CN109181638A - A kind of tungsten disulfide-redox graphene three-dimensional self-assembled structures absorbing material - Google Patents
A kind of tungsten disulfide-redox graphene three-dimensional self-assembled structures absorbing material Download PDFInfo
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- CN109181638A CN109181638A CN201811028527.XA CN201811028527A CN109181638A CN 109181638 A CN109181638 A CN 109181638A CN 201811028527 A CN201811028527 A CN 201811028527A CN 109181638 A CN109181638 A CN 109181638A
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- tungsten disulfide
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Abstract
The invention discloses a kind of tungsten disulfide-redox graphene three-dimensional self-assembled structures absorbing materials, absorbing material is made of tungsten disulfide and redox graphene, it is whole spongy in black, the redox graphene lamella is interspersed in tungsten disulfide lamella, is formed and is interted stacked structure layer by layer.Absorbing material of the invention with paraffin after mixing, in the case where accounting for gross mass 10%, when matching thickness is 3.0mm, in in 2-18GHz frequency range, frequency bandwidth of the reflection loss lower than -10dB is up to 8.74GHz, when maximum value appears in 14.16GHz, reflection loss at this time is -42.86dB.
Description
Technical field
The present invention relates to electromagnetic wave absorbent material preparation technical field, specially a kind of tungsten disulfide-reduction-oxidation graphite
Alkene three-dimensional self-assembled structures absorbing material.
Background technique
Development in terms of current absorbing material is gradually thin to (layer), (matter) is light, (frequency) is wide, (absorbing property) is strong, carbon material
Traditional Ferrite Material is gradually substituted to be used in absorbing material.Graphene is a kind of nano material of two-dimensional structure, is had
Bigger serface, excellent conduction and heating conduction, strong mechanical performance, have a wide range of applications in field of compound material.
Two-dimensional graphene lamella has certain suction wave generally after its area load metal oxide or conducting polymer
Performance, but gained absorbing material (3-5mm) only in the biggish situation of matching thickness just has preferable absorbing property, and
Additive amount is larger (mass ratio 30-50%), so that will cause quality of materials increases larger, and mechanical properties decrease.
In recent years, two-dimensional graphene lamella is formed to the three-dimensional sponge shape oxygen reduction of microcosmic porous structure by hydro-thermal reaction
Graphite alkene is the research hotspot of Material Field, but the absorbing property of three-dimensional sponge construction recovery graphene oxide itself compared with
Difference can not obtain the frequency range for absorbing 10dB or more, therefore many researchs all concentrate on three-dimensional sponge construction recovery oxidation stone
Ferrite is loaded on black alkene to improve absorbing property, but quality of materials greatly improves therewith.Simultaneously because graphene is prepared into
This is very high, therefore graphene price can not have always been high any more, and material, which accounts for main body with graphene, will lead to material preparation cost height, it is difficult to
It promotes.
Summary of the invention
The purpose of the present invention is to provide a kind of tungsten disulfide-redox graphene three-dimensional self-assembled structures to inhale wave material
Material, to solve the problems mentioned in the above background technology.
To achieve the above object, the invention provides the following technical scheme: a kind of tungsten disulfide-redox graphene is three-dimensional
Self-assembled structures absorbing material, the absorbing material are made of tungsten disulfide and redox graphene, and material is integrally in black
Spongy, the graphene sheet layer is interspersed in tungsten disulfide lamella, is formed and is interted stacked structure layer by layer.
Preferably, preparation method includes the following steps:
A, graphene oxide is dispersed in volume ratio is the water of 1:1, in n,N-Dimethylformamide mixed solution, and concentration is
1.0mg/mL；
B, 0.6g tungsten hexachloride is added in the solution of step A and is stirred evenly；
C, 1.2g thioacetamide is added in the solution of step B and is stirred evenly；
D, the homogeneous mixture solotion in step C is put into reaction kettle, 120 DEG C of heating are reacted；
E, by the reaction of step D, tungsten hexachloride is reacted with thioacetamide at this time generates tungsten disulfide nano slices layer, oxygen
Graphite alkene is reduced, and the solid product after reaction is repeatedly centrifuged, and alcohol is washed, washing, and after washing away wherein impurity, it is dry to carry out freezing
It is dry.
