CN110669228B - CoFe/C composite material and preparation method and application thereof - Google Patents
CoFe/C composite material and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a nest-shaped CoxFe4‑xThe preparation method of/C composite material and its application are characterized by that it uses cobalt acetate tetrahydrate and iron chloride hexahydrate as metal source, uses 2, 5-dihydroxy terephthalic acid as organic ligand, and adds a certain quantity of Fe3+Obtaining a nest-shaped structure, taking ultrapure water as a reaction solvent, refluxing for a certain time under an oil bath, centrifuging, washing and drying the obtained black product, and finally performing heat treatment in argon to obtain nest-shaped CoxFe4‑xa/C composite material. CoxFe obtained by the method4‑xthe/C composite material is nest-shaped, and the unique structure and the multiple components of the composite material enable the composite material to be used as a wave-absorbing material to show excellent electromagnetic wave-absorbing performance.
Description
Technical Field
The invention belongs to the field of electromagnetic wave absorption, and particularly relates to a CoFe/C composite material and a preparation method and application thereof.
Background
With the development of radio, television and microwave technologies, electromagnetic pollution caused by excessive electromagnetic radiation has become another major pollution affecting people's health and information security. In general, attenuation and shielding of electromagnetic waves is certainly a good choice in order to reduce the influence of electromagnetic waves. In particular, electromagnetic waves can be more effectively attenuated by converting the electromagnetic waves into heat energy or dissipating the heat energy through interference, and therefore, designing and manufacturing high-performance wave-absorbing materials are the direction of research. In many previous researches, the multi-component wave absorbing material is found to have better wave absorbing performance than a single wave absorbing material, and the porous wave absorbing material can also improve the wave absorbing performance. Therefore, as the wave-absorbing material develops to a design concept of good impedance matching and light weight, more and more researchers focus on multi-component and micro-morphology design. The prior art has the following problems: firstly, from the aspect of the method, the conditions are harsh, and most of the solvent is organic solvent; secondly, the metal particles cannot be uniformly dispersed in the carbon layer, and the smaller volume cavity limits the entering of electromagnetic waves, so that the loss of the electromagnetic waves is reduced; finally, the absorption band of pure metal is relatively narrow, which is related to the eddy current formed by the conductive network structure.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides CoxFe4-x/C composite material, preparation method and application thereof, and prepared CoxFe4-xthe/C composite material has excellent wave-absorbing performance.
The invention is realized by the following technical scheme:
a preparation method of a CoFe/C composite material comprises the following steps:
step 3, carrying out heat treatment on the obtained precipitate at 700-900 ℃ in a protective atmosphere to obtain CoxFe4-xa/C composite material.
Preferably, in step 2, after mixing mixture B and mixture A, 2, 5-dihydroxyterephthalic acid and Co (CH)3COO)2·4H2The molar ratio of O is: 2: (3.4-2.6).
Preferably, in the step 2, the reaction is carried out for 1-3 h at 90-110 ℃.
Preferably, in step 2, the drying is freeze-drying.
Preferably, in step 3, the protective gas is argon.
Preferably, in the step 3, the heat treatment temperature is 700-900 ℃ and the time is 2-5 h.
Preferably, in step 3, the temperature rise rate is 2-5 ℃/min.
The CoFe/C composite material is prepared by the preparation method.
