CN112743098B - Preparation method of nitrogen-doped porous carbon-coated hollow cobalt-nickel alloy composite wave-absorbing material - Google Patents
Preparation method of nitrogen-doped porous carbon-coated hollow cobalt-nickel alloy composite wave-absorbing material Download PDFInfo
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Abstract
The preparation method of the nitrogen-doped porous carbon-coated hollow cobalt-nickel alloy composite wave-absorbing material takes CoNi @ polydopamine as a template, dopamine hydrochloride is polymerized in situ on a hollow CoNi alloy, and the hollow CoNi alloy composite wave-absorbing material coated with the nitrogen-doped porous carbon shell is formed through high-temperature calcination. The composite wave-absorbing material has excellent microwave absorption performance under the condition of thinner thickness, the frequency is 12.8GHz, the matching thickness is 2.0mm, the optimal RL value can reach-47.1 dB, the frequency bandwidth is 4.52GHz, the wave-absorbing performance is excellent, and the application value is very high. The invention has the advantages of simple preparation process, uniform compounding, stable material performance and low production cost, and is suitable for industrial production.
Description
Technical Field
The invention relates to a preparation method of a nitrogen-doped porous carbon-coated hollow cobalt-nickel alloy composite wave-absorbing material, and particularly belongs to the technical field of wave-absorbing materials.
Background
Due to the rapid development of electronic technology, the problem of electromagnetic wave interference is ubiquitous in our daily life, which not only seriously threatens the health of human beings, but also influences the operation of precise electronic instruments. In addition, military equipment is also important for the purpose of stealth by absorbing radar waves. Therefore, it is crucial to develop advanced microwave absorbing materials with "strong, wide, thin, light" functionality to achieve perfect functionality. Magnetic materials (alloys) have attracted much attention because of their high saturation magnetization, simple preparation process, and low cost. However, these magnetic materials generally have poor impedance mismatch and microwave absorption, are easily oxidized, and have high density, which cannot satisfy the requirement of light weight. Therefore, the method of taking the hollow alloy as the core and taking the porous carbon as the shell is an effective method for improving the wave absorption performance of the magnetic material. The CoNi alloy wave absorber prepared by Zhang Shimin et al has no reflection loss value of-10 dB (current Lia, sting Sui, Xiaohui junction, Zhiming Zhang ga, Liangmin Yu. A Sustainable constraint of an effective light microwave International,2019, 18572. 18582.) at all thicknesses, mainly because CoNi has strong magnetism, but has low dielectric, poor impedance matching, which causes electromagnetic waves not to enter the wave absorber and is not beneficial to the absorption of the electromagnetic waves. The cobalt-nickel alloy (Co-Ni) coated hollow glass microsphere light composite powder prepared by luoshami et al reaches-27.25 d B at 7.2GHz, and the bandwidth less than-10 d B is 1.6GHz (luoshami, yuanjun, jacarassian, maxmin, wangxing). The invention reduces the relative density by designing the cobalt-nickel alloy with the hollow structure, and the hollow structure can also adjust impedance matching, enhance the scattering and reflection of electromagnetic waves and improve the attenuation capability. In addition, the polydopamine is used as the shell, so that the density of the material is effectively reduced, the corrosion resistance of the composite wave-absorbing material is improved, the dielectric of the material is improved, and the impedance matching of the material is improved, so that the electromagnetic wave absorption performance of the composite material is obviously improved.
Disclosure of Invention
The invention provides a preparation method of a composite wave-absorbing material of a nitrogen-doped porous carbon-coated hollow cobalt-nickel alloy, aiming at solving the technical problems of complex preparation method, high equipment requirement and high cost of the existing carbon-based microwave absorbing material.
