CN107511478B - Graphite wraps up the alloy cpd Fe that Haas strangles (Heusler) and N doping3Si Nano capsule - Google Patents
Graphite wraps up the alloy cpd Fe that Haas strangles (Heusler) and N doping3Si Nano capsule Download PDFInfo
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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Abstract
The object of the present invention is to provide a kind of novel wave-absorbing material and preparation method thereof, this kind of material is nanoscale Fe3Si@C and N-Fe3Si@C nano capsule, wherein single-phase Fe3The Fe of Si or N doping3Si is as kernel, and nano-graphite is as shell.Such single-phase Nano capsule can largely be prepared by the ex vivo approach such as utilizing, both Nano capsule average grain diameters are in 30-40nm, with good soft magnet performance, this Nano capsule also has good dielectric properties and magnetic property, therefore there is good electromagnetic matching, in entire 2-18GHz frequency range, there is very high reflection loss, the nano wave-absorbing material of this electro-magnetic wave absorption for enabling this kind of material to become in 2-18GHz frequency range.
Description
Technical field
The invention belongs to Material Field, it is related to a kind of cenotype Nano capsule using plasma arc method and provides one
Kind, in situ under state, by introducing catalyzed gas ethyl alcohol or acetonitrile, graphite package soft magnetism Haas can be spontaneously generated and strangle alloy
Fe3The Fe of Si or N doping3The single phase nano capsule of Si, and can be with the preparation method of the such Nano capsule of mass production.
Background technique
In recent years, in the case where being pushed using information propagation as the information revolution of core, competing as the national defence of core using space flight and aviation
It strives under requirement, around how to utilize electromagnetic wave, especially this core of 2-18GHz frequency electromagnetic waves, has carried out numerous studies work
Make.Wave frequency is needed to stride forward from 4GHz to 5GHz in the upgrading of civilian aspect, mechanics of communication, the height of wireless network (wifi)
Effect use is also required to wave frequency and further increases on the basis of 2.4GHz；In terms of national defence, electromagnetism that reconnaissance radar uses
Wave frequency rate is on the basis of 2-5GHz, in order to improve scouting precision, tends to increase frequency to realize wideband detected with high accuracy.However,
From the aspect of opposite, with the raising of electromagnetic wave frequency of use, electromagnetic wave energy per unit area is also greatly improved, and can be produced therewith
Raw forceful electric power electromagnetic pollution, i.e. frequency electromagnetic waves can generate very strong electromagnetic interference, while high frequency to certain important electronic equipment operations
Electromagnetic wave also can cause the imperceptible damage arrived to human body inner tissue, cell and DNA helical structure in a manner of radiation, seriously
Influence the health of the mankind.In terms of national defence, the stealth aircraft and stealthy guided missile needs that China develops avoid being detectd by High Accuracy Radar
It observes, therefore, in recent years it is necessary to have higher magnetic or absorption higher frequency electromagnetic wave absorbing material, and magnetic Nano
Material as new functional, magnetic recording with it is more and more extensive in absorbing material (stealth material) application, therefore develop
More novel nano magnetic materials become the requirement that investigation of materials is increasingly urgent to.Since soft magnetism kernel has high magnetic permeability, and it is sharp
With high magnetic permeability, the electromagnetic matching relationship of adjustable Nano capsule, to obtain better electromagnetic wave absorption performance, therefore fit
In as absorbing material of new generation.
Because it is more difficult to synthesize magnetically soft alloy, early stage scientist is to prepare simple substance using physically or chemically method
Soft magnetic metal or oxidate nano composite material prepare soft magnetic metal or oxide for physically or chemically method as absorbing material
Nanocomposite is described as follows:
Patent CN103305185A discloses a kind of redox graphene/Fe3O4The system of the nano combined absorbing material of/Ag
GO/Fe is made using simplified coprecipitation in Preparation Method3O4, RGO/Fe is then made using wet-chemical reduction method3O4/ Ag ternary
Composite material, Radar Absorbing Properties of Composites obtained is good, can be by adjusting RGO, Fe3O4Ratio, the dosage of reducing agent with Ag
And the thickness of composite material realizes effective absorption of different-waveband.
It is multiple that patent CN102924876A discloses a kind of carbon nanotube-polythiophene that NiCuZn ferrite cladding DBSA is modified
Close the preparation method of absorbing material.This method first uses dodecyl benzene sulfonic acid (DBSA) to be modified multi-walled carbon nanotube,
And with the modified carbon nano-tube, Ni (NO3)2·6H2O、 Cu(NO3)2·3H2O、Zn(NO3)2·6H2O、Fe(NO3)3·9H2O is
Raw material prepares the modified carbon nano tube compound material of NiCuZn ferrite cladding DBSA using hydrothermal synthesis method, then again with
Thiophene monomer prepares the modified carbon nanotube-polythiophene composite wave-absorbing of NiCuZn ferrite cladding DBSA by in-situ polymerization
Material.The composite material has good electromagnetic performance, has important application value in field of microwave absorption.
