CN109289718A - A kind of three-dimensional redox graphene aerogel material and preparation method thereof - Google Patents
A kind of three-dimensional redox graphene aerogel material and preparation method thereof Download PDFInfo
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- CN109289718A CN109289718A CN201811310432.7A CN201811310432A CN109289718A CN 109289718 A CN109289718 A CN 109289718A CN 201811310432 A CN201811310432 A CN 201811310432A CN 109289718 A CN109289718 A CN 109289718A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
Abstract
The invention discloses a kind of three-dimensional redox graphene aerogel materials and preparation method thereof, aerogel material is made of graphene oxide, redox graphene, whole fluffy spongy in black, three-dimensional redox graphene aeroge produces a large amount of micron order hole during forming three-dimensional structure.Aerogel material of the invention with paraffin after mixing, under the dosage for accounting for gross mass 10%, as matching thickness 2.5mm, in 2-18GHz frequency range, the reachable -8.2dB of reflection loss.The preparation process for utilizing the three-dimensional redox graphene aeroge simultaneously, can carry the metal nanoparticles such as ZnO in porous redox graphene internal void, and realization is to preparing the compound of material electromagnetic performance and regulate and control.
Description
Technical field
The present invention relates to aerogel material preparation technical field, specially a kind of three-dimensional redox graphene airsetting glue material
Material and preparation method thereof.
Background technique
Traditional absorbing material is based on absorbing by force, the features such as novel wave-absorbing material will then meet " thin, light, wide, strong ", and not
The absorbing material come should then meet stealthy multiple spectra, environment adaptation, high temperature resistant, marine climate resistant, Antiradiation, shock resistance etc. more
High request, the material of one-component are difficult to meet the requirement of these comprehensive performances.It is normal that the absorbing property of material mainly answers dielectric by it
Several and complex permeability codetermines, multiple material is carried out it is various forms of compound, to adjust the electromagnetic parameter of compound, to reach
To the requirement of impedance matching, wherein compound become of magnetic loss type absorbing material and dielectric loss type absorbing material improves absorbing property
Effective means.
Graphene itself has very strong dielectric loss, especially graphene as basis material, and there are a foregone conclusions with other
Sex-limited absorbing material progress is compound, and such as graphene-supported magnetic material not only can solve the big disadvantage of density, moreover it is possible to widen
It inhales wave frequency section, reaches lightweight, high-strength, wideband wave-absorbing effect.Three-dimensional aeroge is made in graphene, may be implemented in its hole
Other function structure, particle are carried in gap, and then assign this three-dimensional aeroge more functional applications.
Summary of the invention
The purpose of the present invention is to provide a kind of three-dimensional redox graphene aerogel materials and preparation method thereof, with solution
Certainly the problems mentioned above in the background art.
To achieve the above object, the invention provides the following technical scheme: a kind of three-dimensional redox graphene airsetting glue material
Material, aerogel material are made of graphene oxide, redox graphene, nano zine oxide and hole, whole fluffy in black
It is spongy, the carrying of nano-metal-oxide electromagnetic material is realized in the hole of the redox graphene aeroge.
Preferably, a kind of preparation method of three-dimensional redox graphene aerogel material, preparation method includes following
Step:
A, graphite powder is added in the beaker equipped with the 105ml concentrated sulfuric acid, ice bath stirring 3h；
B, potassium permanganate is added in the mixed solution obtained to step A, continues ice bath stirring 2h；
C, step B acquired solution is placed in room temperature water-bath, is slowly added to 210ml deionized water along wall of cup, and with aubergine
Smoke and gas steep and release, add mixed solution after water to continue to stir 30min；
D, 30% hydrogen peroxide of 15ml is slowly added dropwise into the resulting mixed solution of step C, solution left standstill is for 24 hours；
E, the resulting mixed solution of step D is outwelled into supernatant liquor, repeatedly washing centrifugation, the collection of gained graphite oxide is being cultivated
In ware, it is put into the 50 DEG C of dryings of baking oven constant temperature；
F, dry graphite oxide is dissolved in deionized water, is made into 1.5mg/ml solution, ultrasonic 2h；
G, the solution of step F is centrifuged, the supernatant liquor after taking centrifugation can obtain graphene oxide solution；
H, graphene oxide powder is dispersed in deionized water, the dispersion liquid of 3mg/ml to be made by ultrasonic wave；
I, dispersion liquid obtained by step H is placed in hydrothermal reaction kettle, 180 DEG C of heating 12h are cooled to room temperature, take out wet shape object, cold
Jelly is drying to obtain three-dimensional redox graphene aerogel material.
