CN110395716A - A kind of preparation method of the microwave defense material based on graphene - Google Patents
A kind of preparation method of the microwave defense material based on graphene Download PDFInfo
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- CN110395716A CN110395716A CN201910679568.3A CN201910679568A CN110395716A CN 110395716 A CN110395716 A CN 110395716A CN 201910679568 A CN201910679568 A CN 201910679568A CN 110395716 A CN110395716 A CN 110395716A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
Abstract
The present invention relates to electromagnetic protection technical fields, more specifically, it is related to a kind of preparation method of microwave defense material based on graphene, graphene oxide is prepared into redox graphene aeroge, certain pressure is imposed to it using press machine, obtains the microwave defense material based on graphene.The present invention realizes the double control of shielding and absorbing property by impedance matching and multi-layer structure design, on the one hand can carry out designing impedance matching by changing material surface resistivity, adjust its shielding properties；On the other hand, multi-layer structure design is carried out by graphene LBL self-assembly, control its absorbing property, it is adjusted by means such as simple mechanics, calorifics, density degree by changing material can further adjust the surface impedance and multilayered structure of material, and then realize electro-magnetic screen function and inhale the mutual conversion between wave energy that there is practical value.
Description
Technical field
The present invention relates to electromagnetic protection technical fields, more specifically, are related to a kind of electromagnetic protection material based on graphene
The preparation method of material.
Background technique
With the fast development of modern science and technology, each electron-like, the work and life that electrical equipment is people are brought
Great convenience.At the same time, it has been inevitably generated electromagnetic radiation during electronics, electric equipment operation, not only threatened
To the health of the mankind, interfering with each other between electronics, electrical equipment is also created, influences equipment normal operation.When especially 5G
The arriving in generation, electromagnetic radiation develop to high frequency direction, cause more serious harm.Currently, control electromagnetic radiation pollution
Most efficient method is electromagnetic shielding and suction wave.Electromagnetic shielding material inhibits electromagnetism mainly by way of reflection electromagnetic wave
Radiation；Absorbing material is then the energy for converting the energy of electromagnetic wave in the way of dielectric loss and magnetic loss the other forms such as thermal energy
Amount, thoroughly to eliminate electromagnetic radiation.
Shielding material and absorbing material have different applications, and the electromagnetism that shielding material is usually applied to electronic product is simultaneous
It is installed with meter, human body electromagnetic protection and the leakage of anti-electromagnetic information etc.；Absorbing material be then widely used in it is military it is stealthy, microwave is dark
The fields such as room.But material mutually inhibits the reflection and absorption of electromagnetic wave, material is main to the albedo of electromagnetic wave
Depending on the level of impedance match (the intrinsic wave impedance of air is 377 Ω) on its surface and free surrounding space, level of impedance match is got over
Height, reflection when electromagnetic wave incident material surface is weaker, and most of electromagnetic wave can go deep into material internal；Conversely, impedance matching
Degree is lower, and material surface is stronger to the albedo of electromagnetic wave, and corresponding absorbing property will reduce.Therefore, researcher needs
Different shielding or absorbing material are designed according to the actual situation, and same material is difficult to have both efficient electromagnetic shielding and inhales wave
Function.
Graphene is a kind of novel two-dimentional carbon nanomaterial, with great specific surface area and excellent conductive, thermally conductive
Performance.On the one hand, the high conductivity of graphene brings certain electrical loss, and high-specific surface area provides interface abundant,
At these interfaces multiple scattering and phase cancellation occur for part electromagnetic wave, play wave-absorbing effect；On the other hand, high electric conductivity
It will cause graphene surface impedance and air mismatch, improve the albedo to electromagnetic wave.Therefore, graphene is anti-in electromagnetism
Highly researcher goes to explore and develop the potential using value in protector for collar domain.The patent Shen of 108531005 A of Publication No. CN
A kind of graphene electromagnetic screen coating and preparation method thereof please be disclose, it is graphene-doped in resin matrix, it has constructed even
Continuous conductive channel enhances coating to the albedo of electromagnetic wave, and then improves its shield effectiveness.Publication No. CN
The patent application of 106883445 A discloses a kind of preparation method based on modified graphene Wave suction composite material, and use changes
Property grapheme foam as filler be added resin matrix in, prepare the Wave suction composite material of multilayered structure.Graphene material at present
Material is all solely to consider that shielding or absorbing property carry out designing material structure in the relevant application study in electromagnetic protection field, this
The grapheme material that sample is designed often is single shielding material or absorbing material, and material shields once forming
Or absorbing property would become hard to further change.
