CN111960468A - Two-dimensional transition metal chalcogenide wave-absorbing material, preparation method and application thereof - Google Patents

Two-dimensional transition metal chalcogenide wave-absorbing material, preparation method and application thereof Download PDF

Info

Publication number
CN111960468A
CN111960468A CN202010851270.9A CN202010851270A CN111960468A CN 111960468 A CN111960468 A CN 111960468A CN 202010851270 A CN202010851270 A CN 202010851270A CN 111960468 A CN111960468 A CN 111960468A
Authority
CN
China
Prior art keywords
wave
transition metal
absorbing material
metal chalcogenide
dimensional transition
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202010851270.9A
Other languages
Chinese (zh)
Other versions
CN111960468B (en
Inventor
宁明强
满其奎
谭果果
李润伟
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Ningbo Institute of Material Technology and Engineering of CAS
Original Assignee
Ningbo Institute of Material Technology and Engineering of CAS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Ningbo Institute of Material Technology and Engineering of CAS filed Critical Ningbo Institute of Material Technology and Engineering of CAS
Priority to CN202010851270.9A priority Critical patent/CN111960468B/en
Publication of CN111960468A publication Critical patent/CN111960468A/en
Application granted granted Critical
Publication of CN111960468B publication Critical patent/CN111960468B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00Compounds of molybdenum
    • C01G39/06Sulfides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G31/00Compounds of vanadium
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G41/00Compounds of tungsten
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05KPRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K9/00Screening of apparatus or components against electric or magnetic fields
    • H05K9/0073Shielding materials
    • H05K9/0081Electromagnetic shielding materials, e.g. EMI, RFI shielding
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/80Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/85Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/04Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Engineering & Computer Science (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)

Abstract

The invention relates to the field of electromagnetic functional materials, and discloses a two-dimensional transition metal chalcogenide wave-absorbing material, and a preparation method and application thereof. The preparation method of the wave-absorbing material comprises the steps of dissolving a transition metal source and a chalcogen source in a solvent, carrying out thermal reaction on the solution, and finally processing the solution to obtain the two-dimensional transition metal chalcogen compound wave-absorbing material; the solvent is a mixed solution of nitrogen methyl pyrrolidone and an alcohol reagent. According to the invention, the volume ratio of the azomethidone and the alcohol reagent in the reaction solvent is regulated, so that the ratio of the semiconductor phase (2H) to the metal phase (1T) in the prepared wave-absorbing material is accurately regulated, and the wave-absorbing material with significant advantages in indexes such as matching characteristics, maximum reflectivity, effective bandwidth and the like is obtained.

