CN109732078A - A kind of Fe-based nanocrystalline magnetically soft alloy micro mist radio-radar absorber and preparation method thereof - Google Patents
A kind of Fe-based nanocrystalline magnetically soft alloy micro mist radio-radar absorber and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of Fe-based nanocrystalline magnetically soft alloy micro mist radio-radar absorber, and alloy powder ingredient expression formula is FeaSibBcCudMe, M is one or more of Al, Cr, Co, Ni, P and C element in formula, and a, b, c, d and e respectively indicate the atom percentage content of each corresponding component, and meet 80≤a≤90,1≤b≤15,3≤c≤15,0≤d≤2.5,0≤e≤5.The present invention also provides a kind of preparation methods of Fe-based nanocrystalline magnetically soft alloy micro mist radio-radar absorber, comprising the following steps: step 1: preparing the raw material preparation of alloy powder;Step 2: the preparation of nanometer crystal alloy micro mist;It chooses the raw material for preparing alloy powder of the diameter less than 300 μm and is packed into ball grinder, inert gas shielding is filled with after vacuumizing, ball milling is carried out and alloy powder is made.Technical solution of the present invention solves the shortcoming of existing radio-radar absorber and preparation method thereof.
Description
Technical field
The present invention relates to new material technology fields, specifically, more particularly to a kind of Fe-based nanocrystalline magnetically soft alloy micro mist
Radio-radar absorber and preparation method thereof.
Background technique
Electronics and information industry technology is constantly progressive in recent years, modern electronic equipment towards micromation, integrated and high frequency
Direction is developed.With new generation of wireless communication, the progress of the emergence of wireless charging technology and the radar exploration technique, frequency electromagnetic waves
(such as frequency is in GHz range) industry, medical treatment and military field in using more and more.The raising of wave frequency and energy
The enhancing of amount in addition to influencing equipment and operating normally, can also so that electromagnetic interference, electromagnetic pollution and electromagnetic information leakage phenomenon are serious
Seriously threaten the health and safety of the mankind.Electromagnetic wave absorbent material can be consumed by electro-magnetic wave absorption and inside it to reduce electricity
Magnetic wave reflection or transmission are the effective ways for solving electromagnet radiation.Another important application of absorbing material is conduct
The electromagnetic wave that camouflage coating absorbs radar emission is stealthy to achieve the purpose that.With " absorbing property is strong, effective absorption frequency range is wide,
Light weight, thickness are thin " and it is suitable for the electromagnetic wave absorbent material of high band in electromagnetic wave security protection, electromagnetic compatibility and stealthy etc.
Technical field has extensive and urgent demand.
According to electromagnetic wave loss mechanism, absorbing material can be divided into magnetic loss type, dielectric loss type etc..Based on magnetic loss
Ferrite micropowder absorbent be one of common absorbing material.Traditional ferrite wave-absorbing material has under relatively low frequency
There are biggish magnetic loss and good absorbing property and is widely used.Due to the restriction by the Snoke limit, ferrite class magnetic
Property material magnetic conductivity sharply decline with the raising of wave frequency, electromagnetic wave absorption performance be deteriorated and be unable to satisfy high frequency and answer
With.Traditional ferrous alloy micro mist such as FeNi, FeCo and FeSiAl etc. are also typical magnetic electromagnetic wave absorbing material, and temperature is stablized
Property it is preferable, by prepare platelet-like metal micro mist formed high shape anisotropic property structure, improve magnetic conductivity to a certain extent
And natural resonant frequency, it is applicable in frequency and Effective frequency width of absorption increases.But the dielectric constant values of such material are larger, it is difficult to
Good impedance matching is formed with magnetic conductivity, absorbing property has reached theoretical limit.Fe-based nanocrystalline magnetically soft alloy has by receiving
The line and staff control of bcc-Fe and the residual amorphous phase composition of metrical scale, crystallite dimension bcc-Fe nano-crystalline and amorphous appropriate are alternate
Coupling interaction effect is generated, low-alloyed average magnetocrystalline anisotropy is dropped, it is made to show excellent soft magnet performance, is had both high full
There is outstanding advantage compared with traditional magnetic material with the magnetic conductivity under the intensity of magnetization and magnetic conductivity, especially high frequency.In addition, receiving
Rice peritectic alloy contains amorphous phase, and resistivity is higher, and dielectric constant is low, is advantageously implemented impedance matching, and nanometer crystal alloy can be improved
To the absorbent properties of frequency electromagnetic waves.Nanocrystalline radio-radar absorber is receive more and more attention in suction wave field.
FINEMET nanometer crystal alloy has a biggish electromagnetic wave loss ability in gigahertz frequency range, but it is as radio-radar absorber pair
Required coating layer thickness is larger (>3.5mm), effectively absorb frequency range it is relatively narrow (<2.5GHz), and in alloy high-content nonmagnetic elements
Nb reduces saturation magnetization, is also unfavorable for further increasing for magnetic conductivity.Develop high Fe content, the high saturation without Nb addition
The intensity of magnetization, high magnetic permeability nano-crystal soft magnetic alloy micro mist be expected to further increase the comprehensive of nanometer crystal alloy electromagnetic wave agent and inhale
Wave performance.