Preferably, -50 DEG C of temperature are freeze-dried in the step E -- it 55 DEG C, is freeze-dried -26 hours 24 hours.
Compared with prior art, the beneficial effects of the present invention are: the redox graphene dosage used in the present invention is few,
At low cost, redox graphene only accounts for the 10% of gross mass；Absorbing material obtained and paraffin are accounting for always by after mixing
In the case where quality 10%, when matching thickness is 3.0mm, in 2-18GHz frequency range, reflection loss is lower than -10dB's
Frequency bandwidth is up to 8.74GHz, and when maximum value appears in 14.16GHz, reflection loss at this time is -42.86dB.
Detailed description of the invention
Fig. 1 is the absorbing property of embodiment 1.
Fig. 2 is the absorbing property of embodiment 2.
Fig. 3 is the absorbing property of embodiment 3.
Fig. 4 is the absorbing property of comparative example 1.
Fig. 5 is the absorbing property of comparative example 2.
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.
Embodiment one:
The invention provides the following technical scheme: a kind of tungsten disulfide-redox graphene three-dimensional self-assembled structures inhale wave
Material, the absorbing material are made of tungsten disulfide and redox graphene, and material is integrally in spongy, the described stone of black
Black alkene lamella is interspersed in tungsten disulfide lamella, is formed and is interted stacked structure layer by layer.
The preparation method of the present embodiment the following steps are included:
A, graphene oxide is dispersed in volume ratio is the water of 1:1, in n,N-Dimethylformamide mixed solution, and concentration is
1.0mg/mL；
B, 0.6g tungsten hexachloride is added in the solution of step A and is stirred evenly；
C, 1.2g thioacetamide is added in the solution of step B and is stirred evenly；
D, the homogeneous mixture solotion in step C is put into reaction kettle, 120 DEG C of heating are reacted；
E, by the reaction of step D, tungsten hexachloride is reacted with thioacetamide at this time generates tungsten disulfide nano slices layer, oxygen
Graphite alkene is reduced, and the solid product after reaction is repeatedly centrifuged, and alcohol is washed, washing, and after washing away wherein impurity, it is dry to carry out freezing
It is dry.
In the present embodiment, it is freeze-dried -50 DEG C of temperature in step E, is freeze-dried 24 hours.
Tungsten disulfide-redox graphene three-dimensional self-assembled structures absorbing material is uniformly mixed with paraffin, paraffin accounts for
Gross mass 95% is pressed into ring mould and sample is made, wherein ring mould high 2.0mm, outer diameter 7.0mm, internal diameter 3.0mm,
Absorbing property is as shown in Fig. 1.
In Fig. 1, abscissa is the frequency range 2-18GHz of test, and ordinate is reflection loss, and ordinate value is smaller,
Indicate the more of electro-magnetic wave absorption, -10dB is that electromagnetic wave energy has decayed 90%, therefore be more than -10dB region it is referred to as effective
Absorption region.
Embodiment two:
A kind of tungsten disulfide-redox graphene three-dimensional self-assembled structures absorbing material, the absorbing material is by two sulphur
Change tungsten and redox graphene composition, material is integrally in that black is spongy, and the graphene sheet layer is interspersed in tungsten disulfide
In lamella, is formed and intert stacked structure layer by layer.