Patent CN104209531A discloses a kind of cobalt/graphene composite nano wave-absorbing material and preparation method thereof, belongs to
Absorbing material field.The cobalt/graphene composite nano wave-absorbing material is made of cobalt and graphene, and cobalt is carried on the table of graphene
Face.The invention prepares graphene using chemistry redox method, is then loaded and is received on the surface of graphene by the method for chemical plating
Rice cobalt particle.The composite material of preparation in plating 1 hour has wider suction wave frequency section under the conditions of 70 DEG C, when matching thickness is
When 2mm, frequency range of the reflectivity less than -10dB is 12.5-17.5GHz, and at about 15.5GHz, absorption maximum is -12.5dB
Patent CN103846065A is disclosed a kind of combined using direct current arc method-sol-gal process and prepares bivalve layer
BaTiO3The method of/BN/Ni Nano capsule.Direct current arc method is used first, using amorphous Ni-B alloy as anode (Ni-B alloy sun
Pole target is suppressed by the amorphous Ni-B nano-alloy powder of solid state reaction preparation), tungsten is cathode, prepares BN packet
Cover Ni Nano capsule.It is adopted due to anode target material and is suppressed by the amorphous Ni-B nano-alloy powder of solid state reaction preparation,
It solves the problems, such as to be difficult to realize one-step synthesis BN cladding metal nano capsule in customary DC electric arc preparation method；Then in conjunction with
Sol-gel technique prepares bivalve layer BaTiO3/ BN coats Ni Nano capsule, solves ferroelectric material and iron on nanoscale
The problem of magnetic Material cladding.It is that a kind of technique is relatively easy, controllability is strong, improves transmission channel, the reality of electromagnetic wave inside it
The preparation method that existing Nano capsule absorbing material regulates and controls in different-waveband absorbing property.
Patent CN1762590A has invented a kind of transition metal-γ-Fe2O3Nano material and the preparation method and application thereof.
Transition metal-γ-Fe provided by the present invention2O3Nano material, substantially by 1-5 nanometer of transition metal or transition gold
Belong to alloy nano particle and 10-50 nanometers of γ-Fe2O3Nanoparticle composition；The transition metal or transition metal alloy account for
The 0.01-30% of the nano material total weight.Preparation method includes the following steps: 1) to prepare colloidal transition metal；2)
Prepare ferric hydroxide colloid；3) two kinds of colloids are mixed, hydro-thermal process, oxidation drying prepare transition metal-γ-Fe2O3Nanometer
Material.Transition metal γ-Fe of the invention2O3Nano material is that transition metal nano-cluster is answered with what ferric oxide nano particles were formed
Object is closed, due to the synergistic effect between function ingredients and nanoparticle containing two or more, there is very high urge
Change activity and stability, in catalyst, absorbing material, the fields such as Magneto separate have a wide range of applications value.
Patent CN103422192A discloses a kind of Fe-Co alloy/C/C composite nano fiber microwave absorption, including Fe-Co
Alloy nanoparticle and carbon nano-fiber, the Fe-Co alloy/C nano particle are uniformly distributed in inside or the table of carbon nano-fiber
Face, and Fe-Co alloy/C nano particle is graphitized carbon-coating package, the invention also discloses Fe-Co alloy/C/C composite nano fibers
The preparation method of microwave absorption, this method are made using electrostatic spinning combination Post isothermal treatment one-step method, this method technique letter
It is single, low in cost, yield is high, and continuously can largely prepare target product Fe-Co alloy/C/C composite nano fiber microwave absorption.
Fe-Co alloy/C of the invention/C composite nano fiber microwave absorption is a kind of absorbing material of excellent combination property, has matter
Gently, wideband, strong absorption, electromagnetic parameter facilitate the advantages that adjustable, in skills such as electromagnetism stealth, electromagnetic shielding and anti-electromagnetic-radiation interference
Art field has a good application prospect.
Above-mentioned soft magnetic metal or oxidate nano composite material are mainly prepared by chemically or physically synthetic method, soft magnet performance
The requirement of practical technique is not achieved, it is therefore desirable to develop a kind of new Nano capsule with high saturation and magnetic intensity, and can be big
The method for measuring preparation.
