CN115594222A - Two-dimensional FeNi @ MoS 2 Nano-structure electromagnetic wave absorption material and preparation method thereof - Google Patents
Two-dimensional FeNi @ MoS 2 Nano-structure electromagnetic wave absorption material and preparation method thereof Download PDFInfo
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- 229910002555 FeNi Inorganic materials 0.000 title claims abstract description 67
- 238000010521 absorption reaction Methods 0.000 title claims abstract description 26
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 25
- 239000000463 material Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims description 22
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims abstract description 63
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 45
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 38
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- 239000011358 absorbing material Substances 0.000 claims abstract description 21
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 claims abstract description 19
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Abstract
The invention provides FeNi @ MoS 2 The electromagnetic wave absorbing material is prepared by the following steps: firstly, a proper amount of tetrabutylammonium bromide is weighed and dissolved in acetonitrile solution, and ultrasonic treatment is carried out to prepare 8mg/ml solution. Pouring the prepared solution into an electrochemical cell, and stripping molybdenite into single-layer or multi-layer nanosheets; adding a certain amount of NiCl 2 ·6H 2 O and FeCl 3 ·6H 2 Adding O into deionized water, performing ultrasonic treatment until the O is completely dissolved, and adding a certain amount of NaOH and N 2 H 4 ·H 2 O (40 wt%). Putting the above products into waterAfter hydrothermal reaction in the thermal reaction kettle, centrifuging and drying the product, and collecting FeNi @ MoS 2 And (3) obtaining the product. FeNi @ MoS obtained by the invention 2 The wave-absorbing material presents a two-dimensional multi-gap structure, and the shape of the nano material can pass through MoS 2 And (4) regulating and controlling the doping ratio. The multi-gap two-dimensional nano structure and the components of the material enable the material to have more excellent microwave absorption performance.
Description
Technical Field
The invention relates to the field of electromagnetic wave absorbing materials with a nano structure, in particular to two-dimensional FeNi @ MoS 2 A nano-structure electromagnetic wave absorbing material and a preparation method thereof.
Background
With the progress of science and technology, electronic equipment such as mobile phones and computers brings great convenience to people. However, the electromagnetic waves are harmful to the physical health of people, affect the normal operation of mechanical equipment, seriously leak information and harm the information safety of individuals and countries. Therefore, it is of great research significance to find an advanced electromagnetic wave absorbing material to solve the electromagnetic wave pollution caused by electromagnetic wave radiation. As for the current research on electromagnetic wave absorption, electromagnetic wave absorbing materials can be classified into: magnetic loss materials and dielectric loss materials. Magnetic loss materials generally include ferrites, metal oxides, magnetic alloy particles; dielectric lossy materials generally include carbonaceous materials and conductive polymers. The pursuit of the electromagnetic wave absorbing material at present is light weight, wide bandwidth, good attenuation capability and thin thickness. Traditional absorbents, such as metals, have strong electromagnetic wave absorption performance due to high conductivity and dielectric constant, but pure metals have the defects of poor corrosion resistance, high manufacturing cost, high density and the like in practical application. And an ideal electromagnetic wave absorber should have a moderate dielectric constant and high magnetic permeability according to impedance matching conditions. In addition, the multi-gap structure can effectively reflect the electromagnetic waves, and further more electromagnetic waves are lost.
