CN105883921A - Preparation of 3D molybdenum disulfide nano-microparticles with high broadband wave absorption capability - Google Patents

Preparation of 3D molybdenum disulfide nano-microparticles with high broadband wave absorption capability Download PDF

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Publication number
CN105883921A
CN105883921A CN201610232548.8A CN201610232548A CN105883921A CN 105883921 A CN105883921 A CN 105883921A CN 201610232548 A CN201610232548 A CN 201610232548A CN 105883921 A CN105883921 A CN 105883921A
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molybdenum disulfide
nano
preparation
microparticles
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王广胜
章晓娟
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Beihang University
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Beihang University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00—Compounds of molybdenum
    • C01G39/06—Sulfides
    • 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
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N22/00—Investigating or analysing materials by the use of microwaves or radio waves, i.e. electromagnetic waves with a wavelength of one millimetre or more
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/32—Spheres
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • 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
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/003—Additives being defined by their diameter
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives

Abstract

The invention discloses a preparation of 3D molybdenum disulfide nano-microparticles with high broadband wave absorption capability and belongs to the technical field of nano-microparticles and preparation of the nano-microparticles. According to the method, reactants including sodium molybdate and L-cysteine are selected, dissolved in deionized water, stirred uniformly and then placed in a reaction kettle, the reaction kettle is put in a drying oven at the temperature of 200 DEG C, the reaction is performed for 12-20 h, and the 3D molybdenum disulfide nano-microparticles are obtained. The 3D MoS2 nano-microparticles with special shapes are prepared with a simple hydrothermal method and are composited with a high polymer material polyvinylidene fluoride, and the wave absorbing performance of an organic/inorganic nanocomposite at a high frequency band of 18-40 GHz is tested with a waveguide testing method. The preparation method has the advantages of simplicity in operation and high repeatability, and the obtained product has a stable structure and has the high broadband wave absorption capability.