Preferably, in the step G, graphene oxide solution is poured into culture dish, it is dry at 50 DEG C, it can must aoxidize stone
Black alkene powder.
Compared with prior art, the beneficial effects of the present invention are: porous aerogel material structure stable uniform of the invention,
Fluffy, density very little, preparation method is simple；The redox graphene aerogel material after mixing, is being accounted for paraffin
Under the dosage of gross mass 10%, as matching thickness 2.5mm, in 2-18GHz frequency range, the reachable -8.2dB of reflection loss；This
Outside, with the preparation process of the redox graphene aerogel material, three-dimensional redox graphene/zinc oxide electricity can be prepared
Magnetic shielding material, with paraffin after mixing, under the dosage for accounting for gross mass 10%, as matching thickness 0.7mm, Ji Ke
In 2-18GHz frequency range, achieve the effect that shield 90% electromagnetic energy.
Detailed description of the invention
Fig. 1 is the SEM schematic diagram of graphene oxide of the present invention and three-dimensional redox graphene；
Fig. 2 is the Raman spectrogram of graphite oxide GO of the present invention and three-dimensional redox graphene 3D-RGO；
Fig. 3 is graphene oxide GO of the present invention and three-dimensional redox graphene 3D-RGO in the region C 1s xps energy spectrum curve graph；
Fig. 4 is the reflection loss curve graph of the three-dimensional redox graphene of the present invention；
Fig. 5 is present invention three-dimensional redox graphene 3D-RGO and three-dimensional redox graphene/zinc oxide 3D-RGO/ZnO
TEM schematic diagram；
Fig. 6 is that three-dimensional redox graphene/zinc oxide 3D-RGO/ that mass fraction is 10% is added in composite material of the present invention
The electromagnet shield effect schematic diagram of ZnO.
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.
The present invention provides a kind of technical solution: a kind of three-dimensional redox graphene aerogel material, aerogel material by
Graphene oxide, redox graphene, nano zine oxide and hole composition, whole fluffy spongy in black, described goes back
The carrying of nano-metal-oxide electromagnetic material is realized in the hole of former graphite oxide aerogel.
Embodiment one:
The present embodiment the preparation method is as follows: 3g graphite powder is added in the beaker equipped with the 105ml concentrated sulfuric acid, ice bath stirring
3h, then into mixed solution be added 15g potassium permanganate, continue ice bath stirring 2h after change room temperature water-bath into after, it is slow along wall of cup
210ml deionized water is added, continues to stir 30min, then 30% hydrogen peroxide of 15ml, solution left standstill are slowly added dropwise into beaker
For 24 hours, supernatant liquor is outwelled, with deionized water with 4500 turns/min, 15min/ times, repeatedly washing, centrifugation, finally drying is collected
To graphite oxide.Graphite oxide is dissolved in deionized water, 1.5mg/ml solution is made into, 10000 turns/min is centrifuged after ultrasonic 2h,
Supernatant liquor after taking centrifugation can obtain graphene oxide powder after dry；The graphene oxide powder of 60mg is passed through into ultrasonic wave
It being dispersed in the deionized water of 20ml, then this dispersion liquid is placed in hydrothermal reaction kettle, 180 DEG C of heating 12h are cooled to room temperature,
Wet shape object is taken out, is freeze-dried up to three-dimensional redox graphene aerogel material.
The microscopic appearance of material of the invention is as shown in Figure 1.
Embodiment two:
The present embodiment the preparation method is as follows: 3g graphite powder is added in the beaker equipped with the 105ml concentrated sulfuric acid, ice bath stirring
3h, then into mixed solution be added 15g potassium permanganate, continue ice bath stirring 2h after change room temperature water-bath into after, it is slow along wall of cup
210ml deionized water is added, continues to stir 30min, then 30% hydrogen peroxide of 15ml, solution left standstill are slowly added dropwise into beaker
For 24 hours, supernatant liquor is outwelled, with deionized water with 4500 turns/min, 15min/ times, repeatedly washing, centrifugation, finally drying is collected
To graphite oxide.Graphite oxide is dissolved in deionized water, 1.5mg/ml solution is made into, 10000 turns/min is centrifuged after ultrasonic 2h,
Supernatant liquor after taking centrifugation can obtain graphene oxide powder after dry；The graphene oxide powder of 60mg is passed through into ultrasonic wave
It being dispersed in the deionized water of 20ml, then this dispersion liquid is placed in hydrothermal reaction kettle, 180 DEG C of heating 12h are cooled to room temperature,
Wet shape object is taken out, is freeze-dried up to three-dimensional redox graphene aerogel material.
