CN113086965A - Chitosan-based nitrogen-doped carbon aerogel wave-absorbing material and preparation method thereof - Google Patents
Chitosan-based nitrogen-doped carbon aerogel wave-absorbing material and preparation method thereof Download PDFInfo
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- CN113086965A CN113086965A CN202110346255.3A CN202110346255A CN113086965A CN 113086965 A CN113086965 A CN 113086965A CN 202110346255 A CN202110346255 A CN 202110346255A CN 113086965 A CN113086965 A CN 113086965A
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Abstract
The invention discloses a chitosan-based nitrogen-doped carbon aerogel wave-absorbing material and a preparation method thereof, belonging to the technical field of material preparation and microwave absorbing materials. The preparation method specifically comprises the following steps: dissolving chitosan in a dilute acetic acid solvent to obtain a chitosan precursor solution; then pouring the chitosan precursor solution into a chill casting mold for directional chill casting, and freeze-drying after the chill casting is finished to obtain chitosan aerogel; and then carbonizing the chitosan aerogel to obtain the chitosan-based nitrogen-doped carbon aerogel. The chitosan-based nitrogen-doped carbon aerogel prepared by the invention has the performance characteristics of low density, high reflection loss and wide band absorption, is simple in preparation method and controllable in structure, meets the requirement of practical application, and has great application potential in the technical field of microwave absorption materials.
Description
Technical Field
The invention belongs to the technical field of material preparation and microwave absorption materials, and particularly relates to a chitosan-based nitrogen-doped carbon aerogel wave-absorbing material and a preparation method thereof.
Background
The rapid development of wireless communication technology and the wide application of electronic equipment cause serious electromagnetic pollution, become a new type of pollution following noise pollution, air pollution and water pollution, and cause serious threats to human health, precision instrument control, communication system operation and the like, and the development of electromagnetic wave absorbing materials becomes an important technical path for solving the electromagnetic pollution. In the military field, in order to meet the development requirement of the modernization of military equipment, the research of the wave-absorbing material has important significance for reducing the detectability of a weapon system and realizing radar stealth. Based on the important role of the wave-absorbing material in social development and national defense construction, research and development and application of the light, green, low-cost and high-performance electromagnetic wave-absorbing material become increasingly concerned research hotspots of various national researchers.
Compared with the traditional powder electromagnetic wave absorbing material, the carbon aerogel material has the advantages of unique three-dimensional network structure, high specific surface area, low density and the like, can realize the construction of a high-efficiency conductive network under the condition of low filling amount, and further endows the material with stronger electromagnetic wave attenuation capability; the abundant pore structure provides an important structural basis for electromagnetic parameter regulation and control and impedance matching optimization, and the development of the freeze casting technology provides a new technical means for three-dimensional aerogel material pore structure parameter regulation and control. Meanwhile, the application of the biomass material has important significance for realizing green and environment-friendly preparation and low-cost preparation of the electromagnetic wave absorbing material.
Based on the analysis, the chitosan-based nitrogen-doped carbon aerogel prepared by utilizing the chitosan biomass precursor through the processes of freeze casting, freeze drying and carbonization provides a new idea for electromagnetic pollution protection and military stealth, and has an important application prospect in the field of microwave absorption.
Disclosure of Invention
The invention aims to provide a broadband and efficient chitosan-based nitrogen-doped carbon aerogel wave-absorbing material and a preparation method thereof. The material has outstanding wave-absorbing performance, the reflection loss value can reach 68.8dB when the thickness is 5.1mm, and the effective absorption bandwidth can cover the whole X wave band. The material has the advantages of simple preparation process, low cost and high structure controllability, and can realize multi-scale regulation and control of wave absorption performance through precursor concentration, cold casting conditions, carbonization temperature and the like.
The invention adopts the following specific technical scheme:
on one hand, the invention provides a preparation method of a chitosan-based nitrogen-doped carbon aerogel wave-absorbing material, which comprises the following specific steps:
s1: adding chitosan into a dilute acetic acid solvent, and stirring until the chitosan is fully dissolved to obtain a chitosan precursor solution;
s2: performing freeze casting on the chitosan precursor solution, and then performing freeze drying to obtain chitosan aerogel;
s3: and carbonizing the chitosan aerogel in an inert atmosphere, and cooling to obtain the chitosan-based nitrogen-doped carbon aerogel wave-absorbing material.
Preferably, in S1, the dilute acetic acid solvent has a concentration of 1% v/v, and is prepared by adding glacial acetic acid into water.
Preferably, in the S1, the addition amount of the chitosan is 1-4 g.
Preferably, in S1, the stirring speed is 400 r/S.
Preferably, in S2, the chitosan precursor solution is poured into a directional chill casting mold for chill casting, where the directional chill casting mold includes a copper base for realizing temperature conduction between the chitosan precursor solution and a cold source, and a polytetrafluoroethylene square tube for containing the chitosan precursor solution.
Preferably, in S2, the temperature of the freeze casting is-20 ℃ to-196 ℃ and the time is 3 hours.
