
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