Summary of the invention
The object of the present invention is to provide a kind of novel wave-absorbing material, this kind of material is by nanoscale Fe3Si@C, N-Fe3Si@
Generation is prepared in situ under catalysis atmosphere effect in C nano capsule.Nano capsule saturated magnetization with higher at room temperature
Intensity and lower coercivity, in entire 2-18 ghz band, dielectric constant and magnetic conductivity with higher, this makes the material
A kind of novel nano wave-absorbing material in 2-18GHz frequency range can be become.
Technical solution of the present invention is as follows:
One kind strangling (Heusler) magnetically soft alloy compound Fe by graphite package Haas3Si Nano capsule Fe3Si@C, it is special
Sign is: the Nano capsule pattern has spherical, the single Fe of nano-scale3The structure of Si@C nano capsule be with
Shell-core structure feature, wherein graphite is shell, Heusler magnetically soft alloy Fe3Si is shell-core configuration of kernel.
A kind of Haas Le (Heusler) magnetically soft alloy compound Fe by graphite package N doping3Si Nano capsule N-
Fe3Si@C, it is characterised in that: the Nano capsule pattern has spherical, the single Fe of nano-scale3Si@C nano capsule
Structure is with shell-core structure feature, and wherein graphite is shell, and N adulterates Heusler magnetically soft alloy Fe3Si is the shell-of kernel
Core configuration.
The presence stable in the air of both the above Nano capsule simultaneously can be used directly, and have good soft magnet performance, and
Good dielectric properties and magnetic property, therefore there is good electromagnetic matching, in entire 2-18GHz frequency range, have very high
Reflection loss, the nano wave-absorbing material of this electro-magnetic wave absorption for enabling this kind of material to become in 2-18GHz frequency range.It is described
Nano capsule size is preferably distributed in 10-60nm, average grain diameter 30-40nm.
The present invention also provides the preparation methods of described two Nano capsules, it is characterised in that: with high-temperature plasma electricity
Arc evaporation technique is prepared in situ to obtain under working gas；Wherein: using pure carbon electrode for cathode, Fe-Si alloy is anode target
Material, cathode are kept at a distance from 1-10mm between anode target material；The electric current of arc discharge is 60~200A, and voltage is 5~40V；
The electric arc retention time is 5-300 minutes, and working gas used is argon gas, hydrogen, and catalyzed gas used is ethyl alcohol or acetonitrile.
Wherein: the partial pressure of argon gas is 5-60kPa, and the partial pressure of hydrogen is 10-40kPa, the dosage of ethyl alcohol be 5-50ml (preferably
20-30ml), acetonitrile content is 5-50ml (preferably 20-30ml).
The cathode that the present invention uses is preferably the pure graphite electrode that purity is higher than 99.9%；Anode target material is FexSi100-xIt closes
Gold, wherein x=40-60 (preferably 45-55), prepares Fe3Si@C and N-Fe3The optimal anode target of Si@C Nano capsule closes
Golden ingredient is Fe50Si50., the Fe of this optimal components preparation3Si@C and N-Fe3Si@C nano capsule has good single phase property,
Crystalline state is good, and particle diameter distribution is uniform.
The preparation method of Nano capsule of the present invention, it is characterised in that: the anode target material be cylindrical metal block or
Alloy block, a diameter of 10-50mm, with a thickness of 10-30mm.
The preparation method of Nano capsule of the present invention, it is characterised in that: 10-20 DEG C of cooler-water temperature range used.
Using plasma arc evaporation technology of the present invention, electric arc generates very high temperature, while plasma will make instead
It answers in gas after hydrogen decomposition, hydrogen atom is added in liquefied anode molten bath, in evaporation process, promotes anode metal atom
And elementide largely evaporates, these atoms and cluster are after leaving high-temperature region, and mutually collision forms Fe3What Si phase or N were adulterated
Fe3Si phase nano particle, as introducing catalyzed gas ethyl alcohol (C2H5) or acetonitrile (C OH2H3N after), electric arc is broken down into C, H, O, N
Equal atoms, wherein C, H, N dissolve in the Fe-Si alloy of fusing, and in evaporation process, C and N are dissolved in since atomic size is small
The Fe of formation3In Si nano-liquid droplet, while the presence of C atom inhibits the other objects of Fe-Si mutually such as Fe again2Si, Fe5Si3Shape
At promoting single-phase Fe3The formation of Si, on the other hand, N atom can also be solid-solubilized in Fe3In Si lattice, forms N and mix Fe3Si,
Fe3Si drop or the Fe of N doping3During Si Drop Condensation, C atom is precipitated due to supersaturation, in the Fe of solidification3Si nanometers
Particle or the Fe of N doping3Si nano grain surface forms graphite shells, ultimately forms graphite package Fe3Si or N adulterates Fe3Si receives
Rice grain.
