CN110272720A - A kind of double-nucleocapsid structure iron nickel molybdenum base absorbing material and preparation method thereof - Google Patents
A kind of double-nucleocapsid structure iron nickel molybdenum base absorbing material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of graphene oxide cladding lithium aluminium silicon transparent glass cladding iron nickel molybdenum nano wave-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, smelting iron nickel-molybdenum alloy ingot；S2, iron nickel molybdenum magnetic nanometer is prepared；S3, aluminium glue is prepared；S4, lithium aluminium glue is prepared；S5, silica gel is prepared；S6, lithium aluminum silica gel is prepared；S7, lithium aluminium silicon transparent glass cladding iron nickel molybdenum magnetic nanometer is prepared using sintering process；S8, graphene and lithium aluminium silicon transparent glass cladding iron nickel molybdenum are prepared by graphene oxide cladding lithium aluminium silicon transparent glass cladding iron nickel molybdenum magnetic nanoparticle by solvent-thermal method.The invention has the characteristics that the frequency of reflection loss absorption peak is mobile toward high frequency treatment, and impedance matching is also optimized, to significantly improve absorbing property after processing.
Description
Technical field
Magnetic Nano composite wave-suction material field more particularly to a kind of iron nickel molybdenum magnetic nanometer composite material and its preparation side
Method.
Background technique
With increasing sharply for population, the rapid development of electronic industrial technology, various high-frequency electronic elements are in electronic product
Middle use, such as mobile phone, computer, micro-wave oven, television set, automobile, wireless receiver equipment, this is provided for people's lives
While great convenience, the electromagnetic energy density of environment is also greatly improved.It is dirty that this certainly will bring electromagnetic interference, electromagnetism
The problems such as dye.Therefore, absorbing material has huge demand and wide application in terms of solving electromagnetic pollution and electromagnetic pollution
Space, the electro-magnetic wave absorption mechanism of research material have critically important theoretical value and far-reaching for developing excellent absorbing material
Practical significance.
Summary of the invention
The present invention provides one group of iron nickel molybdenum base magnetic nanometer composite materials and preparation method thereof.Firstly, by iron, nickel, molybdenum
Equal element simple substances are prepared into iron nickel molybdenum base ingot by high vacuum arc melting method；Then DC arc plasma is used
Iron nickel molybdenum base ingot is prepared into iron nickel molybdenum base magnetic nanometer.Prepare lithium glue, aluminium glue, silicon respectively by sol-gel method
Glue is prepared by mixing into lithium aluminum silica gel body according to the ratio that molar ratio is 1:1:2.Taking molar ratio is that the iron nickel molybdenum magnetism of 1:0.4 is received
Rice flour and lithium aluminum silica gel body are uniformly mixed, and prepare lithium aluminium silicon transparent glass cladding iron nickel molybdenum magnetic nanometer using sintering process.Most
Solvent-thermal method is used afterwards, one layer of graphene oxide is coated in pyroreaction kettle, obtains the graphene oxide cladding transparent glass of lithium aluminium silicon
Glass coats iron nickel molybdenum magnetic nanometer.Lithium aluminium silicon transparent glass, which is coated, by graphene oxide prepared by this method coats iron nickel molybdenum
The frequency of the reflection loss absorption peak of magnetic Nano absorbing material is mobile toward high frequency treatment, and impedance matching is also optimized, from
And significantly improve absorbing property.
The technical solution of the present invention is as follows:
A kind of iron nickel molybdenum magnetic nanometer composite material, inner core molecule metering-type be quality very: iron 16%, nickel 79%-
84%, molybdenum 0-5%.