The CoFe/C composite material is applied to the aspect of electromagnetic wave absorption.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention adjusts the addition amount of iron ions to ensure that Co is added2+And Fe3The complex is in coordination relation with the ligand, thereby influencing the micro-morphology of the synthesized product and successfully preparing the nest-like Cox/Fe4-xThe MOF-74 bimetal organic framework material adopts water as a solvent, and has the advantages of simple method and high yield. Then the synthesized Co is treated under the protection of argonx/Fe4-xMOF-74 was heat-treated to finally obtain nest-like CoxFe4-xa/C composite material. Of course, when the cobalt-iron ratio exceeds the range, a nest-like structure cannot be formed, and other morphological products can be formed, for example, when the cobalt-iron ratio is 2: 2, the product was short rod-like. The invention has the following improvements: firstly, water is used as a reaction solvent, so that the method is non-toxic and harmless, and is simple and high in yield; secondly, a bird nest-shaped appearance with a cavity with a larger volume is obtained, which is beneficial to the entering of electromagnetic waves; finally, the alloy and carbon are compounded, because the alloy has the characteristics of two components, compared with single-component magnetic metal, the magnetic metal alloy has stronger electron transfer and spin polarization coupling characteristics, has certain advantages in the field of electromagnetic wave absorption, and the carbon material has certain dielectric loss. Moreover, the nest-like Co prepared by the inventionxFe4-xThe material of the/C composite material has uniform appearance and good crystallinity, the electromagnetic wave absorption performance of a sample is tested by a vector network analyzer, and Co can be found to be only 10% in mass fractionxFe4-xthe/C composite material has good wave-absorbing performance,when the frequency is 12.7GHz, the maximum reflection loss reaches-61.8 dB, the effective bandwidth is 8.68GHz, and the matching thickness is 2.8 mm.
Drawings
FIG. 1 is a drawing of (a) bimetallic Co prepared in example 63/Fe1-MOF-74 framework material and (b) Co after heat treatment3Fe1SEM pictures of the/C composite.
Fig. 2 shows the cobalt-iron ratio 2 of comparative example 1: 2 time bimetal Co2/Fe2-MOF-74 framework material and Co after heat treatment2Fe2SEM pictures of the/C composite.
FIG. 3 shows Co after heat treatment in example 63Fe1XRD pattern of the/C composite material.
FIG. 4 shows Co prepared in example 63Fe1Co with a/C composite filling of 10 wt%3Fe1Reflection loss value of the/C composite material.
FIG. 5 shows Co prepared in comparative example 12Fe2Co with a/C composite filling of 10 wt%2Fe2Reflection loss value of the/C composite material.
FIG. 6 shows Co prepared in example 63Fe1Cole-Cole circle diagram and C0 diagram of/C composite material.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
The invention relates to CoxFe4-xThe preparation method of the/C composite material comprises the following steps:
(1) weighing x mmol Co (CH)3COO)2·4H2O and (4-x) mmol FeCl3·6H2Dissolving O (x is 3.4-2.6) in 50mL of ultrapure water sufficiently after ultrasonic dispersion for half an hour to obtain a mixed solution A;
(2) weighing 2mmol of 2, 5-dihydroxy terephthalic acid, dissolving in a single-neck flask filled with 50mL of ultrapure water, and performing ultrasonic dispersion for half an hour to fully dissolve to obtain a mixed solution B;
(3) transferring the mixed solution B into an oil bath pan, slowly adding the mixed solution A into the mixed solution B, reacting for 0.5-3 h at 90-110 ℃, washing with ultrapure water and absolute ethyl alcohol, and freeze-drying for 24h to obtain a black precipitate.
(4) And placing the obtained black precipitate in a corundum porcelain boat, and carrying out heat treatment under the argon atmosphere, wherein the heat treatment temperature is 700-900 ℃, the heating rate is 2-5 ℃/min, and the heat preservation time is 2-5 h.
Example 1
The invention relates to CoxFe4-xThe preparation method of the/C composite material comprises the following steps:
(1) 3.4mmol of Co (CH) are weighed3COO)2·4H2O and 0.6mmol FeCl3·6H2Dissolving O in 50mL of ultrapure water fully after ultrasonic dispersion for half an hour to obtain a mixed solution A;
(2) weighing 2mmol of 2, 5-dihydroxy terephthalic acid, dissolving in a single-neck flask filled with 50mL of ultrapure water, and performing ultrasonic dispersion for half an hour to fully dissolve to obtain a mixed solution B;
(3) transferring the mixed solution B into an oil bath pan, slowly adding the solution A into the solution B, reacting at 90 ℃ for 1h, washing with ultrapure water and absolute ethyl alcohol, and freeze-drying for 24h to obtain a black precipitate (bimetal Co)3.4/Fe0.6-MOF-74 metal organic framework material);
(4) placing the obtained black precipitate in a corundum porcelain boat, and carrying out heat treatment under argon atmosphere at the heat treatment temperature of 700 ℃, the heating rate of 2 ℃/min and the heat preservation time of 2h to obtain Co3.4Fe0.6a/C composite material.