The present invention also provides the Fe3Si@C and N-Fe3Si@C nano capsule as 2-18GHz under room temperature or low temperature it
Between frequency range absorbing material application.The Fe of 40wt.%, 50wt.%, 60wt.%3Si@C nano capsule and 60wt.%,
The paraffin (medium for not inhaling electromagnetic wave) of 50wt.%, 40wt.% mix, the electromagnetic property measured at room temperature, and dielectric is normal
Number real part ε ' within the scope of 2-18GHz between 6-70, imaginary part of dielectric constant ε " within the scope of 2-18GHz between 0.7-60,
Complex permeability real part μ ' is between 0.85-1.5 within the scope of 2-18GHz, and complex permeability imaginary part μ " is in 2-18 GHz range
It is interior between 0.01-0.3.The Fe of 40wt.%, 50wt.%, 60wt.%3Si@C and N-Fe3The reflection loss of Si@C Nano capsule
Best wave-absorbing effect can achieve the absorption of -50dB Yu -18dB.
Detailed description of the invention
Fig. 1 .Fe3Si@C X-ray diffraction spectrum.
Fig. 2 .Fe3The transmission photo of Si@C nano capsule, (a) pattern photo；(b) high-resolution photo.
Fig. 3 .Fe3The stereoscan photograph (40000 times of amplification) of Si@C nano capsule.
Fig. 4 (a) Fe3The x-ray photoelectron feature power spectrum of Fe2p 3/2 in Si@C nano capsule；(b) Fe3Si@C receives
The x-ray photoelectron feature power spectrum of Si2p 3/2 in rice glue capsule.
Fig. 5 .Fe3Si@C nano capsule and the Fe for mixing N3The Raman spectrum of Si@C nano capsule illustrates that its graphite shells has
Orderly graphite-structure also has unordered defect sturcture.
Fig. 6 .Fe3The hysteresis loop of Si@C nano capsule at different temperatures, curve show that its display is soft from 5K to room temperature
Magnetic characteristic.
Fig. 7 different proportion Fe3Variation relation of the electromagnetic parameter of Si@C nano capsule with frequency, (a) real part of permittivity
With the variation relation of frequency, (b) imaginary part of dielectric constant is with the variation relation of frequency, and (c) magnetic conductivity real part is with the variation with frequency
Relationship, (d) magnetic conductivity imaginary part is with the variation relation with frequency.
Fig. 8 different proportion Fe3Variation relation of the reflection loss of Si@C nano capsule with frequency, the Fe of (a) 40%3Si@C
The reflection loss of Nano capsule is with the variation relation of frequency, (b) 50% Fe3The reflection loss of Si@C nano capsule is with frequency
Variation relation, (c) 60% Fe3The reflection loss of Si@C nano capsule with frequency variation relation.
Fig. 9 mixes the Fe of N3Si@C nano capsule X-ray diffraction spectrum.
Figure 10 mixes the Fe of N3Photo, (a) pattern photo are returned in the transmission of Si@C nano capsule；(b) high-resolution photo.
Figure 11 mixes the Fe of N3The stereoscan photograph (80000 times of amplification factor) of Si@C nano capsule.Figure 12 (a) mixes N
Fe3The x-ray photoelectron feature power spectrum of Fe2p 3/2 in Si@C nano capsule；(b) Fe of N is mixed3In Si@C nano capsule
The x-ray photoelectron feature power spectrum of Si 2p3/2；(c) Fe of N is mixed3The x-ray photoelectron of N 1s in Si@C nano capsule is special
Levy power spectrum.
Figure 13 .Fe3Si@C nano capsule and the Fe for mixing N3The Raman spectrum of Si@C nano capsule.
Figure 14 mixes the Fe of N3The hysteresis loop of Si@C nano capsule at different temperatures, curve show from 5K to room temperature it
Show soft magnetic characteristic, saturation magnetization 93.8emu/g, coercivity 124Oe.
The Fe of the doping N of Figure 15 different proportion3With the variation relation of frequency, (a's electromagnetic parameter of Si@C nano capsule) is situated between
Electric constant real part is with the variation relation of frequency, and (b) imaginary part of dielectric constant is with the variation relation of frequency, (c) magnetic conductivity real part with
The variation relation of frequency, (d) magnetic conductivity imaginary part is with the variation relation with frequency.
