CN110669474A - NiCo/C @ CNT double-conductive-network hierarchical structure material and preparation method and application thereof - Google Patents
NiCo/C @ CNT double-conductive-network hierarchical structure material and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a NiCo/C @ CNT double-conducting-network hierarchical structure material and a preparation method and application thereof, wherein nickel acetate tetrahydrate and cobalt acetate tetrahydrate are used as metal sources, 2, 5-dihydroxyterephthalic acid is used as an organic ligand, ultrapure water is used as a reaction solvent, an orange-yellow precipitate is obtained after a certain reflux reaction at a temperature of 80-110 ℃ for a period of time, the obtained product is centrifuged, washed and dried, and finally the product is calcined at a temperature of 500-800 ℃ for 1-4 hours in an inert atmosphere to obtain the NiCo/C @ CNT double-conducting-network wave-absorbing material. The NiCo/C @ CNT double-conductive-network wave-absorbing material obtained by the method forms a hierarchical structure after the carbon nano tubes are generated in situ, so that the NiCo/C @ CNT double-conductive-network wave-absorbing material as a wave-absorbing material shows excellent electromagnetic wave-absorbing performance.
Description
Technical Field
The invention belongs to the field of electromagnetic wave absorption, and particularly relates to a NiCo/C @ CNT double-conductive-network hierarchical structure material as well as a preparation method and application thereof.
Background
In the 21 st century, information technology is the leading era, and in recent years, with the development of science and technology, televisions, computers, electromagnetic waves, microwave ovens, mobile phones and the like have been deeply involved in daily life of people, and the rapid development of information technology and electronic communication equipment brings great convenience and rapidness to the production and life style of people, but also brings certain threats to the living environment of people. The wave-absorbing material can convert electromagnetic wave energy into heat energy, and relieve the problem of increasingly serious electromagnetic pollution caused by the wide application of electronic equipment, so the wave-absorbing material has attracted extensive attention in the technical fields of electronic safety systems and national defense stealth. Generally, a superior EMW absorber should meet the requirements of strong lightweight, low strength, broad band absorption, and strong absorption capacity. Previous researches prove that the carbon-based composite material has novel structures such as core-shell, yolk-shell, hollow and layered structures, and the like, which are greatly improved in wave absorbing performance, so that the carbon-based composite material is considered to be a promising candidate material. However, the preparation process of these hierarchical structures is relatively complicated, which is not favorable for industrial application thereof. Therefore, it remains a great challenge to prepare a graded carbon-based absorber in a simple and efficient manner.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a NiCo/C @ CNT double-conductive-network hierarchical structure material, a preparation method and application thereof, the preparation method is simple, and the prepared NiCo/C @ CNT double-conductive-network hierarchical structure material has excellent wave-absorbing performance.
The invention is realized by the following technical scheme:
a preparation method of a NiCo/C @ CNT double-conductive-network hierarchical structure material comprises the following steps:
(1) mixing Co (CH)3COO)2·4H2O and Ni (CH)3COO)2·4H2Dissolving 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 Ni (CH)3COO)2·4H2The molar ratio of O is X: (4-X), X ═ 1-3;
(2) mixing the mixed solution A and the mixed solution B, reacting for 0.5-3 h at the temperature of 80-110 ℃, washing and drying a product to obtain a precipitate;
(3) and carrying out heat treatment on the precipitate in a protective atmosphere at the temperature of 500-800 ℃ to obtain the NiCo/C @ CNT double-conductive-network hierarchical structure material.
Preferably, in the step (2), after the mixture A and the mixture B are mixed, 2, 5-dihydroxyterephthalic acid and Ni (CH)3COO)2·4H2The molar ratio of O is: 2: (1-3).
Preferably, in step (2), the drying is freeze-drying.
Preferably, in step (2), the reaction is carried out under oil bath conditions.
Preferably, in the step (3), the heating rate is 2-5 ℃/min, and the heat preservation time is 1-4 h.
