CN106211728A - A kind of graphene coated Fe3o4the composite wave-suction material preparation method of nano-particle - Google Patents
A kind of graphene coated Fe3o4the composite wave-suction material preparation method of nano-particle Download PDFInfo
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- CN106211728A CN106211728A CN201610536001.7A CN201610536001A CN106211728A CN 106211728 A CN106211728 A CN 106211728A CN 201610536001 A CN201610536001 A CN 201610536001A CN 106211728 A CN106211728 A CN 106211728A
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- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
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Abstract
The invention discloses a kind of graphene coated Fe3O4The composite wave-suction material preparation method of nano-particle, its step: (1). by Fe3O4Nano-particle is dissolved in deionized water and carries out ultrasonic disperse, obtains dispersion liquid A；(2). a certain amount of Graphene is dissolved in deionized water and carries out ultrasonic disperse, obtain dispersion liquid B；(3). dispersion liquid A is added dropwise in the dispersion liquid B being stirred continuously, obtains mixed liquor；Obtain black precipitate after Li Xin, use vacuum filtration, vacuum drying, obtain Graphene cladding Fe for the first time3O4Product (the Fe of nano-particle3O4@G)；(4). the product obtained in step (3) is distributed to the ethanol water of 80ml Graphene, loads in autoclave, hydro-thermal reaction at 180 DEG C, then wash with vacuum filtration ionized water, vacuum drying, obtain Graphene second time cladding Fe3O4The product of nano-particle i.e. obtains graphene coated Fe3O4The composite wave-suction material of nano-particle.The method not only preparation process is simple, and the absorbing material prepared has, and absorbing property is strong, inhale the advantage that ripple frequency range is wide.
Description
Technical field
The invention belongs to absorbing material technical field, be specifically related to a kind of graphene coated Fe3O4The compound suction of nano-particle
Wave material preparation method.
Background technology
Along with the development of modern science and technology, although electrical equipment provides great convenience for social production, but it is extensive
Application defines the electromagnetic radiation environment of complexity, and the normal use of electronic machine and equipment, spoke are not only disturbed in these electromagnetic radiation
Penetrate the health that seriously also can affect the mankind.At present, the effective method solving electromagnetic radiation pollution is to use absorbing material, inhales ripple
Material can absorb, attenuation electromagnetic radiation, converts electromagnetic energy into thermal energy consumption and dissipates.Wherein, Graphene have uniqueness mechanics,
Electricity, optics and magnetic performance attract wide attention, and research shows, graphene oxide sheet and redox graphene exist relatively
Many defects functional group, can improve impedance matching property, promotes to change to fermi level state from adjacent states, beneficially electromagnetism
The infiltration of ripple and absorption, become a kind of novel wave-absorbing material；Fe3O4Nano material typically has dielectric loss as one
With magnetic loss dual function in the dielectric material of one, due to its low cost, the absorbent properties reason such as preferably, it is at electromagnetic shielding
Application with electro-magnetic wave absorption has caused the concern of people.But, simple undressed Fe3O4Nano material is as suction
Wave material, can manifest oxidizable, high density, frequency absorption section are narrow, the problems such as high frequency permeability is low, electro-magnetic wave absorption performance is subject to
Greatly limit.To this end, Chinese scholars is by Graphene and Fe3O4It is combined and prepares composite wave-suction material, make absorbing material have
There are wider suction ripple bandwidth and relatively low reflection loss.Such as, Chinese patent CN104163919A disclose a kind of polyaniline/
Graphene oxide/ferroso-ferric oxide composite wave-suction material, prepared composite 2～18GHz internal reflection loss values less than-
The bandwidth of 10dB is 2.62GHz, and minimal reflection loss value is-46.5GHz.But Graphene and four oxygen in prior art
The preparation process changing three-iron composite wave-suction material is complicated, and the response time is long, and part is combined with poisonous conduction high polymer, preparation
It is not good enough that composite still suffers from absorbing property, less to electro-magnetic wave absorption peak value, absorbs the narrow problem of frequency range, it will usually more than 40
Wt%, even more than 60 wt%, this increases not only the density of absorbing material, increases the weight of absorbent, improves production cost.
Summary of the invention
It is an object of the invention to solve prepared by prior art the technical problem that absorbing material exists, and propose one
Graphene coated Fe3O4The composite wave-suction material preparation method of nano-particle, the method not only preparation process is simple, and adds
Wave absorbing agent content be 30 wt%, prepared absorbing material has that absorbing property is strong, inhale the advantage that ripple frequency range is wide.