Shown method includes:
S1, iron, nickel, molybdenum simple substance are prepared into iron nickel molybdenum ingot by high vacuum arc melting method；
S2, the iron nickel molybdenum ingot that S1 is prepared is put into DC arc plasma metal nano powder Preparation equipment, is taken out true
Sky, hereinafter, using tungsten electrode as electrode, is filled with the mixed gas of hydrogen and argon gas, electric current is in 60-180A, by straight to 0.005Pa
Galvanic electricity arc plasma heating prepares iron nickel molybdenum nano particle；
S3, using sol-gal process at 85 DEG C, prepare aluminium glue, ageing time is 12 hours；
S4, in the aluminium glue prepared, be added lithium nitrate, stir evenly, obtain lithium aluminium glue；
S5, using latex gel method, prepare silica gel；
S6, it selects molar ratio to be the lithium of 1:1:2: aluminium: silicon, is uniformly mixed, obtains lithium aluminum silica gel body；
S7, it takes molar ratio to be uniformly mixed for the iron nickel molybdenum magnetic nanometer and lithium aluminum silica gel body of 1:0.4, lithium is prepared using sintering process
Aluminium silicon transparent glass coats iron nickel molybdenum magnetic nanometer；
S8, solvent-thermal method, at 200 DEG C, heating rate is to keep the temperature in 10 small pyroreaction kettles at present under 5 DEG C/min and coat one
Layer graphene oxide obtains graphene oxide cladding lithium aluminium silicon transparent glass cladding iron nickel molybdenum magnetic nanometer.
Using AgilentPNA-L5230C vector network analyzer test material electromagnetic parameter and calculate reflectivity.With
Graphene oxide cladding iron nickel molybdenum magnetic nanoparticle and paraffin in S3 are mixed according to the ratio of mass ratio 3:2, and outer diameter is made
It is respectively 7mm and 3mm with internal diameter, with a thickness of the coaxial sample of 2.5mm or so.Measure multiple magnetic of the sample in 2-18GHz frequency range
Formula (1) and (2) are respectively adopted in conductance and complex dielectric permittivity, the reflection loss RL and impedance matching Z of the single-layer absorber
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:
The absorbing material that present example provides, prepares iron nickel molybdenum nano particle by DC arc plasma, passes through
After sintering process and solvent-thermal method processing, one layer of graphene oxide and lithium aluminium silicon transparent glass are coated in pyroreaction kettle, is obtained
Graphene oxide coats lithium aluminium silicon transparent glass and coats iron nickel molybdenum magnetic nanometer.The graphene oxide packet prepared by this method
The frequency for covering the reflection loss absorption peak of lithium aluminium silicon transparent glass cladding iron nickel molybdenum magnetic Nano absorbing material is moved toward high frequency treatment
Dynamic, impedance matching is also optimized, to significantly improve absorbing property.
Detailed description of the invention
Fig. 1 is to prepare graphene oxide cladding lithium aluminium silicon transparent glass cladding iron nickel molybdenum magnetic Nano in the present invention to inhale wave material
The process flow chart of material；
Fig. 2 is the impedance of graphene oxide cladding lithium aluminium silicon transparent glass cladding iron nickel molybdenum magnetic Nano absorbing material in the present invention
Matching figure；
Fig. 3 is the solvent of graphene oxide cladding lithium aluminium silicon transparent glass cladding iron nickel molybdenum magnetic Nano absorbing material in the present invention
The comparison diagram of absorbing property after thermal method processing.
Specific embodiment:
For a better understanding of the present invention, clearly, be completely illustrated below in conjunction with the attached drawing in the present embodiment.