In recent years, research shows that molybdenum disulfide (MoS) 2 ) As representative transition metal dihalide compounds (TMDs), they are attractive as microwave absorbing materials because of their excellent electronic characteristics and excellent chemical and physical properties. Two hexagonal (2H) phase MoS 2 Molybdenite from nature. Theoretical research shows that MoS 2 The band gap of (a) increases with decreasing crystal thickness, which can range from an indirect band gap of 1.2eV in bulk to a direct band gap of 1.9eV in single layer band gap. MoS of layered structure 2 By forming stable in-plane bonds through S-Mo-S bonds with 0.62nm interlayer spacing to facilitate rapid passage of sodium ions through the layerIntercalation and deintercalation, indicating that molybdenite can be easily exfoliated into single or few layers of nanoplatelets. In electromagnetic wave absorption applications, moS 2 The interaction between the layers generates polarization behavior and causes dielectric loss of electromagnetic waves, indicating the potential for excellent electromagnetic wave absorption properties. However, pure MoS 2 MoS for impedance matching, which does not have a good effect on electromagnetic wave absorption 2 And compounding with various dielectric materials or magnetic materials.
Disclosure of Invention
The invention aims to prepare a two-dimensional nano-structure FeNi @ MoS with wide effective absorption frequency band and excellent microwave absorption performance 2 Electromagnetic wave absorbing material
The invention provides two-dimensional FeNi @ MoS 2 The preparation method of the nano-structure electromagnetic wave absorption material comprises the following steps:
step 1, stripping molybdenite by adopting an electrochemical method to obtain single-layer or several-layer nanosheets:
pouring an acetonitrile solution of tetrabutylammonium bromide into an electrochemical cell, wherein a platinum electrode and the sheet molybdenite are respectively connected with a positive electrode and a negative electrode of the electrochemical cell; applying voltage to the electrochemical cell to perform electrochemical reaction to obtain stripped molybdenite;
taking out the stripped molybdenite from the electrochemical cell, and cleaning;
adding deionized water into the washed molybdenite for freezing treatment, and then drying the molybdenite by a freeze dryer to obtain nano flaky molybdenite;
Preparation of NiCl 2 And FeCl 3 Aqueous solution, and the MoS 2 Dissolved into the NiCl 2 And FeCl 3 Obtaining solution A in the aqueous solution, wherein the NiCl is 2 And FeCl 3 In the aqueous solution, the mass concentration of the Ni element and the Fe element is the same;
mixing NaOH aqueous solution with N 2 H 4 Sequentially adding the aqueous solution into the solution A to obtain a solution B;
will be described in detail1 and the solution B are put into a hydrothermal reaction kettle together for hydrothermal reaction; centrifuging and drying the product after the reaction is finished to obtain FeNi @ MoS 2 。
Preferably, in the step 1, the concentration of the acetonitrile solution of tetrabutylammonium bromide is 8mg/ml
Preferably, in the step 2, the preparation method of the solution a comprises: mixing a solution of mmolNiCl 2 ·6H 2 O and l mmol FeCl 3 ·6H 2 Dissolving O in 40ml deionized water, adding 40-100 mg MoS 2 And carrying out ultrasonic treatment to obtain a solution A.
Preferably, in the step 2, the preparation method of the solution B comprises: 10ml of a 5mol/L NaOH solution and 8ml of an 80wt% N 2 H 4 ·H 2 The O solution is added into the solution A in sequence.
Preferably, in the step 1, the direct current voltage required by the electrochemical reaction is 12V; in the step 2, the reaction conditions of the hydrothermal reaction are as follows: reaction at 150 ℃ for 8 hours, and drying conditions are as follows: drying in vacuum at 60 deg.C for 12 hr.
Preferably, in the step 1, the voltage applied to the electrochemical cell is a dc voltage of 12V, and the electrochemical reaction is performed for 8 hours.
Preferably, in the step 1, the preparation method of the acetonitrile solution of tetrabutylammonium bromide comprises the following steps: adding tetrabutylammonium bromide into acetonitrile and carrying out ultrasonic treatment to obtain an acetonitrile solution of the tetrabutylammonium bromide;
the invention also provides FeNi @ MoS 2 Nano-structured electromagnetic wave absorbing material, said FeNi @ MoS 2 The nano-structure electromagnetic wave absorption material is formed by stacking a plurality of two-dimensional sheet structures, each two-dimensional sheet structure is nano-sheet molybdenite obtained after molybdenite is stripped, and each nano-sheet molybdenite is formed by single-layer or multi-layer MoS 2 Forming; fe and Ni bimetal alloy particles are distributed between the surface of the two-dimensional sheet structure and the adjacent two-dimensional sheet structure, and a nano-scale gap exists between the stacked two-dimensional sheet structures.