Summary of the invention
In the presence of overcoming the shortcomings of the prior art, the present invention provides a kind of microwave defense material based on graphene
Preparation method, solve existing microwave defense material and have a single function, material once form, structure, which is just difficult to happen, further to be changed
Become, shielding or absorbing property will be unable to or be difficult to be changed.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is as follows:
A kind of preparation method of the microwave defense material based on graphene, comprising the following steps:
S1, it weighs a certain amount of graphene oxide powder and is mixed into distilled water, ultrasonic disperse obtains graphene oxide dispersion；
S2, the graphene oxide dispersion for taking S1 to prepare are transferred in hydrothermal reaction kettle, certain temperature are heated to, when reacting one section
Between after take out, obtain graphene oxide hydrogel；
S3, it after the graphene oxide hydrogel of S2 preparation is impregnated cleaning with ethanol solution, is placed in freeze dryer, it is cold at low temperature
Graphite oxide aerogel is made after dry a period of time is lyophilized；
S4, the S3 graphite oxide aerogel prepared is placed in tube type resistance furnace, under an inert atmosphere with certain heating speed
Rate is heated to high temperature and keeps the temperature a period of time, is cooled to room temperature to tube type resistance furnace, takes out sample, obtain redox graphene
Aeroge；
S5, the S4 redox graphene aeroge prepared is placed in particular manufacturing craft, it is imposed using press machine certain
Pressure obtains the microwave defense material based on graphene.
Further, the concentration of graphene oxide dispersion is 2 ~ 10mg/mL in the S1.
Further, graphene oxide dispersion adds reproducibility reagent after being transferred to hydrothermal reaction kettle in the S2.
Further, the reproducibility reagent is at least one of hydroiodic acid, hydrazine, ascorbic acid, sodium borohydride, dosage
It is 1 ~ 3 times of graphene oxide quality.
Further, hydrothermal temperature is 60 ~ 200 DEG C in the S2, and the hydro-thermal reaction time is 4 ~ 12h.
Further, it is -20 ~ -60 DEG C that temperature is freeze-dried in the S3, and sublimation drying is 1 ~ 4 day in the S3.
Further, heating rate is 1 ~ 8 DEG C/min in the S4, and heating temperature is 1000 ~ 3000 DEG C, and soaking time is
1~3h。
Further, press machine presses to redox graphene aeroge of different sizes in the S5, can obtain
To the thickness microwave defense material based on graphene different from density degree.
Further, the microwave defense material realizes the transformation from suction wave energy to function of shielding by applying pressure；
Microwave defense material passes through high-temperature expansion in an inert atmosphere, realizes the transformation from function of shielding to suction wave energy.
Compared with prior art, the advantageous effect of present invention is that:
The present invention provides a kind of preparation methods of microwave defense material based on graphene, pass through impedance matching and multilayered structure
Design realizes the double control of shielding and absorbing property, on the one hand can carry out impedance by changing material surface resistivity
With design, its shielding properties is adjusted；On the other hand, multi-layer structure design is carried out by graphene LBL self-assembly, controls its suction
Wave performance is adjusted by means such as simple mechanics, calorifics, and the density degree by changing material can be adjusted further
The surface impedance and multilayered structure of material, and then realize electro-magnetic screen function and inhale the mutual conversion between wave energy have real
With value.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of the microwave defense material based on graphene provided by the invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
A kind of preparation method of the microwave defense material based on graphene, comprising the following steps:
S1, it weighs a certain amount of graphene oxide powder and is mixed into distilled water, ultrasonic disperse obtains the oxygen that concentration is 2 ~ 10mg/mL
Graphite alkene dispersion liquid；
S2, the graphene oxide dispersion for taking S1 to prepare are transferred in hydrothermal reaction kettle, can add a certain amount of go back thereto
Immunogenic agent is heated to 60 ~ 200 DEG C, takes out after reacting 4 ~ 12h, obtains graphene oxide hydrogel；
S3, it after the graphene oxide hydrogel of S2 preparation is impregnated cleaning with ethanol solution, is placed in freeze dryer, -20 ~ -60
Graphite oxide aerogel is made after being freeze-dried 1 ~ 4 day at DEG C；
S4, the S3 graphite oxide aerogel prepared is placed in tube type resistance furnace, under an inert atmosphere with the liter of 1 ~ 8 DEG C/min
Warm rate is heated to 1000 ~ 3000 DEG C and keeps the temperature 1 ~ 3h, is cooled to room temperature to tube type resistance furnace, takes out sample, obtain oxygen reduction
Graphite alkene aeroge；
S5, the S4 redox graphene aeroge prepared is placed in particular manufacturing craft, it is imposed using press machine certain
Pressure obtains the microwave defense material based on graphene.
In the present embodiment, the reproducibility reagent be at least one of hydroiodic acid, hydrazine, ascorbic acid, sodium borohydride,
Dosage is 1 ~ 3 times of graphene oxide quality.