The Fe of Figure 16 different proportion N doping3Variation relation of the reflection loss of Si@C nano capsule with frequency, (a) 40%
N doping Fe3The reflection loss of Si@C nano capsule is with the variation relation of frequency, (b) 50% Fe of N doping3Si@C nano
The reflection loss of capsule is with the variation relation of frequency, (c) 60% Fe of N doping3The reflection loss of Si@C nano capsule is with frequency
The variation relation of rate.
Specific embodiment
In the examples below, such as non-specified otherwise, being all made of the graphite electrode that purity is 99.9% is cathode, used to disappear
Consuming anode target material is cylindrical alloy pig.Catalysis reaction gas used is ethyl alcohol, for mixing the Fe of N3The catalysis that Si is used is anti-
Answering gas is acetonitrile.
Embodiment 1
Plasma arc coevaporation technology prepares graphite package Fe3Nano capsule (the Fe of Si3Si@C):
In plasma arc electric discharge evaporation process, consumable anode target used is diameter 20mm with a thickness of 10mm's
Fe50Si50Alloy cylindrical body, graphite cathode and anode target material spacing are 1.5mm.Cavity is vacuumized up to 5 × 10-3After Pa, true
It is passed through argon gas 20kPa, hydrogen 10kPa and ethyl alcohol 15ml in cavity body, connects DC power supply, adjusting voltage is 18-20V, anode
Arc discharge occurs between target and cathode, the electric current for generating arc discharge is 80A, adjust during arc discharge operating current with
Voltage keeps relative stability, and the electric arc retention time is 50 minutes, and Fe and Si evaporates jointly, is prepared in above-mentioned reaction atmosphere
Graphite wraps up magnetically soft alloy Fe3The Fe of Si3Si@C nano capsule collects powder after extraction gas at vacuum cavity inner wall
Last shape Fe3Si@C nano capsule.
Fig. 1 provides obtained Fe3The X ray diffracting spectrum (XRD) of Si@C nano capsule can be seen that from map
Kernel is single-phase Fe3Si, and the graphite of shell is not shown since quality is smaller in XRD map.
Fig. 2 provides Fe3Si@C transmission electron microscope photo, as can be seen that Fe from Fig. 2 (a)3Si@C nano capsule presents spherical
Particle characteristic, particle diameter distribution 20-80nm, partial size is relatively uniform, and average grain diameter is about 40nm or so.Fe3Si@C nano capsule is in
Now typical core-shell structure feature, Fig. 2 (b) high-resolution photo confirm that shell is graphite, kernel Fe3Si, (002) feature are brilliant
Interplanar distance is 0.282nm.
Fig. 3 provides Fe3The stereoscan photograph of Si@C nano capsule, 40000 times of amplification factor, as can be seen from the figure
Spherical shape is presented in grain, and partial size is highly uniform.
Fig. 4 provides Fe3In Si@C nano capsule in kernel Fe2p 3/2 and Si2p 3/2d under 0-54nm different depth
X-ray photoelectron feature power spectrum, from map it can be seen that, the outer surface 0nm and kernel depth of Fe and Si in Nano capsule
At 54nm, the characteristic peak of Momentum profiles has significant difference, to illustrate shell, there is no Fe3Si, and there are Fe for kernel3Si, outside
The peak of the Fe and Si of shell are as caused by exogenous impurity pollution.
Fig. 5 provides Fe3Si C nano capsule Raman spectrum indicates two characteristic dispersion peaks of graphite shells in figure, point
It Wei Yu not 1319cm-1With 1582cm-1, it is unordered with ordered graphitic structure that this respectively represents face graphite shells, transmits electricity according to front
Mirror photo analysis, it is unordered to represent graphite shells there are more defects, orderly represent carbon atom in graphite shells orderly point
Cloth.
Fig. 6 indicates Fe3Magnetic property of the Si C nano capsule from 5K to room temperature, 5K to room temperature magnetic do not change substantially,
Wherein saturation magnetization is 114emu/g, coercivity 160Oe at room temperature.
Fig. 7 provides 40wt.%, the Fe of 50wt.%, 60wt.% respectively3Si@C nano capsule and 60wt.%,
The paraffin (medium for not inhaling electromagnetic wave) of 50wt.%, 40wt.% mix, the electromagnetic property measured at room temperature, dielectric constant
Real part ε ' within the scope of 2-18GHz between 6-12, imaginary part of dielectric constant ε " in 2-18 GHz range between 0.7-3.7,
Complex permeability real part μ ' is between 0.85-1.4 within the scope of 2-18GHz, and complex permeability imaginary part μ " is in 2-18GHz range
It is interior between 0.01-0.25.
