CN109877333A - A kind of FeNiMo@NiO magnetic Nano absorbing material and preparation method thereof with excellent microwave absorbing property - Google Patents
A kind of FeNiMo@NiO magnetic Nano absorbing material and preparation method thereof with excellent microwave absorbing property Download PDFInfo
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- CN109877333A CN109877333A CN201910000389.2A CN201910000389A CN109877333A CN 109877333 A CN109877333 A CN 109877333A CN 201910000389 A CN201910000389 A CN 201910000389A CN 109877333 A CN109877333 A CN 109877333A
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Abstract
The invention discloses a kind of FeNiMo@NiO magnetic Nano absorbing material and preparation method thereof, inner core molecule metering-type be quality very: Fe 16%, Ni 79%-84%, Mo 0-5%.Preparation method includes: S1, is smelted into FeNiMo alloy pig;S2, powder processed prepare FeNiMo magnetic nanometer using DC arc plasma, are evacuated to 5.0 × 10‑3Pa is filled with 25% hydrogen and 75% argon gas, electric current 60-180A hereinafter, using tungsten electrode as electrode;The FeNiMo magnetic nanoparticle prepared is carried out oxidizing thermal treatment in atmosphere furnace by S3, oxidizing thermal treatment, and atmosphere is the dry air of an atmospheric pressure, and oxidation temperature is from untreated to 400 DEG C, and soaking time is half an hour, and heating rate is 5 DEG C/min.The invention has the characteristics that the impedance matching of absorbing material is optimized after oxidizing thermal treatment, to improve absorbing property significantly.
Description
Technical field
Magnetic Nano absorbing material field more particularly to a kind of FeNiMo@NiO nano wave-absorbing material and preparation method thereof.
Background technique
Absorbing material either suffers from extensive purposes in civilian or military aspect.
At civilian aspect: with the development of science and technology, the development of electronic product Highgrade integration, electromagnetic pollution is increasingly tight
Weight, brings many new social safety problems, is the fourth-largest public hazards after atmosphere pollution, noise pollution and water pollution, electromagnetism
Pollution has the characteristics that biggish harmfulness and is not easy to protect, and causes researcher and greatly pays close attention to.
In military aspect: with modern microelectronic technology, computer technology, antenna technology, modern signal processing technology
It grows rapidly, is detected so that the detection means of radar system become multiband by one-segment.The sea, land and air of countries in the world are military
The survival ability of target and military penetration ability all receive serious threat, all positive hair of developed country and developing country
Open up stealth technology.
Therefore, absorbing material has huge demand in terms of solving electromagnetic pollution and enhancing national security and wide answers
With space, the electro-magnetic wave absorption mechanism of research material has critically important theoretical value and depth for developing excellent absorbing material
Remote practical significance.
Summary of the invention
The present invention provides a kind of FeNiMo@NiO magnetic Nano absorbing materials and preparation method thereof.First by Fe, Ni, Mo
Simple substance element is prepared into FeNiMo ingot by high vacuum arc melting method;Then use DC arc plasma will
FeNiMo ingot is prepared into FeNiMo magnetic nanometer;Finally obtained FeNiMo magnetic nanometer is carried out with atmosphere furnace
Oxidizing thermal treatment obtains FeNiMo@NiO magnetic nanometer.Wave material is inhaled by FeNiMo@NiO magnetic Nano prepared by this method
The impedance matching of material is optimized, to improve absorbing property significantly.
The technical solution of the present invention is as follows: a kind of FeNiMo@NiO magnetic Nano absorbing material, inner core molecule metering-type are
Quality is very: Fe 16%, Ni 79%-84%, Mo 0-5%.
It the described method comprises the following steps.
S11, Fe, Ni, Mo metal simple-substance are prepared into FeNiMo ingot by high vacuum arc melting method.
S12, the FeNiMo ingot that S11 is prepared is put into DC arc plasma metal nano powder Preparation equipment
In, it is evacuated toPa is filled with the mixed gas of hydrogen and argon gas hereinafter, using tungsten electrode as electrode, and electric current exists
60-180A prepares FeNiMo nano particle by DC arc plasma heating.
S13, the FeNiMo nano particle that S12 is prepared is subjected to oxidizing thermal treatment with atmosphere furnace, atmosphere is an atmosphere
The dry air of pressure, oxidation temperature are from untreated to 400 DEG C, and heating rate is 5 DEG C/min, and soaking time is half small
When.