Description

Two-dimensional transition metal chalcogenide wave-absorbing material, preparation method and application thereof
Technical Field
The invention relates to the field of electromagnetic wave absorbing materials, in particular to a two-dimensional transition metal chalcogenide wave absorbing material, a preparation method and application thereof.
Background
At present, with the rapid development of information technology, electromagnetic wave-absorbing materials play an increasingly important role in the fields of military stealth, electronic communication and the like. As a novel two-dimensional material, two-dimensional transition metal chalcogenides (TMDs) have good physicochemical properties, thermal stability, and mechanical flexibility, and related studies in the field of dielectric wave absorption have attracted attention.
In MoS2For representativeness, the applicant prepared and reported two-dimensional molybdenum disulfide (MoS) for the first time in 20152) Dielectric wave-absorbing performance of the nano-sheet. The experimental results show that: MoS2The maximum reflectance loss of the nanoplatelets was-38.4 dB (Nanoscale,2015,7, 15734-15740).
Based on this work, many groups have continued their research into TMDs-type materials. For example, patent application with publication number CN105428820A discloses a graphene and molybdenum disulfide composite material, which can be used as an electromagnetic wave absorbing material for electromagnetic shielding or electromagnetic protection facilities, and has strong electromagnetic wave absorbing performance, light weight, wide absorption frequency band and strong absorption capacity.
Patent application with publication number CN107660114A discloses a MoS2the/Mxene layered composite wave-absorbing material is prepared by mixing molybdenum disulfide and MXene materials and then adopting a hydrothermal reaction to prepare MoS2Washing and drying initial powder of/MXene layered composite material to obtain MoS2the/MXene layered composite wave-absorbing material. The material has good wave absorbing performance in a microwave frequency range.
The patent application with the publication number of CN105883921A discloses a 3D type MoS with wide-band strong wave-absorbing capability2A nano-microsphere wave-absorbing material. The preparation method comprises the steps of dissolving reactants of sodium molybdate and L-cysteine in deionized water, uniformly stirring, and placing the mixture in a reaction kettle for reaction to obtain the 3D molybdenum disulfide nano microspheres. The invention adopts a simple hydrothermal method to prepare the 3D molybdenum disulfide nano-microsphere with special morphology, and the method is to prepare the molybdenum disulfide nano-microsphere with special morphologyThe composite material is compounded with a high polymer material polyvinylidene fluoride, and the wave-absorbing performance of the organic/inorganic nano composite material in a high-frequency band of 18-40 GHz is tested by combining a waveguide test method.
However, most of the currently reported TMDs-based wave-absorbing materials have the defects of poor impedance matching, high wave-absorbing matching thickness (4mm or even 8mm), limited wave-absorbing performance and the like, and are difficult to meet the requirement of rapid development in the electromagnetic field.
Disclosure of Invention
The present invention is directed to providing a method capable of significantly optimizing the impedance matching performance and the wave absorption performance of two-dimensional transition metal chalcogenides (TMDs). Compared with TMDs (transition metal oxides) type wave-absorbing materials prepared by the prior art, the wave-absorbing material prepared by the method has more excellent impedance matching property and wave-absorbing performance.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a two-dimensional transition metal chalcogenide wave-absorbing material comprises the steps of dissolving a transition metal source and a chalcogen source in a solvent, carrying out solvothermal reaction, and carrying out post-treatment to obtain the two-dimensional transition metal chalcogenide wave-absorbing material; the solvent is a mixed solution of nitrogen methyl pyrrolidone and an alcohol reagent.
The invention regulates and controls the reaction polar environment of reactants by regulating and controlling the solvent proportion in solvothermal, thereby accurately controlling the proportion of a semiconductor phase (2H) and a metal phase (1T) in the synthesized TMDS material. The introduction of the 1T phase in the TMDs material can improve the electric conduction loss of the material on one hand, and the introduction of the rich phase interface (2H/1T) can improve the polarization loss of the material on the other hand, thereby obviously optimizing the impedance matching characteristic of the TMDs material and improving the wave-absorbing performance of the wave-absorbing material. The total amount of the reaction solvent is preferably sufficient to dissolve and disperse the transition metal source and the chalcogen source.