Description

A kind of preparation of the 3D molybdenum disulfide nano microsphere with the strong wave-sucking performance of wideband
Technical field
The invention belongs to Nano microsphere and preparing technical field thereof, be specifically related to a kind of 3D with the strong wave-sucking performance of wideband The preparation of molybdenum disulfide nano microsphere.
Background technology
In recent years, big along with various military and civil equipment such as radar, satellite communication system, domestic electronic appliances etc. Amount application, its hazards of electromagnetic radiation brought makes microwave absorbing material receive much attention.Electromagnetic radiation is invisible, Can not touch, hidden people are difficult to discover deeply, but it brings beyond thought harm to the mankind and surrounding thereof.Research Show, electromagnetic radiation not only can interference Instrument properly functioning, cause information leakage, also can affect our healthy.Mesh Before, electromagnetic pollution has been acknowledged as the fourth-largest pollution after atmospheric pollution, water pollution, solid waste pollution.Therefore, respectively Row people from all walks of life are being devoted to study how to reduce electromagnetic radiation intensity, prevent electromagnetic radiation pollution.In consideration of it, research and development Novel wave-absorbing material becomes current hotspot.
Nano material owing to having that density is low, the advantage such as small-size effect and special appearance structure and become a kind of new The absorbing material of type, yet with the restriction of method of testing, the frequency range of major part relevant nano wave-absorbing material research at present All at 2-18GHz, in order to widen the application of absorbing material, it is particularly significant that wideband wave absorbing material is prepared in research.
Summary of the invention
In order to solve to prepare present in prior art that path is complicated, the problem such as to inhale ripple frequency range narrow, the present invention uses simply Hydro-thermal method prepare the 3D MoS with special appearance2Nano microsphere, and by itself and macromolecular material Kynoar (PVDF) being combined, in conjunction with waveguide measurement, test Organic/Inorganic Composite Nanomaterials is at the suction ripple of high band 18-40GHz Performance.
The present invention provides the preparation method of a kind of 3D molybdenum disulfide nano microsphere with the strong wave-sucking performance of wideband, described side Method chooses reactant sodium molybdate and Cys is dissolved in deionized water, after stirring, is placed in reactor, by reactor It is placed in response time 12-20h in 200 DEG C of baking ovens.Products therefrom is cleaned, dries, obtain 3D molybdenum disulfide nano microsphere.
The mass ratio of described sodium molybdate and Cys is 1:2.The described response time is preferably 20h.
Advantages of the present invention or have the beneficial effects that:
(1) simple to operate；
(2) repeatable high；
(3) Stability Analysis of Structures；
(4) wideband；
(5) strong wave-sucking performance.
Accompanying drawing explanation
Figure 1A～Fig. 1 D respectively response time is the 3D MoS that 6h, 8h, 12h and 20h prepare2Nano microsphere SEM schemes；
Fig. 1 E is the 3D MoS that response time 20h prepares2The TEM figure of Nano microsphere；
Fig. 2 A and Fig. 2 B respectively reactant mass ratio is the product image that 1:1 and 1:3 condition prepares.
Fig. 3 A～3D is in 18-26.5GHz frequency range, (A) 5wt%；(B) 10wt%；(C) 20wt%；(D) MoS under 30wt% content2/ PVDF composite is at the reflection loss figure of different-thickness.
Fig. 4 A～4D is in 26.5-40GHz frequency range, (A) 5wt%；(B) 10wt%；(C) 20wt%；(D) MoS under 30wt% content2/ PVDF composite is at the reflection loss figure of different-thickness.
Fig. 5 MoS2The wave-absorbing mechanism schematic diagram of/PVDF nano composite material.
Detailed description of the invention
The present invention is described in detail with embodiment below in conjunction with the accompanying drawings.
The present invention provides the preparation method of a kind of 3D molybdenum disulfide nano microsphere with the strong wave-sucking performance of wideband, specifically For: sodium molybdate and Cys are dissolved in deionized water, after stirring, are placed in reactor, reactor is placed in 160 ～200 DEG C of baking ovens react 12-20h.Products therefrom is cleaned, dries, obtain 3D molybdenum disulfide nano microsphere.