Example 2
The invention relates to CoxFe4-xThe preparation method of the/C composite material comprises the following steps: (1) 3.4mmol of Co (CH) are weighed3COO)2·4H2O and 0.6mmol FeCl3·6H2Dispersing O in 50mL of ultrapure water by ultrasonic for half an hour, and fully dissolving to obtain a mixed solution A;
(2) weighing 2mmol of 2, 5-dihydroxy terephthalic acid, dissolving in a single-neck flask filled with 50mL of ultrapure water, and performing ultrasonic dispersion for half an hour to fully dissolve to obtain a mixed solution B;
(3) transferring the mixed solution B into an oil bath pan, slowly adding the solution A into the solution B, reacting at 110 ℃ for 3h, washing with ultrapure water and absolute ethyl alcohol, and freeze-drying for 24h to obtain black precipitate (bimetal Co)3.4/Fe0.6-MOF-74 metal organic framework material);
(4) placing the obtained black precipitate in a corundum porcelain boat, and carrying out heat treatment under argon atmosphere at the heat treatment temperature of 900 ℃, the heating rate of 5 ℃/min and the heat preservation time of 5h to obtain Co3.4Fe0.6a/C composite material.
Example 3
The invention relates to CoxFe4-xThe preparation method of the/C composite material comprises the following steps:
(1) 3.4mmol of Co (CH) are weighed3COO)2·4H2O and 0.6mmol FeCl3·6H2Dissolving O in 50mL of ultrapure water fully after ultrasonic dispersion for half an hour to obtain a mixed solution A;
(2) weighing 2mmol of 2, 5-dihydroxy terephthalic acid, dissolving in a single-neck flask filled with 50mL of ultrapure water, and performing ultrasonic dispersion for half an hour to fully dissolve to obtain a mixed solution B;
(3) transferring the mixed solution B into an oil bath pan, slowly adding the solution A into the solution B, reacting at 100 ℃ for 2h, washing with ultrapure water and absolute ethyl alcohol, and freeze-drying for 24h to obtain black precipitate (bimetal Co)3.4/Fe0.6-MOF-74 metal organic framework material);
(4) placing the obtained black precipitate in a corundum porcelain boat, and carrying out heat treatment under the argon atmosphere, wherein the heat treatment temperature is 800 ℃, the heating rate is 3 ℃/min, and the heat preservation time is 3h to obtain Co3.4Fe0.6a/C composite material.
Example 4
CoxFe4-xThe preparation method of the/C composite material comprises the following steps:
(1) 3mmol of Co (CH) are weighed3COO)2·4H2O and 1mmol FeCl3·6H2Dissolving O in 50mL of ultrapure water fully after ultrasonic dispersion for half an hour to obtain a mixed solution A;
(2) weighing 2mmol of 2, 5-dihydroxy terephthalic acid, dissolving in a single-neck flask filled with 50mL of ultrapure water, and performing ultrasonic dispersion for half an hour to fully dissolve to obtain a mixed solution B;
(3) transferring the mixed solution B into an oil bath pan, slowly adding the solution A into the solution B, reacting at 90 deg.C for 0.5h, washing with ultrapure water and anhydrous ethanol, and freeze-drying for 24h to obtain black precipitate (bimetal Co)3/Fe1-MOF-74 metal organic framework material);
(4) placing the obtained black precipitate in a corundum porcelain boat, and carrying out heat treatment under argon atmosphere at the heat treatment temperature of 700 ℃, the heating rate of 2 ℃/min and the heat preservation time of 2h to obtain Co3Fe1a/C composite material.