The volume ratio of the N-methyl pyrrolidone to the alcohol reagent is 1-40: 1, preferably 2-30: 1. In the process of solvothermal reaction, the solvent is used for dissolving corresponding reaction precursors and transferring and assembling highly dispersed reaction atoms or molecules through a liquid medium. The dielectric constant is an important parameter for measuring the polarity of the reaction solvent. The reaction solvent with proper dielectric constant can effectively adjust the relaxation degree of chemical bonds in reactants, change the arrangement matching of atoms and molecules and induce new physical and chemical changes, thereby influencing the phase composition of the synthetic material. Considering the different solvent polarity characteristics of the N-methyl pyrrolidone and the alcohol reagent, the mixed reagents with different volume ratios can obtain solvothermal reaction environments with different polarities, thereby providing conditions for preparing TMDS materials with different phase contents. The method comprises the step of setting the polarity range of a controllable system with the volume ratio of the N-methyl pyrrolidone to the alcohol reagent of 1-40: 1, so as to control the relative content of 2H and 1T in the material. The materials with different contents have different influences on the wave-absorbing performance, and the wave-absorbing performance of the material is finally controlled by controlling the proportion of the solvent.
The alcohol reagent includes but is not limited to one or more of methanol, ethanol, isopropanol.
Preferably, the alcohol reagent is ethanol. The polarity of the ethanol is intermediate, the polarity of a solvothermal reaction system can be adjusted by the cooperation of the ethanol and the N-methyl pyrrolidone, and the relative content of 2H and 1T phases in the material can be easily adjusted. The wave-absorbing performance and the impedance matching performance of the material are adjusted. Under the selection of the raw materials, when the volume ratio of the two is in the range, the mixed solvent in the ratio has the optimal polarity, and thus the two-dimensional transition metal chalcogenide wave-absorbing material with excellent impedance matching characteristic and excellent wave-absorbing performance is prepared.
The transition metal source comprises one or more of a sodium salt, a chloride salt, or a thioammonium salt of a transition metal.
Wherein the transition metal includes, but is not limited to, one or more metal elements selected from Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Zr, Nb, Mo, Hf, Ta, W, Re.
The chalcogen in the chalcogen source comprises sulfur, selenium and tellurium, and preferably the chalcogen source comprises one or more of thiourea, selenourea and telluride.
Further preferably, the transition metal source is a thioammonium salt of a transition metal, and the chalcogen source is thiourea. The synergistic effect of the two is good, and the impedance matching characteristic and the wave absorbing performance of the material can be adjusted conveniently.
Further preferably, when the transition metal source is ammonium thiomolybdate, the volume ratio of the N-methyl pyrrolidone to the alcohol reagent is 2-15: 1; and when the transition metal source is ammonium thiogallate or ammonium thiotungstate, the volume ratio of the N-methyl pyrrolidone to the alcohol reagent is 15-30: 1.
The molar ratio of the transition metal source to the chalcogen source is 1: 3-6; considering the polar easy-dissolution characteristic of the chalcogen element in the thermochemical reaction process of the related solvent, properly increasing the relative molar content of the chalcogen element is favorable for making up the deficiency of the chalcogen element in the reaction process and improving the crystallinity of the reaction product.
The molar ratio of the transition metal source to the chalcogen source is 180-220 ℃, and the reaction time is 8-24 hours. Generally speaking, as the reaction temperature is increased, the solubility of the transition metal source in the solvent is gradually increased, and the distribution of the relevant metal ions in the solvent is more likely to be commented on, which is favorable for the homogeneous phase reaction. Meanwhile, the improvement of the reaction time is beneficial to improving the crystallinity and the two-dimensional characteristics of the reaction product, so that the wave-absorbing property of the material is improved.
The post-treatment includes conventional purification steps of centrifugation, washing, drying, etc. to improve the purity and yield of the material.
The invention also provides the two-dimensional transition metal chalcogenide wave-absorbing material prepared by the preparation method, wherein the mass ratio of the semiconductor phase (2H) to the metal phase (1T) in the two-dimensional transition metal chalcogenide wave-absorbing material is 1: 0.2 to 3, preferably 1: 0.5 to 1.5. When the proportion of the two phases is in the range, the impedance matching characteristic and the comprehensive wave absorbing performance of the prepared material are optimal.