According to above-mentioned method, 0.1g sodium molybdate and 0.2g Cys being dissolved in 50ml deionized water, stirring is all After even, being placed in reactor (100ml), be placed in by reactor in 200 DEG C of baking ovens, the adjustment response time is respectively 6h, 8h, 12h And 20h, obtain product SEM figure respectively as Figure 1A～1D, only response time be 12h and 20h when, 3D bis-sulfur obtained Changing molybdenum is Nano microsphere structure, TEM image as referring to figure 1e, and when the response time is 20h, 3D molybdenum bisuphide is Nano microsphere tool Having the flake structure of self assembly, mean diameter is about 150-200nm.
Maintaining reaction temperature is 200 DEG C, and the response time is 20h, adjusts reactant sodium molybdate and Cys mass ratio Example is respectively 1:1 and 1:3, acquired results as shown in Figure 2 A and 2B, when reactant ratio is 1:1, owing to system has bigger Reaction compartment, the Nano microsphere particle diameter of generation is bigger and has more hierarchy；And when reactant ratio is 1:3, Owing to system does not has enough reaction compartments to make the nanometer sheet of generation be self-assembled into Nano microsphere, therefore product is that a pile is random The nanometer sheet of pattern.
With the response time as 20h, the 3D MoS for preparing for 1:2 of reactant mass ratio2Nano microsphere is filler, passes through Simple solvent blending method is prepared content and is respectively the MoS of 5wt%, 10wt%, 20wt% and 30wt%2/ PVDF nanometer is multiple Closing thin film, its key step is as follows:
First, appropriate Kynoar (PVDF) is dissolved in organic solvent DMF (DMF) or N, N- In dimethyl acetylamide (DMAc), it is continuously agitated under room temperature；
Secondly, after solution clear, according to mass percent 5wt%, 10wt%, 20wt% and 30wt% etc. are respectively Add MoS2Nano microsphere, continues stirring a period of time；
Finally, above-mentioned solution is all poured in culture dish, be placed in baking oven, take out, i.e. after solvent evaporation completely Obtain MoS2/ PVDF composite.
Subsequently by MoS2/ PVDF composite is put in particular mold, first heats it, treats that temperature is raised to 210 DEG C After, maintain 5min；Then begin to be forced into 5MPa, and pressurize 10 minutes, finally stop heating, after it drops to room temperature, take out Square piece, the square piece of extrusion has two kinds of specifications, and the longest 10.60mm × wide 4.20mm, long 7.10mm × wide 3.50mm, thickness can Adjust, in test process, respectively both square pieces are put in corresponding waveguide fixture, connect Network Analyzer subsequently and carry out accordingly The suction ripple test of wave band (18-26.5GHz, 26.5-40GHz).
Suction ripple test result is as shown in Fig. 3 A～3D and Fig. 4 A～4D, by regulation MoS2MoS in/PVDF composite2's Weight/mass percentage composition, can obtain all band high frequency absorbing material, at MoS2Weight/mass percentage composition 10wt% under conditions of, MoS2The absorbing property of/PVDF nano composite material is best, and in 18-26.5GHz frequency range, its minimum reflection loss value exists -46.8dB (26.0GHz) can be reached under 7.5mm thickness, correspond approximately to the electromagnetism wave energy of 99.99% and absorbed；At 26.5- In 40GHz frequency range, its minimum reflection loss value can reach-33.2dB (34.8GHz) under 8.0mm thickness, corresponds approximately to The electromagnetism wave energy of 99.9% is absorbed.Thus can obtain, MoS2/ PVDF nano composite material has excellent broadband absorbing performance.
Suction ripple result according to gained, conducts in-depth analysis to the wave-absorbing mechanism of material, is specifically related to five most of: One, polarity effect, mainly includes dipole polarization, interfacial polarization and interfacial polarization, and these Polarization Mechanism show electromagnetic wave Heat energy can be converted into soon and dissipate after injecting material；Two, interfere cancellation, be primarily referred to as inciding Nano microsphere The electromagnetic wave of sheet surface and the electromagnetic wave reflected are owing to having identical frequency and opposite in phase, thus interfere cancellation Phenomenon, advantageously reduces electromagnetic wave；Three, interface scattering, this is due to MoS2It is normal that Nano microsphere and PVDF have different dielectrics Number causes, and is also beneficial to electromagnetic wave and is absorbed；Four, multiple reflections, due to MoS2Nano microsphere is by large amount of thin sheets self assembly Form, thus cause the electromagnetic wave of incidence that multiple reflections occurs between different lamellas, extend electromagnetic wave in the material Transmit path, and then the most more electromagnetic wave is converted into heat energy and dissipates；Five, cooperative effect, MoS2Nano microsphere There is certain absorbing property with PVDF, cooperative effect can be produced after the two is compound, promote absorbing property to obtain further Promote, as shown in Figure 5.