Preferably, in step (3), the protective atmosphere is argon.
The NiCo/C @ CNT double-conductive-network hierarchical structure material obtained by the preparation method.
The NiCo/C @ CNT double-conductive-network hierarchical structure material is applied to the aspect of electromagnetic wave absorption.
Compared with the prior art, the invention has the following beneficial technical effects:
the nano-rod-shaped Ni/Co-MOF-74 metal organic framework material is prepared by a simple method, and the hierarchical structure material of the NiCo/C @ CNT double-conductive network can be obtained by heat treatment in a protective atmosphere. By adjusting the Ni/Co molar ratio of the precursor NiCo-MOF-74 nanorod, a hierarchical NiCo/C @ CNTs hierarchical structure with different chemical compositions, densities and CNTs lengths can be obtained after heat treatment, and the hierarchical structure is composed of the carbon nanorod, metal particles on the carbon nanorod, the carbon nanotube and metal particles on the carbon nanotube. The method has the advantages of low reaction temperature, short reaction time, simple equipment operation, low energy consumption, continuous operation, easy control of process conditions, green synthesis and the like.
The nano-rod-shaped Ni/Co-MOF-74 derived NiCo/C @ CNT double-conductive network prepared by the method has the advantages of high purity, good crystallinity and uniform appearance of the hierarchical structure material, and compared with other wave-absorbing materials, the conductivity of the nano-rod-shaped Ni/Co-MOF-74 derived NiCo/C @ CNT double-conductive network is greatly improved due to the fact that carbon nano-tubes are generated under the catalytic action of nickel and cobalt, so that the nano-rod-shaped Ni/Co-MOF-74 derived NiCo/C @ CNT double-conductive network has the advantages of high reflection loss value, wide frequency bandwidth. The electromagnetic wave absorption performance of the sample is tested by a vector network analyzer, and it can be found that when the mass fraction is only 5%, the nickel-cobalt ratio is 2: 2 has the best wave-absorbing performance. The maximum reflection loss reaches-58.8 dB, the effective bandwidth is 6.5GHz (11.5-18GHz), and the matching thickness is 2.6 mm.
Drawings
FIG. 1(a) is an SEM photograph of a nanorod NiCo-MOF-74 precursor prepared in example 3; FIG. 1(b) is an SEM photograph of a nanorod NiCo-MOF-74 precursor prepared in example 6; FIG. 1(c) is an SEM photograph of a nanorod NiCo-MOF-74 precursor prepared in example 9;
FIG. 2 is (a) SEM and (b) TEM pictures of a hierarchical structure material of a NiCo/C @ CNT two-conductor network prepared in example 6.
FIG. 3 shows the values of the reflection loss at a loading of 5 wt% for the hierarchical structure material of a NiCo/C @ CNT dual conductive network prepared in example 6.
FIG. 4 is a Cole-Cole ring diagram of the hierarchical structure material of NiCo/C @ CNT dual conductive network prepared in example 6, and C0.
FIG. 5 is a schematic structural diagram of a hierarchical structure material of a NiCo/C @ CNT double-conductive network and a TEM image of the material of example 6.
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 discloses a preparation method and application of a NiCo/C @ CNT double-conductive-network hierarchical structure material, which comprises the following steps:
(1) weighing X mmolCo (CH)3COO)2·4H2O and (4-X) mmolNi (CH)3COO)2·4H2Dissolving O in 50mL of ultrapure water fully after ultrasonic dispersion for half an hour to obtain a mixed solution A; wherein, X is 1-3;
(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 the temperature of 80-110 ℃, washing with ultrapure water and absolute ethyl alcohol, and freeze-drying for 24h to obtain an orange yellow precipitate;
(4) and placing the obtained orange-yellow precipitate in a corundum porcelain boat, and carrying out heat treatment under the argon atmosphere, wherein the heat treatment temperature is 500-800 ℃, the heating rate is 2-5 ℃/min, and the heat preservation time is 1-4 h.