Embodiment 1
(1) ingredient
Iron: nickel: molybdenum=16:82:2(mass percent)
(2) preparation method
Step 1: to be with purity99.5% fe, nickel, molybdenum are raw material, by iron: nickel: molybdenum=16:82:2(mass percentage
Than) proportion；
Step 2: proportioned raw material is put into high vacuum electric arc melting equipment, in the case where electric current is 100-280A melt back 5 times,
Obtain uniform iron nickel molybdenum ingot；
Step 3: the iron nickel molybdenum ingot that step 2 obtains being put into DC arc plasma metal nano powder equipment, is taken out true
Sky is to 0.005pa hereinafter, being 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 complete in cavity
After discharge, the Ar of 50 KPa is filled with as protective gas, is passivated every the dry air that half an hour is filled with 5 KPa, directly
Gas to cavity reaches a standard atmospheric pressure.After passivation 8 hours, the powder of collection is sieved by the sieve of 200 mesh
Point, obtain iron nickel molybdenum magnetic nanoparticle；
Step 5: using sol-gal process, at 85 DEG C, preparing aluminium glue, ageing time is 12 hours；
Step 6: by molar ratio lithium: aluminium is that the lithium nitrate of 1:1 is put into the aluminium glue prepared in step 5, stirs evenly, obtains lithium
Aluminium glue；
Step 7: using sol-gal process, by molar ratio aluminium: silicon is that first tetraethyl orthosilicate of 1:2 is prepared into silica gel；
Step 8: by the colloid prepared in step 6,7 according to molar ratio be 1:1:2 ratio lithium: aluminium: silicon is prepared by mixing into lithium aluminium
Colloidal silica；
Step 9: taking molar ratio to be uniformly mixed for the iron nickel molybdenum magnetic nanometer and lithium aluminum silica gel body of 1:0.4, using sintering legal system
Standby lithium aluminium silicon transparent glass coats iron nickel molybdenum magnetic nanometer；
Step 10: the lithium aluminium silicon transparent glass cladding iron nickel molybdenum magnetic nanometer that graphene and step 9 are obtained is according to 0.04:1
(mass ratio) is matched, and is uniformly mixed within mechanical stirring 0.5 hour.It is put into 100ml pyroreaction kettle, 200 DEG C, heating rate
For 5 DEG C/min, react within soaking time 10 hours, obtained product is washed for several times with dehydrated alcohol, 40 DEG C of vacuum dryings.Obtain oxygen
Graphite alkene coats lithium aluminium silicon transparent glass and coats iron nickel molybdenum magnetic nanoparticle.
(3) it characterizes
Using AgilentPNA-L5230C vector network analyzer test material electromagnetic parameter and calculate reflectivity.With step 5
The ratio mixing that the graphene oxide that solvent-thermal method obtains coats iron nickel molybdenum nano particle and paraffin according to mass ratio 3:2 is carried out,
It is respectively 7mm and 3mm that outer diameter and inner diameter, which is made, with a thickness of the coaxial sample of 2.5mm or so.Sample is measured in 2-18GHz frequency range
On magnetic conductivity and dielectric constant, the reflection loss RL and impedance matching Z of the single-layer absorber be respectively adopted formula (1) and
(2) calculating simulation is carried out:
(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
For embodiment 2 difference from example 1 is that in step 10, graphene and lithium aluminium silicon transparent glass coat iron nickel molybdenum
The ratio of nano particle is different, other schemes are same as Example 1.
In step 10, lithium aluminium silicon transparent glass cladding iron nickel molybdenum magnetic nanometer that graphene and step 9 are obtained according to
0.01:1(mass ratio) it is matched.
Embodiment 3
For embodiment 3 difference from example 1 is that in step 10, graphene and lithium aluminium silicon transparent glass coat iron nickel molybdenum
The ratio of nano particle is different, other schemes are same as Example 1.
In step 10, lithium aluminium silicon transparent glass cladding iron nickel molybdenum magnetic nanometer that graphene and step 9 are obtained according to
0.02:1(mass ratio) it is matched.
Embodiment 4
For embodiment 4 difference from example 1 is that in step 10, graphene and lithium aluminium silicon transparent glass coat iron nickel molybdenum
The ratio of nano particle is different, other schemes are same as Example 1.
In step 10, lithium aluminium silicon transparent glass cladding iron nickel molybdenum magnetic nanometer that graphene and step 9 are obtained according to
0.03:1(mass ratio) it is matched.
