CN108559249A - A kind of graphene modified molybdenum disulfide wave absorbing agent and preparation method thereof - Google Patents
A kind of graphene modified molybdenum disulfide wave absorbing agent and preparation method thereof Download PDFInfo
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- CN108559249A CN108559249A CN201810394200.8A CN201810394200A CN108559249A CN 108559249 A CN108559249 A CN 108559249A CN 201810394200 A CN201810394200 A CN 201810394200A CN 108559249 A CN108559249 A CN 108559249A
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- molybdenum disulfide
- modified molybdenum
- graphene modified
- graphene
- absorbing agent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
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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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3009—Sulfides
Abstract
The invention discloses a kind of graphene modified molybdenum disulfide wave absorbing agent and preparation method thereof, the graphene modified molybdenum disulfide is rendered as nanometer sheet under microcosmic, has efficient absorbing property.Invention additionally discloses a kind of preparation methods of graphene modified molybdenum disulfide wave absorbing agent, and the preparation method is simple for process, at low cost, without complicated synthesis device, can be produced in enormous quantities with scale.
Description
Technical field
The present invention relates to electromagnetic wave absorbent material technical field, specially a kind of graphene modified molybdenum disulfide wave absorbing agent and
Preparation method.
Background technology
With the rapid development of electronic information technology, the electromagnetic radiation and electromagnetic interference that are faced in people's production and life are asked
Topic is on the rise.Development absorbing material is one of the important channel for protecting electromagnetic radiation and electromagnetic interference problem.Absorbing material is
By electromagnetic radiation transform into it is other it is non-radiative can dissipate, avoid secondary pollution.Therefore, Development of Novel absorbing material exists
Military field and civil field are of great significance.
In recent years, microwave defense material started to change to lightweight, the carbon-based electromagnetic screen of lightweight especially represented with graphene
Cover material.The conductivity of graphene is higher, this causes using single graphene to be the electromagnetic shielding material of key component to entering radio
The reflection loss of magnetic wave is excessive, is unfavorable for electromagnetic radiation in electromagnetic camouflage and environment and eliminates.(M.S.Cao,X.X.Wang,
W.Q.Cao, et al.J.Mater.Chem.C, 2015,3,6589.) however, graphene is a kind of modified to improve other materials electricity
The high efficiency method of magnetic loss.(F.Wu, A.Xie, M.Sun, et al.J.Mater.Chem.A, 2015,3,14358.) curing
Molybdenum is a kind of two-dimensional layer material of new generation of similar graphene, has unique optics, electrical properties.However it is not but one
The excellent absorbing material of kind, mainly since its conductivity is too low.If graphene is combined with molybdenum disulfide, it is expected to design height
Imitate absorbing material.
Invention content
The purpose of the present invention is to provide a kind of graphene modified molybdenum disulfide wave absorbing agents and preparation method thereof, in solution
State the problem of being proposed in background technology.
To achieve the above object, the present invention provides the following technical solutions：A kind of graphene modified molybdenum disulfide wave absorbing agent, institute
Stating graphene modified molybdenum disulfide wave absorbing agent is made of graphene modified molybdenum disulfide and macromolecule resin, and graphene is modified two
Molybdenum sulfide is dispersed in macromolecule resin.
Preferably, preparation method includes the following steps：
A, graphene oxide is dispersed in water, prepares certain density graphene oxide water solution, then addition mole
Than being 1:1 thiocarbamide and ammonium molybdate, 200 degree of solvent thermal reactions 12 hours are obtained by processes such as filtering, washing, vacuum drying
Graphene modified molybdenum disulfide black powder；
B, macromolecule resin is heated to melting, the graphene modified molybdenum disulfide prepared in step A is added and is sufficiently mixed,
Cooling obtains graphene modified molybdenum disulfide wave absorbing agent.
Preferably, the concentration range of graphene oxide described in the step A is 0.1-10mg/mL.
Preferably, macromolecule resin described in the step B is made of polyurethane, epoxy resin, polyethers, natural resin.