Example 5
CoxFe4-xThe preparation method of the/C composite material comprises the following steps:
(1) 3mmol of Co (CH) are weighed3COO)2·4H2O and 1mmol FeCl3·6H2Dissolving O in 50mL of ultrapure water fully after ultrasonic dispersion for half an hour to obtain a mixed solution A;
(2) weighing 2mmol of 2, 5-dihydroxy terephthalic acid, dissolving in a single-neck flask filled with 50mL of ultrapure water, and performing ultrasonic dispersion for half an hour to fully dissolve to obtain a mixed solution B;
(3) transferring the mixed solution B into an oil bath pan, slowly adding the solution A into the solution B, reacting at 110 ℃ for 3h, washing with ultrapure water and absolute ethyl alcohol, and freeze-drying for 24h to obtain black precipitate (bimetal Co)3/Fe1-MOF-74 metal organic framework material);
(4) placing the obtained black precipitate in a corundum porcelain boat, carrying out heat treatment in argon atmosphere at the heat treatment temperature of 900 ℃ and the heating rate of 5 ℃/min,keeping the temperature for 5h to obtain Co3Fe1a/C composite material.
Example 6
CoxFe4-xThe preparation method of the/C composite material comprises the following steps:
(1) 3mmol of Co (CH) are weighed3COO)2·4H2O and 1mmol FeCl3·6H2Dissolving O in 50mL of ultrapure water fully after ultrasonic dispersion for half an hour to obtain a mixed solution A;
(2) weighing 2mmol of 2, 5-dihydroxy terephthalic acid, dissolving in a single-neck flask filled with 50mL of ultrapure water, and performing ultrasonic dispersion for half an hour to fully dissolve to obtain a mixed solution B;
(3) transferring the mixed solution B into an oil bath pan, slowly adding the solution A into the solution B, reacting at 100 ℃ for 2h, washing with ultrapure water and absolute ethyl alcohol, and freeze-drying for 24h to obtain black precipitate (bimetal Co)3/Fe1-MOF-74 metal organic framework material);
(4) placing the obtained black precipitate in a corundum porcelain boat, and carrying out heat treatment under the argon atmosphere, wherein the heat treatment temperature is 800 ℃, the heating rate is 3 ℃/min, and the heat preservation time is 3h to obtain Co3Fe1a/C composite material.
Example 7
CoxFe4-xThe preparation method of the/C composite material comprises the following steps:
(1) 2.6mmol of Co (CH) are weighed3COO)2·4H2O and 1.4mmol FeCl3·6H2Dissolving O in 50mL of ultrapure water fully after ultrasonic dispersion for half an hour to obtain a mixed solution A;
(2) weighing 2mmol of 2, 5-dihydroxy terephthalic acid, dissolving in a single-neck flask filled with 50mL of ultrapure water, and performing ultrasonic dispersion for half an hour to fully dissolve to obtain a mixed solution B;
(3) transferring the mixed solution B into an oil bath pan, slowly adding the solution A into the solution B, reacting at 90 ℃ for 1h, washing with ultrapure water and absolute ethyl alcohol, and freeze-drying for 24h to obtain blackPrecipitate (bimetal Co)2.6/Fe1.4-MOF-74 metal organic framework material);
(4) placing the obtained black precipitate in a corundum porcelain boat, and carrying out heat treatment under argon atmosphere at the heat treatment temperature of 700 ℃, the heating rate of 2 ℃/min and the heat preservation time of 2h to obtain Co2.6Fe1.4a/C composite material.
Example 8
CoxFe4-xThe preparation method of the/C composite material comprises the following steps:
(1) 3mmol of Co (CH) are weighed3COO)2·4H2O and 1mmol FeCl3·6H2Dissolving O in 50mL of ultrapure water fully after ultrasonic dispersion for half an hour to obtain a mixed solution A;
(2) weighing 2mmol of 2, 5-dihydroxy terephthalic acid, dissolving in a single-neck flask filled with 50mL of ultrapure water, and performing ultrasonic dispersion for half an hour to fully dissolve to obtain a mixed solution B;
(3) transferring the mixed solution B into an oil bath pan, slowly adding the solution A into the solution B, reacting at 110 ℃ for 3h, washing with ultrapure water and absolute ethyl alcohol, and freeze-drying for 24h to obtain black precipitate (bimetal Co)3/Fe1-MOF-74 metal organic framework material);
(4) placing the obtained black precipitate in a corundum porcelain boat, and carrying out heat treatment under argon atmosphere at the heat treatment temperature of 900 ℃, the heating rate of 5 ℃/min and the heat preservation time of 5h to obtain Co3Fe1a/C composite material.
