CN114390880A - MXene microsphere composite wave-absorbing material modified by thorn-shaped Ni simple substance and preparation and application thereof - Google Patents

MXene microsphere composite wave-absorbing material modified by thorn-shaped Ni simple substance and preparation and application thereof Download PDF

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CN114390880A
CN114390880A CN202111526727.XA CN202111526727A CN114390880A CN 114390880 A CN114390880 A CN 114390880A CN 202111526727 A CN202111526727 A CN 202111526727A CN 114390880 A CN114390880 A CN 114390880A
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pmma
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车仁超
文彩月
张捷
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Fudan University
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Abstract

The invention relates to an MXene microsphere composite wave-absorbing material modified by thorn-shaped Ni simple substances, and preparation and application thereof. According to the invention, polymethyl methacrylate (PMMA) is used as a spherical template, MXene is combined on the surface of PMMA through a hydrogen bond acting force, and then a spine-shaped Ni simple substance with high anisotropy grows in situ on the surface of the PMMA by a hydrothermal method to prepare the material with the sea urchin-shaped appearance. The MXene @ Ni material provided by the invention has excellent microwave absorption performance, and the strongest reflection loss value can reach-59.6 dB when the thickness is only 1.5 mm. The invention has simple synthesis process and excellent material performance, and has wide application prospect in the field of microwave absorption.

Description

MXene microsphere composite wave-absorbing material modified by thorn-shaped Ni simple substance and preparation and application thereof
Technical Field
The invention belongs to the technical field of wave-absorbing materials, and relates to an MXene microsphere composite wave-absorbing material modified by thorn-shaped Ni simple substances, and preparation and application thereof.
Background
With the rapid development of electronic devices and the internet, the amount of electromagnetic waves diffused in the air is increasing. These flooded electromagnetic waves not only interfere with the proper operation of the equipment, but also can present a potential threat to human health. To solve the increasing electromagnetic wave pollution, the development of high-efficiency microwave absorbing materials is considered to have important value. Recently, MXene, a novel two-dimensional material, has attracted much attention from researchers because of its advantages such as a large specific surface area, many reactive functional groups, and easy surface modification. However, like other two-dimensional materials such as graphene and the like, MXene seriously self-stacking inhibits the generation of an active surface thereof, and aggregation between sheet layers is not favorable for electron transport, thereby causing a decrease in wave absorption performance. In addition, the single dielectric loss mechanism of MXene can limit the improvement of the wave absorbing performance, and the important significance is given to how to effectively introduce the magnetic component so as to widen the microwave loss mechanism of the wave absorbing material.
For example, patent CN110290691A introduces magnetic cobalt ferrite between MXene layers, which improves the magnetic loss in the system, but the serious self-stacking phenomenon of MXene itself is still not solved, and it is unable to realize a strong reflection loss value at a light weight.
Disclosure of Invention
The invention aims to provide an MXene microsphere composite wave-absorbing material modified by a spiky Ni simple substance, and preparation and application thereof.
The purpose of the invention can be realized by the following technical scheme:
one of the technical schemes of the invention provides a preparation method of an MXene microsphere composite wave-absorbing material modified by thorn-shaped Ni simple substance, which comprises the following steps:
(1) weighing polymethyl methacrylate, dispersing the polymethyl methacrylate in deionized water, dropwise adding MXene suspension under the stirring condition, centrifuging, washing and drying the obtained mixed solution to obtain PMMA @ MXene powder;
(2) dispersing PMMA @ MXene powder into deionized water again, adding nickel chloride hexahydrate, stirring, then adding a reducing agent, and continuing stirring to obtain a precursor solution;
(3) and carrying out hydrothermal reaction on the precursor solution, washing and drying the obtained reaction product to obtain the target product.
Further, in the step (1), the mass ratio of the polymethyl methacrylate to the MXene is 4: 1-10: 1.
Further, in the step (1), the ratio of the amount of the polymethyl methacrylate to the deionized water is (120-240) mg: 12 mL.
Further, in the step (2), the mass ratio of PMMA @ MXene powder to nickel chloride hexahydrate is (40-100) mg: (0.4-0.5) g.
Further, in the step (2), the reducing agent is hydrazine hydrate. Furthermore, in the step (2), the concentration of hydrazine hydrate is 80-90 wt%, and the ratio of the hydrazine hydrate to the addition amount of PMMA @ MXene powder is (6-8) mL: (40-100) mg.