The preparation method of the present embodiment the following steps are included:
A, graphene oxide is dispersed in volume ratio is the water of 1:1, in n,N-Dimethylformamide mixed solution, and concentration is
1.0mg/mL；
B, 0.6g tungsten hexachloride is added in the solution of step A and is stirred evenly；
C, 1.2g thioacetamide is added in the solution of step B and is stirred evenly；
D, the homogeneous mixture solotion in step C is put into reaction kettle, 120 DEG C of heating are reacted；
E, by the reaction of step D, tungsten hexachloride is reacted with thioacetamide at this time generates tungsten disulfide nano slices layer, oxygen
Graphite alkene is reduced, and the solid product after reaction is repeatedly centrifuged, and alcohol is washed, washing, and after washing away wherein impurity, it is dry to carry out freezing
It is dry.
In the present embodiment, it is freeze-dried -55 DEG C of temperature in step E, is freeze-dried 26 hours.
Tungsten disulfide-redox graphene self-assembled structures absorbing material is uniformly mixed with paraffin, paraffin accounts for total matter
Amount 90% is pressed into ring mould and sample is made, wherein ring mould high 2.0mm, outer diameter 7.0mm, internal diameter 3.0mm inhale wave
Performance is as shown in Fig. 2.
Embodiment three:
A kind of tungsten disulfide-redox graphene three-dimensional self-assembled structures absorbing material, the absorbing material is by two sulphur
Change tungsten and redox graphene composition, material is integrally in that black is spongy, and the graphene sheet layer is interspersed in tungsten disulfide
In lamella, is formed and intert stacked structure layer by layer.
The preparation method of the present embodiment the following steps are included:
A, graphene oxide is dispersed in volume ratio is the water of 1:1, in n,N-Dimethylformamide mixed solution, and concentration is
1.0mg/mL；
B, 0.6g tungsten hexachloride is added in the solution of step A and is stirred evenly；
C, 1.2g thioacetamide is added in the solution of step B and is stirred evenly；
D, the homogeneous mixture solotion in step C is put into reaction kettle, 120 DEG C of heating are reacted；
E, by the reaction of step D, tungsten hexachloride is reacted with thioacetamide at this time generates tungsten disulfide nano slices layer, oxygen
Graphite alkene is reduced, and the solid product after reaction is repeatedly centrifuged, and alcohol is washed, washing, and after washing away wherein impurity, it is dry to carry out freezing
It is dry.
In the present embodiment, it is freeze-dried -52 DEG C of temperature in step E, is freeze-dried 25 hours.
Tungsten disulfide-redox graphene self-assembled structures absorbing material is uniformly mixed with paraffin, paraffin accounts for total matter
Amount 85% is pressed into ring mould and sample is made, wherein ring mould high 2.0mm, outer diameter 7.0mm, internal diameter 3.0mm inhale wave
Performance is as shown in Fig. 3.
Comparative example 1: 0.6g tungsten hexachloride is dissolved in 60mL n,N-Dimethylformamide solution, it is thio to add 1.2g
Acetamide is dispersed in uniformly, and mixed solution is put into reaction kettle, and 120 DEG C of heating are reacted；Solid product warp after reaction
Centrifugation, alcohol are washed, and are washed, and after washing away wherein impurity, -50 DEG C of freeze-dryings obtain simple tungsten disulfide three-dimensional self assembly knot in 24 hours
Structure absorbing material.
Simple tungsten disulfide three-dimensional self-assembled structures absorbing material is uniformly mixed with paraffin, paraffin accounts for gross mass 90%,
Sample is made in indentation ring mould, wherein the high 2.0mm of ring mould, outer diameter 7.0mm, internal diameter 3.0mm, absorbing property is such as
Shown in attached drawing 4.
Comparative example 2: dispersing graphene oxide in 60mL water, concentration 1.0mg/mL.It is put into reaction kettle and adds for 120 DEG C
Heat is taken out after 12 hours, and -50 DEG C of freeze-dryings obtain simple redox graphene three-dimensional self-assembled structures in 24 hours.
