CN111960468B - 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 PDFInfo
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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
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, and 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 excellent physicochemical properties, thermal stability, and mechanical flexibility, and their research on the field of dielectric wave absorption has attracted attention.
In MoS 2 For representativeness, the applicant prepared and reported two-dimensional molybdenum disulfide (MoS) for the first time in 2015 2 ) Dielectric wave-absorbing performance of the nano-sheet. The experimental results show that: moS 2 The maximum reflectance loss of the nanoplatelets is-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 and applied to electromagnetic shielding or electromagnetic protection facilities, and the material has strong electromagnetic wave absorption performance, and is a novel wave absorbing material with light weight, wide absorption frequency band and strong absorption capacity.
Patent application with publication number CN107660114A discloses a MoS 2 The Mxene layered composite wave-absorbing material is prepared by mixing molybdenum disulfide and MXene materials and adopting a hydrothermal reaction to prepare MoS 2 The initial powder of the/MXene layered composite material is washed and dried to obtain MoS 2 the/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 CN105883921A discloses a 3D type MoS with broadband strong wave-absorbing capability 2 A 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 method adopts a simple hydrothermal method to prepare the 3D molybdenum disulfide nano-microspheres with special morphology, compounds the 3D molybdenum disulfide nano-microspheres with a high polymer material polyvinylidene fluoride, and combines a waveguide test method to test the wave absorbing performance of the organic/inorganic nano-composite material at a high frequency range of 18-40 GHz.
However, most of the currently reported TMDs-type wave-absorbing materials have the defects of poor impedance matching, high wave-absorbing matching thickness (4 mm or even 8 mm), 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 wave-absorbing material 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 realize 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 a 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 to 30. 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 regulate the chemical bond relaxation degree of reactant, change the arrangement and matching of atoms and molecules and induce new physical and chemical change to affect 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 invention sets the volume ratio of N-methyl pyrrolidone to alcohol reagent as 1-40, and controls the polarity range of the controllable system, thereby controlling the relative contents 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 materials 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 centered, so that the polarity of a solvothermal reaction system can be adjusted by cooperating with the azomethyl pyrrolidone, and the relative content of 2H and 1T phases in the material can be easily adjusted and controlled. 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 proportion has the optimal polarity, and then 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 or 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.
More preferably, when the transition metal source is ammonium thiomolybdate, the volume ratio of the N-methylpyrrolidone to the alcohol reagent is 2-15; 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.
The molar ratio of the transition metal source to the chalcogen source is 1:3 to 6; considering the polar easy-to-dissolve characteristic of the chalcogen element in the thermochemical reaction process of the relevant solvent, properly increasing the relative molar content of the chalcogen element is favorable for making up the loss 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 tends to be more commented, which is favorable for homogeneous 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 a 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 2GHz. 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 graph of example 2 preparation of 2H/1T-1 2 The TEM appearance of the wave-absorbing material is characterized;
FIG. 3 is 2H/1T-1 of example 1 2 Wave-absorbing material is inA reflection loss map in the 2-18GHz frequency band;
FIG. 4 is the 2H/1T-1 of example 2 2 Reflection loss spectrum of the wave-absorbing material in the frequency band of 2-18 GHz;
FIG. 5 is 2H/1T-1 of example 3 2 Reflection loss spectrum of the wave-absorbing material in the frequency band of 2-18 GHz;
FIG. 6 is 2H/1T-1 2 Reflection loss spectrum of the wave-absorbing material at the temperature of minus 220 ℃ in a frequency band of 2-18 GHz;
FIG. 7 is 2H/1T-1 of example 5 2 The wave-absorbing material reflects a loss spectrum within 2-18 GHz;
FIG. 8 is 2H/1T-1 of example 6 2 The wave-absorbing material reflects a loss pattern within 2-18 GHz;
FIG. 9 is 2H-MoS of comparative example 1 2 The reflection loss spectrum of the wave-absorbing material within 2-18 GHz;
FIG. 10 is 1T-MoS of comparative example 2 2 The reflection loss spectrum of the wave-absorbing material within 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 do not 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 were weighed according to the molar ratio of 1. Adding 20mL of N-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 centrifuge tube for high-speed centrifugation at 10000rpm for 20min, taking the tube bottom product, washing the tube bottom product with deionized water and absolute ethyl alcohol for 2-3 times 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 2 And (3) a wave-absorbing material.