The invention also provides application of the two-dimensional transition metal chalcogenide wave-absorbing material prepared by the preparation method in the fields of high-frequency electromagnetic compatibility and protection. The wave-absorbing material has obvious advantages in indexes such as matching characteristics, maximum reflectivity, effective coverage bandwidth and the like, and can be applied to relevant fields such as darkroom protection, 5G communication, electromagnetic stealth protection and the like.
Compared with the prior art, the invention has the following beneficial effects:
the two-dimensional transition metal chalcogenide wave-absorbing material provided by the invention has excellent impedance matching characteristics in a broadband frequency band of 2-18 GHz; when the matching thickness is 3.0mm, the maximum reflectivity is-43 dB, and the effective absorption bandwidth with the reflectivity value less than-10 dB is 2 GHz. Compared with the existing wave-absorbing material, the TMDS wave-absorbing material has obvious advantages in indexes such as matching characteristics, maximum reflectivity, effective coverage bandwidth and the like, and is expected to be applied in the fields of 5G communication, stealth protection and the like.
Drawings
FIG. 1 is a XPS crystal phase composition characterization map of the wave-absorbing material prepared in example 2 and comparative examples 1 and 2, wherein (a) is comparative example 1, (b) is example 2, and (c) is comparative example 2;
FIG. 2 is a schematic representation of the preparation of 2H/1T-1:1-MoS in example 22The TEM appearance of the wave-absorbing material is characterized;
FIG. 3 is the 2H/1T-1:1.6-MoS of example 12A reflection loss spectrum of the wave-absorbing material in a frequency band of 2-18 GHz;
FIG. 4 shows 2H/1T-1:1-MoS of example 22A reflection loss spectrum of the wave-absorbing material in a frequency band of 2-18 GHz;
FIG. 5 is the 2H/1T-1:0.4-MoS of example 32A reflection loss spectrum of the wave-absorbing material in a frequency band of 2-18 GHz;
FIG. 6 is the 2H/1T-1:1-MoS of example 42A reflection loss spectrum of the wave-absorbing material at the temperature of-220 ℃ in a frequency band of 2-18 GHz;
FIG. 7 shows 2H/1T-1:1-VS in example 52The wave-absorbing material reflects a loss spectrum within 2-18 GHz;
FIG. 8 shows 2H/1T-1:1-WS of example 62The wave-absorbing material reflects a loss spectrum within 2-18 GHz;
FIG. 9 is 2H-MoS of comparative example 12The reflection loss spectrum of the wave-absorbing material in 2-18 GHz;
FIG. 10 is 1T-MoS of comparative example 22The reflection loss spectrum of the wave-absorbing material in 2-18 GHz;
FIG. 11 is a comparison graph of impedance matching factors of the wave-absorbing materials prepared in examples 2 and 5 and comparative examples 1 and 2 in a frequency range of 2-18 GHz.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. Those skilled in the art should understand that they can make modifications and equivalents without departing from the spirit and scope of the present invention, and all such modifications and equivalents are intended to be included within the scope of the present invention.
Example 1
(1) Ammonium thiomolybdate and thiourea in corresponding mass are weighed according to the molar ratio of 1:5 and placed in a 50mL beaker. Adding 20mL of nitrogen methyl pyrrolidone and 5mL of ethanol, and fully stirring for 1h to obtain a mixed solution; the obtained reaction solution was transferred to a solvothermal reaction inner bushing with a capacity of 50mL, the inner bushing was sealed in a stainless steel outer bushing, and the reaction was carried out at 200 ℃ for 15 hours.
(2) After the reaction is finished, placing the product in a centrifugal tube for high-speed centrifugation at 10000rpm for 20min, taking the tube bottom product, washing the tube bottom product for 2-3 times by deionized water and absolute ethyl alcohol respectively, and then placing the tube bottom product in a 50 ℃ drying oven for drying for 15H to obtain a final product 2H/1T-1:1.6-MoS2And (3) a wave-absorbing material.
Example 2
The preparation process of example 1 is followed, with the difference that: the reaction solvent in the step (1) is changed into 27mL of nitrogen methyl pyrrolidone and 3mL of ethanol to prepare 2H/1T-1:1-MoS2And (3) a wave-absorbing material.
Example 3
The preparation process of example 1 is followed, with the difference that: the reaction solvent in the step (1) is changed into 28mL of nitrogen methyl pyrrolidone and 2mL of ethanol to prepare 2H/1T-1:0.4-MoS2And (3) a wave-absorbing material.
Example 4
The procedure of example 2 was followed except that: the reaction temperature in the step (1) is changed to 220 ℃ to prepare 2H/1T-1:1-MoS2-220 ℃ wave-absorbing material.
Example 5
The procedure of example 2 was followed except that: the ammonium thiomolybdate in step (1) of example 2 was replaced with equimolar ammonium thiovanadate; the reaction solvent in step (1) of example 2 was changed to 28.5mL of N-methylpyrrolidone and 1.5mL of ethanol to give 2H/1T-1:1-VS2And (3) a wave-absorbing material.
Example 6
The procedure of example 2 was followed except that: replacing ammonium thiomolybdate in step (1) of example 2 with equimolar ammonium thiotungstate; the reaction solvent in step (1) of example 2 was changed to 28.5mL of N-methylpyrrolidone and 1.5mL of ethanol to prepare 2H/1T-1:1-WS2And (3) a wave-absorbing material.
Comparative example 1