Example 1
A preparation method of a NiCo/C @ CNT double-conductive-network hierarchical structure material comprises the following steps:
(1) weighing 3mmol Ni (CH)3COO)2·4H2O and 1mmol of Co (CH)3COO)2·4H2Dissolving O in 50mL of ultrapure water, and fully dissolving the O 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 80 ℃ for 0.5h, washing with ultrapure water and absolute ethyl alcohol, and freeze-drying for 24h to obtain an orange yellow precipitate;
(4) and placing the obtained orange-yellow precipitate in a corundum porcelain boat, and carrying out heat treatment under the argon atmosphere, wherein the heat treatment temperature is 500 ℃, the heating rate is 2 ℃/min, and the heat preservation time is 1 h.
Example 2
A preparation method of a NiCo/C @ CNT double-conductive-network hierarchical structure material comprises the following steps:
(1) 3mmol of Ni (CH) are weighed3COO)2·4H2O and 1mmol of Co (CH)3COO)2·4H2Dissolving O in 50mL of ultrapure water, and fully dissolving the O after ultrasonic dispersion for half an hour to obtain a mixed solutionA；
(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 for 3h at 110 ℃, washing with ultrapure water and absolute ethyl alcohol, and freeze-drying for 24h to obtain an orange yellow precipitate;
(4) and placing the obtained orange-yellow 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 5 ℃/min, and the heat preservation time is 4 h.
Example 3
A preparation method of a NiCo/C @ CNT double-conductive-network hierarchical structure material comprises the following steps:
(1) 3mmol of Ni (CH) are weighed3COO)2·4H2O and 1mmol of Co (CH)3COO)2·4H2Dissolving O in 50mL of ultrapure water, and fully dissolving the O 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 for 2h at 100 ℃, washing with ultrapure water and absolute ethyl alcohol, and freeze-drying for 24h to obtain an orange yellow precipitate;
(4) and placing the obtained orange-yellow precipitate in a corundum porcelain boat, and carrying out heat treatment under the argon atmosphere, wherein the heat treatment temperature is 700 ℃, the heating rate is 3 ℃/min, and the heat preservation time is 2 h.
Example 4
A preparation method of a NiCo/C @ CNT double-conductive-network hierarchical structure material comprises the following steps:
(1) weighing 2mmol of Ni (CH)3COO)2·4H2O and 2mmol of Co (CH)3COO)2·4H2Dissolving O in 50mL of ultrapure water, and ultrasonically separatingAfter half an hour of dispersion, fully dissolving the mixture 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 80 ℃ for 0.5h, washing with ultrapure water and absolute ethyl alcohol, and freeze-drying for 24h to obtain an orange yellow precipitate;
(4) and placing the obtained orange-yellow precipitate in a corundum porcelain boat, and carrying out heat treatment under the argon atmosphere, wherein the heat treatment temperature is 500 ℃, the heating rate is 2 ℃/min, and the heat preservation time is 1 h.
Example 5
A preparation method of a NiCo/C @ CNT double-conductive-network hierarchical structure material comprises the following steps:
(1) weighing 2mmolNi (CH)3COO)2·4H2O and 2mmolCo (CH)3COO)2·4H2Dissolving O in 50mL of ultrapure water, and fully dissolving the O 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 for 3h at 110 ℃, washing with ultrapure water and absolute ethyl alcohol, and freeze-drying for 24h to obtain an orange yellow precipitate;
(4) and placing the obtained orange-yellow 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 5 ℃/min, and the heat preservation time is 4 h.
Example 6
A preparation method of a NiCo/C @ CNT double-conductive-network hierarchical structure material comprises the following steps:
(1) weighing 2mmol of Ni (CH)3COO)2·4H2O and 2mmol of Co (CH)3COO)2·4H2Dissolving O in 50mL of ultrapure water, and fully dissolving the O 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 for 2h at 100 ℃, washing with ultrapure water and absolute ethyl alcohol, and freeze-drying for 24h to obtain an orange yellow precipitate;
(4) and placing the obtained orange-yellow precipitate in a corundum porcelain boat, and carrying out heat treatment under the argon atmosphere, wherein the heat treatment temperature is 700 ℃, the heating rate is 3 ℃/min, and the heat preservation time is 2 h.