This invention is achieved through the following technical solutions:
A kind of graphene coated Fe3O4The composite wave-suction material preparation method of nano-particle, including step in detail below:
(1). by a certain amount of Fe3O4Nano-particle is dissolved in deionized water and carries out ultrasonic disperse, and ultrasonic 10-20min obtains
Dispersion liquid A;
(2). a certain amount of Graphene is dissolved in deionized water and carries out ultrasonic disperse, ultrasonic 10-20min, obtain dispersion liquid B；
(3). the dispersion liquid A obtained in step (1) is added dropwise in the step (2) being stirred continuously in the dispersion liquid B obtained,
Obtain mixed liquor；By mixed liquor centrifugal 10-20min under 5000-10000r/min, obtain black precipitate, use vacuum filtration, use
Deionized water is washed, and is vacuum dried at 40-60 DEG C, obtains Graphene cladding Fe for the first time3O4The product of nano-particle
(Fe3O4@G)；
(4). 80mg graphite oxide is dissolved in 80mL ethanol and ethanol water that water volume ratio is 1:1, obtains Graphene
Ethanol water, the product (Fe that will obtain in step (3)3O4@G) it is distributed in the ethanol water of 80ml Graphene, obtain
Uniform mixed liquor, loads in autoclave, hydro-thermal reaction at 180 DEG C, and the response time is 6-12h, then uses vacuum filtration
After, wash with deionized water, be vacuum dried at 45 DEG C, obtain Graphene second time cladding Fe3O4The product of nano-particle
(Fe3O4@G) i.e. obtain graphene coated Fe3O4The composite wave-suction material of nano-particle.
In ethanol water described in above-mentioned steps (4), wherein, the volume ratio of second alcohol and water is 1:2.
The present invention compared with prior art has a following beneficial effect:
The method of the present invention uses the anti-self assembly of hydro-thermal, and Graphene is coated with Fe twice3O4Composite wave-absorbing prepared by nano-particle
Manufacture of materials is with low cost, and preparation technology is simple, and the used time is shorter, and the wave absorbing agent content of addition is less than 30wt%, and material lightweight, energy is many
Secondary reflection, suction ripple are strong, and regulation absorbing material thickness can realize the electro-magnetic wave absorption under different frequency.
Accompanying drawing explanation
Fig. 1 is the graphite oxide cladding Fe of preparation in embodiment 13O4The reflection loss of the composite wave-suction material of nano-particle
Figure.
Fig. 2 is the thermal expansion graphene coated Fe of preparation in embodiment 23O4The reflection loss of the composite of nano-particle
Figure.
Fig. 3 is the redox graphene cladding Fe of preparation in embodiment 33The reflection of the composite of O nano-particle is damaged
Consumption figure.
Detailed description of the invention
Below by way of particular specific embodiment and accompanying drawing, the present invention is made the most in detail.
Graphene (G) described in the embodiment of the present invention is in graphite oxide, thermal expansion Graphene, redox graphene
One, after it is specifically stated:
Embodiment 1
A kind of graphene coated Fe of the present invention3O4The composite wave-suction material preparation method of nano-particle, wherein, Graphene (G)
For graphite oxide, specifically comprise the following steps that
(1). weigh 0.076g Fe3O4Nano-particle is dissolved in 200ml deionized water and carries out ultrasonic disperse, ultrasonic 10-
20min, obtains dispersion liquid A；
(2). weigh 25mg graphite oxide and be dissolved in 250ml deionized water and carry out ultrasonic disperse, ultrasonic 10-20min, obtain
Dispersion liquid B；
(3). in the dispersion liquid B that the step (2) that the dispersion liquid A obtained in step (1) is added dropwise to be stirred continuously obtains, obtain
Mixed liquor；By mixed liquor centrifugal 0-20min under 8000r/min, obtain black precipitate, with vacuum filtration, clean with deionized water,
It is vacuum dried at 45 DEG C, obtains graphite oxide cladding Fe for the first time3O4Product (the Fe of nano-particle3O4@GO)；
(4). 80mg graphite oxide is dissolved in 80mL ethanol and ethanol water that water volume ratio is 1:1, obtains Graphene
Ethanol water, the product (Fe that will prepare in step (3)3O4@GO) evenly spread to the ethanol water of 30ml graphite oxide
In, above-mentioned uniform mixed liquor is loaded pyroreaction still, at a temperature of 180 DEG C, processes 12h, then with after vacuum filtration, spend
Ionized water is washed, and is vacuum dried at 45 DEG C, obtains Graphene second time cladding Fe3O4Product (Fe3O4@GO/GO), i.e. obtain
Graphene oxide cladding Fe3O4The composite wave-suction material of nano-particle.