Take above-mentioned gained three-dimensional redox graphene aeroge and raw material graphene oxide, test its Raman spectrum and
X-ray photoelectron spectroscopy, it is as shown in Figures 2 and 3 respectively.
There are typical D at 1347 and 1581cm-1 for graphene oxide and three-dimensional redox graphene in Fig. 2
Band and G band.Graphene oxide layer is after hydrothermal reduction, and the intensity of D band and G band is than rising to hydro-thermal from 1.62 before hydro-thermal
Afterwards 1.93, although this is primarily due to eliminate oxygen-containing group from carbon-coating, be no longer on the moiety site of graphene layer
Complete six-membered ring structure, so as to cause the lattice structure defects of carbon.
The region the C 1s xps energy spectrum curve of graphene oxide is by carbon skeleton C-C(284.8eV), oxygen-containing functional group C- in Fig. 3
O(286.6 eV), C=O(288.0 eV), O C=O (289.2 eV)) composition, show in graphene oxide structure containing abundant
Oxygen-containing functional group.And in the region the C 1s xps energy spectrum curve of three-dimensional redox graphene aeroge, although there are still oxygen-containing
Functional group, but its intensity be far from graphene oxide oxygen-containing luminous energy group peak intensity, this also indicate that by hydro-thermal reaction incited somebody to action
Graphene oxide reduction.
Embodiment three:
The present embodiment the preparation method is as follows: 3g graphite powder is added in the beaker equipped with the 105ml concentrated sulfuric acid, ice bath stirring
3h, then into mixed solution be added 15g potassium permanganate, continue ice bath stirring 2h after change room temperature water-bath into after, it is slow along wall of cup
210ml deionized water is added, continues to stir 30min, then 30% hydrogen peroxide of 15ml, solution left standstill are slowly added dropwise into beaker
For 24 hours, supernatant liquor is outwelled, with deionized water with 4500 turns/min, 15min/ times, repeatedly washing, centrifugation, finally drying is collected
To graphite oxide.Graphite oxide is dissolved in deionized water, 1.5mg/ml solution is made into, 10000 turns/min is centrifuged after ultrasonic 2h,
Supernatant liquor after taking centrifugation can obtain graphene oxide powder after dry；The graphene oxide powder of 60mg is passed through into ultrasonic wave
It being dispersed in the deionized water of 20ml, then this dispersion liquid is placed in hydrothermal reaction kettle, 180 DEG C of heating 12h are cooled to room temperature,
Wet shape object is taken out, is freeze-dried up to three-dimensional redox graphene aerogel material.
Three-dimensional redox graphene aeroge is uniformly mixed with paraffin, paraffin accounts for gross mass 90%, is pressed into ring mould
Sample is made in (high 2.0mm, outer diameter 7.0mm, internal diameter 3.0mm), electromagnetic absorption performance is as shown in Figure 4.
In Fig. 4, abscissa is the frequency range 2-18GHz of test, and ordinate is reflection loss (Reflection
Loss).Ordinate is smaller, indicates the more of electro-magnetic wave absorption, and electromagnetic absorption performance is better.As matching thickness 2.5mm, in
In 2-18GHz frequency range, the reachable -8.2dB of reflection loss.
Comparative example 1: by the graphene oxide powder ultrasonic disperse of 60mg in 20ml N-methyl pyrrolidones (NMP) and ethyl alcohol
Mixed solution (volume ratio 1:1) in.The ZnO of 10mg is dispersed in the ethanol solution of 10ml by ultrasonic wave, and by this point
Dispersion liquid is added dropwise in graphene oxide dispersion under fast stirring, under ultraviolet lamp irradiation condition after high-speed stirred 4h,
Resulting materials mixture is dispersed in water by filtering drying again, forms the dispersion liquid of 1mg/ml.A certain amount of dispersion liquid is set
In hydrothermal reaction kettle, 180 DEG C of heating are cooled to room temperature afterwards for 24 hours, are taken out wet shape object, be can be obtained three-dimensional reduction after freeze-drying
Graphene oxide/zinc oxide aerogel material, it is as shown in Figure 5 with the TEM photo comparison of three-dimensional redox graphene material.
In Fig. 5, Zinc oxide nanoparticle is attached to the surface of redox graphene, free zinc oxide does not occur
Nano particle.