Further, in the step (2), the addition amount of PMMA @ MXene powder and deionized water is (40-100) mg: 60 mL.
Further, in the step (3), the temperature of the hydrothermal reaction is 140-160 ℃, and the time is 10-15 h.
The second technical scheme of the invention provides an MXene microsphere composite wave-absorbing material modified by thorn-shaped Ni simple substance, which is prepared by the preparation method. Polymethyl methacrylate (PMMA) is adopted as a spherical template, a few layers of MXene materials obtained after etching and stripping are combined on the surface of the PMMA through hydrogen bond acting force, a spiny Ni simple substance grown in situ on the surface of the MXene materials through a hydrothermal reaction chemical synthesis method has high anisotropy, and the ternary material with the double-layer core-shell structure is sea urchin-shaped.
The third technical scheme of the invention is the application of the thorn-shaped Ni simple substance modified MXene microsphere composite wave-absorbing material in the microwave absorption field.
According to the invention, researches show that the two-dimensional material MXene is easy to self-accumulate, so that a large amount of active functional groups on the surface are lost, and the possibility of surface modification is reduced. Meanwhile, MXene is a dielectric material, and its own generated dielectric loss is one of microwave energy attenuation mechanisms. However, in order to realize better wave-absorbing performance, the introduction of a magnetic component into the system so as to enhance the magnetic loss is an effective solution. Based on the above problems, the self-stacking phenomenon can be alleviated to some extent by constructing MXene into microspheres having a three-dimensional structure by using a spherical template method. Meanwhile, the exposure of a large number of active functional groups on the surface of the MXene microspheres is successfully realized, and the introduction of the magnetic simple substance Ni with high anisotropy by utilizing a hydrothermal reaction method through electrostatic interaction force is facilitated. The formed thorn-shaped Ni forms a strong magnetic coupling effect, generates stronger magnetic loss and plays an important role in improving the integral wave absorption performance of the material.
The invention successfully realizes the combination between the PMMA template and MXene by adopting a simple method, the spherical shape of the MXene microspheres can still be maintained in the process of generating the spiny Ni simple substance in situ in the subsequent hydrothermal reaction, and the spiny Ni simple substance forms high anisotropic arrangement. The Ti modified by the thorn-shaped Ni simple substance3C2TxThe MXene microsphere composite wave-absorbing material shows excellent comprehensive performance in the field of microwave absorption.
Compared with the prior art, the invention has the following advantages:
(1) the MXene microsphere material modified by the magnetic simple substance Ni provided by the invention is applied to the field of microwave absorption, has the advantages of high reflection loss and thin thickness, and has the strongest reflection loss value of-59.6 dB and the thickness of only 1.5 mm.
(2) The synthesis method is novel, and successfully synthesizes the sea urchin-shaped magnetic simple substance Ni-coated MXene microspheres.
Drawings
FIG. 1 is a schematic diagram of synthesis of a thorn-shaped Ni simple substance modified MXene microsphere composite wave-absorbing material PMMA @ MXene @ Ni.
FIG. 2 is a scanning electron micrograph of each sample: (a) PMMA @ MXene @ Ni material; (b) PMMA @ MXene material; (c) MXene/Ni material.
FIG. 3 is a transmission electron micrograph of each sample: (a) PMMA @ MXene @ Ni material; (b) PMMA @ MXene material; (c) MXene/Ni material.
FIG. 4 is an X-ray diffraction spectrum of the thorn-shaped Ni simple substance modified MXene microsphere composite wave-absorbing material PMMA @ MXene @ Ni.
FIG. 5 shows the relative complex dielectric constants of the respective samples: (a) real part of relative complex permittivity; (b) relative complex dielectric constant imaginary part; (c) real part of relative complex permeability and (d) imaginary part of relative complex permeability.
Fig. 6 shows the values of the reflection loss for different thicknesses of the samples: (a) PMMA @ MXene @ Ni material; (b) PMMA @ MXene material; (c) MXene/Ni material.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
MXene suspensions (Ti) used in the examples below3C2TxMXene suspensions) were prepared in the literature (Carbon 2021,175, 509-518).
Otherwise, unless otherwise specified, all the materials or processing techniques are conventional commercial products or conventional processing techniques in the art.