The preparation process of example 1 is followed, with the difference that: the reaction solvent in the step (1) is changed into 30mL of nitrogen methyl pyrrolidone, and the 2H-MoS is prepared2And (3) a wave-absorbing material.
Comparative example 2
The preparation process of example 1 is followed, with the difference that: the reaction solvent in the step (1) is changed into 10mL of nitrogen methyl pyrrolidone and 20mL of ethanol to prepare 1T-MoS2And (3) a wave-absorbing material.
And (3) testing the structure:
the crystal phase composition of the product was tested by X-ray photoelectron spectroscopy. As shown in fig. 1: from the peak separation results, it can be seen that MoS was obtained in example 2 and comparative examples 1 and 22The wave-absorbing material has different crystal phase compositions which are respectively 2H/1T-1:1 (b in figure 1), 100% -2H (a in figure 1) and 100% -1T (c in figure 1).
And (3) characterizing the micro-topography of the wave-absorbing material prepared in the example 2 by using a transmission electron microscope (JEOL-2011). As shown in fig. 2: the prepared 2H/1T-1:1-MoS2The material exhibits typical two-dimensional material properties with dimensions of about 500 nm.
Performance testing
The wave-absorbing materials prepared in the embodiments 1-6 and the comparative examples 1 and 2 are respectively and uniformly mixed with paraffin according to the mass ratio of 1:1 (namely, the content of the absorbent is 50%), and then the mixture is pressed into a standard coaxial sample ring with the inner diameter of 3.0mm, the outer diameter of 7.04mm and the thickness of 2.0mm in a special mould. The electromagnetic absorption properties of the samples were tested in the 2-18GHz range using a vector network analyzer (agilent n5234A), respectively.
Using 2H/1T-1:1.6-MoS as described in example 12The electromagnetic wave absorption performance of the sample prepared by the wave-absorbing material is shown in figure 3. The wave-absorbing material has a maximum reflectivity of-12 dB and an effective bandwidth of 2GHz when the matching thickness is 3.0mm in a frequency band of 2-18 GHz.
Using the 2H/1T-1:1-MoS described in example 22The electromagnetic wave absorption performance of the sample prepared by the wave-absorbing material is shown in figure 4. The wave-absorbing material has a maximum reflectivity of-43 dB and an effective bandwidth of 2GHz when the matching thickness is 3.0mm in a frequency band of 2-18 GHz.
Using 2H/1T-1:0.4-MoS as described in example 32The electromagnetic wave absorption performance of the sample prepared by the wave-absorbing material is shown in figure 5. The wave-absorbing material has the maximum reflectivity of-12.5 dB and the effective bandwidth of 3GHz within the frequency band of 2-18GHz when the matching thickness is 3.0 mm.
Using 2H/1T-1:1-MoS as described in example 42The electromagnetic wave absorption performance of a sample prepared by the wave-absorbing material at the temperature of-220 ℃ is shown in figure 6. The wave-absorbing material has the maximum reflectivity of-28.5 dB and the effective bandwidth of 2.4GHz within the frequency band of 2-18GHz when the matching thickness is 3.0 mm.
Using 2H/1T-1:1-VS as described in example 52The electromagnetic wave absorption performance of the sample prepared by the wave-absorbing material is shown in figure 7. The wave-absorbing material has the maximum reflectivity of-38 dB and the effective bandwidth of 1.8GHz within the frequency band of 2-18GHz and the matching thickness of 3 mm.
Using 2H/1T-1:1-WS as described in example 62The electromagnetic wave absorption performance of the sample prepared by the wave-absorbing material is shown in figure 8. The wave-absorbing material has the maximum reflectivity of-36 dB and the effective bandwidth of 2GHz when the matching thickness is 3mm in the frequency band of 2-18 GHz.
Utilizing the 2H-MoS as described in comparative example 12The electromagnetic wave absorption performance of the sample prepared by the wave-absorbing material is shown in figure 9. When the matching thickness is 3.0mm, the maximum reflectivity is-8 dB in 2-18GHz, and the effective loss bandwidth is 0 GHz.
Utilizing the 1T-MoS as described in comparative example 22The electromagnetic wave absorption performance of the sample prepared by the wave-absorbing material is shown in figure 10. When the matching thickness is 3.0mm, the maximum reflectivity of the antenna is-12 dB within 2-18GHz, and the effective bandwidth is 1 GHz.
The samples prepared in the embodiments 2 and 5 and the comparative examples 1 and 2 are used for calculating an impedance matching factor Z (Z represents an impedance matching parameter which represents the difficulty of incident electromagnetic waves entering the wave-absorbing material, and the numerical value of the impedance matching parameter is closer to 1 which represents that the incident electromagnetic waves are easier to enter the material, thereby being beneficial to the attenuation of the electromagnetic waves). As shown in fig. 11: examples 2 and 5 and comparative examples 1 and 2 the Z of the prepared samples varies with the relative content of 2H and 1T in the material, and the two-dimensional transition metal chalcogenide having a 1:1 phase composition has excellent impedance matching characteristics.