Fig. 8 provides 40wt.%, the Fe of 50wt.%, 60wt.%3The reflection loss of Si@C nano capsule with frequency variation
Relation curve, curve illustrate that such Nano capsule has good wave-absorbing effect, with measurement content from 40wt.% to 60wt.%,
Its wave-absorbing effect gradually increases, and best wave-absorbing effect can achieve -50dB (absorption for being equivalent to 99.999%).
Embodiment 2
Plasma arc coevaporation technology prepares the graphite package Fe of N doping3Nano capsule (the N-Fe of Si3Si@C):
In plasma arc electric discharge evaporation process, consumable anode target used is diameter 20mm with a thickness of 10mm's
Fe50Si50Metal cylinder is closed, graphite cathode and anode target material spacing are 1.5mm.Cavity is vacuumized up to 5 × 10-3After Pa,
It is passed through argon gas 20kPa, hydrogen 10kPa and acetonitrile 10ml in plasma arc discharging chamber, connects DC power supply, adjusts voltage
For 18-20V, arc discharge occurs between anode target material and cathode, the electric current for generating arc discharge is 80A, during arc discharge
It adjusts operating current to keep relative stability with voltage, the electric arc retention time is 90 minutes, and Fe and Si evaporates jointly, in above-mentioned reaction
The graphite package magnetically soft alloy Fe of N doping is prepared in atmosphere3The N-Fe of Si3Si@C nano capsule, in extraction gas
Afterwards, powdered N-Fe is collected at vacuum cavity inner wall3Si@C nano capsule.
Fig. 9 provides obtained N-Fe3The X ray diffracting spectrum (XRD) of Si@C nano capsule, can from map
Out, kernel is single-phase Fe3Si, and the graphite of shell is not shown since quality is smaller in XRD map.
Figure 10 provides N-Fe3Si@C transmission electron microscope photo, it can be seen from the figure that N-Fe3Si@C nano capsule presents spherical
Particle characteristic, particle diameter distribution 10-80nm, partial size is relatively uniform, and average grain diameter is about 50nm or so.N-Fe3Si@C nano capsule
Typical core-shell structure feature is presented, shell is graphite, and kernel is the Fe for mixing N3Si, (220) feature interplanar distance are
0.21nm。
Figure 11 provides N-Fe3The stereoscan photograph of Si@C nano capsule, 80000 times of amplification factor, can from figure
Spherical shape is presented in particle out, and partial size is highly uniform.
Figure 12 provides N-Fe3Fe2p 3/2, Si2p 3/2 are different in 0-30nm from N1s in kernel in Si@C nano capsule
X-ray photoelectron feature power spectrum under depth, from map it can be seen that, Fe and Si Nano capsule outer surface 0nm with it is interior
At core depth 15nm, the characteristic peak of Momentum profiles has significant difference, to illustrate shell, there is no Fe3Si, and kernel exists
Fe3Si, the peak of the Fe and Si of shell are as caused by exogenous impurity pollution.N1s map also illustrates kernel Fe simultaneously3Si lattice
In mixed N element.
Figure 13 provides N-Fe3Si C nano capsule Raman spectrum indicates two characteristic dispersions of graphite shells in figure
Peak is located at 1319cm-1With 1582cm-1, it is unordered with ordered graphitic structure that this respectively represents face graphite shells, according to front
Transmission electron microscope photo analysis, it is unordered to represent graphite shells there are more defects, orderly represent carbon atom in graphite shells
Orderly distribution.Wherein, it respectively represents unordered with the ratio of orderly peak intensity and undoped with the Fe of N3The ratio phase of Si@C nano capsule
When, illustrate N atom not largely doping enter graphite shells, form a large amount of defect.
Figure 14 indicates N-Fe3Magnetic property of the Si C nano capsule from 5K to room temperature, 5K to room temperature magnetic do not become substantially
Change, wherein saturation magnetization is 93.8emu/g, coercivity 124Oe at room temperature.
Figure 15 provides 40wt.%, the N-Fe of 50wt.%, 60wt.% respectively3Si@C nano capsule and 60wt.%,
The paraffin (medium for not inhaling electromagnetic wave) of 50wt.%, 40wt.% mix, the electromagnetic property measured at room temperature, dielectric constant
Real part ε ' is between 9-65 within the scope of 2-18GHz, and imaginary part of dielectric constant ε " is within the scope of 2-18GHz between 5-60, plural number
Magnetic conductivity real part μ ' is situated between within the scope of 2-18GHz within the scope of 2-18GHz between 0.85-1.45, complex permeability imaginary part μ "
In -0.01-0.3.
Figure 16 provides 40wt.%, the N-Fe of 50wt.%, 60wt.%3The reflection loss of Si@C nano capsule is with frequency
Variation relation curve, curve illustrate that such Nano capsule has good wave-absorbing effect, best wave-absorbing effect can achieve-
18dB (absorption for being equivalent to 99.0%).