Example 2
The preparation process of example 1 is followed, with the difference that: and (2) replacing the reaction solvent in the step (1) by 27mL of nitrogen methyl pyrrolidone and 3mL of ethanol to prepare 2H/1T-1 2 And (3) a wave-absorbing material.
Example 3
The preparation process of example 1 is followed, with the difference that: the reaction solvent in step (1) was changed to 28mL of aminomethylpyrrolidone and 2mL of ethanol to produce a 2H/1T-1 2 And (3) wave-absorbing materials.
Example 4
The procedure of example 2 was followed except that: the reaction temperature in the step (1) is changed to 220 ℃, and the reaction temperature of 2H/1T-1 2 -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 prepare 2H/1T-1 2 And (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 2 And (3) wave-absorbing materials.
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 to prepare 2H-MoS 2 And (3) a wave-absorbing material.
Comparative example 2
The procedure of example 1 was followed except that: the reaction solvent in the step (1) is changed into 10mL of nitrogen methyl pyrrolidone and 20mL of ethanol to prepare 1T-MoS 2 And (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 2 2 The wave-absorbing material has different crystal phase compositions of 2H/1T-1 (b in figure 1), 100% -2H (a in figure 1) and 100% -1T (c in figure 1), respectively.
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: 2H/1T-1 produced 2 The material exhibits typical two-dimensional material properties with dimensions of about 500nm.
Performance testing
The wave-absorbing materials prepared in the above examples 1 to 6 and comparative examples 1 and 2 are respectively and uniformly mixed with paraffin according to the mass ratio of 1. The electromagnetic absorption properties of the samples were tested in the 2-18GHz range using a vector network analyzer (agilent n 5234A), respectively.
Using 2H/1T-1 as described in example 1 2 The 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 within a frequency band of 2-18GHz when the matching thickness is 3.0 mm.
Using the 2H/1T-1 described in example 2 2 The 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 within a frequency band of 2-18GHz when the matching thickness is 3.0 mm.
Using 2H/1T-1 as described in example 3 2 The electromagnetic wave absorption performance of the sample prepared by the wave-absorbing material is shown in figure 5. The wave-absorbing material has a maximum reflectivity of-12.5 dB and an effective bandwidth of 3GHz within a frequency band of 2-18GHz when the matching thickness is 3.0 mm.
Using 2H/1T-1 as described in example 4 2 The 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 and the matching thickness of 3.0 mm.
Using 2H/1T-1 as described in example 5 2 The 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 as described in example 6 2 The 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 minus 36dB 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 1 2 The 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 the range of 2-18GHz, and the effective loss bandwidth is 0GHz.
1T-MoS as described in comparative example 2 2 The 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 in the range of 2-18GHz, and the effective bandwidth is 1GHz.
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 contents of 2H and 1T in the material, and the two-dimensional transition metal chalcogenide having phase 1.
Claims (9)
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; the volume ratio of the N-methyl pyrrolidone to the alcohol reagent is 1-40: 1;
the ratio of the nitrogen methyl pyrrolidone to the alcohols in the solvent can adjust the content ratio of the metal phase to the semiconductor phase in the two-dimensional transition metal chalcogenide wave-absorbing material.
2. 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.
3. 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.
4. 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.
5. The method for preparing 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-methylpyrrolidone to the alcohol reagent is 2-15; 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.
6. 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.
7. The method for preparing 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.
8. A two-dimensional transition metal chalcogenide wave-absorbing material prepared according to any one of claims 1 to 7, wherein the mass ratio of the semiconductor phase to the metal phase in the two-dimensional transition metal chalcogenide wave-absorbing material is 1:0.2 to 3.
9. The two-dimensional transition metal chalcogenide wave-absorbing material obtained according to the method in claim 8 is applied to the fields of high-frequency electromagnetic compatibility and protection.
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