Example 7
A preparation method of a NiCo/C @ CNT double-conductive-network hierarchical structure material comprises the following steps:
(1) weighing 1mmol of Ni (CH)3COO)2·4H2O and 3mmol Co (CH)3COO)2·4H2Dissolving O in 50mL of ultrapure water, and fully dissolving the O 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 80 ℃ for 0.5h, washing with ultrapure water and absolute ethyl alcohol, and freeze-drying for 24h to obtain an orange yellow precipitate;
(4) and placing the obtained orange-yellow precipitate in a corundum porcelain boat, and carrying out heat treatment under the argon atmosphere, wherein the heat treatment temperature is 500 ℃, the heating rate is 2 ℃/min, and the heat preservation time is 1 h.
Example 8
A preparation method of a NiCo/C @ CNT double-conductive-network hierarchical structure material comprises the following steps:
(1) weighing 1mmol Ni (CH)3COO)2·4H2O and 3mmolCo (CH)3COO)2·4H2Dissolving O in 50mL of ultrapure water, and fully dissolving the O 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 for 3h at 110 ℃, washing with ultrapure water and absolute ethyl alcohol, and freeze-drying for 24h to obtain an orange yellow precipitate;
(4) and placing the obtained orange-yellow 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 5 ℃/min, and the heat preservation time is 4 h.
Example 9
A preparation method of a NiCo/C @ CNT double-conductive-network hierarchical structure material comprises the following steps:
(1) weighing 1mmol Ni (CH)3COO)2·4H2O and 3mmolCo (CH)3COO)2·4H2Dissolving O in 50mL of ultrapure water, and fully dissolving the O 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 for 2h at 100 ℃, washing with ultrapure water and absolute ethyl alcohol, and freeze-drying for 24h to obtain an orange yellow precipitate;
(4) and placing the obtained orange-yellow precipitate in a corundum porcelain boat, and carrying out heat treatment under the argon atmosphere, wherein the heat treatment temperature is 700 ℃, the heating rate is 3 ℃/min, and the heat preservation time is 2 h.
FIG. 1 shows SEM pictures of nano-rod-shaped Ni/Co-MOF-74 precursors synthesized by different Ni and Co ratios, wherein (a) is Ni1Co3-MOF-74, (b) is Ni2Co2-MOF-74，(c) Is Ni3Co1-MOF-74. As can be seen from the figure, the samples obtained were all samples in the shape of a nanorod.
FIG. 2 shows SEM (a) and TEM (b) pictures of the hierarchical structure material of NiCo/C @ CNT two-conductive network prepared in example 6. As can be seen from the figure, the carbon nanotubes are grown in situ by heat-treating the nanorod precursors, and have a high aspect ratio and a high density. The carbon nano-tube which grows in situ is grown on the original nano-rod, part of the carbon component in the ligand is converted into nano-rod graphitic carbon and still keeps the appearance of the original nano-rod, and part of the carbon is converted into the carbon nano-tube under the bimetallic catalysis of Ni and Co, so that the hierarchical structure of the carbon nano-tube growing on the carbon nano-rod is formed. FIG. 5 is a schematic structural diagram and a TEM comparison with example 6.
FIG. 3 shows the material of the hierarchical structure of a NiCo/C @ CNT two-conductor network prepared in example 6, with RL values calculated for different thicknesses (in mm) at a 5 wt% fill rate, according to transmission line theory. As can be seen from the figure, the maximum RL value of the embodiment 3 is-58.8 dB (14.0GHz), the corresponding frequency bandwidth is 6.5GHz (11.5-18GHz), and the matching thickness is 2.6 mm.