The composite wave-suction material of preparation in the present embodiment 1 is mixed with the ratio of 3:7 with paraffin, uses Agilent Technologies to have
Limit company produces, and model is that the transmission/reflection vector Network Analyzer of N5245A carries out absorbing property test, obtains different
Join graphite oxide cladding Fe under thickness3O4The reflection loss of nano-particles reinforcement absorbing material, as it is shown in figure 1, can be seen by Fig. 1
Going out, when composite wave-suction material coating layer thickness is 2mm, reflection loss (RL) is-35.5dB；Coating layer thickness is 2.0-5.5mm change
Time, effectively inhale ripple (RL <-10dB) frequency coverage 4-18GHz.
Embodiment 2
A kind of graphene coated Fe of the present invention3O4The composite wave-suction material preparation method of nano-particle, wherein, Graphene is heat
Expanded graphite alkene, specifically comprises the following steps that
(1). weigh 0.076g Fe3O4Nano-particle is dissolved in 200ml deionized water and carries out ultrasonic disperse, ultrasonic 10-
20min, obtains dispersion liquid A；
(2). weigh thermal expansion Graphene prepared by 25mg and be dissolved in 250ml deionized water and carry out ultrasonic disperse, ultrasonic 10-
20min, obtains dispersion liquid B；
(3). under rapid stirring, the dispersion liquid A obtained in step (1) is added dropwise to the step (2) being stirred continuously
In the dispersion liquid B obtained, obtain mixed liquor；By mixed liquor centrifugal 0-20min under 8000r/min, obtain black precipitate, use vacuum
Sucking filtration, cleans with deionized water, obtains Graphene cladding Fe for the first time 45 DEG C of vacuum drying3O4The product of nano-particle
(Fe3O4@r-GO)；
(4). 80mg thermal expansion Graphene is dissolved in 80mL ethanol and ethanol water that water volume ratio is 1:1, obtains graphite
The ethanol water of alkene,
Product (the Fe that will prepare in step (3)3O4@r-GO) evenly spread to the ethanol water of 30ml thermal expansion Graphene
In, above-mentioned uniform mixed liquor is loaded pyroreaction still, at a temperature of 180 DEG C, processes 12h, then with after vacuum filtration, spend
Ionized water is washed, and is vacuum dried at 45 DEG C, obtains Graphene second time cladding Fe3O4Product (Fe3O4@r-GO/r-GO), i.e.
Obtain thermal expansion graphene coated Fe3O4The composite wave-suction material of nano-particle.
Being mixed with the ratio of 3:7 with paraffin by the composite wave-suction material of preparation in the present embodiment 2, employing model is N5245A
Transmission/reflection vector Network Analyzer carry out absorbing property test, obtain thermal expansion graphene coated under Different matching thickness
Fe3O4The reflection loss of ferroferric oxide nano granules composite wave-suction material, as in figure 2 it is shown, as seen from Figure 2, composite wave-absorbing
When material coating thickness is 4mm, reflection loss (RL) is-39dB；When coating layer thickness is 2.0-5.5mm change, effectively inhale ripple (RL
<-10dB) frequency coverage 4.7-18GHz.
Embodiment 3
A kind of graphene coated Fe of the present invention3O4The composite wave-suction material preparation method of nano-particle, wherein, Graphene is for also
Former graphene oxide, specifically comprises the following steps that
(1). weigh 0.076g Fe3O4Nano-particle is dissolved in 200ml deionized water and carries out ultrasonic disperse, ultrasonic 10-
15min, obtains dispersion liquid A；
(2). weigh redox graphene prepared by 25mg and be dissolved in 250ml deionized water and carry out ultrasonic disperse, ultrasonic 10-
20min, obtains dispersion liquid B；
(3). under rapid stirring, the dispersion liquid A obtained in step (1) is added dropwise to the step (2) being stirred continuously
In the dispersion liquid B obtained, obtain mixed liquor；By mixed liquor centrifugal 0-20min under 8000r/min, obtain black precipitate, use vacuum
Sucking filtration, cleans with deionized water, obtains Graphene cladding Fe for the first time 45 DEG C of vacuum drying3O4The product of nano-particle
(Fe3O4@RGO)；
(4). 80mg redox graphene is dissolved in 80mL ethanol and ethanol water that water volume ratio is 1:1, obtains stone
The ethanol water of ink alkene, the product (Fe that will prepare in step (3)3O4@RGO) evenly spread to 30ml redox graphene
Ethanol water in, above-mentioned uniform mixed liquor is loaded pyroreaction still, processes 12h at a temperature of 180 DEG C, then take out by vacuum
After filter, wash with deionized water, be vacuum dried at 45 DEG C, obtain Graphene secondary cladding Fe3O4Product (Fe3O4@RGO/
RGO) redox graphene cladding Fe is i.e. obtained3O4The composite wave-suction material of nano-particle.