The preparation method of the nitrogen-doped porous carbon-coated hollow cobalt-nickel alloy composite wave-absorbing material takes CoNi @ PDA (polydopamine) as a template to prepare the porous carbon-coated hollow cobalt-nickel alloy-doped composite wave-absorbing material, and comprises the following specific steps:
step 1: adding CoCl2·6H2O、NiCl2·6H2Dissolving O and polyvinylpyrrolidone in ethylene glycol, continuously stirring for 30min, then adding the mixture into a hydrazine hydrate solution with the mass concentration of 50-80% under the stirring condition, continuously stirring for 20min, transferring the obtained suspension into a stainless steel reaction kettle with a tetrafluoroethylene lining, and preserving heat for 6h under the condition of 160-200 ℃; after the reaction product is adsorbed and collected by a magnet, washing the reaction product with deionized water and ethanol for at least three times respectively, and then drying the reaction product in vacuum for 8 hours at the temperature of 60 ℃ to obtain CoNi alloy microspheres;
in g/mL, CoCl2·6H2The ratio of O to glycol is 0.45-0.50: 34-38, NiCl2·6H2The ratio of O to glycol is 0.45-0.50: 34-38, and the ratio of polyvinylpyrrolidone to glycol is 0.8-1.2: 34-38; according to mL/mL, the ratio of hydrazine hydrate to glycol is 0.5-1.5: 5-7;
step 2: dispersing CoNi alloy microspheres and dopamine hydrochloride into a trihydroxymethyl aminomethane buffer solution with the pH value of 8.5, stirring the reaction mixed solution for reaction for 24 hours, collecting precipitates in the reaction product by using a magnet, washing the precipitates with deionized water and ethanol for three times respectively, and drying the precipitates at the temperature of 60 ℃ overnight to obtain CoNi @ PDA;
in the reaction mixed liquid, the ratio of CoNi alloy microspheres to water is 0.18-0.22: 180-220, the ratio of dopamine hydrochloride to water is 0.22-0.26: 180-220, and the ratio of tris (hydroxymethyl) aminomethane to water is 0.22-0.26: 180-220 in g/mL; the mass ratio of the CoNi alloy microspheres to the dopamine hydrochloride to the tris (hydroxymethyl) aminomethane is 0.18-0.22: 0.22-0.26;
and step 3: the CoNi @ PDA is heated to 600-800 ℃ from room temperature at the heating rate of 5-10 ℃/min in the nitrogen atmosphere, is roasted for 2-4 hours, and is naturally cooled to room temperature in the nitrogen atmosphere, so that the nitrogen-doped porous carbon-coated hollow cobalt-nickel alloy composite wave-absorbing material is obtained.
The invention has the beneficial effects that:
1. the invention overcomes the defect of large alloy density by preparing the hollow cobalt-nickel alloy, so as to reduce the weight of the wave-absorbing material and achieve the purpose of light weight.
2. The invention generates polydopamine by in-situ polymerization reaction on the hollow CoNi alloy, can prevent the CoNi alloy from being oxidized, and improves the corrosion resistance of the material. The hollow CoNi alloy composite material is coated by the nitrogen-doped porous carbon shell obtained by high-temperature calcination to adjust the dielectric constant and magnetic conductivity of the composite material, so that the impedance matching of the material is adjusted, the microwave absorption performance of the composite material is improved, and the density of the composite material is further reduced.
3. The nitrogen-doped porous carbon-coated hollow cobalt-nickel alloy composite wave-absorbing material disclosed by the invention is relatively low in density and strong in corrosion resistance, has strong electromagnetic wave absorption capacity and wide effective bandwidth under the condition of thin thickness, is excellent in microwave absorption performance, has the matching thickness of 2.0mm at the frequency of 12.8GHz, can reach-47.1 dB at the optimal RL value and has a high application value at the frequency bandwidth of 4.52 GHz.
4. The invention has the advantages of simple preparation process, uniform compounding, stable material performance and low production cost, and is suitable for industrial production.
Drawings
FIG. 1 is an X-ray diffraction pattern of CoNi @ NC-700 of the present invention;
in the figure, 700 represents the pyrolysis temperature of CoNi @ PDA;
FIG. 2 is an XPS spectrum of CoNi @ NC-700 of example 1 of the present invention;
FIG. 3 is an SEM of CoNi @ NC-700 of example 1 of the present invention;
FIG. 4 is a TEM image of CoNi @ NC-700 of example 1 of the present invention;
FIG. 5 is a reflection loss spectrum of the CoNi @ NC-700 composite wave-absorbing material in embodiment 1 of the invention.
Detailed Description
Example 1
The method for preparing the CoNi @ NC composite wave-absorbing material by taking CoNi @ PDA as a template comprises the following steps:
step 1: 0.48g of CoCl2·6H2O, 0.48g of NiCl2·6H2O and 1g polyvinylpyrrolidone (PVP) were dissolved in 36mL of ethylene glycol, and stirring was continued for 30min, and then 6mL of 60% hydrazine hydrate solution was dropped into the above solutions in turn under strong stirring and stirred for 20 min. The resulting suspension was transferred to a tetrafluoroethylene lined stainless steel reaction kettle and held at 180 ℃ in an air oven for 6 h. After the reaction is finished, collecting the obtained product, and respectively washing the product with deionized water and ethanol for at least three times to remove residual impurities; and finally, placing the microspheres in a vacuum oven, and drying the microspheres for 8 hours at the temperature of 60 ℃ under a vacuum condition to obtain the hollow CoNi alloy microspheres.
Step 2: 0.2g of CoNi alloy microspheres and 0.24g of dopamine hydrochloride were dispersed in (0.24g of tris, 200 mL of deionized water) tris buffer (pH 8.5) and stirred continuously for 24h, and then the precipitate was collected with a magnet, washed three times with deionized water and ethanol, respectively, and dried at 60 ℃ overnight to give CoNi @ PDA.
And step 3: and (3) heating the prepared CoNi @ PDA from room temperature to 700 ℃ under the conditions of nitrogen atmosphere and heating rate of 5 ℃/min, roasting for 2h, and naturally cooling to room temperature under the nitrogen atmosphere to obtain CoNi @ NC-700.
