CN105858625B - One kind nitridation Fe nanowire and preparation method thereof - Google Patents
One kind nitridation Fe nanowire and preparation method thereof Download PDFInfo
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- 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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Abstract
The present invention relates to one kind nitridation Fe nanowire and preparation method thereof.The invention prepares Fe nanowire using electrodeposition process on aluminum oxide substrate in a cell；Fe nanowire is taken out, is placed in heat-treatment furnace, O is passed through with constant speed2, 1 10h is aoxidized at 300 ~ 400 DEG C, to obtain iron oxide nano-wire；Hydrogen is passed through, 4 20h are reduced at 300 ~ 400 DEG C, to regain Fe nanowire；Ammonia is passed through, 1 ~ 30h is nitrogenized at 120 ~ 200 DEG C, obtains high α " Fe16N2The nitridation Fe nanowire of content.This method prepares nitrided iron by the wire iron powder of nanoscale, and it is very small in diametric(al) size, is advantageous to nitrogenize.
Description
Technical field
The present invention relates to one kind nitridation Fe nanowire and preparation method thereof, belong to field of material preparation.
Background technology
With wide hysteresis curve, high-coercive force, high remanent magnetism, the material of constant magnetic can be kept once magnetization.It is also known as hard
Magnetic material.In practicality, the second quadrant demagnetization part of hysteresis curve after permanent-magnet material works in depth magnetic saturation and magnetized.Permanent magnetism
Material includes ferrite permanent-magnet, rare earth permanent magnet（Rare-Earth Cobalt, neodymium iron boron etc.）, aluminium nickel cobalt, siderochrome cobalt, the material such as ferro-aluminum, wherein most
Conventional, dosage 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,
There is the good reputation of " magnetic king ".But neodymium iron boron is in itself and imperfect, shortcoming is equally obvious, such as：Content of rare earth is high, and price is high, resistance to
Corrosivity is poor.Therefore, people are actively finding permanent-magnet material of new generation always.And the appearance of nitrided iron, turning into everything can
Energy.
With the change of nitrogen content, nitrided iron has different structure and performance, mainly including interstitial solid solution（Alpha, gamma, ε）,
Compound phase（γ´-Fe4N, ε-Fe3N）With steady phase (α '-martensite and the α "-Fe of being situated between16N2).All nitrided irons are all metastable phase, meeting
Resolve into Fe and N2.But the dynamic process that it is decomposed below 400 DEG C is very slow, is limited by dynamic process, nitrided iron
It can be mutually stabilized in room temperature.α "-Fe among these16N2Saturation magnetization value be 2.83 T, far above other materials, draw
Play people's keen interest.
For many years, numerous scientists have used a variety of methods, such as：Nitrogenize annealing method, eutectrol process, ion implantation, chemistry
Vapour deposition process, physical vaporous deposition etc..What is unfortunately failed always prepares single-phase α "-Fe16N2。
One is the reason for possible：α"-Fe16N2It is metastable phase, α+γ '-Fe is easily decomposed into when temperature is more than 200 DEG C4N.And Fe4N,
Fe3N is stable phase, during Fe-N films are prepared with traditional film deposition techniques, has relatively low saturated magnetization strong
The Fe of degree4N, Fe3N compounds are than metastable phase α "-Fe16N2It is more likely formed, so preparing pure single-phase α "-Fe16N2It is relatively difficult
's.1989, Sugita of FDAC research institute et al. was with molecular beam epitaxy in In0.2Ga0.8As (001) monocrystalline base
α "-Fe are successfully prepared on piece16N2Monocrystal thin films, and it is 2.9T to measure its saturation magnetization value with vibrating specimen magnetometer.
In recent years, using Nano-sized Ferric Oxide Powder, using H2Reduction, NH3Nitridation is prepared also by extensive concern.But this method
One shortcoming is H2The iron powder activity obtained after reduction is big, mutually reunites serious, hinders nitridation process.In order to overcome nanometer
The reunion of particle, the method for many scientists Nano-sized Ferric Oxide Powder outer cladding aluminum oxide or silica, and achieve
Certain effect.But the problem of new, occurs, and aluminum oxide and silica are non magnetic constituent element, reduce the intensity of magnetization of system.
In fact, the material of same volume, the surface area that circular shape is obtained is minimum, than cylinder, thin slice etc.