FIG. 4 shows a Cole-Cole ring diagram of the hierarchical structure material of NiCo/C @ CNT two-conductor network prepared in example 6, along with C0. As can be seen from the Cole-Cole circle diagram, the example 3 sample has many semicircles, indicating that the enhancement of the imaginary part of the dielectric constant of example 3 is attributable to conduction loss. For the sample of example 3, the high aspect ratio and density of the carbon nanotubes more readily form a network structure between the intertwined carbon nanotubes. For absorbers that are radiated by electromagnetic waves, more micro-current is generated, and more micro-current through the network structure generates more significant conduction loss. As can be seen from C0, the C0 curve exhibits several formants in the low and high frequency regions, indicating that the magnetic loss originates from natural resonance and exchange resonance.
FIG. 5 is a schematic structural diagram of a hierarchical structure material of a NiCo/C @ CNT double-conductive network and a TEM image of the material of example 6. As can be seen from the figure, the obtained lattice stripes are stripes of NiCo alloy, and a part of the nickel-cobalt alloy particles are wrapped by carbon nanotubes, and thus, the hierarchical structure of NiCo/C @ CNT double conductive network has various loss mechanisms.
Claims (8)
1. A preparation method of a NiCo/C @ CNT double-conductive-network hierarchical structure material is characterized by comprising the following steps of:
step 1, mixing Co (CH)3COO)2·4H2O and Ni (CH)3COO)2·4H2Dissolving 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 Ni (CH)3COO)2·4H2The molar ratio of O is X: (4-X), X ═ 1-3;
step 2, mixing the mixed solution A and the mixed solution B, reacting for 0.5-3 h at 80-110 ℃, washing and drying a product to obtain a precipitate;
and 3, carrying out heat treatment on the precipitate in a protective atmosphere at the temperature of 500-800 ℃ to obtain the NiCo/C @ CNT double-conductive-network hierarchical structure material.
2. The method for preparing a NiCo/C @ CNT double-conducting-wire network hierarchical structure material as claimed in claim 1, wherein in the step 2, after the mixed liquor A and the mixed liquor B are mixed, 2, 5-dihydroxyterephthalic acid and Ni (CH)3COO)2·4H2The molar ratio of O is: 2: (1-3).
3. The method for preparing a NiCo/C @ CNT double-conductive-network hierarchical structure material according to claim 1, wherein in the step 2, the drying is freeze drying.
4. The method for preparing a NiCo/C @ CNT double conductive network hierarchical structure material according to claim 1, wherein in the step 2, the reaction is performed under oil bath conditions.
5. The method for preparing a NiCo/C @ CNT double-conductive-network hierarchical structure material according to claim 1, wherein in the step 3, the temperature rise rate is 2-5 ℃/min, and the heat preservation time is 1-4 h.
6. The method for preparing a NiCo/C @ CNT double-conductive-network hierarchical structure material according to claim 1, wherein in the step 3, the protective atmosphere is argon.
7. A NiCo/C @ CNT double conductive network hierarchical structure material obtained by the preparation method of any one of claims 1 to 6.
8. Use of the NiCo/C @ CNT double conductive network hierarchical structure material of claim 7 for electromagnetic wave absorption.
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| CN114346250A (en) * | 2021-12-31 | 2022-04-15 | 广东技术师范大学 | Metal-carbon composite particle and preparation method and application thereof |
| CN114346250B (en) * | 2021-12-31 | 2023-09-26 | 广东技术师范大学 | Metal-carbon composite particles and preparation method and application thereof |
| CN114956014A (en) * | 2022-05-24 | 2022-08-30 | 合肥工业大学 | Preparation method and application of cobalt selenide/tin selenide @ porous carbon nanorod |
| CN114956014B (en) * | 2022-05-24 | 2023-09-26 | 合肥工业大学 | Preparation method and application of cobalt selenide/tin selenide@porous carbon nanorod |
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