Claims (10)

1. A preparation method of a two-dimensional transition metal chalcogenide wave-absorbing material is characterized in that a transition metal source and a chalcogen source are dissolved in a solvent, and the two-dimensional transition metal chalcogenide wave-absorbing material is obtained through the thermal reaction of the solvent and the post-treatment; the solvent is a mixed solution of nitrogen methyl pyrrolidone and an alcohol reagent.
2. The preparation method of the two-dimensional transition metal chalcogenide wave-absorbing material according to claim 1, wherein the volume ratio of the N-methyl pyrrolidone to the alcohol reagent is 1-40: 1.
3. the method for preparing a two-dimensional transition metal chalcogenide wave-absorbing material according to claim 1, wherein the alcohol reagent comprises one or more of methanol, ethanol and isopropanol.
4. The method according to claim 1, wherein the transition metal source comprises one or more of a sodium salt, a chloride salt or a thioammonium salt of a transition metal.
5. The method for preparing the two-dimensional transition metal chalcogenide wave-absorbing material according to claim 1, wherein the chalcogen source comprises one or more of thiourea, selenourea or telluride.
6. The preparation method of the two-dimensional transition metal chalcogenide wave-absorbing material according to claim 1, wherein when the transition metal source is ammonium thiomolybdate, the volume ratio of the N-methyl pyrrolidone to the alcohol reagent is 2-15: 1; and when the transition metal source is ammonium thiogallate or ammonium thiotungstate, the volume ratio of the N-methyl pyrrolidone to the alcohol reagent is 15-30: 1.
7. The method for preparing the two-dimensional transition metal chalcogenide wave-absorbing material according to claim 1, wherein the molar ratio of the transition metal source to the chalcogen source is 1: 3 to 6.
8. The preparation method of the two-dimensional transition metal chalcogenide wave-absorbing material according to claim 1, wherein the solvothermal reaction temperature is 180-220 ℃ and the reaction time is 8-24 hours.
9. A two-dimensional transition metal chalcogenide wave-absorbing material prepared according to any one of claims 1 to 8, wherein the mass ratio of a semiconductor phase to a metal phase in the two-dimensional transition metal chalcogenide wave-absorbing material is 1: 0.2 to 3.
10. The two-dimensional transition metal chalcogenide wave-absorbing material obtained according to claim 9 is applied to the field of high-frequency electromagnetic compatibility and protection.
CN202010851270.9A 2020-08-21 2020-08-21 Two-dimensional transition metal chalcogenide wave-absorbing material, preparation method and application thereof Active CN111960468B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010851270.9A CN111960468B (en) 2020-08-21 2020-08-21 Two-dimensional transition metal chalcogenide wave-absorbing material, preparation method and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010851270.9A CN111960468B (en) 2020-08-21 2020-08-21 Two-dimensional transition metal chalcogenide wave-absorbing material, preparation method and application thereof