The existing method for preparing nano-crystal soft magnetic alloy micro mist has atomization, band crush method and high-energy ball milling method etc..
A large amount of alloyed powders can be disposably made in atomization, but the diameter of particle uniformity is poor;Band crush method is usually to first pass through melt
Quick quenching technique (getting rid of band method) obtains noncrystalline alloy strip, using heat treatment, the broken nanocrystalline micro mist of acquisition.Both the above method
Not only needed alloy that there is sufficiently high amorphous formation ability, but also to the more demanding of equipment, technique is relative complex.Pass through high energy ball
Mill method carries out mechanical alloying, can directly prepare nano-crystal soft magnetic alloy micro mist, amorphous formation ability of this method to alloy
It is required that it is relatively low, amorphous/nanocrystalline structure can be obtained in broader alloy component range, operation also low to equipment requirement
Simply, can be mass-produced alloyed powder, the disadvantage is that the time for directly carrying out mechanical alloying nanometer crystal powder is longer, production efficiency
It is lower.
In conjunction with the status of current magnetically soft alloy micro mist radio-radar absorber, invent a kind of in high frequency with strong electromagnetic wave suction
The receipts ability and simple nano-crystal soft-magnetic radio-radar absorber of preparation process will be of great significance.
Summary of the invention
According to the shortcoming of existing radio-radar absorber set forth above and preparation method thereof, and provide a kind of saturation magnetic
Change intensity is high, high frequency absorbing property is excellent, simple production process Fe-based nanocrystalline magnetically soft alloy micro mist radio-radar absorber and
Preparation method.
The technological means that the present invention uses is as follows:
A kind of Fe-based nanocrystalline magnetically soft alloy micro mist radio-radar absorber,
Alloy powder ingredient expression formula is FeaSibBcCudMe, in formula M be one of Al, Cr, Co, Ni, P and C element or
Several, a, b, c, d and e respectively indicate the atom percentage content of each corresponding component, and meet 80≤a≤90,1≤b≤15,3
≤ c≤15,0≤d≤2.5,0≤e≤5.
Further, alloy powder is made of the spheric granules that diameter is 2~15 μm, and has nanocrystalline/amorphous two-phase
Line and staff control, crystallite dimension, which is that the bcc-Fe of 5~20nm is nanocrystalline, to be evenly distributed in noncrystal substrate.
The present invention also provides a kind of preparation method of Fe-based nanocrystalline magnetically soft alloy micro mist radio-radar absorber, alloy powders
Preparation the following steps are included:
Step 1: preparing the raw material preparation of alloy powder;
Step 2: the preparation of nanometer crystal alloy micro mist;
It chooses the raw material for preparing alloy powder of the diameter less than 300 μm and is packed into ball grinder, be filled with inert gas after vacuumizing
Protection carries out ball milling and alloy powder is made.
Further, the preparation process of step 1 includes: the powder that each component is weighed according to the nominal composition of the alloy powder
Body raw material alloyage melts the powder of each component using induction melting furnace or non-consumable arc furnace under atmosphere of inert gases
Raw material obtain the master alloy ingot of chemical homogeneous, and master alloy ingot preliminary mechanical are crushed to the raw material for obtaining preparing alloy powder.
Further, the preparation process of step 1 includes: according to the nominal composition of the alloy powder, directly selection diameter
The powder raw material of each component less than 300 μm obtain preparing the raw material of alloy powder.
Further, the inert gas is argon gas or nitrogen.
It further, is hard alloy steel ball for the abrading-ball of ball milling;The ratio of grinding media to material of mechanical milling process is 20:1, and revolving speed is
300~400rpm, Ball-milling Time are 30~120h.
Further, further include step 3: the heat treatment of alloy powder, for adjusting the structure of alloy powder and then regulating and controlling
Its electromagnetic wave absorption performance;
By the alloy powder, isothermal annealing, isothermal temperature are 300~450 DEG C in vacuum annealing furnace, and soaking time is
30~60min is then cooled to room temperature.
Compared with the prior art, the invention has the following advantages that
1, Fe-based nanocrystalline magnetically soft alloy micro mist radio-radar absorber provided by the invention, saturation magnetization and magnetic conductivity
High, dielectric constant fits that medium, high frequency absorbing property is excellent, and the saturation magnetization of the nano-crystal soft magnetic alloy micro mist is 178.3~
197.8emu/g, magnetic conductivity real part is 2.18~2.49 under 2GHz frequency, and highest magnetic conductivity imaginary part is 0.68~0.99,8GHz
Lower real part of permittivity is 7.2~8.6, be made after which is mixed with paraffin by 3:1 mass ratio with a thickness of 2.0~
2.3mm sample has strong electromagnetic wave absorbability within the scope of 6.5~14.7GHz, and reflection loss peak RLmin is reachable-
53.9dB, Effective frequency width of absorption (i.e. reflection loss be better than -10dB) are not less than 4.5GHz, can cover entire X-band (8~
12GHz)。
2, the preparation method of Fe-based nanocrystalline magnetically soft alloy micro mist radio-radar absorber provided by the invention combines master alloy
Melting and high-energy ball milling prepare nanometer crystal alloy micro mist, and preparation process is simple, and Ball-milling Time is short, and high production efficiency industrially may be used
Produce in enormous quantities.
3, the preparation method of Fe-based nanocrystalline magnetically soft alloy micro mist radio-radar absorber provided by the invention, by changing ball
It consumes time and heat treatment process is combined to can control the pattern of alloy powder, particle size and nanocrystalline structure (including nanocrystal
Size, volume fraction etc.), so realize to nanometer crystal alloy micro mist electromagnetic wave absorption performance (including reflection loss peak, effectively
Absorb bandwidth, coating layer thickness etc.) Effective Regulation.
To sum up, using radio-radar absorber provided by the invention and preparation method thereof, in high frequency there is strong electromagnetic wave to inhale
Receipts ability and preparation process is simple.Therefore, the present invention solves the deficiency of existing radio-radar absorber and preparation method thereof
Place.
The present invention can be widely popularized in the fields such as camouflage coating and electromagnetic wave security protection in X-band based on the above reasons.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to do simply to introduce, it should be apparent that, the accompanying drawings in the following description is this hair
Bright some embodiments for those of ordinary skill in the art without any creative labor, can be with
It obtains other drawings based on these drawings.
Fig. 1 is 1 (Fe of the embodiment of the present invention80.7Si4B13Cu2.3) alloy powder after 40h ball milling XRD spectrum.
Fig. 2 is 1 (Fe of the embodiment of the present invention80.7Si4B13Cu2.3) alloy powder after 40h ball milling DSC curve.
Fig. 3 is 1 (Fe of the embodiment of the present invention80.7Si4B13Cu2.3) alloy powder after 40h ball milling SEM figure.
Fig. 4 is 1 (Fe of the embodiment of the present invention80.7Si4B13Cu2.3) alloy powder after 40h ball milling hysteresis loop figure.
Fig. 5 is 1 (Fe of the embodiment of the present invention80.7Si4B13Cu2.3) alloy powder/paraffin composite sample after 40h ball milling
Complex permeability real part μ ' and imaginary part μ " 2~18GH frequency range change curve.
Fig. 6 is 1 (Fe of the embodiment of the present invention80.7Si4B13Cu2.3) alloy powder/paraffin composite sample after 40h ball milling
Complex dielectric permittivity real part ε ' and imaginary part ε " 2~18GH frequency range change curve.
Fig. 7 is 1 (Fe of the embodiment of the present invention80.7Si4B13Cu2.3) through 40h, 80h ball milling and first through 80h ball milling again through 300 DEG C
Keep the temperature 60min after alloy powder/paraffin composite sample reflection loss 2~18GH frequency range change curve.
Specific embodiment
It should be noted that in the absence of conflict, the feature in embodiment and embodiment in the present invention can phase
Mutually combination.The present invention will be described in detail below with reference to the accompanying drawings and embodiments.
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is only
It is only a part of the embodiment of the present invention, instead of all the embodiments.It is real to the description of at least one exemplary embodiment below
It is merely illustrative on border, never as to the present invention and its application or any restrictions used.Based on the reality in the present invention
Example is applied, every other embodiment obtained by those of ordinary skill in the art without making creative efforts all belongs to
In the scope of protection of the invention.
Following non-limiting embodiments can with a person of ordinary skill in the art will more fully understand the present invention, but not with
Any mode limits the present invention.
Test method described in following embodiments is unless otherwise specified conventional method;The reagent and material, such as
Without specified otherwise, commercially obtain.
The present invention provides a kind of Fe-based nanocrystalline magnetically soft alloy micro mist radio-radar absorber,
Alloy powder ingredient expression formula is FeaSibBcCudMe, in formula M be one of Al, Cr, Co, Ni, P and C element or
Several, a, b, c, d and e respectively indicate the atom percentage content of each corresponding component, and meet 80≤a≤90,1≤b≤15,3
≤ c≤15,0≤d≤2.5,0≤e≤5.
Further, alloy powder is made of the spheric granules that diameter is 2~15 μm, and has nanocrystalline/amorphous two-phase
Line and staff control, crystallite dimension, which is that the bcc-Fe of 5~20nm is nanocrystalline, to be evenly distributed in noncrystal substrate.
The present invention also provides a kind of preparation method of Fe-based nanocrystalline magnetically soft alloy micro mist radio-radar absorber, alloy powders
Preparation the following steps are included:
Step 1: preparing the raw material preparation of alloy powder;
Step 2: the preparation of nanometer crystal alloy micro mist;
It chooses the raw material for preparing alloy powder of the diameter less than 300 μm and is packed into ball grinder, be filled with inert gas after vacuumizing
Protection carries out ball milling and alloy powder is made.