The invention has the advantages of
(1) The experimental and theoretical results of the invention show that the molybdenite is stripped into single-layer or multi-layer nano sheets by means of ion intercalation, and the two-dimensional nano structure material obtained by compounding the nano sheets with FeNi alloy particles can show more excellent electromagnetic wave absorption performance. Wherein, in the electrochemical reaction process, the concentration of tetrabutylammonium bromide is 8mg/mL, the stripping time is 8h, and the best effect is achieved 2 The nano material shows excellent microwave absorption performance and wider effective absorption frequency band, and is an ideal microwave absorption material.
(2) The shape of the nano material can be determined by MoS 2 The doping ratio is regulated and controlled, and then the two-dimensional multi-gap structure FeNi @ MoS is obtained 2 A nano-material. The two-dimensional multi-gap structure can generate a larger surface area, which can enhance multiple reflection and scattering of incident waves and provide more contact points for electromagnetic waves. Therefore, the invention can realize stronger reflection loss and wider effective absorption frequency band.
(3) Meanwhile, the preparation method does not need to use a highly toxic chemical reagent, has simple steps, strong controllability and low cost, and can be used for large-scale industrial production. The important result also provides a powerful theoretical basis and experimental basis for the research and development of ideal microwave absorbing materials.
(4) The invention provides a two-dimensional nanostructure FeNi @ MoS 2 The preparation method of the electromagnetic wave absorbing material does not need to use a highly toxic organic solvent, has simple steps, strong controllability and low cost, and can be used for large-scale industrial production.
Drawings
In order to illustrate more clearly the embodiments or solutions of the present invention in the prior art, reference will now be made briefly to the attached drawings, which are used in the description of the embodiments or solutions in the prior art, and in which some specific embodiments of the invention will be described in detail, by way of example and not by way of limitation, with reference to the attached drawings. The same reference numbers in the drawings identify the same or similar elements or components. Those skilled in the art will appreciate that the drawings are not necessarily to scale. In the drawings:
FIG. 1 shows FeNi and MoS prepared by the invention 2 And FeNi @ MoS 2 X-ray diffraction patterns of (a);
FIG. 2 shows a MoS of the present invention 2 SEM pictures after being peeled;
FIG. 3 shows FeNi @ MoS obtained in example 1 of the present invention 2 -SEM picture of 40;
FIG. 4 shows FeNi @ MoS obtained in example 2 of the present invention 2 SEM photograph of-70
FIG. 5 is FeNi @ MoS obtained in example 3 of the present invention 2 -SEM picture of 100;
FIG. 6 is FeNi @ MoS obtained in example 2 of the present invention 2 -TEM pictures of 70;
FIG. 7 shows FeNi @ MoS obtained in example 1 of the present invention 2 -a reflection loss map of 40;
FIG. 8 is FeNi @ MoS obtained in example 2 of the present invention 2 -a reflection loss map of 70;
FIG. 9 shows FeNi @ MoS obtained in example 3 of the present invention 2 -a reflection loss map of 100.
Detailed Description
In order to make the objects, technical solutions and advantages of the present application more apparent, the present application is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the present application and are not intended to limit the present application. In the present invention, unless otherwise specified, all the raw materials and equipments used are commercially available or commonly used in the art, and the methods in the examples are conventional in the art unless otherwise specified.