Simple redox graphene three-dimensional self-assembled structures absorbing material is uniformly mixed with paraffin, paraffin accounts for gross mass
90%, it is pressed into ring mould and sample is made, wherein ring mould high 2.0mm, outer diameter 7.0mm, internal diameter 3.0mm, wave absorbtion
It can be as shown in Fig. 5.
The redox graphene dosage used in the present invention is few, and at low cost, redox graphene only accounts for gross mass
10%；Absorbing material obtained and paraffin are pressed after mixing, in the case where accounting for gross mass 10%, when matching thickness is
When 3.0mm, in 2-18GHz frequency range, frequency bandwidth of the reflection loss lower than -10dB occurs up to 8.74GHz, maximum value
In 14.16GHz, reflection loss at this time is -42.86dB.
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 tungsten disulfide-redox graphene three-dimensional self-assembled structures absorbing material, it is characterised in that: the suction wave material
Material is made of tungsten disulfide and redox graphene, and material is integrally in that black is spongy, and the graphene sheet layer is interspersed in
In tungsten disulfide lamella, is formed and intert stacked structure layer by layer.
2. realizing a kind of tungsten disulfide-redox graphene three-dimensional self-assembled structures absorbing material described in claim 1
Preparation method, it is characterised in that: preparation method includes the following steps:
A, graphene oxide is dispersed in volume ratio is the water of 1:1, in n,N-Dimethylformamide mixed solution, and concentration is
1.0mg/mL；
B, 0.6g tungsten hexachloride is added in the solution of step A and is stirred evenly；
C, 1.2g thioacetamide is added in the solution of step B and is stirred evenly；
D, the homogeneous mixture solotion in step C is put into reaction kettle, 120 DEG C of heating are reacted；
E, by the reaction of step D, tungsten hexachloride is reacted with thioacetamide at this time generates tungsten disulfide nano slices layer, aoxidizes stone
Black alkene is reduced, and the solid product after reaction is repeatedly centrifuged, and alcohol is washed, and washing after washing away wherein impurity, is freeze-dried.
3. a kind of tungsten disulfide according to claim 1-redox graphene three-dimensional self-assembled structures absorbing material
Preparation method, it is characterised in that: -50 DEG C of temperature are freeze-dried in the step E -- it 55 DEG C, is freeze-dried -26 hours 24 hours.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111704125A (en) * | 2020-06-16 | 2020-09-25 | 齐齐哈尔大学 | WS (WS)2Preparation method of (N-styrene-butadiene-styrene)/CNTs (carbon nanotubes) hybrid wave-absorbing material |
Citations (3)
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| CN106356202A (en) * | 2016-09-28 | 2017-01-25 | 上海电力学院 | Graphene/tungsten disulfide film flexible super capacitor and manufacturing method and application thereof |
| CN106952737A (en) * | 2017-03-02 | 2017-07-14 | 中山大学 | A kind of preparation method of tungsten disulfide flake nano material |
| CN108428565A (en) * | 2017-02-13 | 2018-08-21 | 中国科学院宁波材料技术与工程研究所 | Tungsten disulfide/graphene oxide composite material, preparation method and application |
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2018
- 2018-09-05 CN CN201811028527.XA patent/CN109181638A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106356202A (en) * | 2016-09-28 | 2017-01-25 | 上海电力学院 | Graphene/tungsten disulfide film flexible super capacitor and manufacturing method and application thereof |
| CN108428565A (en) * | 2017-02-13 | 2018-08-21 | 中国科学院宁波材料技术与工程研究所 | Tungsten disulfide/graphene oxide composite material, preparation method and application |
| CN106952737A (en) * | 2017-03-02 | 2017-07-14 | 中山大学 | A kind of preparation method of tungsten disulfide flake nano material |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111704125A (en) * | 2020-06-16 | 2020-09-25 | 齐齐哈尔大学 | WS (WS)2Preparation method of (N-styrene-butadiene-styrene)/CNTs (carbon nanotubes) hybrid wave-absorbing material |
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