Example 9
CoxFe4-xThe preparation method of the/C composite material comprises the following steps:
(1) 3mmol of Co (CH) are weighed3COO)2·4H2O and 1mmol FeCl3·6H2Dissolving O in 50mL of ultrapure water fully after ultrasonic dispersion for half an hour to obtain a mixed solution A;
(2) weighing 2mmol of 2, 5-dihydroxy terephthalic acid, dissolving in a single-neck flask filled with 50mL of ultrapure water, and performing ultrasonic dispersion for half an hour to fully dissolve to obtain a mixed solution B;
(3) transferring the mixed solution B into an oil bath pan, slowly adding the solution A into the solution B, reacting at 100 ℃ for 2h, washing with ultrapure water and absolute ethyl alcohol, and freeze-drying for 24h to obtain black precipitate (bimetal Co)3/Fe1-MOF-74 metal organic framework material);
(4) placing the obtained black precipitate in a corundum porcelain boat, and carrying out heat treatment under the argon atmosphere, wherein the heat treatment temperature is 800 ℃, the heating rate is 3 ℃/min, and the heat preservation time is 3h to obtain Co3Fe1a/C composite material.
Comparative example 1
CoxFe4-xThe preparation method of the/C composite material comprises the following steps:
(1) weighing 2mmol of Co (CH)3COO)2·4H2O and 2mmol FeCl3·6H2Dissolving O in 50mL of ultrapure water fully after ultrasonic dispersion for half an hour to obtain a mixed solution A;
(2) weighing 2mmol of 2, 5-dihydroxy terephthalic acid, dissolving in a single-neck flask filled with 50mL of ultrapure water, and performing ultrasonic dispersion for half an hour to fully dissolve to obtain a mixed solution B;
(3) transferring the mixed solution B into an oil bath pan, slowly adding the solution A into the solution B, reacting at 100 ℃ for 2h, washing with ultrapure water and absolute ethyl alcohol, and freeze-drying for 24h to obtain black precipitate (bimetal Co)2/Fe2-MOF-74 metal organic framework material);
(4) placing the obtained black precipitate in a corundum porcelain boat, and carrying out heat treatment under the argon atmosphere, wherein the heat treatment temperature is 800 ℃, the heating rate is 3 ℃/min, and the heat preservation time is 3h to obtain Co3Fe1a/C composite material.
FIG. 1 shows the bimetallic Co prepared in example 63/Fe1-MOF-74 Metal-organic framework Material (a) and Co after Heat treatment3Fe1SEM (b) photograph and TEM (C) photograph of/C composite material. As can be seen from the figure, Co was preparedx/Fe4-x-MOF-7The 4 metal organic framework material presents obvious bird nest-like microscopic morphology, which shows that the MOF material with the morphology can be successfully prepared by the method. After heat treatment in argon, it is evident that the heat treated product retains the microscopic appearance of the precursor and also exhibits a more pronounced bird's nest-like shape, but the heat treated product has a pronounced shrinkage due to the decomposition of the organic components in the metal organic framework material, which leads to a reduction in the mass of the heat treated product relative to the precursor. As can be seen from the TEM photographs, the metal particles are embedded in the carbon layer, and many cavities are formed, which is advantageous for enhancing the electromagnetic wave absorption.
FIG. 2 shows bimetallic Co prepared in comparative example 12/Fe2-MOF-74 Metal-organic framework Material and Co after Heat treatment2Fe2SEM pictures of the/C composite. As can be seen from the figure, when the cobalt iron ratio is 2: 2, the microscopic morphology of the product is obviously changed, and the product becomes a relatively agglomerated short rod-shaped product. Thus, the proportion of cobalt and iron must be reasonably controlled to prepare the nest-shaped product.