Example 1
Referring to the flow shown in fig. 1, the preparation of the thorn-shaped Ni simple substance modified MXene microsphere composite wave-absorbing material PMMA @ MXene @ Ni:
first, 120mg of PMMA powder is weighed and dispersed in 12mL of deionized water, and the PMMA powder is uniformly dispersed by ultrasonic. Then 10mL of MXene solution (3mg/mL) was slowly added dropwise and mixed well under magnetic stirring. And carrying out centrifugal separation on the obtained solution containing the flocculent precipitate, washing the lower-layer precipitate with deionized water for 1-2 times, and drying the finally obtained precipitate by using a freeze dryer.
40mg of PMMA @ MXene powder prepared was weighed, dispersed in 60mL of deionized water, and mixed well under magnetic stirring. 0.4754g of nickel chloride hexahydrate are then added and stirring is continued for 30 minutes. Then 8mL of hydrazine hydrate reducing agent (85% by mass) is slowly added dropwise, and the reaction is continued for 30 minutes under magnetic stirring. And finally, transferring the obtained solution into a high-pressure reaction kettle, and continuously reacting for 15 hours at the temperature of 160 ℃. And after the reaction is finished, washing and drying the obtained precipitate to obtain the target product PMMA @ MXene @ Ni material.
Comparative example 1
Preparing a non-thorn-shaped Ni simple substance modified PMMA @ MXene microsphere material:
compared with example 1, the method is mostly the same except that the hydrothermal reaction condition by adding nickel chloride hexahydrate is lacked.
Comparative example 2
Preparation of MXene/Ni material without spherical template PMMA support:
compared to example 1, is largely identical except for the absence of the condition for adding PMMA powder.
The micro-morphology of the materials in the above examples was characterized using a scanning electron microscope (SEM, Hitachi SEM S-4800), sample preparation method: and ultrasonically dispersing the powder sample in ethanol, and then dripping the powder sample on a conductive silicon wafer to be dried for testing. A series of composite material microstructures can be characterized by a transmission electron microscope (TEM, JEOL JEM-2100F), and a sample preparation method comprises the following steps: and ultrasonically dispersing the powder sample in ethanol, and then dripping the powder sample on a carbon-supported copper net for drying to test. The X-ray diffraction spectra were measured on a bruker d8 Advance instrument. The complex relative permittivity and permeability in the range of 2.0-18.0GHz was tested using a vector network analyzer model N5230C.
FIG. 2 is a scanning electron microscope picture of MXene microspheres with different components, wherein a is the micro-morphology of PMMA @ MXene @ Ni, b is the micro-morphology of PMMA @ MXene, and c is the micro-morphology of MXene/Ni materials. It can be observed that MXene is coated on the surface of the spherical template PMMA, the sphere still maintains a relatively complete spherical shape, and the size distribution of the microspheres is uniform. After a layer of compact magnetic thorn-shaped Ni grows on the surface of the sea urchin microsphere through hydrothermal reaction, the spine-shaped Ni layer with high anisotropy surrounds the surface of the microsphere, and the final sea urchin microsphere is formed. After the supporting function of the spherical template PMMA is lost, Ni spikes directly grown on the surface of the lamellar MXene wholly present a disordered distribution and arrangement (figure 2c), and a serious self-stacking phenomenon is generated among MXene layers.
FIG. 3 is a transmission electron microscope image of PMMA @ MXene @ Ni, PMMA @ MXene and MXene/Ni materials obtained in the above example 1, comparative example 1 and comparative example 2. From fig. 3b it is evident that the surface-coated layer MXene has approximately up to a dozen or so layers. The figure a shows that the morphology of the sea urchin microsphere with the Ni spikes grown on the surface is consistent with that of an SEM picture, and the successful regulation and control of the morphology of the material are proved. The figure c shows the morphology of MXene/Ni material synthesized after spherical template PMMA is lost, and thorn-shaped Ni attracts each other due to magnetic interaction, so that obvious aggregation is caused, and good dispersion of magnetic components cannot be realized.