FeNi @ MoS obtained by preparation method of invention 2 The wave-absorbing material presents a two-dimensional multi-gap structure, and the shape of the nano material can pass through MoS 2 And regulating and controlling the doping ratio. FeNi @ MoS 2 The preparation process comprises the following steps: firstly, a proper amount of tetrabutylammonium bromide is weighed and dissolved in acetonitrile solution, and ultrasonic treatment is carried out to prepare 8mg/ml solution. Pouring the prepared solution into an electrochemical cell, and stripping molybdenite into single-layer or multi-layer nanosheets; a certain amount of NiCl is added 2 ·6H 2 O and FeCl 3 ·6H 2 Adding O into deionized water, performing ultrasonic treatment until the O is completely dissolved, and adding a certain amount of NaOH and N 2 H 4 ·H 2 O (40 wt%). Putting the products obtained in the step 1 into a hydrothermal reaction kettle together for hydrothermal reaction. Under the environment of high temperature and high pressure, a large amount of products are synthesized by a hydrothermal method, and FeNi @ MoS can be collected by centrifuging and drying the products 2 And (3) obtaining the product.
The invention FeNi @ MoS 2 The preparation method of the wave-absorbing material specifically comprises the following steps:
example 1
Step 1, firstly, weighing a proper amount of tetrabutylammonium bromide, dissolving the tetrabutylammonium bromide in an acetonitrile solution, and carrying out ultrasonic treatment to prepare a solution of 8mg/ml. The prepared solution is poured into an electrochemical cell, and a platinum electrode and the flaky molybdenite are respectively connected with the anode and the cathode of the electrochemical cell. A voltage of 12V was applied to the cell and the cell was peeled off for 8 hours. After the stripping is finished, the stripped molybdenite is taken out and washed twice by deionized water and absolute ethyl alcohol respectively. Putting the cleaned molybdenite into a test tube, adding a proper amount of deionized water, putting the test tube into a refrigerator for freezing, putting the frozen molybdenite into a freeze dryer for drying and collecting.
Example 2
Step 1, firstly, weighing a proper amount of tetrabutylammonium bromide, dissolving the tetrabutylammonium bromide in an acetonitrile solution, and carrying out ultrasonic treatment to prepare a solution with the concentration of 8mg/ml. The prepared solution is poured into an electrochemical cell, and a platinum electrode and the flaky molybdenite are respectively connected with the anode and the cathode of the electrochemical cell. A voltage of 12V was applied to the cell and the cell was peeled off for 8 hours. After the stripping is finished, the stripped molybdenite is taken out and washed twice by deionized water and absolute ethyl alcohol respectively. Putting the cleaned molybdenite into a test tube, adding a proper amount of deionized water, putting the test tube into a refrigerator for freezing, putting the frozen molybdenite into a freeze dryer for drying and collecting.
Example 3
Step 1, firstly, weighing a proper amount of tetrabutylammonium bromide, dissolving the tetrabutylammonium bromide in an acetonitrile solution, and carrying out ultrasonic treatment to prepare a solution of 8mg/ml. The prepared solution is poured into an electrochemical cell, and a platinum electrode and the flaky molybdenite are respectively connected with the anode and the cathode of the electrochemical cell. A voltage of 12V was applied to the cell and the cell was peeled off for 8 hours. After the stripping is finished, the stripped molybdenite is taken out and washed twice by deionized water and absolute ethyl alcohol respectively. Putting the cleaned molybdenite into a test tube, adding a proper amount of deionized water, putting the test tube into a refrigerator for freezing, putting the frozen molybdenite into a freeze dryer for drying and collecting.
FIG. 1 shows FeNi, moS 2 And FeNi @ MoS 2 XRD pattern of (a). The standard pattern corresponding to all diffraction peaks is as follows: feNi (JCPDS 47-1417) and MoS 2 (JCPDS 37-1492). From the XRD pattern of fig. 1, diffraction peaks at 2 θ =43.920 °, 50.140 °, and 75.317 ° correspond to (111), (200), and (220) of FeNi. Diffraction peaks at 2 θ =14.378 °, 29.026 °, 44.151 °, 60.144 °, and 77.570 ° correspond to MoS 2 (002), (004), (006), (008), and (0010). In composite material FeNi @ MoS 2 FeNi and MoS appeared 2 The main diffraction peak. The diffraction peak in FIG. 1 is sharp and high in intensity, indicating FeNi @ MoS 2 Has good crystallinity. XRD pattern shows that FeNi @ MoS is successfully synthesized 2 A composite material.