Publications (2)

Publication Number Publication Date
CN111960468A true CN111960468A (en) 2020-11-20
CN111960468B CN111960468B (en) 2022-12-06

Family

ID=73389959

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010851270.9A Active CN111960468B (en) 2020-08-21 2020-08-21 Two-dimensional transition metal chalcogenide wave-absorbing material, preparation method and application thereof

Country Status (1)

Country Link
CN (1) CN111960468B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114804218A (en) * 2022-05-19 2022-07-29 郑州大学 Microwave absorbing material with multilevel heterostructure and preparation method thereof

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102603006A (en) * 2011-12-20 2012-07-25 上海大学 Method for synthetizing nanometer molybdenum disulfide transparent colloid
CN104108755A (en) * 2014-07-25 2014-10-22 深圳新宙邦科技股份有限公司 Curved-surface molybdenum disulfide nanosheet and preparation method thereof
CN105217567A (en) * 2015-09-07 2016-01-06 复旦大学 A kind of molybdenum disulfide nano sheet/graphene nano belt composite and preparation method thereof
CN106082304A (en) * 2016-06-07 2016-11-09 上海师范大学 A kind of preparation method of flower-shaped copper sulfide N-methyl ketopyrrolidine dispersant
CN106675516A (en) * 2016-11-30 2017-05-17 中国人民解放军国防科学技术大学 Transition metal chalcogenide-carbonyl iron powder composite microwave absorbent and preparation method thereof
CN108585042A (en) * 2018-07-02 2018-09-28 陕西科技大学 A kind of extra small flower-shaped VS of nanometer sheet self assembly2Powder and preparation method thereof
CN108996478A (en) * 2018-08-22 2018-12-14 郑州轻工业学院 A kind of MNxSuper crystal and its preparation method and application
CN109037641A (en) * 2018-08-07 2018-12-18 河源广工大协同创新研究院 A kind of lithium ion battery MoS2The preparation method of negative electrode material
CN110684507A (en) * 2019-10-09 2020-01-14 中国科学院宁波材料技术与工程研究所 Core-shell structure type wave-absorbing material and preparation method and application thereof