Comparative example 2: material preparation is identical as comparative example 2
Three-dimensional redox graphene gas/oxidation gel of zinc is uniformly mixed with paraffin, paraffin accounts for gross mass 90%, indentation annular
Sample is made in mold (high 2.0mm, outer diameter 7.0mm, internal diameter 3.0mm), electromagnet shield effect is as shown in Figure 6.
In Fig. 6, when thickness of composite material is only 0.7mm, in 2-18GHz frequency range, total electromagnetism of the material
The electromagnetic wave energy that shield effectiveness is all larger than 10dB(90% is shielded).And when thickness reaches 1.6 and 3.7mm, the material it is total
Electromagnet shield effect has been more than that the electromagnetic wave energy of 20dB(99% is shielded respectively) and the electromagnetic wave energy of 30dB(99.9% shielded
It covers).
In conclusion porous aerogel material structure stable uniform of the invention, fluffy, density very little, preparation method letter
It is single；The redox graphene aerogel material after mixing, under the dosage for accounting for gross mass 10%, is working as matching with paraffin
When thickness 2.5mm, in 2-18GHz frequency range, the reachable -8.2dB of reflection loss；In addition, with the redox graphene
The preparation process of aerogel material can prepare three-dimensional redox graphene/zinc oxide electromagnetic shielding material, mix with paraffin
After uniformly, under the dosage for accounting for gross mass 10%, as matching thickness 0.7mm, screen can be reached in 2-18GHz frequency range
Cover the effect of 90% electromagnetic energy.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (3)
1. a kind of three-dimensional redox graphene aerogel material, it is characterised in that: aerogel material is by graphene oxide, reduction
Graphene oxide, nano zine oxide and hole composition, the whole redox graphene airsetting fluffy spongy, described in black
The carrying of nano-metal-oxide electromagnetic material is realized in the hole of glue.
2. realizing a kind of preparation method of three-dimensional redox graphene aerogel material described in claim 1, feature exists
In: preparation method includes the following steps:
A, graphite powder is added in the beaker equipped with the 105ml concentrated sulfuric acid, ice bath stirring 3h；
B, potassium permanganate is added in the mixed solution obtained to step A, continues ice bath stirring 2h；
C, step B acquired solution is placed in room temperature water-bath, is slowly added to 210ml deionized water along wall of cup, and with aubergine
Smoke and gas steep and release, add mixed solution after water to continue to stir 30min；
D, 30% hydrogen peroxide of 15ml is slowly added dropwise into the resulting mixed solution of step C, solution left standstill is for 24 hours；
E, the resulting mixed solution of step D is outwelled into supernatant liquor, repeatedly washing centrifugation, the collection of gained graphite oxide is being cultivated
In ware, it is put into the 50 DEG C of dryings of baking oven constant temperature；
F, dry graphite oxide is dissolved in deionized water, is made into 1.5mg/ml solution, ultrasonic 2h；
G, the solution of step F is centrifuged, the supernatant liquor after taking centrifugation can obtain graphene oxide solution；
H, graphene oxide powder is dispersed in deionized water, the dispersion liquid of 3mg/ml to be made by ultrasonic wave；
I, dispersion liquid obtained by step H is placed in hydrothermal reaction kettle, 180 DEG C of heating 12h are cooled to room temperature, take out wet shape object, cold
Jelly is drying to obtain three-dimensional redox graphene aerogel material.
3. one kind according to claim 1, it is characterised in that: in the step G, graphene oxide solution is poured into culture
It is dry at 50 DEG C in ware, graphene oxide powder can be obtained.
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| CN110240731A (en) * | 2019-05-23 | 2019-09-17 | 东南大学 | A kind of preparation method of graphene with high specific surface-metal oxide composite sponge |
| CN110395716A (en) * | 2019-07-26 | 2019-11-01 | 中国电子科技集团公司第三十三研究所 | A kind of preparation method of the microwave defense material based on graphene |
| CN115594232A (en) * | 2022-10-21 | 2023-01-13 | 中国科学院宁波材料技术与工程研究所（Cn） | Three-dimensional directional porous aerogel loaded with hollow oxide nano-boxes as well as preparation method and application of three-dimensional directional porous aerogel |
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| CN110240731A (en) * | 2019-05-23 | 2019-09-17 | 东南大学 | A kind of preparation method of graphene with high specific surface-metal oxide composite sponge |
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| CN115594232B (en) * | 2022-10-21 | 2024-03-08 | 中国科学院宁波材料技术与工程研究所 | Three-dimensional directional porous aerogel loaded with hollow oxide nano boxes and preparation method and application thereof |
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Application publication date: 20190201 |