FIG. 3 shows Co after heat treatment in example 63Fe1XRD pattern of the/C composite material. As can be seen from the figure, three characteristic peaks of XRD of the heat-treated sample correspond to iron metal particles of bcc structure (PDF card: 06-0696). At this time, the diffraction peak of the cobalt metal simple substance is not obviously shown, because the unit cell of the iron atom effectively adjusts the unit cell of the cobalt atom, so that the diffraction peak of the cobalt cannot be obviously shown. Indicating that the iron incorporation is dominant and masking the diffraction peaks of cobalt metal.
FIG. 4 shows Co after heat treatment in example 63Fe1RL value of the/C composite material when the mass fraction is only 10%. As can be seen from the figure, in example 6, the maximum reflection loss reaches-61.8 dB at the frequency of 12.7GHz, the effective frequency bandwidth is 8.68GHz, and the matching thickness is 2.8 mm.
FIG. 5 shows the heat-treated Co of comparative example 12Fe2RL value of the/C composite material when the mass fraction is only 10%. As can be seen from the graph, comparative example 1 has a frequency of 13.92GHz, which is the most importantThe large reflection loss reaches-47.5 dB, the effective frequency bandwidth is 8.68GHz, and the matching thickness is 2.5 mm.
FIG. 6 shows Co after heat treatment in example 63Fe1The cole-cole circle diagram and the C0 diagram of the/C composite material when the mass fraction is only 10%. As shown in fig. 6(a), several Cole-Cole semicircles were found in the curves of the samples, indicating that the debye relaxation process is favorable for improving the dielectric properties of the three samples, and that the Cole-Cole semicircles are distorted, indicating that in addition to debye relaxation, mechanisms such as electron polarization and dipole polarization exist in these composites. As can be seen from the TEM photograph of fig. 1(c), a part of the metal particles are coated with carbon to form a shell structure, so that the propagating microwave generates rich interface polarization and is repeatedly scattered, resulting in absorption and loss of the microwave. FIG. 6(b) shows Co3Fe1/The C0 curve for the C composite clearly shows that as the frequency increases, the C0 for all samples fluctuates significantly, indicating that eddy current losses are not the only magnetic loss mechanism, and that both exchange resonance and natural resonance contribute to the magnetic loss.
Claims (8)
1. A preparation method of a CoFe/C composite material is characterized by comprising the following steps:
step 1, mixing Co (CH)3COO)2·4H2O and FeCl3·6H2Dissolving O in water to obtain a mixed solution A; dissolving 2, 5-dihydroxy terephthalic acid in water to obtain a mixed solution B; wherein, Co (CH)3COO)2·4H2O and FeCl3·6H2The molar ratio of O is x: (4-x), wherein x is 3.4-2.6; the solute of the mixed solution A is Co (CH)3COO)2·4H2O and FeCl3·6H2O composition;
step 2, mixing the mixed solution B and the mixed solution A, reacting for 0.5-3 h at 90-110 ℃, washing and drying the obtained product to obtain a precipitate;
step 3, carrying out heat treatment on the obtained precipitate at 700-900 ℃ in a protective atmosphere to obtain CoxFe4-xa/C composite material;
in step 2, after the mixed solution B and the mixed solution A are mixed, 2, 5-dihydroxyterephthalic acid and Co (CH)3COO)2·4H2The molar ratio of O is: 2: (3.4-2.6).
2. The method for preparing the CoFe/C composite material according to claim 1, wherein in the step 2, the reaction is carried out at 90-110 ℃ for 1-3 h.
3. The method of claim 1, wherein the drying in step 2 is freeze-drying.
4. The method of claim 1, wherein in step 3, the shielding gas is argon.
5. The method for preparing the CoFe/C composite material according to claim 1, wherein in the step 3, the heat treatment temperature is 700-900 ℃ and the time is 2-5 h.
6. The method of claim 1, wherein in step 3, the temperature rise rate is 2-5 ℃/min.
7. A CoFe/C composite material obtained by the production process according to any one of claims 1 to 6.
8. Use of the CoFe/C composite material of claim 7 for electromagnetic wave absorption.
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