According to the above method, by changing S5 pressure, the shield effectiveness of the microwave defense material obtained based on graphene
It is as shown in table 1 with absorbing property comparison:
The shield effectiveness and absorbing property of the microwave defense material based on graphene prepared under 1 different pressures of table compare
| Pressure (MPa) | Shield effectiveness (dB) | Absorbing property (dB) |
| 0 | 53 | 48 |
| 50 | 55 | 45 |
| 100 | 59 | 40 |
| 150 | 61 | 34 |
| 200 | 65 | 23 |
| 250 | 68 | 15 |
| 300 | 72 | 9 |
Embodiment 1
S1, the graphene oxide powder for weighing 200mg are mixed into 100mL distilled water, and ultrasonic disperse obtains the oxidation stone of 2mg/mL
Black alkene dispersion liquid；
S2, the graphene oxide dispersion for taking S1 to prepare are transferred in hydrothermal reaction kettle, and 200mg hydroiodic acid is added, is heated to 60
DEG C, 4h is reacted, graphene oxide hydrogel is obtained；
S3, it after the graphene oxide hydrogel of S2 preparation is impregnated cleaning with ethanol solution, is placed in freeze dryer, at -60 DEG C
After freeze-drying 1 day, graphite oxide aerogel is made；
S4, the S3 graphite oxide aerogel prepared is placed in tube type resistance furnace, under an inert atmosphere with the heating of 1 DEG C/min
Rate is heated to 1000 DEG C and keeps the temperature 1 h, is cooled to room temperature to tube type resistance furnace, takes out sample, obtain redox graphene
Aeroge；
S5, the S4 redox graphene aeroge prepared is placed in particular manufacturing craft, 300MPa is imposed to it using press machine
Pressure, obtain the microwave defense material based on graphene.
Embodiment 2
S1, the graphene oxide powder for weighing 300mg are mixed into 100mL distilled water, and ultrasonic disperse obtains the oxidation stone of 3mg/mL
Black alkene dispersion liquid；
S2, the graphene oxide dispersion for taking S1 to prepare are transferred in hydrothermal reaction kettle, and 900mg ascorbic acid and hydrazine mixing is added
Object (mass ratio 1:1) is heated to 80 DEG C, reacts 6h, obtains graphene oxide hydrogel；
S3, it after the graphene oxide hydrogel of S2 preparation is impregnated cleaning with ethanol solution, is placed in freeze dryer, at -40 DEG C
After freeze-drying 2 days, graphite oxide aerogel is made；
S4, the S3 graphite oxide aerogel prepared is placed in tube type resistance furnace, under an inert atmosphere with the heating of 2 DEG C/min
Rate is heated to 1500 DEG C and keeps the temperature 3h, is cooled to room temperature to tube type resistance furnace, takes out sample, obtains redox graphene gas
Gel；
S5, the S4 redox graphene aeroge prepared is placed in particular manufacturing craft, 200MPa is imposed to it using press machine
Pressure, obtain the microwave defense material based on graphene.
Embodiment 3
S1, the graphene oxide powder for weighing 500mg are mixed into 100mL distilled water, and ultrasonic disperse obtains the oxidation stone of 5mg/mL
Black alkene dispersion liquid；
S2, the graphene oxide dispersion for taking S1 to prepare are transferred in hydrothermal reaction kettle, and 1000mg sodium borohydride is added, is heated to
100 DEG C, 8h is reacted, obtains graphene oxide hydrogel；
S3, it after the graphene oxide hydrogel of S2 preparation is impregnated cleaning with ethanol solution, is placed in freeze dryer, at -30 DEG C
After freeze-drying 3 days, graphite oxide aerogel is made；
S4, the S3 graphite oxide aerogel prepared is placed in tube type resistance furnace, under an inert atmosphere with the heating of 5 DEG C/min
Rate is heated to 3000 DEG C and keeps the temperature 1 .5 h, is cooled to room temperature to tube type resistance furnace, takes out sample, obtain reduction-oxidation graphite
Alkene aeroge；
S5, the S4 redox graphene aeroge prepared is placed in particular manufacturing craft, 100MPa is imposed to it using press machine
Pressure, obtain the microwave defense material based on graphene.
Embodiment 4
S1, the graphene oxide powder for weighing 1000mg are mixed into 100mL distilled water, and ultrasonic disperse obtains the oxidation of 10mg/mL
Graphene dispersing solution；
S2, the graphene oxide dispersion for taking S1 to prepare are transferred in hydrothermal reaction kettle, are added without any reproducibility reagent, are heated
To 180 DEG C, 12h is reacted, obtains graphene oxide hydrogel；
S3, it after the graphene oxide hydrogel of S2 preparation is impregnated cleaning with ethanol solution, is placed in freeze dryer, at -20 DEG C
After freeze-drying 4 days, graphite oxide aerogel is made；
S4, the S3 graphite oxide aerogel prepared is placed in tube type resistance furnace, under an inert atmosphere with the heating of 8 DEG C/min
Rate is heated to 2000 DEG C and keeps the temperature 2 h, is cooled to room temperature to tube type resistance furnace, takes out sample, obtain redox graphene
Aeroge；
S5, without applying any pressure to redox graphene aeroge prepared by S4, obtain the electromagnetism based on graphene
Protective materials.