Claims (5)

1. the preparation of a 3D molybdenum disulfide nano microsphere with the strong wave-sucking performance of wideband, it is characterised in that:
Choose reactant sodium molybdate and Cys is dissolved in deionized water, after stirring, be placed in reactor, will reaction Still is placed in response time 12-20h in 200 DEG C of baking ovens；Products therefrom is cleaned, dries, obtain 3D molybdenum disulfide nano microsphere.
The preparation of a kind of 3D molybdenum disulfide nano microsphere with the strong wave-sucking performance of wideband the most according to claim 1, its It is characterised by: the mass ratio of described sodium molybdate and Cys is 1:2；The described response time is 20h.
3. a 3D molybdenum disulfide nano microsphere with the strong wave-sucking performance of wideband, it is characterised in that: 3D molybdenum bisuphide is nanometer Microsphere has the flake structure of self assembly, and mean diameter is about 150-200nm.
4.MoS2The preparation method of/PVDF nano compound film, it is characterised in that: with the response time as 20h, reactant mass ratio The 3D MoS prepared for 1:22Nano microsphere is filler, prepares MoS by solvent blending method2/ PVDF is nano combined thin Film, specifically comprises the following steps that
First, Kynoar is dissolved in organic solvent DMF or N,N-dimethylacetamide, in room temperature Under be continuously agitated；
Secondly, after solution clear, add MoS according to mass percent 5wt%～30wt%2Nano microsphere, continues to stir Mix；
Finally, above-mentioned solution is all poured in culture dish, be placed in baking oven, take out after solvent evaporation completely, i.e. obtain MoS2/ PVDF composite.
5. the suction ripple method of testing of a 3D molybdenum disulfide nano microsphere with the strong wave-sucking performance of wideband, it is characterised in that: first First prepare MoS according to the method described in claim 42/ PVDF composite；
Subsequently by MoS2/ PVDF composite is put in particular mold, first heats it, after temperature is raised to 210 DEG C, and dimension Hold 5min；Then begin to be forced into 5MPa, and pressurize 10 minutes, finally stop heating, after it drops to room temperature, take out square piece, Square piece is put in corresponding waveguide fixture, connect Network Analyzer subsequently and carry out 18-26.5GHz wave band, 26.5-40GHz ripple The suction ripple test of section；
At MoS2Weight/mass percentage composition 10wt% under conditions of, MoS2The absorbing property of/PVDF nano composite material is best, In 18-26.5GHz frequency range, its minimum reflection loss value can reach-46.8dB under 7.5mm thickness；At 26.5-40GHz In frequency range, minimum reflection loss value can reach-33.2dB under 8.0mm thickness.
CN201610232548.8A 2016-04-14 2016-04-14 Preparation of 3D molybdenum disulfide nano-microparticles with high broadband wave absorption capability Pending CN105883921A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110498447A (en) * 2019-08-05 2019-11-26 河南师范大学 A kind of synthetic method of tennis shape molybdenum disulfide micro Nano material and its preparing the application in photo-thermal anticancer drug
CN115975314A (en) * 2022-12-26 2023-04-18 北京工商大学 Preparation method of composite material with adjustable wave-absorbing function under low filling amount condition
CN116135311A (en) * 2023-04-20 2023-05-19 山西省煤炭地质物探测绘院有限公司 Nanometer material based on molybdenum disulfide network structure and preparation method and application thereof

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CN104681815A (en) * 2015-02-11 2015-06-03 深圳新宙邦科技股份有限公司 Spherical molybdenum disulfide composite material and preparation method and application thereof
CN105062417A (en) * 2015-07-15 2015-11-18 北京新怡源环保科技有限公司 Organic-inorganic composite nano microwave absorbing material and preparation method thereof

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CN104681815A (en) * 2015-02-11 2015-06-03 深圳新宙邦科技股份有限公司 Spherical molybdenum disulfide composite material and preparation method and application thereof
CN105062417A (en) * 2015-07-15 2015-11-18 北京新怡源环保科技有限公司 Organic-inorganic composite nano microwave absorbing material and preparation method thereof

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110498447A (en) * 2019-08-05 2019-11-26 河南师范大学 A kind of synthetic method of tennis shape molybdenum disulfide micro Nano material and its preparing the application in photo-thermal anticancer drug
CN115975314A (en) * 2022-12-26 2023-04-18 北京工商大学 Preparation method of composite material with adjustable wave-absorbing function under low filling amount condition
CN116135311A (en) * 2023-04-20 2023-05-19 山西省煤炭地质物探测绘院有限公司 Nanometer material based on molybdenum disulfide network structure and preparation method and application thereof
CN116135311B (en) * 2023-04-20 2023-08-04 山西省煤炭地质物探测绘院有限公司 Nanometer material based on molybdenum disulfide network structure and preparation method and application thereof

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