Embodiment 5
For embodiment 5 difference from example 1 is that in step 10, graphene and lithium aluminium silicon transparent glass coat iron nickel molybdenum
The ratio of nano particle is different, other schemes are same as Example 1.
In step 10, lithium aluminium silicon transparent glass cladding iron nickel molybdenum magnetic nanometer that graphene and step 9 are obtained according to
0.05:1(mass ratio) it is matched.
Embodiment 6
(1) ingredient
Iron: nickel=16:84(mass percent)
(2) preparation method
Embodiment 6 is difference from example 1 is that iron, nickel, molybdenum quality are very different, other schemes and 1 phase of embodiment
Together.
Embodiment 7
(1) ingredient
Iron: nickel=16:84(mass is very)
(2) preparation method
Embodiment 7 from embodiment 2 the difference is that iron, nickel, molybdenum quality are very different, other schemes and 2 phase of embodiment
Together.
Embodiment 8
(1) ingredient
Iron: nickel=16:84(mass is very)
(2) preparation method
Embodiment 8 from embodiment 3 the difference is that iron, nickel, molybdenum quality are very different, other schemes and 3 phase of embodiment
Together.
Embodiment 9
(1) ingredient
Iron: nickel=16:84(mass is very)
(2) preparation method
Embodiment 9 from embodiment 4 the difference is that iron, nickel, molybdenum quality are very different, other schemes and 4 phase of embodiment
Together.
Embodiment 10
(1) ingredient
Iron: nickel=16:84(mass is very)
(2) preparation method
Embodiment 10 from embodiment 5 the difference is that iron, nickel, molybdenum quality are very different, other schemes and 5 phase of embodiment
Together.
Embodiment 11
(1) ingredient
Iron: nickel: molybdenum=16:79:5(mass is very)
(2) preparation method
Embodiment 11 is difference from example 1 is that iron, nickel, molybdenum quality are very different, other schemes and 1 phase of embodiment
Together.
Embodiment 12
(1) ingredient
Iron: nickel: molybdenum=16:79:5(mass is very)
(2) preparation method
Embodiment 12 from embodiment 2 the difference is that iron, nickel, molybdenum quality are very different, other schemes and 2 phase of embodiment
Together.
Embodiment 13
(1) ingredient
Iron: nickel: molybdenum=16:79:5(mass is very)
(2) preparation method
Embodiment 13 from embodiment 3 the difference is that iron, nickel, molybdenum quality are very different, other schemes and 3 phase of embodiment
Together.
Embodiment 14
(1) ingredient
Iron: nickel: molybdenum=16:79:5(mass is very)
(2) preparation method
Embodiment 14 from embodiment 4 the difference is that iron, nickel, molybdenum quality are very different, other schemes and 4 phase of embodiment
Together.
Embodiment 15
(1) ingredient
Iron: nickel: molybdenum=16:79:5(mass is very)
(2) preparation method
Embodiment 15 from embodiment 5 the difference is that iron, nickel, molybdenum quality are very different, other schemes and 5 phase of embodiment
Together.
Experimental result:
It is saturating that graphene oxide cladding lithium aluminium silicon is prepared by DC arc plasma and sintering process and solvent-thermal method
Bright glass fluxing technique iron nickel molybdenum nano particle.The material has had both the high magnetic permeability of iron nickel molybdenum super-permalloy and by core-shell structure copolymer knot
The advantages of high dielectric constant caused by high interfacial polarization caused by structure.So that the frequency of reflection loss absorption peak is past high
It is moved at frequency, optimizes impedance matching, further improve absorbing property.Pass through AgilentPNA-L5230C vector network point
The magnetic conductivity and dielectric constant that analyzer test material obtains, the square reflection loss RL and impedance matching Z of the single-layer absorber
Formula (1) is respectively adopted 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.Iron nickel molybdenum base before and after the oxidizing thermal treatment being calculated
Impedance matching Z and reflection loss RL such as Fig. 2 and 3 of magnetic nanoparticle.From fig. 2 it can be seen that when with a thickness of 1.5 mm,
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 matching
The curve of Z obviously compares without horizontal line when oxidizing thermal treatment close to y=1, and impedance matching Z has obtained apparent optimization.From
When in Fig. 3 as can be seen that without oxidizing thermal treatment, the minimum value of reflection loss is -20.5 dB, by oxidizing thermal treatment
Afterwards, the minimum value of reflection loss has reached -40.7 dB, and the frequency for absorbing peak-to-peak value is mobile toward high frequency treatment, and absorbing property obtains
Apparent raising is arrived.