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102603006A (en) * 2011-12-20 2012-07-25 上海大学 Method for synthetizing nanometer molybdenum disulfide transparent colloid
CN104108755A (en) * 2014-07-25 2014-10-22 深圳新宙邦科技股份有限公司 Curved-surface molybdenum disulfide nanosheet and preparation method thereof
CN105217567A (en) * 2015-09-07 2016-01-06 复旦大学 A kind of molybdenum disulfide nano sheet/graphene nano belt composite and preparation method thereof
CN106082304A (en) * 2016-06-07 2016-11-09 上海师范大学 A kind of preparation method of flower-shaped copper sulfide N-methyl ketopyrrolidine dispersant
CN106675516A (en) * 2016-11-30 2017-05-17 中国人民解放军国防科学技术大学 Transition metal chalcogenide-carbonyl iron powder composite microwave absorbent and preparation method thereof
CN108585042A (en) * 2018-07-02 2018-09-28 陕西科技大学 A kind of extra small flower-shaped VS of nanometer sheet self assembly2Powder and preparation method thereof
CN109037641A (en) * 2018-08-07 2018-12-18 河源广工大协同创新研究院 A kind of lithium ion battery MoS2The preparation method of negative electrode material
CN108996478A (en) * 2018-08-22 2018-12-14 郑州轻工业学院 A kind of MNxSuper crystal and its preparation method and application
CN110684507A (en) * 2019-10-09 2020-01-14 中国科学院宁波材料技术与工程研究所 Core-shell structure type wave-absorbing material and preparation method and application thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114804218A (en) * 2022-05-19 2022-07-29 郑州大学 Microwave absorbing material with multilevel heterostructure and preparation method thereof

Also Published As

Publication number Publication date
CN111960468B (en) 2022-12-06

Similar Documents

Publication Publication Date Title
CN110684507B (en) Core-shell structure type wave-absorbing material and preparation method and application thereof
CN112961650B (en) Three-metal organic framework derived iron-nickel alloy/porous carbon ultrathin wave absorber and preparation method thereof
Wei et al. Defect-induced insulator-metal transition and negative permittivity in La1-xBaxCoO3 perovskite structure
CN110790268B (en) Boron and nitrogen co-doped graphene wave-absorbing material and preparation method and application thereof
CN109019688A (en) Magnetic molybdenum disulfide microwave absorbent doped with transition metal elements and preparation method thereof
CN111960468B (en) Two-dimensional transition metal chalcogenide wave-absorbing material, preparation method and application thereof
CN114449877A (en) Core-shell Ni/Co alloy @ nitrogen-doped carbon-based wave-absorbing composite material and preparation method thereof
CN114715947A (en) SrNdMnO wave absorbing material and preparation method thereof
CN115784317A (en) LaCaFeO wave-absorbing material and preparation method thereof
CN114634208A (en) Oxide composite material and preparation method and application thereof
CN112996375B (en) Cu9S5/C composite material and preparation method and application thereof
CN116914411B (en) Magneto-dielectric material optimization-based 5G antenna manufacturing method, device and apparatus
CN113735093A (en) Porous N-doped Co @ C composite material and preparation method and application thereof
CN109574663A (en) A kind of Ni-Ti-Ta base microwave medium ceramic material and preparation method thereof
CN113045304A (en) Ferrite wave-absorbing material with mixed spinel structure and preparation method thereof
CN114524419B (en) Castor-like graphite carbon nitride nanotube/cobalt/carbon composite material and preparation method thereof
Kaur et al. Modulation of microwave properties of La–Sr hexagonal ferrite with doping of Co–Zr and change in thickness
CN114411132A (en) Preparation method of cobalt-nickel alloy particle hydrophilic carbon cloth composite material with corn cob-like heterostructure
CN113415796A (en) Application of Cu/C composite material as electromagnetic wave absorption material
Jalal et al. GPS patch antenna performance by modification of Zn (1− x) Ca x Al 2 O 4-based microwave dielectric ceramics
CN106977203B (en) Zero-temperature-coefficient low-temperature sintering microwave medium and preparation method thereof
CN116904164A (en) One-dimensional MnO 2 @CuS composite electromagnetic wave absorbing material and preparation method and application thereof
CN112342623B (en) Nano-rod-shaped antimony trisulfide electromagnetic wave absorption material, absorber, preparation method and application
CN109534815A (en) Modified BaO-TiO2-La2O3The preparation method of dielectric ceramic
CN112292016B (en) Preparation method of rare earth composite wave-absorbing material

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant