CN113840528A - MOF-derived composite wave-absorbing material and preparation method and application thereof - Google Patents
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Abstract
The invention provides a preparation method of a composite wave-absorbing material derived from MOF. The preparation method is simple in preparation process and low in cost, large-scale mass production can be realized, and the prepared wave-absorbing material has good impedance matching, wide effective absorption bandwidth and strong reflection loss value. According to the invention, MOFs is used as a template to synthesize the ordered porous wave-absorbing material, and magnetic metal, alloy or metal oxide generated after calcination can bring excellent magnetic loss, so that impedance matching and wider effective absorption bandwidth are facilitated.
Description
Technical Field
The invention relates to the technical field of electromagnetic wave absorbing materials, in particular to a composite wave absorbing material derived from MOF (metal organic framework), and a preparation method and application thereof.
Background
Nowadays, people increasingly depend on great convenience brought by electronic products, but the great convenience brings about a plurality of electromagnetic wave interference problems. Studies have shown that the central nervous system, the reproductive system and the immune system are damaged to varying degrees in humans in a long-term environment of electromagnetic radiation. Recently, nano-magnetic metals, alloys, metal oxides, etc. have been successively synthesized. The wave-absorbing material mainly utilizes the interaction between the material and electromagnetic waves to realize the absorption of the electromagnetic waves. The 'strong, wide, light and thin' is a development target of the wave-absorbing material, and in order to achieve the target, researchers develop various composite structures, such as graphene/alloy composite materials, carbon nanotube/ferrite composite materials and the like. However, to achieve excellent wave absorbing capacity of the composite, two key scientific problems must be solved: firstly, the growth mechanism of different nano structures is known, and the construction and regulation of the nano ordered structure are realized; and secondly, the functional structure design of the material is optimized, the superposition of multiple losses of electromagnetic waves is realized, the absorption bandwidth is expanded, and the reflection loss is increased. Therefore, it is urgent to manufacture a new electromagnetic wave absorber to attenuate or even eliminate the radiation of electromagnetic waves.
Disclosure of Invention
The invention provides a preparation method of an MOF (metal organic framework) derived composite wave-absorbing material, aiming at solving the problems of complex synthesis, high density, narrow effective absorption bandwidth and the like of the composite wave-absorbing material in the prior art. The preparation method is simple in preparation process and low in cost, large-scale mass production can be realized, and the prepared wave-absorbing material has good impedance matching, wide effective absorption bandwidth and strong reflection loss value.
In order to achieve the purpose, the invention adopts the following technical scheme:
a composite absorbing material derived from MOF is prepared by the following steps:
(1) preparation of FeNi-MIL-101:
h is to be2BDC (terephthalic acid) is dissolved in DMF (N, N-dimethylformamide), stirred and added with FeCl3·6H2O and Ni (acac)2Ultrasonically mixing uniformly, transferring the obtained mixture into a stainless steel autoclave for hydrothermal reaction for 1-32 h (preferably 8h) at 110-130 ℃ (preferably 120 ℃), cooling to room temperature, performing centrifugal separation to obtain brown precipitates, washing the brown precipitates with DMF or ethanol respectively, and drying overnight to obtain FeNi-MIL-101; the described Ni (acac)2、FeCl3·6H2O and H2The mass ratio of BDC is 1: 1-3: 1 to 3 (preferably 1: 2: 2);
(2) preparing a FeNiC-X composite wave-absorbing material:
and (2) putting the FeNi-MIL-101 prepared in the step (1) into a tube furnace, and calcining for 1-4 h (preferably 2h) at the speed of 1-10 ℃/min (preferably 5 ℃/min) in a protective atmosphere (such as inert gas or nitrogen, preferably nitrogen) to 600-800 ℃ (preferably 700 ℃), so as to obtain the MOF-derived composite wave-absorbing material, namely the black FeNiC-X composite wave-absorbing material.
Further, in the step (1), the volume of DMF is expressed by H2The mass of the BDC is 0.1-0.5 mL/mg (0.1L/g).
Preferably, in step (1), said H2The time for stirring BDC dissolved in DMF is 10-60 min.
Preferably, in the step (1), the time for ultrasonic uniform mixing is 10-60 min.
Preferably, in the step (1), the number of washing is 1 to 10.
Preferably, in the step (1), the drying is performed at a temperature of 60 to 80 ℃.
The heating rate is more favorable for keeping the original microstructure when 5 ℃/min, and the wave absorbing effect is obviously improved.
Compared with the prior art, the invention has the beneficial effects that:
1. compared with the prior preparation technology of most wave-absorbing materials, the wave-absorbing material synthesized by the MOF derivation method has the advantages of light weight, large specific surface area, porous structure and various structures, and particularly, effective impedance matching, namely a proper loss tangent value can be obtained by realizing proper balance between dielectric loss and magnetic loss so as to obtain excellent electromagnetic wave attenuation capability. MOFs are an ideal sacrificial precursor for the synthesis of highly dispersed metals/metal compounds/carbon materials or composites thereof by a calcination-thermal decomposition strategy. The MOF is used as a precursor for preparing the wave-absorbing material, and 1) the preparation of a sample is simpler and more convenient; 2) the pore structure and diameter of the MOF can be adjusted; 3) the porous structure of the MOF allows other substances within the pores to enter and polymerize; 4) a large number of MOFs having different compositions and multiple topologies can be further converted into target MOF-derived materials; 5) the carbon substrate derived from the decomposition of the organic ligand can prevent the aggregation of the metal/metal compound particles or the collapse of the integrated structure during calcination; 6) The MOF derived material can retain the original form of the MOF under appropriate conditions. In addition, the ordered porous wave-absorbing material is synthesized by taking MOFs as a template, and magnetic metal, alloy or metal oxide generated after calcination can bring excellent magnetic loss, so that impedance matching and wider effective absorption bandwidth are facilitated.
2. The FeNiC-X composite wave-absorbing material prepared by the invention has a unique microstructure, and the hollow spindle structure not only greatly reduces the weight and the density, but also can cause electromagnetic waves to be reflected and scattered for multiple times so as to dissipate energy. In addition, the porous structure also reduces the dielectric constant, so that the material obtains better impedance matching to enhance the attenuation of electromagnetic waves.
3. The FeNiC-X composite wave-absorbing material prepared by the invention has excellent electromagnetic absorption performance. The reflection loss value of the FeNiC-X composite wave-absorbing material reaches-62.7 through dielectric loss derived from conductivity loss and polarization loss and high magnetic loss generated by natural resonance and exchange resonance
dB。
Drawings
FIG. 1 is an XRD pattern of the FeNiC-X composite wave-absorbing material prepared in example 1.
FIG. 2 is an SEM image of the FeNiC-X composite wave-absorbing material prepared in example 1.
FIG. 3 is a Raman diagram of the FeNiC-X composite wave-absorbing material prepared in example 1 of the present invention.
FIG. 4 is a Reflection Loss (RL) curve of the FeNiC-X composite wave-absorbing material prepared in example 1 of the present invention.
FIG. 5 is a Reflection Loss (RL) curve of the FeNiC-X composite wave-absorbing material prepared in example 2 of the present invention.
FIG. 6 is a Reflection Loss (RL) curve of the FeNiC-X composite wave-absorbing material prepared in example 3 of the present invention.
Detailed Description
To facilitate an understanding of the present invention by those skilled in the art, specific embodiments thereof are described below with reference to the accompanying drawings. It is to be understood that the following text is merely illustrative of one or more specific embodiments of the invention and does not strictly limit the scope of the invention as specifically claimed.
XRD (PANalytical X' Pert PRO) analysis was used to determine the phase and crystal structure of the wave-absorbing material. And analyzing the appearance and the microstructure of the wave-absorbing material by a TEM (JEOL JEM-2100). The graphitization degree of the wave-absorbing material is analyzed by Raman spectroscopy by using a Raman spectrometer (Raman WITec Alpha300R) system with an excitation wavelength of 532 nm. The dielectric constant and permeability of the material in the frequency range of 2-18GHz were measured using a vector network analyzer (Agilent PNA N5234A) with a test step size of 0.08 GHz. The test sample preparation procedure was as follows: firstly, 0.03g of material to be tested and 0.07g of paraffin are weighed and added into a beaker with preset 2mL of normal hexane, the paraffin is completely dissolved in the normal hexane by ultrasonic treatment for 5min, and meanwhile, the test powder is uniformly dispersed. Then the beaker was placed in a water bath at 70 ℃ and n-hexane was volatilized while stirring to obtain a uniform paraffin-coated powder. And finally, putting the powder into a die, applying certain pressure to press the powder into a circular test sample. The test specimen had an outer diameter of 7mm and an inner diameter of 3.04 mm. The reflection loss caused by the electromagnetic wave entering the wave-absorbing coating can be calculated by the following equation:
in the formula, z0Is the free space wave impedance, murIs magnetic permeability, epsilonrIs the dielectric constant, f is the frequency of the electromagnetic wave, d is the coating thickness, and c is the speed of light in vacuum.
Example 1
A preparation method of a composite absorbing material derived from MOF comprises the following steps:
(1): 166mg (1mmol) of H2The BDC powder was dissolved in 16.6mL DMF solution, the mixture was stirred on a magnetic stirrer at 1000rpm for 10min, and after stirring 270mg (1mmol) FeCl was added3·6H2O and 128mg (0.5mmol) of Ni (acac)2And (3) carrying out ultrasonic treatment on the powder for 20min, uniformly mixing, transferring the mixture into a stainless steel autoclave, and carrying out hydrothermal reaction at 120 ℃ for 12 h. Hydrothermal reactionAfter completion, it was cooled to room temperature and centrifuged to give a brown precipitate which was washed 6 times with DMF and ethanol. Finally, the brown product was dried in an oven at 70 ℃ overnight.
(2): and (2) placing the FeNi-MIL-101 prepared in the step (1) into a tube furnace, heating to 700 ℃ at a heating rate of 5 ℃/min in a nitrogen atmosphere, calcining for 2h, and obtaining the final black FeNiC-X composite wave-absorbing material after calcining.
XRD test is carried out on the FeNiC-X composite wave-absorbing material prepared in the example 1. The test results are shown in FIG. 1, and the diffraction peaks indicate that the NiFe alloy and the NiFe have been successfully synthesized2O4Ferrite. The diffraction peaks at 35.5, 44.7 and 45.6, 50.7 and 74.9 respectively point to NiFe2O4(JCPDS No.10-0325) and Fe0.64Ni0.36Alloy (JCPDS No. 47-1405).
SEM test is carried out on the FeNiC-X composite wave-absorbing material prepared in the example 1. As shown in FIG. 2, the FeNiC-X is a spindle-shaped composite material having a length of about 2.5 μm and a width of 0.5. mu.m. A number of magnetic nanoparticles are uniformly dispersed on the carbon backbone, with an average diameter of about 70 nm. In addition, the cracked sample in fig. 1 confirms that the calcined sample has a hollow structure. The special structure not only greatly reduces the weight and the density, but also can cause the electromagnetic wave to be reflected and scattered for enhancing the attenuation.
The FeNiC-X composite wave-absorbing material prepared in example 1 was subjected to Raman testing. The test results are shown in fig. 3. About 1330cm-1And-1590 cm-1The two peaks at (A) correspond to the D and G bands of carbon, respectively, and the intensity ratio of the D and G bands (I)D/IG) The degree of graphitization is disclosed. I of FeNiC-XD/IGA value of 0.78 indicates a higher degree of graphitization, providing the possibility of attenuation of electromagnetic waves.
Electromagnetic wave-absorbing performance calculation is carried out on the FeNiC-X composite wave-absorbing material prepared in the embodiment 1, and a Reflection Loss (RL) curve of the absorber under the thickness of 1.6-5.5 mm is shown in FIG. 4. The effective absorption bandwidth and the minimum Reflection Loss (RL) are generally used as parameters for evaluating the wave absorption performance of the material. When the RL value is less than-10B, 90% of the electromagnetic wave energy is absorbedAnd a frequency bandwidth of less than-10 dB is referred to as an effective absorption bandwidth. As can be seen from FIG. 4, the FeNiC-X composite wave-absorbing material shows excellent electromagnetic wave-absorbing performance, when the frequency is 17.6GHz, the RL value reaches-62.7 dB, and the effective absorption bandwidth reaches 7.5 GHz. The excellent electromagnetic wave absorption performance of the material is mainly attributed to the fact that the material has a hollow structure, strong dielectric loss and magnetic loss. First, the hollow porous structure not only significantly reduces weight and density, but also causes multiple reflections and scattering to dissipate energy. In addition, the porous structure significantly reduces the dielectric constant, resulting in better impedance matching values. Second, the presence of a large number of small-sized nanoparticles in the carbon layer can cause dipole polarization, resulting in strong dielectric losses. Finally, a large amount of NiFe and NiFe2O4The nanoparticles provide high magnetic losses from magnetic resonance. Therefore, the FeNiC-X composite wave-absorbing material has strong electromagnetic wave attenuation performance.
Example 2
A preparation method of a composite absorbing material derived from MOF comprises the following steps:
(1): 166mg (1mmol) of H2The BDC powder was dissolved in 16.6mL DMF solution, the mixture was stirred on a magnetic stirrer at 1000rpm for 10min, and after stirring 270mg (1mmol) FeCl was added3·6H2O and 128mg (0.5mmol) of Ni (acac)2And (3) carrying out ultrasonic treatment on the powder for 20min, uniformly mixing, transferring the mixture into a stainless steel autoclave, and carrying out hydrothermal reaction at 120 ℃ for 12 h. After the hydrothermal reaction, the mixture was cooled to room temperature, centrifuged to obtain a brown precipitate, and washed with DMF and ethanol 6 times. Finally, the brown product was dried in an oven at 70 ℃ overnight.
(2): and (2) placing the FeNi-MIL-101 prepared in the step (1) into a tube furnace, heating to 600 ℃ at a heating rate of 5 ℃/min in a nitrogen atmosphere, calcining for 2h, and obtaining the final black FeNiC-X composite wave-absorbing material after calcining.
Electromagnetic wave-absorbing performance calculation is carried out on the FeNiC-X composite wave-absorbing material prepared in the embodiment 2, a Reflection Loss (RL) curve of an absorber with the thickness of 1.6-5.5 mm is shown in fig. 5, and compared with the material prepared in the embodiment 1, the FeNiC-X composite wave-absorbing material prepared in the embodiment 2 has the advantages that the whole effective absorption bandwidth is increased, but the wave-absorbing performance is slightly reduced, wherein the effective absorption bandwidth of the material is 7.6GHz, and the minimum reflection loss value is-40.9 dB. The reason is that the composite material has small values of complex dielectric constant and complex magnetic permeability, so that the dielectric loss and the magnetic loss of the material are reduced, and the wave absorbing performance is reduced.
Example 3
A preparation method of a composite absorbing material derived from MOF comprises the following steps:
(1): 166mg (1mmol) of H2The BDC powder was dissolved in 16.6mL DMF solution, the mixture was stirred on a magnetic stirrer at 1000rpm for 10min, and after stirring 270mg (1mmol) FeCl was added3·6H2O and 128mg (0.5mmol) of Ni (acac)2And (3) carrying out ultrasonic treatment on the powder for 20min, uniformly mixing, transferring the mixture into a stainless steel autoclave, and carrying out hydrothermal reaction at 120 ℃ for 12 h. After the hydrothermal reaction, the mixture was cooled to room temperature, centrifuged to obtain a brown precipitate, and washed with DMF and ethanol 6 times. Finally, the brown product was dried in an oven at 70 ℃ overnight.
(2): and (2) placing the FeNi-MIL-101 prepared in the step (1) into a tube furnace, heating to 800 ℃ at a heating rate of 5 ℃/min in a nitrogen atmosphere, calcining for 2h, and obtaining the final black FeNiC-X composite wave-absorbing material after calcining.
Electromagnetic wave-absorbing performance calculation is carried out on the FeNiC-X composite wave-absorbing material prepared in the embodiment 3, a Reflection Loss (RL) curve of the absorber with the thickness of 1.6-5.5 mm is shown in fig. 6, and compared with the materials prepared in the embodiments 1 and 2, the FeNiC-X composite wave-absorbing material prepared in the embodiment 3 has greatly reduced integral wave-absorbing performance, the effective absorption bandwidth of the material is 4.6GHz, and the minimum reflection loss value is-18.6 dB. This is because when the calcination temperature is increased to 800 ℃, the electrical conductivity of the composite material is enhanced, which results in mismatching of the impedance of the material, and a large amount of electromagnetic waves are reflected, thereby reducing the wave-absorbing performance.
The embodiments of the present invention have been described in detail with reference to the examples, but the present invention is not limited thereto in any way. It will be apparent to those skilled in the art that, after learning the present disclosure, numerous modifications and substitutions can be made without departing from the principles of the invention and these equivalents are to be considered as within the scope of the invention.
Claims (10)
1. A composite absorbing material derived from MOF is characterized in that the composite absorbing material derived from MOF is prepared by the following method:
(1) preparation of FeNi-MIL-101:
h is to be2BDC is dissolved in DMF, stirred and added with FeCl3·6H2O and Ni (acac)2Ultrasonically mixing uniformly, transferring the obtained mixture into a stainless steel autoclave for hydrothermal reaction at the temperature of 110-; the described Ni (acac)2、FeCl3·6H2O and H2Mass ratio of BDC 1: 1-3: 1-3;
(2) preparing a FeNiC-X composite wave-absorbing material:
and (2) putting the FeNi-MIL-101 prepared in the step (1) into a tube furnace, heating to 600-800 ℃ at a speed of 1-10 ℃/min in a protective atmosphere, and calcining for 1-4 h to obtain the MOF-derived composite wave-absorbing material.
2. The MOF-derived composite wave absorbing material of claim 1, wherein: in the step (1), the volume of DMF is expressed as H2The BDC powder is 0.1-0.5 mL/mg in mass.
3. The MOF-derived composite wave absorbing material of claim 1, wherein: in the step (1), the hydrogen atom2The time for stirring BDC dissolved in DMF is 10-60 min.
4. The MOF-derived composite wave absorbing material of claim 1, wherein: in the step (1), the time for ultrasonic mixing is 10-60 min.
5. The MOF-derived composite wave absorbing material of claim 1, wherein: in the step (1), the washing times are 1-10 times.
6. The MOF-derived composite wave absorbing material of claim 1, wherein: in the step (1), the drying is carried out at a temperature of 60-80 ℃.
7. The MOF-derived composite wave absorbing material of claim 1, wherein: in the step (1), the temperature of the hydrothermal reaction is 120 ℃ and the time is 8 h.
8. The MOF-derived composite wave absorbing material of claim 1, wherein: in the step (1), the Ni (acac)2、FeCl3·6H2O and H2The molar ratio of BDC is 1: 2: 2.
9. the MOF-derived composite wave absorbing material of claim 1, wherein: the rate of temperature rise in step (2) is 5 ℃/min.
10. The MOF-derived composite wave absorbing material of claim 1, wherein: the temperature of the calcination in the step (2) is 700 ℃.
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| CN115537180A (en) * | 2022-09-29 | 2022-12-30 | 浙江工业大学 | Two-dimensional conductive MOF wave-absorbing material and preparation method and application thereof |
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| CN115537180A (en) * | 2022-09-29 | 2022-12-30 | 浙江工业大学 | Two-dimensional conductive MOF wave-absorbing material and preparation method and application thereof |
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