Shape will be much smaller.And nitriding result directly depends on surface area.Therefore, if preparing nitridation using the iron powder of wire
Iron material, what efficiency of nitridation should be good is more.It is well known that electrodeposition process is to prepare one of common method of Fe nanowire.Therefore,
The purpose of the present invention is using aluminum oxide as template, uses electrodeposition process to prepare the iron nanometer in diametric(al) for nano-scale
Line, advantage is provided for nitridation, and then by aoxidizing, reducing, nitrogenizing, acquisition α "-Fe16N2Phase, improve iron nitride material
Magnetic.
The content of the invention
It is an object of the invention to provide a kind of high α "-Fe16N2The nitridation Fe nanowire of content, while a kind of use is provided
Electrodeposition process is the Fe nanowire of nano-scale to prepare in diametric(al), and then by aoxidizing, reducing and nitrogenize, is nitrogenized
The preparation method of Fe nanowire.
The present invention's concretely comprises the following steps：
The first step：It is prepared by Fe nanowire
Fe nanowire is prepared using electrodeposition process in a cell：One side electrode is alumina formwork, and another side electrode is
Steel disc, after adding deposition liquid, lead to 10V alternating voltages, deposit 20 minutes or so, after the completion of deposition, with saturation SnCl2Solution dissolves
Aluminium base is removed, nanowire is discharged after alumina formwork is dissolved with NaOH solution, is then washed to neutrality with distillation；
Described deposition liquid composition is：FeSO4·7H2O、HBO3、(NH4)2SO4And vitamin C；
In this deposition formula of liquid, HBO3As the pH value of buffer stably depositing liquid, (NH is added4)2SO4Be in order to
Metal ion is set to be easier to deposit in the nano pore of aluminum oxide, it is to prevent Fe to deposit and add vitamin C in liquid2+By oxygen
Change；
Second step：Oxidation, reduction
Fe nanowire is taken out, is placed in heat-treatment furnace, O is passed through with constant speed2, 1- is aoxidized at 300 ~ 400 DEG C
10h, to obtain iron oxide nano-wire；
Hydrogen is passed through, 4-20h is reduced at 300 ~ 400 DEG C, to regain Fe nanowire；
3rd step：Nitridation
Ammonia is passed through, 1 ~ 30h is nitrogenized at 120 ~ 200 DEG C；Cooling, cool to room temperature with the furnace, take out sample, you can obtain nitrogen
Change Fe nanowire, its phase composition is mainly α "-Fe16N2, and include part α-Fe phases.
The advantage of the invention is that：Nitrided iron is prepared by the wire iron powder of nanoscale, it is non-in diametric(al) size
It is often small, be advantageous to nitrogenize.
Embodiment
With reference to embodiment, the present invention will be described in detail, so as to more fully understand the purpose of the present invention, feature and
Advantage.Although the present invention is described with reference to the specific embodiment, it is not intended that the invention be limited to described
Specific embodiment.On the contrary, the embodiment that can be included in the protection domain defined in the claims in the present invention is carried out
Replacement, improvement and equivalent embodiment, belong to protection scope of the present invention.For the technological parameter not marked especially,
Routinely technology it can carry out.
The present invention's concretely comprises the following steps：
The first step：It is prepared by Fe nanowire
Fe nanowire is prepared using electrodeposition process in a cell：One side electrode is alumina formwork, and another side electrode is
Steel disc, after adding deposition liquid, lead to 10V alternating voltages, deposit 20 minutes or so, after the completion of deposition, with saturation SnCl2Solution dissolves
Aluminium base is removed, nanowire is discharged after alumina formwork is dissolved with NaOH solution, is then washed to neutrality with distillation；
Described deposition liquid composition is：FeSO4·7H2O、HBO3、(NH4)2SO4And vitamin C；
In this deposition formula of liquid, HBO3As the pH value of buffer stably depositing liquid, (NH is added4)2SO4Be in order to
Metal ion is set to be easier to deposit in the nano pore of aluminum oxide, it is to prevent Fe to deposit and add vitamin C in liquid2+By oxygen
Change；
Second step：Oxidation, reduction
Fe nanowire is taken out, is placed in heat-treatment furnace, O is passed through with constant speed2, 1- is aoxidized at 300 ~ 400 DEG C
10h, to obtain iron oxide nano-wire；
Hydrogen is passed through, 4-20h is reduced at 300 ~ 400 DEG C, to regain Fe nanowire；
3rd step：Nitridation
Ammonia is passed through, 1 ~ 30h is nitrogenized at 120 ~ 200 DEG C；Cooling, cool to room temperature with the furnace, take out sample.
α "-Fe can be prepared by the present invention16N2The high nitridation Fe nanowire of content.
Embodiment 1：
Step is：
The first step：It is prepared by Fe nanowire
Fe nanowire is prepared using electrodeposition process in a cell：Prepare electrodeposit liquid, its formula is：FeSO4·7H2O、
HBO3、(NH4)2SO4And vitamin C；One side electrode is alumina formwork, and another side electrode is steel disc, after adding deposition liquid, is led to
10V alternating voltages, deposit 20 minutes or so, after the completion of deposition, with saturation SnCl2Solution dissolving removes aluminium base, uses NaOH solution
Nanowire is discharged after alumina formwork is dissolved, is then washed to neutrality with distillation；
Second step：Oxidation, reduction
Fe nanowire is taken out, is placed in heat-treatment furnace, O is passed through with constant speed2, 10h is aoxidized at 300 DEG C, to obtain
Obtain iron oxide nano-wire；
Hydrogen is passed through, in 300 DEG C of reductase 12 0h, to regain Fe nanowire；
3rd step：Nitridation
Ammonia is passed through, 30h is nitrogenized at 120 DEG C；Cooling, cool to room temperature with the furnace, take out sample.
XRD and SEM is carried out to the sample prepared by embodiment 1 to characterize, and detects α "-Fe16N2Phase, and find nitrided iron
Pattern is nano wire.
Embodiment 2：
Step is：
The first step：It is prepared by Fe nanowire
Fe nanowire is prepared using electrodeposition process in a cell：Prepare electrodeposit liquid, its formula is：FeSO4·7H2O、
HBO3、(NH4)2SO4And vitamin C；One side electrode is alumina formwork, and another side electrode is steel disc, after adding deposition liquid, is led to
10V alternating voltages, deposit 20 minutes or so, after the completion of deposition, with saturation SnCl2Solution dissolving removes aluminium base, uses NaOH solution
Nanowire is discharged after alumina formwork is dissolved, is then washed to neutrality with distillation；
Second step：Oxidation, reduction
Fe nanowire is taken out, is placed in heat-treatment furnace, O is passed through with constant speed2, 8h is aoxidized at 320 DEG C, to obtain
Iron oxide nano-wire；
Hydrogen is passed through, 16h is reduced at 320 DEG C, to regain Fe nanowire；
3rd step：Nitridation
Ammonia is passed through, 16h is nitrogenized at 140 DEG C；Cooling, cool to room temperature with the furnace, take out sample.
XRD and SEM is carried out to the sample prepared by embodiment 2 to characterize, and detects α "-Fe16N2Phase, and find nitrided iron
Pattern is nano wire.
Embodiment 3：
Step is：
The first step：It is prepared by Fe nanowire
Fe nanowire is prepared using electrodeposition process in a cell：Prepare electrodeposit liquid, its formula is：FeSO4·7H2O、
HBO3、(NH4)2SO4And vitamin C；One side electrode is alumina formwork, and another side electrode is steel disc, after adding deposition liquid, is led to
10V alternating voltages, deposit 20 minutes or so, after the completion of deposition, with saturation SnCl2Solution dissolving removes aluminium base, uses NaOH solution
Nanowire is discharged after alumina formwork is dissolved, is then washed to neutrality with distillation；
Second step：Oxidation, reduction
Fe nanowire is taken out, is placed in heat-treatment furnace, O is passed through with constant speed2, 6h is aoxidized at 340 DEG C, to obtain
Iron oxide nano-wire；
Hydrogen is passed through, 12h is reduced at 340 DEG C, to regain Fe nanowire；
3rd step：Nitridation
Ammonia is passed through, 8h is nitrogenized at 160 DEG C；Cooling, cool to room temperature with the furnace, take out sample.
XRD and SEM is carried out to the sample prepared by embodiment 3 to characterize, and detects α "-Fe16N2Phase, and find nitrided iron
Pattern is nano wire.
Embodiment 4：
Step is：
The first step：It is prepared by Fe nanowire
Fe nanowire is prepared using electrodeposition process in a cell：Prepare electrodeposit liquid, its formula is：FeSO4·7H2O、
HBO3、(NH4)2SO4And vitamin C；One side electrode is alumina formwork, and another side electrode is steel disc, after adding deposition liquid, is led to
10V alternating voltages, deposit 20 minutes or so, after the completion of deposition, with saturation SnCl2Solution dissolving removes aluminium base, uses NaOH solution
Nanowire is discharged after alumina formwork is dissolved, is then washed to neutrality with distillation；
Second step：Oxidation, reduction
Fe nanowire is taken out, is placed in heat-treatment furnace, O is passed through with constant speed2, 4h is aoxidized at 360 DEG C, to obtain
Iron oxide nano-wire；
Hydrogen is passed through, 8h is reduced at 360 DEG C, to regain Fe nanowire；
3rd step：Nitridation
Ammonia is passed through, 4h is nitrogenized at 170 DEG C；Cooling, cool to room temperature with the furnace, take out sample.
XRD and SEM is carried out to the sample prepared by embodiment 4 to characterize, and detects α "-Fe16N2Phase, and find nitrided iron
Pattern is nano wire.
Embodiment 5：
Step is：
The first step：It is prepared by Fe nanowire
Fe nanowire is prepared using electrodeposition process in a cell：Prepare electrodeposit liquid, its formula is：FeSO4·7H2O、
HBO3、(NH4)2SO4And vitamin C；One side electrode is alumina formwork, and another side electrode is steel disc, after adding deposition liquid, is led to
10V alternating voltages, deposit 20 minutes or so, after the completion of deposition, with saturation SnCl2Solution dissolving removes aluminium base, uses NaOH solution
Nanowire is discharged after alumina formwork is dissolved, is then washed to neutrality with distillation；
Second step：Oxidation, reduction
Fe nanowire is taken out, is placed in heat-treatment furnace, O is passed through with constant speed2, 2h is aoxidized at 380 DEG C, to obtain
Iron oxide nano-wire；
Hydrogen is passed through, 6h is reduced at 380 DEG C, to regain Fe nanowire；
3rd step：Nitridation
Ammonia is passed through, 2h is nitrogenized at 180 DEG C；Cooling, cool to room temperature with the furnace, take out sample.
XRD and SEM is carried out to the sample prepared by embodiment 5 to characterize, and detects α "-Fe16N2Phase, and find nitrided iron
Pattern is nano wire.
Embodiment 6：
Step is：
The first step：It is prepared by Fe nanowire
Fe nanowire is prepared using electrodeposition process in a cell：Prepare electrodeposit liquid, its formula is：FeSO4·7H2O、
HBO3、(NH4)2SO4And vitamin C；One side electrode is alumina formwork, and another side electrode is steel disc, after adding deposition liquid, is led to
10V alternating voltages, deposit 20 minutes or so, after the completion of deposition, with saturation SnCl2Solution dissolving removes aluminium base, uses NaOH solution
Nanowire is discharged after alumina formwork is dissolved, is then washed to neutrality with distillation；
Second step：Oxidation, reduction
Fe nanowire is taken out, is placed in heat-treatment furnace, O is passed through with constant speed2, 1h is aoxidized at 400 DEG C, to obtain
Iron oxide nano-wire；
Hydrogen is passed through, 4h is reduced at 400 DEG C, to regain Fe nanowire；
3rd step：Nitridation
Ammonia is passed through, 1h is nitrogenized at 200 DEG C；Cooling, cool to room temperature with the furnace, take out sample.
XRD and SEM is carried out to the sample prepared by embodiment 6 to characterize, and detects α "-Fe16N2Phase, and find nitrided iron
Pattern is nano wire.
Claims (1)
- A kind of 1. preparation method for nitrogenizing Fe nanowire, it is characterised in that：The main phase of nitrided iron is α "-Fe16N2, and include portion Divide α-Fe phases；Nitrided iron pattern is wire, a diameter of nanoscale；The preparation process of the nitrided iron is：The first step：It is prepared by Fe nanowireFe nanowire is prepared using electrodeposition process in a cell：One side electrode is alumina formwork, and another side electrode is steel disc, After adding deposition liquid, lead to 10V alternating voltages, deposit 20 minutes or so, after the completion of deposition, with saturation SnCl2Solution dissolving removes Aluminium base, nanowire is discharged after alumina formwork is dissolved with NaOH solution, is then washed to neutrality with distillation；Described deposition liquid composition is：FeSO4·7H2O、HBO3、(NH4)2SO4And vitamin C；Second step：Oxidation, reductionFe nanowire is taken out, is placed in heat-treatment furnace, O is passed through with constant speed2, 1-10h is aoxidized at 300 ~ 400 DEG C, to obtain Obtain iron oxide nano-wire；Hydrogen is passed through, 4-20h is reduced at 300 ~ 400 DEG C, to regain Fe nanowire；3rd step：NitridationAmmonia is passed through, 1 ~ 30h is nitrogenized at 120 ~ 200 DEG C；Cooling, cool to room temperature with the furnace, take out sample, you can obtain nitrided iron Nano wire.
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Citations (4)
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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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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (1)
| Title |
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| Fe16N2的物性研究;黄娟;《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》;20131215(第12期);第3页，第8-9页 * |
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