Further, the preparation process of step 1 includes: the powder that each component is weighed according to the nominal composition of the alloy powder
Body raw material alloyage melts the powder of each component using induction melting furnace or non-consumable arc furnace under atmosphere of inert gases
Raw material obtain the master alloy ingot of chemical homogeneous, and master alloy ingot preliminary mechanical are crushed to the raw material for obtaining preparing alloy powder.
Further, the preparation process of step 1 includes: according to the nominal composition of the alloy powder, directly selection diameter
The powder raw material of each component less than 300 μm obtain preparing the raw material of alloy powder.
Further, the inert gas is argon gas or nitrogen.
It further, is hard alloy steel ball for the abrading-ball of ball milling;The ratio of grinding media to material of mechanical milling process is 20:1, and revolving speed is
300~400rpm, Ball-milling Time are 30~120h.
Further, further include step 3: the heat treatment of alloy powder, for adjusting the structure of alloy powder and then regulating and controlling
Its electromagnetic wave absorption performance;
By the alloy powder, isothermal annealing, isothermal temperature are 300~450 DEG C in vacuum annealing furnace, and soaking time is
30~60min is then cooled to room temperature.
Embodiment 1
Fe80.7Si4B13Cu2.3
(1) preparation of as cast condition master alloy ingot
Each raw material of Fe, Si, B and Cu by purity not less than 99% (mass percent) is weighed by alloy nominal composition
Ingredient, using non-consumable arc furnace, by alloy raw material, melt back three times, obtains the uniform master alloy of ingredient under an argon atmosphere
Ingot casting.
(2) preparation of nanometer crystal alloy micro mist
60 mesh screens are crossed after master alloy ingot is carried out mechanical precrushing, alloy powder of the particle size less than 300 μm is taken to put
Enter ball grinder, setting ratio of grinding media to material is 20:1, is evacuated down to 6 × 10-3Pa is filled with argon gas and makees protective gas, is put into planet after closing
Formula ball mill carries out ball milling, and control drum's speed of rotation is 350rpm, and every mill 30min shuts down 5 minutes and cooled down, Ball-milling Time point
It is not set as 40h, 80h, 120h, reaches taking-up after cooling down 0.5h after setting Ball-milling Time and obtains iron-base nanometer crystal alloy micro mist electricity
Electro-magnetic wave absorption agent.
(3) alloy powder is heat-treated
The alloy powder obtained after ball milling 80h is placed in quartz ampoule and is evacuated to 3 × 10-3It seals after Pa, then puts
Enter in batch-type furnace, setting heat treatment temperature is 300 DEG C, is cooled to room temperature after keeping the temperature 60min, and iron-based the receiving of heat treatment modification is obtained
Rice peritectic alloy radio-radar absorber.
(4) structural characterization of iron-base nanometer crystal alloy radio-radar absorber, morphology observation and performance test
The structure of the alloy powder prepared under the conditions of each using XRD characterization: as shown in Figure 1, the alloy obtained after ball milling 40h
Contain bcc-Fe phase in micro mist, estimates that its crystallite dimension is about 10nm by Scherrer formula.
Using the hot property of differential scanning calorimeter (DSC) beta alloy micro mist: as shown in Fig. 2, obtained after ball milling 40h
Alloy powder has obvious exothermic peak when heated, shows in micro mist with the presence of amorphous phase.
In conjunction with XRD and DSC result it is found that the alloy powder obtained after ball milling 40h have bcc-Fe it is nanocrystalline/amorphous mixing
Tissue.Similarly, by other Ball-milling Time ball millings and heat treatment after alloy powder all have bcc-Fe it is nanocrystalline/amorphous
Line and staff control, bcc-Fe nanocrystalline crystallite dimension are slightly reduced with the increase of Ball-milling Time, and crystallite dimension changes after heat treatment
Less, heat treatment main function is to remove the internal stress generated in mechanical milling process, improves soft magnet performance.
The pattern of nanocrystalline micro mist is observed using scanning electron microscope (SEM): as shown in figure 3, the alloy obtained after ball milling 40h is micro-
Powder is made of the subsphaeroidal particle that average particle size particle size is 9 μm.Similarly, the alloy powder after other Ball-milling Time ball millings
Equal almost spherical, particle size gradually decrease in 3~15 μ ms with the increase of Ball-milling Time, and distributing homogeneity increases.
Micro powder granule pattern is basically unchanged after heat treatment.
The saturation magnetization of nanocrystalline micro mist is tested using vibrating specimen magnetometer (VSM): as shown in figure 4, ball milling 40h
The nanocrystalline micro mist obtained afterwards shows typical soft magnetic characteristic, and saturation magnetization reaches 181.9emu/g.Similarly, pass through
Nanocrystalline micro mist after other Ball-milling Time ball millings all has biggish saturation magnetization, in 178.3~183.4emu/g model
It encloses.