Embodiment 3
Plasma arc coevaporation technology prepares graphite package Fe3Nano capsule (the Fe of Si3Si@C):
In plasma arc electric discharge evaporation process, consumable anode target used is diameter 20mm with a thickness of 10mm's
Fe40Si60Or Fe60Si40Alloy cylindrical body, graphite cathode and anode target material spacing are 1.5mm.Cavity is vacuumized up to 5 × 10-3After Pa, it is passed through argon gas 20kPa, hydrogen 10kPa and ethyl alcohol 50ml in vacuum cavity, connects DC power supply, adjusting voltage is
Arc discharge occurs between anode target material and cathode for 18-20V, and the electric current for generating arc discharge is 80A, adjusts during arc discharge
Section operating current keeps relative stability with voltage, and the electric arc retention time is 50 minutes, and Fe and Si evaporates jointly, in above-mentioned reaction gas
Graphite package magnetically soft alloy Fe is prepared in atmosphere3The Fe of Si3Si@C nano capsule and Fe3C@C nano capsule, hollow carbon sphere
Phase.Due to Fe40Si60Or Fe60Si40Ingredient deviates the ingredient Fe of optimization50Si50Farther out, and more ethyl alcohol is used, thus cannot
Obtain single-phase Fe3Si@C Nano capsule.
Embodiment 4
Plasma arc coevaporation technology prepares the graphite package Fe of N doping3Nano capsule (the N-Fe of Si3Si@C):
In plasma arc electric discharge evaporation process, consumable anode target used is diameter 20mm with a thickness of 10mm's
Fe40Si60Or Fe60Si40Alloy cylindrical body, graphite cathode and anode target material spacing are 1.5mm.Cavity is vacuumized up to 5 × 10- 3After Pa, it is passed through argon gas 20kPa, hydrogen 10kPa and acetonitrile 40ml in plasma arc discharging chamber, connects DC power supply,
Adjusting voltage is 18-20V, and arc discharge occurs between anode target material and cathode, and the electric current for generating arc discharge is 80A, and arc light is put
Operating current is adjusted in electric process to keep relative stability with voltage, the electric arc retention time is 90 minutes, and Fe and Si evaporates jointly,
The graphite package magnetically soft alloy Fe of N doping is prepared in above-mentioned reaction atmosphere3The N-Fe of Si3Si@C nano capsule, and
FeN, FeC, the miscellaneous phases such as hollow carbon sphere, due to Fe40Si60Or Fe60Si40Ingredient deviates the ingredient Fe of optimization50Si50Farther out, and make
With more acetonitrile, so that the graphite package Fe of single-phase N doping cannot be obtained3Nano capsule (the N-Fe of Si3Si@C)。
Comparative example 1
In gas ions arc discharge cavity, consumable anode target used is diameter 20mm, highly for 10mm's
Fe50Si50Metal cylinder is closed, black cathode and anode target material spacing are 1.5mm.Cavity is vacuumized up to 5 × 10-3It is being waited after Pa
It is passed through argon gas 20kPa, hydrogen 10kPa in gas ions arc discharge cavity, is not put into ethyl alcohol, connects DC power supply, adjusts voltage
For 18-20V, arc discharge occurs between anode target material and cathode, the electric current for generating arc discharge is 80A, during arc discharge
It adjusts operating current to keep relative stability with voltage, the electric arc retention time is 50 minutes, and Fe and Si evaporates jointly, due to not anti-
Gas alcohol vapor is answered, so that the Fe that a large amount of C atom is dissolved into fusing cannot be generated50Si50In metal bath, it cannot be catalyzed
Single-phase Fe3Si nano particle generates, but forms Fe3Si5, Fe2The multiphases nano particle such as Si.
Comparative example 2
In gas ions arc discharge cavity, it is highly the Fe of 10mm that consumable anode target used, which is diameter 20mm,50Si50
Metal cylinder is closed, black cathode and anode target material spacing are 1.5mm.Cavity is vacuumized up to 5 × 10-3In plasma electricity after Pa
It is passed through argon gas 20kPa, hydrogen 10kPa in arc discharge cavity, is not put into acetonitrile, connects DC power supply, adjusting voltage is 18-
Arc discharge occurs between anode target material and cathode for 20V, and the electric current for generating arc discharge is 80A, and work is adjusted during arc discharge
Make electric current to keep relative stability with voltage, the electric arc retention time is 90 minutes, and Fe and Si evaporates jointly, due to not having reaction gas
Acetonitrile vapors, so that the Fe that a large amount of C atom is dissolved into fusing cannot be generated50Si50In metal bath, while it can not generate
A large amount of N atom generates single-phase Fe to cannot be catalyzed3Si, and N atom not can enter Fe3Si lattice cannot finally form N
The single-phase Fe of doping3Si Nano capsule.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention
Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.