FIGS. 2,3,4,5 are MoS, respectively 2 、FeNi@MoS 2 -40、FeNi@MoS 2 -70 and FeNi @ MoS 2 SEM photograph of-100, as can be seen in FIG. 2, moS after exfoliation 2 Is a two-dimensional sheet structure, as can be seen in FIGS. 3,4 and 5, with MoS 2 The more the amount added, the more FeNi @ MoS is obtained 2 Composite sheet structures are becoming more and more apparent.
FIG. 6 is FeNi @ MoS 2 From fig. 6, it can be seen that the FeNi alloy particles coat MoS 2 Some FeNi alloy particles of the nano-sheets are agglomerated.
FIG. 7 shows FeNi @ MoS 2 Reflection loss plot of-40, from FIG. 7 it can be seen that FeNi @ MoS 2 40 shows good microwave absorption performance, the maximum reflection loss can reach-62.50 dB when the matching thickness is 2.47mm and the frequency is 11.96 GHz; at a thickness of 2.8mm, the optimum effective bandwidth is 5.24GHz.
FIG. 8 shows FeNi @ MoS 2 Reflection loss map of-70, feNi @ MoS can be seen from FIG. 8 2 -70 shows excellent microwave absorption properties, matching thickness of 3.18mm, frequency of 6.24GHz,the maximum reflection loss can reach-67.81 dB; at a thickness of 1.68mm, the optimum effective bandwidth is 5.88GHz.
FIG. 9 shows FeNi @ MoS 2 Reflection loss map of-100, feNi @ MoS can be seen from FIG. 9 2 100 shows general microwave absorption performance, the maximum reflection loss can reach-11.50 dB when the matching thickness is 1.90mm and the frequency is 9.60 GHz; at a thickness of 2.08mm, the optimum effective bandwidth is 1.32GHz.
The invention is FeNi @ MoS 2 The electromagnetic wave absorbing material is MoS obtained by electrochemically stripping molybdenite 2 The nano sheet is compounded with FeNi alloy particles to obtain FeNi @ MoS 2 A composite material. FeNi @ MoS 2 In the composite electromagnetic wave absorbing material, the FeNi alloy improves the magnetic permeability of the composite material, so that the impedance matching is further optimized. Therefore, the invention can still achieve stronger reflection loss and wider effective absorption frequency band under the condition of lower thickness.
The invention is FeNi @ MoS 2 The wave absorbing performance of the composite material mainly comes from MoS 2 The interface with the alloy particles polarizes, scatters and magnetically loses, both of which cause the incident electromagnetic wave to be dissipated. The strong electrical conductivity properties ensure a relatively high dielectric constant of the material at low thicknesses. The presence of multiple loss mechanisms ensures strong absorption of the incident electromagnetic wave.