Claims (5)
1. a kind of iron nickel molybdenum base magnetic nanometer composite material with excellent microwave absorbing property, it is characterised in that: described in it
Composite material is iron nickel molybdenum magnetic nanoparticle, lithium aluminium silicon transparent glass and graphene oxide respectively.
2. iron nickel molybdenum magnetic nanometer composite material as described in claim 1, it is characterised in that: iron nickel molybdenum magnetic nanoparticle is
Kernel, lithium aluminium silicon transparent glass are first layer inner casing, and graphene oxide is shell.
3. iron nickel molybdenum magnetic nanoparticle kernel as claimed in claim 2, it is characterised in that: inner core molecule metering-type is quality
Very: iron 16%, nickel 79%-84%, molybdenum 0-5%.
4. the preparation method of the iron nickel molybdenum magnetic nanometer composite material as described in claim 1 and 2, it is characterised in that: including with
Lower step:
S1, the elemental metals such as iron, nickel, molybdenum are prepared by iron nickel molybdenum ingot by electric arc melting；
S2, the iron nickel molybdenum ingot that S1 is prepared is made by iron nickel molybdenum magnetic by direct current-arc plasma metal nano powder the preparation method
Property nano particle；
S3, lithium glue, aluminium glue, silica gel are prepared respectively by sol-gel method, is mixed with according to the ratio that molar ratio is 1:1:2
At lithium aluminum silica gel body；
S4, iron nickel molybdenum magnetic nanoparticle and lithium aluminum silica gel body is made in molar ratio in the iron nickel molybdenum ingot that S2 and S3 are prepared
It is uniformly mixed for the ratio of 1:0.4, in a nitrogen atmosphere by sintering process, temperature is 500 DEG C, and heating rate is 5 DEG C/min, is protected
The warm time be 1 it is small at present, be prepared for lithium aluminium silicon transparent glass cladding iron nickel molybdenum magnetic nanoparticle；
S5, the lithium aluminium silicon transparent glass for taking a certain amount of graphene and S4 to prepare coat iron nickel molybdenum magnetic nanoparticle ratio machine
Tool stir 12 hours, then by solvent-thermal method at 200 DEG C, heat preservation 10 it is small prepare at present graphene oxide cladding lithium aluminium silicon it is transparent
Glass fluxing technique iron nickel molybdenum magnetic nanoparticle.
5. the iron nickel molybdenum magnetic nanoparticle mixing that a certain amount of graphene and S2 as described in claim requires 4 prepare,
It is characterized by: the proportional region of graphene and iron nickel molybdenum magnetic nanoparticle is 0.01 ~ 0.05:1.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113321423A (en) * | 2021-05-24 | 2021-08-31 | 吴尚荣 | Glass brick with magnetic adsorption effect and preparation method thereof |
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2019
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113321423A (en) * | 2021-05-24 | 2021-08-31 | 吴尚荣 | Glass brick with magnetic adsorption effect and preparation method thereof |
| CN113321423B (en) * | 2021-05-24 | 2023-01-06 | 苏州鱼得水电气科技有限公司 | Glass brick with magnetic adsorption effect and preparation method thereof |
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