Claims (15)
1. a kind of strangle magnetically soft alloy compound Fe by graphite package Haas3The Nano capsule Fe of Si3Si@C, it is characterised in that: described
Nano capsule pattern is spherical, the single Fe of nano-scale3The structure of Si@C nano capsule has shell-core structure feature,
Middle graphite is shell, and Haas strangles magnetically soft alloy compound Fe3Si is kernel；
The Nano capsule Fe3Si@C's the preparation method comprises the following steps:
With high-temperature plasma arc evaporation technology, it is prepared in situ to obtain under working gas；Wherein: using high pure graphite electrode
For cathode, FexSi100-xAlloy is anode target material, x=40-60, and cathode is kept at a distance from 1-10mm between anode target material；Electricity
The electric current of arc discharge is 60~200A, and voltage is 5~40V；The electric arc retention time is 5-300 minutes, and working gas used is argon
Gas and hydrogen, catalyzed gas used are ethyl alcohol.
2. according to Nano capsule Fe described in claim 13Si@C, it is characterised in that: the Nano capsule Fe3The distribution of Si@C size
In 10-60nm, average grain diameter 30-40nm.
3. according to Nano capsule Fe described in claim 13Si@C, it is characterised in that: the partial pressure of argon gas is 5-60kPa, point of hydrogen
Pressure is 10-40kPa, and the dosage of ethyl alcohol is 5-50ml.
4. according to Nano capsule Fe described in claim 13Si@C, it is characterised in that: the anode target material FexSi100-xX in alloy
=45-55, the dosage of ethyl alcohol are 20-30ml.
5. according to Nano capsule Fe described in claim 13Si@C, it is characterised in that: Fe-Si alloy is in the anode target material
Fe50Si50。
6. according to Nano capsule Fe described in claim 13Si@C, it is characterised in that: the anode target material is cylindrical alloy block,
A diameter of 10-50mm, with a thickness of 10-30mm.
7. according to Nano capsule Fe described in claim 13Si@C, it is characterised in that: Nano capsule Fe3It is adopted in Si@C preparation method
With 10-20 DEG C of cooler-water temperature range.
8. a kind of Haas by graphite package N doping strangles magnetically soft alloy compound Fe3Si Nano capsule N-Fe3Si@C, feature
Be: the Nano capsule pattern is spherical, the single N-Fe of nano-scale3The structure of Si@C nano capsule has shell-core
Structure feature, wherein graphite is shell, and N doping Haas strangles magnetically soft alloy Fe3Si is kernel；
The Nano capsule N-Fe3Si@C's the preparation method comprises the following steps:
With high-temperature plasma arc evaporation technology, it is prepared in situ to obtain under working gas；Wherein: using high pure graphite electrode
For cathode, FexSi100-xAlloy is anode target material, x=40-60, and cathode is kept at a distance from 1-10mm between anode target material；Electricity
The electric current of arc discharge is 60~200A, and voltage is 5~40V；The electric arc retention time is 5-300 minutes, and working gas used is argon
Gas and hydrogen, catalyzed gas used are acetonitrile.
9. according to Nano capsule N-Fe described in claim 83Si@C, it is characterised in that: the Nano capsule N-Fe3Si@C size
It is distributed in 10-60nm, average grain diameter 30-40nm.
10. according to Nano capsule N-Fe described in claim 83Si@C, it is characterised in that: the partial pressure of argon gas is 5-60kPa, hydrogen
Partial pressure be 10-40kPa, acetonitrile content 5-50ml.
11. according to Nano capsule N-Fe described in claim 83Si@C, it is characterised in that: the anode target material FexSi100-xAlloy
Middle x=45-55, the dosage of acetonitrile are 20-30ml.
12. according to Nano capsule N-Fe described in claim 83Si@C, it is characterised in that: Fe-Si alloy is in the anode target material
Fe50Si50。
13. according to Nano capsule N-Fe described in claim 83Si@C, it is characterised in that: the anode target material is cylindrical alloy
Block, a diameter of 10-50mm, with a thickness of 10-30mm.
14. according to Nano capsule N-Fe described in claim 83Si@C, it is characterised in that: Nano capsule N-Fe3Si@C preparation method
It is middle to use 10-20 DEG C of cooler-water temperature range.
15. a kind of application of claim 1 or 8 Nano capsule as frequency range absorbing material between 2-18GHz at room temperature.
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