Using the electromagnetic parameter of vector network analyzer beta alloy micro mist: by nanocrystalline micro mist obtained and paraffin according to
It is 7mm that the ratio of mass ratio 3:1 is pressed into outer diameter after mixing, and internal diameter 3mm utilizes arrow with a thickness of the Both ring sam of 2mm
Amount Network Analyzer tests complex permeability μ=μ '-j μ " and complex dielectric permittivity of the composite sample in 2~18GHz frequency range
ε=ε '-j ε ".As shown in figure 5, the alloy powder obtained after ball milling 40h/paraffin composite sample has biggish complex permeability real
Portion μ ' and imaginary part μ ", μ ' is up to 2.18 at 2GHz, and with the increase of frequency, the real part μ ' of magnetic conductivity is gradually decreased, imaginary part
First increase reduces μ " afterwards, and maximum value 0.77 is reached near 12GHz.Complex dielectric permittivity is as shown in fig. 6, in 2~18GH frequency model
Enclose interior variation less, imaginary part ε " is close to 0, and real part ε ' is 7.3 at 8GHz, shows it mainly based on magnetic loss.It is similar
Ground, by other Ball-milling Time ball millings and heat treatment after alloy powder/paraffin composite sample all have biggish magnetic conductivity and
Dielectric constant appropriate, under 2GHz frequency magnetic conductivity real part μ ' be 2.18~2.33, maximum permeability imaginary part μ " be 0.68~
Real part of permittivity ε ' is 7.3~8.6 at 0.79,8GHz.Electromagnetism can also be joined by adjusting Ball-milling Time and heat treatment temperature
Number is regulated and controled.
The reflection loss of the electromagnetic parameters Alloy micropowder electromagnetic wave absorbent measured is combined according to transmission line principle
(RL) curve evaluates its electromagnetic wave absorption performance: as shown in fig. 7, obtained after different Ball-milling Time ball millings and heat treatment
The absorbing property that alloy powder/paraffin composite sample is excellent in, when counter sample thinner thickness can have biggish RL and
Effective frequency width of absorption, the alloy powder test sample that ball milling 40h is obtained are corresponding with a thickness of RL peak value (RL when 2.1mmmin) be-
39.1dB, Effective frequency width of absorption can reach 5.7GHz (9.0~14.7GHz).RL when corresponding to after ball milling 80h with a thickness of 2.2mm
RL is obtained at 10.3GHminFor -40.7dB, Effective frequency width of absorption 5.0GHz, the alloy powder through 300 DEG C of heat preservation 60min, by
In eliminating the influence for generating internal stress in mechanical milling process, absorbing property is further improved, RLminIt can reach -46.0dB,
Effective frequency width of absorption is widened as 5.4GHz.Similarly, the alloy powder sample after other Ball-milling Time ball millings is shown
Excellent absorbing property.With a thickness of 2.1~2.3mm nanometer crystal alloy micro mist/paraffin composite material in 7.5~14.7GHz model
There is stronger electro-magnetic wave absorption ability in enclosing, entire X-band (8~12GHz), RL can be coveredminFor -39.1~-46.0dB,
Effective frequency width of absorption is 4.5~5.7GHz.
Embodiment 2
Fe89Si7B3Cu1
(1) preparation of as cast condition master alloy ingot
The step is the same as embodiment 1.
(2) preparation of nanometer crystal alloy micro mist
The step is the same as embodiment 1.The present embodiment is unlike the first embodiment: Ball-milling Time is respectively set to 60h and 90h,
And without heat treatment.
(3) structural characterization of iron-base nanometer crystal alloy radio-radar absorber, morphology observation and performance test
The step is the same as embodiment 1.
Nanocrystalline/amorphous mixed structure, bcc-Fe phase are all had in the alloy powder obtained after different time ball milling
Crystallite dimension be about 12nm;Alloy powder is in subsphaeroidal pattern, and particle size is in 2~10 μ ms;Alloy powder has
Typical soft magnetic characteristic, saturation magnetization is within the scope of 192.6~196.0emu/g;Alloy powder/paraffin composite sample
μ ' at 2GHz for 2.25~2.40, μ " maximum value near 6GHz, being worth is 0.86~0.91, ε ' 8GHz at be 7.8~
8.5, there is stronger electro-magnetic wave absorption ability within the scope of 6.5~12.3GHz with a thickness of the composite sample of 2.2~2.3mm,
RLminFor -42.7~-48.2dB, Effective frequency width of absorption is 5.3~5.5GHz.
Embodiment 3
Fe90Si7B3
(1) preparation of as cast condition master alloy ingot
The step is the same as embodiment 1.
(2) preparation of nanometer crystal alloy micro mist
The step is the same as embodiment 1.The present embodiment is unlike the first embodiment: Ball-milling Time is set as 90h.
(3) alloy powder is heat-treated
The step is the same as embodiment 1.The present embodiment is unlike the first embodiment: by the alloy powder obtained after ball milling 90h into
Row heat treatment, heat treatment temperature is respectively 300 DEG C and 450 DEG C, soaking time 30min.
(4) structural characterization of iron-base nanometer crystal alloy radio-radar absorber, morphology observation and performance test
The step is the same as embodiment 1.