Compared with prior art, the beneficial effects of the invention are as follows：Graphene modified molybdenum disulfide of the present invention so that curing
The absorbing property of molybdenum is obviously improved；Preparation method of the present invention is simple for process, at low cost, without complicated synthesis device, Ke Yigui
Modelling is produced in enormous quantities.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of graphene modified molybdenum disulfide in the present invention；
Fig. 2 is the transmission electron microscope picture of graphene modified molybdenum disulfide in invention；
Fig. 3 is the powder x-ray diffraction figure of graphene modified molybdenum disulfide in invention；
Fig. 4 is the x-ray photoelectron spectroscopy figure of graphene modified molybdenum disulfide in invention；
Fig. 5 is the reflection loss collection of illustrative plates of sample 1 made from the embodiment of the present invention 1；
Fig. 6 is the reflection loss collection of illustrative plates of sample 2 made from the embodiment of the present invention 2；
Fig. 7 is the reflection loss collection of illustrative plates of sample 3 made from the embodiment of the present invention 3.
Specific implementation mode
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 describes, 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 the following technical solutions：A kind of graphene modified molybdenum disulfide wave absorbing agent, the graphene are modified two
Molybdenum sulfide wave absorbing agent is made of graphene modified molybdenum disulfide and macromolecule resin, and graphene modified molybdenum disulfide is dispersed in height
In molecule resin；The macromolecule resin is made of polyurethane, epoxy resin, polyethers, natural resin.
Embodiment 1
The preparation method of graphene modified molybdenum disulfide wave absorbing agent sample 1, includes the following steps in the present invention：
A, graphene oxide is dispersed in water, prepares the graphene oxide water solution (100mL) of 0.5mg/mL.Then plus
Enter thiocarbamide (10mmol) and ammonium molybdate (10mmol), stirring and dissolving, 200 degree of solvent thermal reactions 12 hours, by filtering, washing,
The processes such as vacuum drying obtain graphene modified molybdenum disulfide black powder.
B, 0.9 gram of polyurethane is heated to melting, the graphene modified molybdenum disulfide (0.1 gram) prepared in step A is added
It is sufficiently mixed, cooling obtains graphene modified molybdenum disulfide wave absorbing agent, is denoted as sample 1.Graphene modified molybdenum disulfide in sample 1
Mass fraction be 10%.
Embodiment 2
The concentration of the graphene oxide water solution of step 1 in embodiment 1 is changed to 2mg/mL, other implementation conditions are the same as implementation
Example 1 obtains sample 2.
Embodiment 3
Polyurethane in step 2 in embodiment 1 is changed to epoxy resin, other implementation conditions obtain sample 3. with embodiment 1
Fig. 1 is the scanning electron microscope (SEM) photograph of graphene modified molybdenum disulfide in the present invention, it can be seen that graphene is modified curing
The microcosmic upper presentation nano-sheet of molybdenum.
Fig. 2 is the transmission electron microscope picture of graphene modified molybdenum disulfide in invention, further determines that graphene is modified curing
The nanometer sheet pattern of molybdenum.
Fig. 3 is the powder x-ray diffraction figure of graphene modified molybdenum disulfide in invention, determines that graphene is modified curing
The crystal characteristic of molybdenum.
Fig. 4 is the x-ray photoelectron spectroscopy figure of graphene modified molybdenum disulfide in invention, determines that graphene is modified two sulphur
Change the presence of carbon, element sulphur, molybdenum element in molybdenum.
Fig. 5 is the reflection loss collection of illustrative plates of sample 1 made from the embodiment of the present invention 1, it can be seen that sample 1 shows excellent
Absorbing property.When thickness is 2mm, the best reachable -20dB of reflection loss.
Fig. 6 is the reflection loss collection of illustrative plates of sample 2 made from the embodiment of the present invention 2, it can be seen that sample 2 has excellent
Absorbing property.When thickness is 2mm, the best reachable -60dB of reflection loss, the absorption frequency range less than -10dB is less than
5.2GHz concentrates on X-band and Ku wave bands.
Fig. 7 is the reflection loss collection of illustrative plates of sample 3 made from the embodiment of the present invention 3, it can be seen that sample 3 shows excellent
Absorbing property.When thickness is 2mm, the best reachable -40dB of reflection loss, the absorption frequency range less than -10dB is more than
4.6GHz is concentrated in X-band and Ku wave bands.