Being mixed with the ratio of 3:7 with paraffin by the composite wave-suction material of preparation in the present embodiment 3, employing model is N5245A
Transmission/reflection vector Network Analyzer carry out absorbing property test, obtain under Different matching thickness graphite oxide cladding Fe3O4
The reflection loss of nano-particles reinforcement absorbing material, as it is shown on figure 3, as seen from Figure 3, composite wave-suction material coating layer thickness is
During 3.0mm, reflection loss (RL) is-42dB；When coating layer thickness is 2.0-5.5mm change, effectively inhale ripple (RL <-10dB) frequency
Coverage 4.1-18GHz.
Claims (2)
1. a graphene coated Fe3O4The composite wave-suction material preparation method of nano-particle, it is characterised in that the method includes
Step in detail below:
By a certain amount of Fe3O4Nano-particle is dissolved in deionized water and carries out ultrasonic disperse, and ultrasonic 10-20min obtains dispersion liquid A
；
A certain amount of Graphene is dissolved in deionized water and carries out ultrasonic disperse, ultrasonic 10-20min, obtain dispersion liquid B；
The dispersion liquid A obtained in step (1) is added dropwise in the step (2) being stirred continuously in the dispersion liquid B obtained, is mixed
Close liquid；By mixed liquor centrifugal 10-20min under 5000-10000r/min, obtain black precipitate, use vacuum filtration, use deionization
Water is washed, and is vacuum dried at 40-60 DEG C, obtains Graphene cladding Fe for the first time3O4Product (the Fe of nano-particle3O4@G)；
80mg graphite oxide is dissolved in 80mL ethanol and ethanol water that water volume ratio is 1:1, obtains the ethanol of Graphene
Aqueous solution, the product (Fe that will obtain in step (3)3O4@G) it is distributed in the ethanol water of 80ml Graphene, obtain uniformly
Mixed liquor, load in autoclave, hydro-thermal reaction at 180 DEG C, the response time is 6-12h, then with after vacuum filtration, uses
Deionized water is washed, and is vacuum dried at 45 DEG C, obtains Graphene second time cladding Fe3O4Product (the Fe of nano-particle3O4@G)
I.e. obtain graphene coated Fe3O4The composite wave-suction material of nano-particle.
A kind of graphene coated Fe the most according to claim 13O4The composite wave-suction material preparation method of nano-particle, its
Being characterised by, the ethanol water described in above-mentioned steps (4), wherein, the volume ratio of second alcohol and water is 1:2.
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| CN109936974A (en) * | 2019-04-03 | 2019-06-25 | 厦门大学 | A kind of synthetic method of sandwich structure CoFe@C/ graphene electromagnetic wave absorbent material |
| CN110278702A (en) * | 2019-06-04 | 2019-09-24 | 江南石墨烯研究院 | A kind of high stretching high resiliency electromagnetic shielding composite material and preparation method thereof |
| CN111777063A (en) * | 2020-07-09 | 2020-10-16 | 西安交通大学 | Preparation method of nano material |
| CN112724641A (en) * | 2021-01-12 | 2021-04-30 | 电子科技大学 | Preparation method of polar polymer doped nano particles and composite wave-absorbing material containing same |
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| CN112724641A (en) * | 2021-01-12 | 2021-04-30 | 电子科技大学 | Preparation method of polar polymer doped nano particles and composite wave-absorbing material containing same |
| CN113015423A (en) * | 2021-02-22 | 2021-06-22 | 山东大学 | Fe/Fe with high electromagnetic wave absorption performance4N/Fe3O4-rGO nano material, preparation method and application |
| CN113015423B (en) * | 2021-02-22 | 2022-04-15 | 山东大学 | Fe/Fe with high electromagnetic wave absorption performance4N/Fe3O4-rGO nano material, preparation method and application |
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