Nanocrystalline/amorphous mixed structure, bcc-Fe are all had in the alloy powder obtained after 90h ball milling and heat treatment
The crystallite dimension of phase is about 12nm;Alloy powder is in subsphaeroidal pattern, and particle size is in 2~10 μ ms;It is brilliant after heat treatment
Particle size and micro powder granule pattern are basically unchanged.Alloy powder has a typical soft magnetic characteristic, saturation magnetization 195.7~
Within the scope of 197.8emu/g;For 2.43~2.49, μ, " maximum value is in 6GHz at 2GHz by alloy powder/paraffin composite sample μ '
Near, being worth is 0.92~0.99, and ε ' is 7.8~8.0 at 8GHz, with a thickness of 2.0~2.1mm composite sample 6.9~
There is stronger electro-magnetic wave absorption ability, RL within the scope of 13.5GHzminFor -44.8~-51.2dB, Effective frequency width of absorption 6.1
~6.2GHz.
Embodiment 4
Fe85.5Si4B8P2Cu0.5
(1) preparation of as cast condition master alloy ingot
The step is the same as embodiment 1.
(2) preparation of nanometer crystal alloy micro mist
The step is the same as embodiment 1.The present embodiment is unlike the first embodiment: Ball-milling Time is set as 60h.
(3) alloy powder is heat-treated
The step is the same as embodiment 1.The present embodiment is unlike the first embodiment: by the alloy powder obtained after ball milling 60h into
Row heat treatment, heat treatment temperature are set as 300 DEG C, soaking time 30min.
(4) structural characterization of iron-base nanometer crystal alloy radio-radar absorber, morphology observation and performance test
The step is the same as embodiment 1.
There is complete amorphous in the alloy powder that the present embodiment obtains after 60h ball milling unlike the first embodiment
Phase structure, alloy powder are in subsphaeroidal pattern, and particle size is in 3~10 μ ms;It is mixed that nanocrystalline/amorphous is obtained after heat treatment
Structure is closed, the crystallite dimension of bcc-Fe phase is about 10nm;Alloy powder has typical soft magnetic characteristic, and saturation magnetization is
184.3emu/g;Alloy powder/paraffin composite sample μ ' is 2.46, μ " maximum value at 2GHz near 12GHz, is worth and is
0.84, ε ' are 7.2 at 8GHz, have stronger electromagnetism within the scope of 8.5~13.9GHz with a thickness of the composite sample of 2.1mm
Wave absorbability, RLminFor -53.9dB, Effective frequency width of absorption 5.4GHz.
Embodiment 5
Embodiment 5:Fe82.5Co5B11Si1Cu0.5
(1) preparation of as cast condition master alloy ingot
The step is the same as embodiment 1.
(2) preparation of nanometer crystal alloy micro mist
The step is the same as embodiment 1.The present embodiment is unlike the first embodiment: Ball-milling Time is set as 50h, and without heat
Processing.
(3) structural characterization of iron-base nanometer crystal alloy radio-radar absorber, morphology observation and performance test
The step is the same as embodiment 1.
There is nanocrystalline/amorphous mixed structure, the crystal grain ruler of bcc-Fe phase in the alloy powder obtained after 50h ball milling
Very little about 12nm;Alloy powder is in subsphaeroidal pattern, and particle size is in 3~13 μ ms;Alloy powder has typical soft
Magnetic characteristic, saturation magnetization 186.7emu/g;Alloy powder/paraffin composite sample μ ' at 2GHz for 2.31, μ " most
For big value near 9GHz, being worth is 0.76, and ε ' is 8.1 8GHz at, with a thickness of 2.0mm composite sample in 8.3~13.6GHz model
There is stronger electro-magnetic wave absorption ability, RL in enclosingminFor -39.6dB, Effective frequency width of absorption 5.3GHz.
Embodiment 6
Embodiment 6:Fe83.3Ni3.7B8Si4Al1
(1) preparation of as cast condition master alloy ingot
The step is the same as embodiment 1.
(2) preparation of nanometer crystal alloy micro mist
The step is the same as embodiment 1.The present embodiment is unlike the first embodiment: Ball-milling Time is set as 40h, and without heat
Processing.
(3) structural characterization of iron-base nanometer crystal alloy radio-radar absorber, morphology observation and performance test
The step is the same as embodiment 1.
There is nanocrystalline/amorphous mixed structure, the crystal grain ruler of bcc-Fe phase in the alloy powder obtained after 40h ball milling
Very little about 12nm;Alloy powder is in subsphaeroidal pattern, and particle size is in 2~13 μ ms;Alloy powder has typical soft
Magnetic characteristic, saturation magnetization 182.5emu/g;Alloy powder/paraffin composite sample μ ' at 2GHz for 2.34, μ " most
For big value near 12GHz, being worth is 0.78, and ε ' is 8.3 8GHz at, with a thickness of 2.0mm composite sample in 7.9~12.9GHz
There is stronger electro-magnetic wave absorption ability, RL in rangeminFor -36.4dB, Effective frequency width of absorption 5.0GHz.
Embodiment 7
Embodiment 7:Fe87Si7B4Cr2
(1) preparation of as cast condition master alloy ingot
The step is the same as embodiment 1.
(2) preparation of nanometer crystal alloy micro mist
The step is the same as embodiment 1.The present embodiment is unlike the first embodiment: Ball-milling Time is set as 45h, and without heat
Processing.
(3) structural characterization of iron-base nanometer crystal alloy radio-radar absorber, morphology observation and performance test
The step is the same as embodiment 1.
There is nanocrystalline/amorphous mixed structure, the crystal grain ruler of bcc-Fe phase in the alloy powder obtained after 45h ball milling
Very little about 10nm;Alloy powder is in subsphaeroidal pattern, and particle size is in 3~15 μ ms;Alloy powder has typical soft
Magnetic characteristic, saturation magnetization 189.1emu/g;Alloy powder/paraffin composite sample μ ' at 2GHz for 2.30, μ " most
For big value near 7GHz, being worth is 0.85, and ε ' is 7.9 8GHz at, with a thickness of 2.0mm composite sample in 7.4~12.2GHz model
There is stronger electro-magnetic wave absorption ability, RL in enclosingminFor -42.6dB, Effective frequency width of absorption 4.8GHz.
Embodiment 8
Embodiment 8:Fe80.5Si4B15Cu0.5
(1) raw material preparation of alloy powder is prepared
According to the nominal composition of the alloy powder, selection purity is not less than 99% (mass percent) and particle size is small
Obtain preparing the raw material of alloy powder in each micro mist raw material of 300 μm Fe, Si, B and Cu.
(2) preparation of nanometer crystal alloy micro mist
The raw material for preparing alloy powder is directly loadable into ball grinder and carries out ball milling under inert gas protection, Ball-milling Time is set
It is set to 70h, and without heat treatment.
(3) structural characterization of iron-base nanometer crystal alloy radio-radar absorber, morphology observation and performance test
The step is the same as embodiment 1.
There is nanocrystalline/amorphous mixed structure, the crystal grain ruler of bcc-Fe phase in the alloy powder obtained after 70h ball milling
Very little about 10nm;Alloy powder is in subsphaeroidal pattern, and particle size is in 3~15 μ ms;Alloy powder has typical soft
Magnetic characteristic, saturation magnetization 179.1emu/g;Alloy powder/paraffin composite sample μ ' at 2GHz for 2.23, μ " most
For big value near 12GHz, being worth is 0.75, and ε ' is 7.4 8GHz at, with a thickness of 2.0mm composite sample in 8.5~13.1GHz
There is stronger electro-magnetic wave absorption ability, RL in rangeminFor -38.2dB, Effective frequency width of absorption 4.6GHz.
Embodiment 9
Embodiment 9:Fe82Si15B3
(1) preparation of as cast condition master alloy ingot
The step is the same as embodiment 1.
(2) preparation of nanometer crystal alloy micro mist
The step is the same as embodiment 1.The present embodiment is unlike the first embodiment: Ball-milling Time is set as 30h, and without heat
Processing.
(3) structural characterization of iron-base nanometer crystal alloy radio-radar absorber, morphology observation and performance test
The step is the same as embodiment 1.
There is nanocrystalline/amorphous mixed structure, the crystal grain ruler of bcc-Fe phase in the alloy powder obtained after 30h ball milling
Very little about 10nm;Alloy powder is in subsphaeroidal pattern, and particle size is in 3~15 μ ms;Alloy powder has typical soft
Magnetic characteristic, saturation magnetization 178.4emu/g;Alloy powder/paraffin composite sample μ ' at 2GHz for 2.19, μ " most
For big value near 10GHz, being worth is 0.71, and ε ' is 7.2 8GHz at, with a thickness of 2.1mm composite sample in 8.9~13.4GHz
There is stronger electro-magnetic wave absorption ability, RL in rangeminFor -40.1dB, Effective frequency width of absorption 4.5GHz.
Embodiment 10
Fe83Si11B3C2Cu1
(1) preparation of as cast condition master alloy ingot
The step is the same as embodiment 1.
(2) preparation of nanometer crystal alloy micro mist
The step is the same as embodiment 1.The present embodiment is unlike the first embodiment: Ball-milling Time is set as 60h, and without heat
Processing.
(3) structural characterization of iron-base nanometer crystal alloy radio-radar absorber, morphology observation and performance test
The step is the same as embodiment 1.
There is nanocrystalline/amorphous mixed structure, the crystal grain ruler of bcc-Fe phase in the alloy powder obtained after 60h ball milling
Very little about 10nm;Alloy powder is in subsphaeroidal pattern, and particle size is in 3~15 μ ms;Alloy powder has typical soft
Magnetic characteristic, saturation magnetization 185.7emu/g;Alloy powder/paraffin composite sample μ ' at 2GHz for 2.21, μ " most
For big value near 7GHz, being worth is 0.83, and ε ' is 7.5 8GHz at, with a thickness of 2.3mm composite sample in 7.1~12.4GHz model
There is stronger electro-magnetic wave absorption ability, RL in enclosingminFor -43.3dB, Effective frequency width of absorption 5.3GHz.
Comparative example 1
Comparative example 1 is selected from bibliography [J.Alloys Compd.542 (2012) 90].Data in analytical table 1 were it is found that should
The saturation magnetization of radio-radar absorber is 96.1emu/g, RLminFor -22.2dB.Embodiment disclosed by the invention is compared with
Example 1 is compared, and has higher saturation magnetization, and reflection loss peak is lower, shows that electro-magnetic wave absorption ability is stronger.
Comparative example 2
Comparative example 2 is selected from bibliography [J.Ind.Eng.Chem.16 (2010) 437].The saturation of the radio-radar absorber
The intensity of magnetization is 109.3emu/g, although RLminValue reaches -50.3dB, but Effective frequency width of absorption only 2.5GHz, and the thickness of sample
Degree reaches 3.7mm.Embodiment disclosed by the invention has higher saturation magnetization, broader effective suction compared with comparative example 2
The advantages that receiving bandwidth and thinner thickness of sample.
Comparative example 3
Comparative example 3 is selected from bibliography [J.Magn.Magn.Mater.322 (2010) 794].Although its thickness of sample compared with
It is thin, only 1.0mm, but its RLminBe worth relatively low, only -8.4dB, in addition be not achieved electromagnetic wave is effectively absorbed loss value (-
10dB)。
See Table 1 for details for the detailed data of embodiment 1-10 and comparative example 1-3.
In conclusion a kind of Fe-based nanocrystalline magnetically soft alloy micro mist radio-radar absorber provided by the invention has saturation magnetic
Change intensity and magnetic conductivity are high, strong to the absorbability of frequency electromagnetic waves, effectively absorption frequency range is wide, absorbing property is controllable, produce
Outstanding advantages of simple process, the fields such as camouflage coating and electromagnetic wave security protection have broad prospect of application in X-band.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations;To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement;And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (8)
1. a kind of Fe-based nanocrystalline magnetically soft alloy micro mist radio-radar absorber, which is characterized in that
Alloy powder ingredient expression formula is FeaSibBcCudMe, M is one of Al, Cr, Co, Ni, P and C element or several in formula
Kind, a, b, c, d and e respectively indicate the atom percentage content of each corresponding component, and meet 80≤a≤90,1≤b≤15,3≤c
≤ 15,0≤d≤2.5,0≤e≤5.
2. Fe-based nanocrystalline magnetically soft alloy micro mist radio-radar absorber according to claim 1, which is characterized in that alloy is micro-
Powder is that 2~15 μm of spheric granules is constituted, and has nanocrystalline/amorphous bipolar mixture tissue by diameter, crystallite dimension is 5~
The bcc-Fe of 20nm is nanocrystalline to be evenly distributed in noncrystal substrate.
3. a kind of preparation method of Fe-based nanocrystalline magnetically soft alloy micro mist radio-radar absorber as described in claim 1, special
Sign is, the preparation of alloy powder the following steps are included:
Step 1: preparing the raw material preparation of alloy powder;
Step 2: the preparation of nanometer crystal alloy micro mist;
It chooses the raw material for preparing alloy powder of the diameter less than 300 μm and is packed into ball grinder, be filled with inert gas shielding after vacuumizing,
It carries out ball milling and alloy powder is made.
4. the preparation method of Fe-based nanocrystalline magnetically soft alloy micro mist radio-radar absorber according to claim 3, feature
It is, the preparation process of step 1 includes: to prepare according to the powder raw material that the nominal composition of the alloy powder weighs each component
Alloy is melted the powder raw material of each component under atmosphere of inert gases using induction melting furnace or non-consumable arc furnace, obtained
The master alloy ingot of chemical homogeneous, and master alloy ingot preliminary mechanical is crushed to the raw material for obtaining preparing alloy powder.
5. the preparation method of Fe-based nanocrystalline magnetically soft alloy micro mist radio-radar absorber according to claim 3, feature
It is, the preparation process of step 1 includes: according to the nominal composition of the alloy powder, and directly selection diameter is each less than 300 μm
The powder raw material of component obtain preparing the raw material of alloy powder.
6. according to Fe-based nanocrystalline magnetically soft alloy micro mist radio-radar absorber described in any one of claim 3-5 claim
Preparation method, which is characterized in that the inert gas is argon gas or nitrogen.
7. the preparation method of Fe-based nanocrystalline magnetically soft alloy micro mist radio-radar absorber according to claim 6, feature
It is, the abrading-ball for ball milling is hard alloy steel ball;The ratio of grinding media to material of mechanical milling process is 20:1, and revolving speed is 300~400rpm, ball
Time consuming is 30~120h.
8. the preparation method of Fe-based nanocrystalline magnetically soft alloy micro mist radio-radar absorber according to claim 3, feature
It is, further includes step 3: the heat treatment of alloy powder, for adjusting the structure of alloy powder and then regulating and controlling its electro-magnetic wave absorption
Performance;
By the alloy powder in vacuum annealing furnace isothermal annealing, isothermal temperature be 300~450 DEG C, soaking time be 30~
60min is then cooled to room temperature.
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