The principle of synthesizing graphite alkene modified molybdenum disulfide in the present invention：Surface of graphene oxide had into many oxygen-containing functions
Group, such as carboxyl, hydroxyl, epoxy, can adsorb thiocarbamide and ammonium molybdate in the solution.Under solvent thermal environment, graphene oxide
By in-situ reducing, the molybdenum disulfide constantly deposition being formed simultaneously on the surface of graphene, eventually forms the stone of sandwich structure
Black alkene modified molybdenum disulfide.Graphene is coated on outer layer as kernel, molybdenum disulfide.The graphene modified molybdenum disulfide it is micro-
Pattern scanning electron microscope and transmission electron microscope observation are seen, elemental analysis is determined with x-ray photoelectron spectroscopy, crystal characteristic powder
X-ray diffraction determines.
Graphene modified molybdenum disulfide is prepared in situ using hydrothermal technique one-step method in the present invention, significantly improves molybdenum disulfide
Conduction property, and then obtain excellent absorbing property.Preparation method simple process and low cost of the present invention is suitable for industrialization
Production.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding without departing from the principles and spirit of the present invention can carry out these embodiments a variety of variations, modification, replace
And modification, the scope of the present invention is defined by the appended.
Claims (4)
1. a kind of graphene modified molybdenum disulfide wave absorbing agent, it is characterised in that：The graphene modified molybdenum disulfide wave absorbing agent is
It is made of graphene modified molybdenum disulfide and macromolecule resin, graphene modified molybdenum disulfide is dispersed in macromolecule resin.
2. realizing a kind of preparation method of graphene modified molybdenum disulfide wave absorbing agent described in claim 1, it is characterised in that：Its
Preparation method includes the following steps：
A, graphene oxide is dispersed in water, prepares certain density graphene oxide water solution, molar ratio, which is then added, is
1:1 thiocarbamide and ammonium molybdate, 200 degree of solvent thermal reactions 12 hours obtain graphite by processes such as filtering, washing, vacuum drying
Alkene modified molybdenum disulfide black powder；
B, macromolecule resin is heated to melting, the graphene modified molybdenum disulfide prepared in step A is added and is sufficiently mixed, it is cooling
Obtain graphene modified molybdenum disulfide wave absorbing agent.
3. a kind of preparation method of graphene modified molybdenum disulfide wave absorbing agent according to claim 2, it is characterised in that：Institute
The concentration range for stating graphene oxide described in step A is 0.1-10mg/mL.
4. a kind of preparation method of graphene modified molybdenum disulfide wave absorbing agent according to claim 2, it is characterised in that：Institute
Macromolecule resin described in step B is stated to be made of polyurethane, epoxy resin, polyethers, natural resin.
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| CN201810394200.8A CN108559249A (en) | 2018-04-27 | 2018-04-27 | A kind of graphene modified molybdenum disulfide wave absorbing agent and preparation method thereof |
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| CN201810394200.8A CN108559249A (en) | 2018-04-27 | 2018-04-27 | A kind of graphene modified molybdenum disulfide wave absorbing agent and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110903636A (en) * | 2019-12-18 | 2020-03-24 | 万华化学集团股份有限公司 | Polyurethane elastomer and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106398056A (en) * | 2016-09-05 | 2017-02-15 | 北京航空航天大学 | Composite material with excellent wave absorption and electromagnetic shielding performances and preparation method thereof |
| CN106700820A (en) * | 2016-08-31 | 2017-05-24 | 北京科技大学 | Preparation method of lightweight three-dimensional molybdenum disulfide/graphene composite wave absorbing coating |
-
2018
- 2018-04-27 CN CN201810394200.8A patent/CN108559249A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106700820A (en) * | 2016-08-31 | 2017-05-24 | 北京科技大学 | Preparation method of lightweight three-dimensional molybdenum disulfide/graphene composite wave absorbing coating |
| CN106398056A (en) * | 2016-09-05 | 2017-02-15 | 北京航空航天大学 | Composite material with excellent wave absorption and electromagnetic shielding performances and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| L.Z. BAI，ET AL.: "Enhanced electromagnetic wave absorption properties of MoS2-graphene hybrid nanosheets prepared by a hydrothermal method", 《J. SOL. GEL SCI. TECHNOL.》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110903636A (en) * | 2019-12-18 | 2020-03-24 | 万华化学集团股份有限公司 | Polyurethane elastomer and preparation method and application thereof |
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Application publication date: 20180921 |