FIG. 4 is an X-ray diffraction (XRD) analysis of PMMA @ MXene @ Ni, PMMA @ MXene, and MXene/Ni materials prepared in example 1, comparative example 1, and comparative example 2. In the figure, example 1 detects (002), (004) and (110) crystal planes corresponding to MXene components and (111), (200) and (220) crystal planes corresponding to Ni components (JCPDS No.87-0712), and confirms the component integrity of the synthesized structure. The doublets appearing at 7.1 ° and 61 ° in comparative example 1 correspond to the (002) and (110) crystal planes in MXene. In addition, a relatively blunt broad peak appears around 15 °, which corresponds to the less crystalline PMMA component. The peaks appearing in comparative example 2 were substantially in agreement with those of example 1, confirming the presence of both MXene and Ni components in the structure.
FIG. 5 is a graph showing real and imaginary parts of complex dielectric constant (ε ', ε ") and complex permeability (μ', μ") of PMMA @ MXene @ Ni, PMMA @ MXene, and MXene/Ni materials obtained in example 1, comparative example 1, and comparative example 2, which shows the mechanism of their excellent wave absorption properties. The wave absorbing performance of the composite material mainly derives from polarization loss capacity and magnetic loss. From fig. 5a, b it can be seen that the PMMA @ MXene material of comparative example 1 has the highest values of e' and e ", indicating the strongest dielectric polarization capability. When the magnetic component is introduced into the system, the dielectric index of the material is obviously reduced, the epsilon 'value of the PMMA @ MXene @ Ni material in example 1 is reduced from 15.5 to 8.6, and the epsilon' value is changed from 2.6 to 3.5. In addition, it can be seen from the figure that the material of example 1 has stronger dielectric polarization capability than the material of comparative example 2, which is attributed to the structure of spherical morphology, and a large number of magnetic-dielectric interfaces contained in the structure induce stronger interface polarization behavior. Fig. 5c, d show the real and imaginary values (μ', μ ″) of the complex permeability of example 1, comparative example 1, and comparative example 2. Since the PMMA @ MXene material of comparative example 1 does not contain a magnetic component, it can be found that the values of μ' and μ ″ thereof approach to 1 and 0, indicating that comparative example 1 has almost no magnetic loss behavior. In contrast, the PMMA @ MXene @ Ni material of example 1 had higher values of μ 'and μ "with the μ' value decreasing from 1.3 to 1.0 and the μ" value varying from 0.25 to 0.02. Meanwhile, the MXene/Ni material of the comparative example 2 is compared with that of the example 1 and the comparative example 2, and the magnetic permeability value of the MXene/Ni material of the comparative example 2 is low due to the fact that the magnetic simple substance Ni in the structure has low density and is not uniformly distributed, and the locally agglomerated particles block the reflection of magnetic lines of force of the material, so that the MXene/Ni material shows weak magnetism.
FIG. 6 shows the values of the reflection loss at frequencies of 2.0 to 18.0GHz for the PMMA @ MXene @ Ni, PMMA @ MXene and MXene/Ni materials prepared in the above examples 1 to 2 comparative examples at thicknesses of 1.0 to 5.0 mm. It can be seen that the PMMA @ MXene @ Ni material of example 1 exhibits the best wave absorbing performance, the reflection loss value of-59.6 dB is realized only when the thickness is 1.5mm, and the effective absorption bandwidth can reach 4.48 GHz. In contrast, the PMMA @ MXene material of comparative example 1 had a maximum reflection loss value of-23.8 dB, corresponding to a thickness of 2.5 mm. The MXene/Ni material of comparative example 2 had a maximum reflection loss value of-34.1 dB, corresponding to a thickness of 2.7 mm. It can be seen that the material of example 1 has the most excellent wave-absorbing property.
In general, the Ti modified by spiked Ni simple substance of the invention3C2TxThe MXene microsphere composite wave-absorbing material shows excellent electromagnetic wave loss capability in the frequency range of 2.0-18.0 GHz. According to the invention, polymethyl methacrylate (PMMA) is used as a spherical template, MXene is combined on the surface of PMMA through a hydrogen bond acting force, and then a spine-shaped Ni simple substance with high anisotropy grows in situ on the surface of the PMMA by a hydrothermal method to prepare the sea urchin-shaped material. The invention has simple synthesis process and excellent material performance, and has wide application prospect in the field of microwave absorption.
Example 2:
compared with example 1, most of them are the same except that the amount of MXene solution is adjusted so that the mass ratio of polymethyl methacrylate to MXene is 4: 1.
Example 3:
compared with example 1, most of them were the same except that the amount of MXene solution was adjusted so that the mass ratio of polymethyl methacrylate to MXene was 10: 1.