The above description is only a part of the embodiments of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Claims (8)
1. Two-dimensional FeNi @ MoS 2 The preparation method of the nano-structure electromagnetic wave absorption material is characterized by comprising the following steps:
step 1, stripping molybdenite by adopting an electrochemical method to obtain a single-layer or multi-layer nanosheet:
pouring acetonitrile solution of tetrabutylammonium bromide into an electrochemical cell, wherein a platinum electrode and sheet molybdenite are respectively connected with a positive electrode and a negative electrode of the electrochemical cell; applying voltage to the electrochemical cell to carry out electrochemical reaction to obtain stripped molybdenite;
taking out the stripped molybdenite from the electrochemical cell, and cleaning;
adding deionized water into the washed molybdenite for freezing treatment, and then drying the molybdenite by a freeze dryer to obtain nano flaky molybdenite;
step 2, preparation of FeNi @ MoS 2 :
Preparation of NiCl 2 And FeCl 3 Aqueous solution, and the MoS 2 Dissolved in the NiCl 2 And FeCl 3 Obtaining solution A in the aqueous solution, wherein the NiCl is 2 And FeCl 3 In the aqueous solution, the mass concentration of the Ni element and the Fe element is the same;
mixing aqueous NaOH solution and N 2 H 4 Sequentially adding the aqueous solution into the solution A to obtain a solution B;
putting the nano flaky molybdenite obtained in the step 1 and the solution B into a hydrothermal reaction kettle for hydrothermal reaction; centrifuging and drying the product after the reaction is finished to obtain FeNi @ MoS 2 。
2. The two-dimensional FeNi @ MoS of claim 1 2 A method for preparing a nano-structure electromagnetic wave absorbing material is characterized in that,
in the step 1, the concentration of the acetonitrile solution of tetrabutylammonium bromide is 8mg/ml.
3. A two dimensional FeNi @ MoS as claimed in claim 2 2 A method for preparing a nano-structure electromagnetic wave absorption material is characterized in that,
in the step 2, the preparation method of the solution A comprises the following steps: mixing a solution of mmolNiCl 2 ·6H 2 O and l mmol FeCl 3 ·6H 2 Dissolving O in 40ml deionized water, adding 40-100 mg MoS 2 And carrying out ultrasonic treatment to obtain a solution A.
4. The two-dimensional FeNi @ MoS of claim 3 2 Nanostructure electromagnetic wave absorptionThe preparation method of the material is characterized in that in the step 2, the preparation method of the solution B comprises the following steps: 10ml of a 5mol/L NaOH solution and 8ml of an 80wt% N 2 H 4 ·H 2 The O solution is added into the solution A in sequence.
5. The two-dimensional FeNi @ MoS of claim 1 2 A method for preparing a nano-structure electromagnetic wave absorption material is characterized in that,
in the step 1, the direct current voltage required by the electrochemical reaction is 12V;
in the step 2, the reaction conditions of the hydrothermal reaction are as follows: the reaction was carried out at 150 ℃ for 8 hours,
the drying conditions are as follows: drying at 60 deg.C for 12 hr under vacuum.
6. The two-dimensional FeNi @ MoS of claim 1 2 A method for preparing a nano-structure electromagnetic wave absorbing material is characterized in that,
in the step 1, the voltage applied to the electrochemical cell is 12V, and the electrochemical reaction is performed for 8 hours.
7. The two-dimensional FeNi @ MoS of claim 1 2 A method for preparing a nano-structure electromagnetic wave absorption material is characterized in that,
in the step 1, the preparation method of the acetonitrile solution of tetrabutylammonium bromide comprises the following steps: adding tetrabutylammonium bromide into acetonitrile and carrying out ultrasonic treatment to obtain an acetonitrile solution of the tetrabutylammonium bromide.
8. Use of the two-dimensional FeNi @ MoS of any one of claims 1 to 6 2 FeNi @ MoS prepared by preparation method of electromagnetic wave absorbing material with nano structure 2 The electromagnetic wave absorbing material with the nano structure is characterized in that:
the FeNi @ MoS 2 The nano-structure electromagnetic wave absorbing material is formed by stacking a plurality of two-dimensional sheet structures, each two-dimensional sheet structure is obtained by stripping molybdenite to obtain nano-sheet molybdeniteThe nano flaky molybdenite consists of single-layer or multi-layer MoS 2 Composition is carried out;
fe and Ni bimetal alloy particles are distributed between the surface of the two-dimensional sheet structure and the adjacent two-dimensional sheet structure, and a nano-scale gap exists between the stacked two-dimensional sheet structures.
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