Using AgilentPNA-L5230C vector network analyzer test material electromagnetic parameter and calculate reflectivity.With
FeNiMo@NiO nano powder and paraffin in S13 are mixed according to the ratio of mass ratio 3:2, and it is respectively 7mm that outer diameter and inner diameter, which is made,
And 3mm, with a thickness of the coaxial sample of 2.5mm or so.It is normal to measure complex permeability and multiple dielectric of the sample in 1-18GHz frequency range
Number, formula (1) is respectively adopted in the reflection loss RL and impedance matching Z of the single-layer absorber and (2) carry out calculating simulation:
(1)
(2)
In above formula,、It is respectively the complex dielectric permittivity, complex permeability and thickness of absorbing material with d, f is the frequency of electromagnetic wave
Rate, c are the spread speed of electromagnetic wave in a vacuum, and j is imaginary unit.
Compared with prior art, the advantages and positive effects of the present invention are: present example provide absorbing material,
FeNiMo nano particle, after oxidizing thermal treatment, the Ni element oxide on surface are prepared by DC arc plasma
At NiO shell, apparent nucleocapsid structure is formed, impedance matching is optimized, improves absorbing property.
Detailed description of the invention
Fig. 1 is the process flow chart that FeNiMo@NiO magnetic Nano absorbing material is prepared in the present invention.
Fig. 2 is the X-ray diffractogram of FeNiMO@NiO magnetic Nano absorbing material in the present invention.
Fig. 3 is the projection electron microscope of FeNiMo@NiO magnetic Nano absorbing material in the present invention.
Fig. 4 is the impedance matching figure of FeNiMO@NiO magnetic Nano absorbing material in the present invention.
Fig. 5 is the comparison of absorbing property after the oxidizing thermal treatment of FeNiMo@NiO magnetic Nano absorbing material in the present invention
Figure.
Specific embodiment
For a better understanding of the present invention, clearly, completely said below in conjunction with the attached drawing in the present embodiment
It is bright.
Embodiment 1
(1) ingredient
Fe16Ni82Mo2(mass is very).
(2) preparation method
Step 1: being with purity99.5% simple substance Fe, Ni, Mo is raw material, is very Ni by quality82Fe16Mo2Matched
Than.
Step 2: proportioned raw material being put into high vacuum electric arc melting equipment, the melt back in the case where electric current is 100-280A
5 times, obtain uniform FeNiMo ingot.
Step 3: the FeNiMo ingot that step 2 obtains is put into DC arc plasma metal nano powder equipment,
It is evacuated toPa is hereinafter, be filled with the H of 15 KPa2With the Ar of 45 KPa, with the current arc of 38 A, after stablizing,
By current regulation to 80A-160A.
Step 4: after the nano powder that step 3 is prepared precipitates completely, the processing of the row's of progress hydrogen.It will be other in cavity
After being completely exhausted out, the Ar of 50 KPa is filled with as protective gas, is carried out every the dry air that half an hour is filled with 5 KPa blunt
Change, until the gas of cavity reaches a standard atmospheric pressure.Passivation 8 hours after, by the powder of collection by 200 mesh sieve into
Row screening, obtains FeNiMo magnetic nanoparticle.
Step 5: the FeNiMo nano particle that step 3 obtains being put into atmosphere furnace and carries out oxidizing thermal treatment, is passed through one
The dry air of standard atmospheric pressure, oxidizing thermal treatment temperature are 200-450 DEG C, and heating rate is 5 DEG C/min, and soaking time is
Half an hour obtains FeNiMo@NiO magnetic nanoparticle.
(3) it characterizes
Using ANalytical-Empyrean type X-ray diffractometer, the FeNiMo@NiO magnetic nanoparticle that step 4 is obtained
Mutually detected.
Using Tecnai G2 F20 S-TWIN (200KV) type transmission electron microscope to step 4 gained FeNiMo@NiO
The shape characteristic 6 of nano powder is characterized.
Using AgilentPNA-L5230C vector network analyzer test material electromagnetic parameter and calculate reflectivity.With
FeNiMo@NiO nano powder and paraffin after step 4 passivation are mixed according to the ratio of mass ratio 3:2, and outer diameter and inner diameter difference is made
For 7mm and 3mm, with a thickness of the coaxial sample of 2.5mm or so.It is normal to measure magnetic conductivity and dielectric of the sample in 1-18GHz frequency range
Number, formula (1) is respectively adopted in the reflection loss RL and impedance matching Z of the single-layer absorber and (2) carry out calculating simulation.
(1)
(2)
In above formula,、It is respectively the complex dielectric permittivity, complex permeability and thickness of absorbing material with d, f is the frequency of electromagnetic wave
Rate, c are the spread speed of electromagnetic wave in a vacuum, and j is imaginary unit.
Embodiment 2
(1) ingredient
Fe16Ni84(quality is very).
(2) preparation method
Embodiment 2 is difference from example 1 is that Fe, Ni, Mo mass are very different, other schemes and 1 phase of embodiment
Together.
Embodiment 3
(1) ingredient
Fe16Ni79Mo5(quality is very).
Embodiment 3 is difference from example 1 is that Fe, Ni, Mo mass are very different, other schemes and embodiment
1 phase.
Experimental result:
FeNiMo@NiO magnetic nanoparticle, the material are obtained by the method for DC arc plasma and oxidizing thermal treatment
The Gao Jie caused by the high magnetic permeability of FeNiMo super-permalloy and the high interfacial polarization by caused by nucleocapsid structure is had both
The advantages of electric constant.To optimize impedance matching, absorbing property is further improved.
By PANalytical-Empyrean type X-ray diffractometer, the FeNiMO@NiO magnetism that Cu target is collected is received
The X ray diffracting data of rice grain, as shown in Figure 2.Visible main phase composition is FeNi in figure3Phase, after oxidizing thermal treatment,
There is NiO phase.
The shape characteristic of sample is characterized by AgilentPNA-L5230C type transmission electron microscope, as shown in Figure 3.From
In Fig. 3 as it can be seen that after oxidizing thermal treatment, FeNiMo@NiO magnetic nanoparticle shows apparent nucleocapsid structure pattern.
The magnetic conductivity and dielectric constant obtained by AgilentPNA-L5230C vector network analyzer test material, institute
Formula (1) is respectively adopted in the square reflection loss RL and impedance matching Z for stating single-layer absorber and (2) carry out calculating simulation:
(1)
(2)
In above formula,、It is respectively the complex dielectric permittivity, complex permeability and thickness of absorbing material with d, f is the frequency of electromagnetic wave
Rate, c are the spread speed of electromagnetic wave in a vacuum, and j is imaginary unit.FeNiMo@before and after the oxidizing thermal treatment being calculated
Impedance matching Z and reflection loss the RL such as Figure 4 and 5 of NiO magnetic nanoparticle.It can be seen from figure 4 that when with a thickness of 2.0 mm
When, when not oxidised heat treatment, the curve of impedance matching Z is far from the horizontal line of y=1;After oxidizing thermal treatment, impedance
The curve of matching Z obviously compares without horizontal line when oxidizing thermal treatment close to y=1, and impedance matching Z has obtained apparent excellent
Change.From figure 5 it can be seen that the minimum value of reflection loss is -17.6 dB, by the heat of oxidation when without oxidizing thermal treatment
After processing, the minimum value of reflection loss has reached -33.6 dB, and absorbing property is significantly improved.
Claims (4)
1. a kind of FeNiMo@NiO magnetic Nano absorbing material, it is characterised in that the kernel described in it is FeNiMo, shell NiO.
2. magnetic Nano absorbing material according to claim 1, it is characterised in that its inner core molecule metering-type is quality hundred
Divide hundred: Fe 16%, Ni 79%-84%, Mo 0-5%.
3. a kind of method for preparing magnetic Nano absorbing material described in claim 1, which comprises the following steps:
(1) Fe, Ni, Mo metal simple-substance are prepared into FeNiMo ingot by high vacuum arc melting method;
(2) melted ingot is put into DC arc plasma metal nano powder Preparation equipment, it is evacuated to 5.0 ×
10-3Pa is filled with the mixed gas of hydrogen and argon gas hereinafter, using tungsten electrode as electrode, and electric current passes through direct-current arc in 60-180A
Plasma heating method prepares FeNiMo nano particle;
(3) resulting FeNiMo nano particle is put into atmosphere furnace and carries out oxidizing thermal treatment at different temperatures.
4. according to the method described in claim 3, it is characterized in that, its atmosphere of the oxidizing thermal treatment is an atmospheric pressure
Dry air, heating rate are 5 DEG C/min, and soaking time is half an hour.
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CN113151796A (en) * | 2021-04-26 | 2021-07-23 | 广东工业大学 | Microwave absorbing material and preparation method thereof |
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