And 4, step 4: the prepared hollow CoNi @ NC-700 composite wave-absorbing material and a paraffin base are uniformly mixed to prepare a circular ring, and the mass of the CoNi @ NC-700 composite wave-absorbing material and the mass of the paraffin are 0.05g and 0.05g respectively.
The electromagnetic parameters of the material are measured by a vector network analyzer, and according to the transmission line theory, the reflection loss of the material to electromagnetic waves is calculated by the complex dielectric constant and the complex permeability under given frequency and the thickness of the wave-absorbing material through the following equation.
Zin＝Z0(μr/εr)1/2tanh[j(2πfd/c)(μr/εr)1/2],
RL(dB)＝20log|(Zin－1)/(Zin+1)|。
According to the X-ray diffraction pattern of CoNi @ NC-700 shown in figure 1 of the invention, XRD analysis is carried out to study that the synthesized compound shows three peaks which are respectively positioned at 44.4 degrees (111), 51.7 degrees (500) and 76.3 degrees (220), and the requirement of face-centered cubic structure Co (PDF #15-0806) and Ni (PDF #04-0850) is met. Each diffraction peak is a unique peak indicating that the material is not a mixture of Co and Ni, but is present in the alloy in the form of a unit cell.
From the XPS plot of FIG. 2, it can be seen that the presence of C, N, O, Co and Ni elements in CoNi @ NC-700 demonstrates the successful preparation of CoNi @ NC-700. The morphology of CoNi @ NC-700 can be seen as a spherical structure in the SEM image of FIG. 3. From the TEM image of FIG. 4, it can be seen that CoNi @ NC-700 has a hollow structure. As can be seen in FIGS. 3 and 4, CoNi @ NC-700 has a core-shell structure. As can be seen from FIG. 5, the optimum RL value of the product CoNi @ NC-700 at a frequency of 12.8GHz with a matching thickness of 2.0mm can reach-47.1 dB, and the frequency bandwidth with a RL less than-10 dB is 4.52 GHz. The RL value can reach-37.6 dB when the thickness is 1.7mm, and the frequency bandwidth of the RL less than-10 dB is 5.10 GHz.
Claims (1)
1. The preparation method of the nitrogen-doped porous carbon-coated hollow cobalt-nickel alloy composite wave-absorbing material is characterized by comprising the following steps of: the preparation method takes CoNi @ PDA as a template to prepare the nitrogen-doped porous carbon-coated hollow cobalt-nickel alloy composite wave-absorbing material, and comprises the following specific steps:
step 1: adding CoCl2·6H2O、NiCl2·6H2Dissolving O and polyvinylpyrrolidone in ethylene glycol, continuously stirring for 30min, then adding the mixture into a hydrazine hydrate solution with the mass concentration of 50-80% under the stirring condition, continuously stirring for 20min, transferring the obtained suspension into a stainless steel reaction kettle with a tetrafluoroethylene lining, and preserving heat for 6h under the condition of 160-200 ℃; after the reaction product is adsorbed and collected by a magnet, washing the reaction product with deionized water and ethanol for at least three times respectively, and then drying the reaction product in vacuum at 60 ℃ for 8 hours to obtain CoNi alloy microspheres;
in g/mL, CoCl2·6H2The ratio of O to glycol is 0.45-0.50: 34-38, NiCl2·6H2The ratio of O to glycol is 0.45-0.50: 34-38, and the ratio of polyvinylpyrrolidone to glycol is 0.8-1.2: 34-38; according to mL/mL, the ratio of hydrazine hydrate to glycol is 0.5-1.5: 5-7;
step 2: dispersing CoNi alloy microspheres and dopamine hydrochloride into a trihydroxymethyl aminomethane buffer solution with the pH value of 8.5, stirring the reaction mixed solution for reaction for 24 hours, collecting precipitates in the reaction product by using a magnet, washing the precipitates with deionized water and ethanol for three times respectively, and drying the precipitates at the temperature of 60 ℃ overnight to obtain CoNi @ PDA;
in the reaction mixed liquid, the ratio of CoNi alloy microspheres to water is 0.18-0.22: 180-220, the ratio of dopamine hydrochloride to water is 0.22-0.26: 180-220, and the ratio of tris (hydroxymethyl) aminomethane to water is 0.22-0.26: 180-220 in g/mL; the mass ratio of the CoNi alloy microspheres to the dopamine hydrochloride to the tris (hydroxymethyl) aminomethane is 0.18-0.22: 0.22-0.26;
and step 3: the CoNi @ PDA is heated to 600-800 ℃ from room temperature at the heating rate of 5-10 ℃/min in the nitrogen atmosphere, is roasted for 2-4 hours, and is naturally cooled to room temperature in the nitrogen atmosphere, so that the nitrogen-doped porous carbon-coated hollow cobalt-nickel alloy composite wave-absorbing material is obtained.
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