Example 4:
compared to example 1, the mass of PMMA @ MXene powder was adjusted to 100 mg.
Example 5:
compared to example 1, the mass was largely the same except that the mass of PMMA @ MXene powder was adjusted to 60 mg.
Example 6:
most of them were the same as in example 1, except that the amount of hydrazine hydrate added was adjusted to 6 mL.
Example 7:
compared with example 1, the most part is the same except that the amount of hydrazine hydrate added is adjusted to 7 mL.
Example 8:
compared with example 1, the hydrothermal reaction was conducted at 140 ℃ for 10 hours.
Example 9:
compared with example 1, the hydrothermal reaction was conducted at 150 ℃ for 12 hours.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.

Claims (10)

1. A preparation method of an MXene microsphere composite wave-absorbing material modified by a thorn-shaped Ni simple substance is characterized by comprising the following steps:
(1) weighing polymethyl methacrylate, dispersing the polymethyl methacrylate in deionized water, dropwise adding MXene suspension under the stirring condition, centrifuging, washing and drying the obtained mixed solution to obtain PMMA @ MXene powder;
(2) dispersing PMMA @ MXene powder into deionized water again, adding nickel chloride hexahydrate, stirring, then adding a reducing agent, and continuing stirring to obtain a precursor solution;
(3) and carrying out hydrothermal reaction on the precursor solution, washing and drying the obtained reaction product to obtain the target product.
2. The preparation method of the MXene microsphere composite wave-absorbing material modified by the thorn-shaped Ni simple substance according to claim 1, wherein in the step (1), the mass ratio of the polymethyl methacrylate to the MXene is 4: 1-10: 1.
3. The method for preparing MXene microsphere composite wave-absorbing material modified by spiked Ni element as claimed in claim 1, wherein in step (1), the ratio of the amount of polymethyl methacrylate and deionized water is (120-240) mg: 12 mL.
4. The preparation method of the MXene microsphere composite wave-absorbing material modified by the thorn-shaped Ni simple substance according to claim 1, wherein in the step (2), the mass ratio of PMMA @ MXene powder to nickel chloride hexahydrate is (40-100) mg: (0.4-0.5) g.
5. The method for preparing the MXene microsphere composite wave-absorbing material modified by the spiky Ni simple substance according to claim 1, wherein in the step (2), the reducing agent is hydrazine hydrate.
6. The preparation method of the MXene microsphere composite wave-absorbing material modified by the spiky Ni simple substance according to claim 5, wherein in the step (2), the concentration of hydrazine hydrate is 80-90 wt%, and the addition amount ratio of the hydrazine hydrate to the PMMA @ MXene powder is (6-8) mL: (40-100) mg.
7. The preparation method of the MXene microsphere composite wave-absorbing material modified by the thorn-shaped Ni simple substance according to claim 1, wherein in the step (2), the addition amount of PMMA @ MXene powder and deionized water is (40-100) mg: 60 mL.
8. The preparation method of the MXene microsphere composite wave-absorbing material modified by the spiky Ni simple substance according to claim 1, wherein in the step (3), the temperature of the hydrothermal reaction is 140-160 ℃ and the time is 10-15 h.
9. An MXene microsphere composite wave-absorbing material modified by thorn-shaped Ni simple substance, which is prepared by the preparation method of any one of claims 1-8.
10. The MXene microsphere composite wave-absorbing material modified by spiky Ni element substance according to claim 9, and the application thereof in the microwave absorption field.
CN202111526727.XA 2021-12-14 2021-12-14 MXene microsphere composite wave-absorbing material modified by thorn-shaped Ni simple substance and preparation and application thereof Pending CN114390880A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115500066A (en) * 2022-08-18 2022-12-20 中国地质大学（武汉） Microsphere-based heat storage and wave absorption integrated material of sea urchin-shaped core-shell minerals and preparation method and application thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115500066A (en) * 2022-08-18 2022-12-20 中国地质大学（武汉） Microsphere-based heat storage and wave absorption integrated material of sea urchin-shaped core-shell minerals and preparation method and application thereof
CN115500066B (en) * 2022-08-18 2024-05-10 中国地质大学（武汉） Sea urchin-shaped core-shell mineral microsphere-based heat-storage wave-absorbing integrated material and preparation method and application thereof

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