In the above-described embodiments, by simply changing the size of pressure applied, i.e., the thickness of controllable material prepared
Degree and density degree, and then regulate and control its reflection and absorbability to electromagnetic wave.As shown in Figure 1, when to redox graphene
When aeroge applies a higher pressure, since the distance between graphene sheet layer shortens, redox graphene aeroge
Become finer and close, electric conductivity is substantially improved, and surface impedance matching degree declines the shield effectiveness, it can be achieved that high；When to reduction
When graphite oxide aerogel application pressure is smaller, redox graphene gel possesses interface abundant, and electromagnetic wave is at interface
Upper generation multiple scattering and phase cancellation, realize high absorbing property.In addition, applying to the graphene absorbing material of S5 preparation
Pressure carries out other similar processing, makes lamella hypotelorism, it can be achieved that being changed from suction wave energy to function of shielding；In indifferent gas
High-temperature heat expansion or other similar processing are carried out to the graphene absorbing material of S5 preparation under atmosphere, increase piece interlamellar spacing, it can be real
Now from function of shielding to wave energy transformation is inhaled, shown in Fig. 1, (a) is graphene shielding material made of high pressure compacting in figure；(b)
For graphene absorbing material made of low pressure compacting.
Only presently preferred embodiments of the present invention is explained in detail above, but the present invention is not limited to above-described embodiment,
Within the knowledge of a person skilled in the art, it can also make without departing from the purpose of the present invention each
Kind variation, various change should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of preparation method of the microwave defense material based on graphene, which comprises the following steps:
S1, graphene oxide powder is mixed into distilled water, ultrasonic disperse obtains graphene oxide dispersion；
S2, the graphene oxide dispersion for taking S1 to prepare are transferred in hydrothermal reaction kettle, and heating is taken out after reaction a period of time, are obtained
Obtain graphene oxide hydrogel；
S3, it after the graphene oxide hydrogel of S2 preparation is impregnated cleaning with ethanol solution, is placed in freeze dryer, it is cold at low temperature
Dry rear obtained graphite oxide aerogel is lyophilized；
S4, the S3 graphite oxide aerogel prepared is placed in tube type resistance furnace, is heated to high temperature under an inert atmosphere and protects
It warm a period of time, is cooled to room temperature to tube type resistance furnace, takes out sample, obtain redox graphene aeroge；
S5, the S4 redox graphene aeroge prepared is placed in mold, is pressed, is obtained based on graphene using press machine
Microwave defense material.
2. a kind of preparation method of microwave defense material based on graphene according to claim 1, it is characterised in that: institute
The concentration for stating graphene oxide dispersion in S1 is 2 ~ 10mg/mL.
3. a kind of preparation method of microwave defense material based on graphene according to claim 1, it is characterised in that: institute
It states after graphene oxide dispersion in S2 is transferred to hydrothermal reaction kettle and adds reproducibility reagent.
4. a kind of preparation method of microwave defense material based on graphene according to claim 3, it is characterised in that: institute
Stating reproducibility reagent is at least one of hydroiodic acid, hydrazine, ascorbic acid, sodium borohydride, and dosage is the 1 of graphene oxide quality
~ 3 times.
5. a kind of preparation method of microwave defense material based on graphene according to claim 1, it is characterised in that: institute
Stating hydrothermal temperature in S2 is 60 ~ 200 DEG C, and the hydro-thermal reaction time is 4 ~ 12h.
6. a kind of preparation method of microwave defense material based on graphene according to claim 1, it is characterised in that: institute
Stating and being freeze-dried temperature in S3 is -20 ~ -60 DEG C, and sublimation drying is 1 ~ 4 day in the S3.
7. a kind of preparation method of microwave defense material based on graphene according to claim 1, it is characterised in that: institute
Stating heating rate in S4 is 1 ~ 8 DEG C/min, and heating temperature is 1000 ~ 3000 DEG C, and soaking time is 1 ~ 3h.
8. a kind of preparation method of microwave defense material based on graphene according to claim 1, it is characterised in that: institute
It states press machine in S5 and presses to redox graphene aeroge of different sizes, available thickness is different from density degree
The microwave defense material based on graphene.
9. a kind of preparation method of microwave defense material based on graphene according to claim 1, it is characterised in that: institute
Microwave defense material is stated by applying pressure, realizes the transformation from suction wave energy to function of shielding；Microwave defense material is in inertia
By high-temperature expansion in atmosphere, the transformation from function of shielding to suction wave energy is realized.
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Cited By (1)
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