Preferably, in S2, the freeze-drying is performed in a freeze-dryer at-84 deg.C for 24 h.
Preferably, in S3, the carbonization treatment is specifically as follows:
heating from room temperature to 650-700 ℃ at the heating rate of 2 ℃/min, preserving heat for 1h, and then naturally cooling to room temperature.
Preferably, the inert atmosphere is an argon atmosphere.
In a second aspect, the invention provides a chitosan-based nitrogen-doped carbon aerogel wave-absorbing material prepared by any one of the preparation methods.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the invention, the biomass material chitosan is selected as the precursor, the raw materials are easy to obtain, the production cost is low, and in-situ nitrogen doping is realized under the condition that an external nitrogen source is not used, so that the improvement of the electromagnetic wave attenuation capability of the material is facilitated;
(2) according to the invention, the micron-sized directional pore canal is successfully constructed in the material by means of a freeze casting-freeze drying process, the structure controllability is strong, and the multi-scale regulation and control of the electromagnetic property and the wave absorption property of the material are facilitated;
(3) the chitosan-based nitrogen-doped carbon aerogel wave-absorbing material prepared by the invention is low in density (43 mg/cm)3) Low filling amount of (<5 wt.%), the effective absorption bandwidth can cover the whole X-band, and the application requirement of the current electromagnetic wave absorption material of light, thin, wide and strong is well met.
Drawings
FIG. 1 is an XPS total spectrum of a chitosan-based nitrogen-doped carbon aerogel wave-absorbing material in example 1;
FIG. 2 is an SEM picture of the chitosan-based nitrogen-doped carbon aerogel wave-absorbing material in example 1;
FIG. 3 is a reflection loss curve of the chitosan-based nitrogen-doped carbon aerogel wave-absorbing material in example 1 at different thicknesses;
fig. 4 is a reflection loss curve (thickness 5mm) of the chitosan-based nitrogen-doped carbon aerogel wave-absorbing materials prepared in example 1, example 2, example 3 and example 4.
Detailed Description
The invention will be further elucidated and described with reference to the drawings and the detailed description. The technical features of the embodiments of the present invention can be combined correspondingly without mutual conflict.
The invention provides a preparation method of a chitosan-based nitrogen-doped carbon aerogel wave-absorbing material, which comprises the following steps:
s1: first, a dilute acetic acid solvent having a concentration of 1% v/v was prepared by adding glacial acetic acid to water. Adding 1-4 g of chitosan into a dilute acetic acid solvent, and fully stirring the chitosan and the dilute acetic acid solvent at room temperature until the chitosan is fully dissolved in the dilute acetic acid solvent to obtain a chitosan precursor solution.
S2: pouring 16g of the chitosan precursor solution prepared in the step S1 into an oriented cold casting mold for freezing casting, wherein a cold source used for freezing casting can adopt a low-temperature test chamber or liquid nitrogen, the temperature for freezing casting can be-20 ℃ to-196 ℃, and the time for freezing casting can be 3 hours. And (3) putting the product obtained after freezing and casting into a freeze dryer for freeze drying, wherein the freeze drying temperature can be-84 ℃, and the freeze drying time can be 24 hours. After freeze drying treatment, the final product is chitosan aerogel.
The directional cold casting mold adopts a self-designed mold, the mold comprises an upper part and a lower part, namely a copper base and a polytetrafluoroethylene square tube, the polytetrafluoroethylene square tube is used for containing a chitosan precursor solution, and the copper base is used for realizing temperature conduction between the chitosan precursor solution and a cold source.
S3: carbonizing the prepared chitosan aerogel in an inert atmosphere (such as an argon atmosphere), namely heating from room temperature to 650-700 ℃ at a heating rate of 2 ℃/min, preserving heat for 1h, and naturally cooling to room temperature. And cooling to obtain the chitosan-based nitrogen-doped carbon aerogel wave-absorbing material.
Example 1
The embodiment prepares the chitosan-based nitrogen-doped carbon aerogel wave-absorbing material, and the specific implementation steps are as follows:
s1: 1mL of glacial acetic acid is measured and added into 100mL of deionized water to prepare a dilute acetic acid solvent with the concentration of 1% (v/v).
S2: and 3g of chitosan is weighed and added into all the diluted acetic acid solvent prepared in the S1, and the mixture is mechanically stirred at the rotating speed of 400r/S at room temperature until the chitosan is fully dissolved, so that a chitosan precursor solution is obtained.
S3: and (4) pouring 16g of the chitosan precursor solution prepared in the step S2 into an oriented cold casting mold for freezing casting, wherein the used cold source is a low-temperature test box, the cold casting temperature is-60 ℃, and the cold casting time is 3 hours. And transferring the mixture to a freeze drier after the cold casting is finished, and drying the mixture at a low temperature of-84 ℃ for 24 hours to obtain the chitosan aerogel.
In this embodiment, the directional chill mold comprises two parts, namely a copper base and a teflon square tube, wherein the size of the copper base is 100 × 5mm, the thickness of the teflon square tube is 5mm, and the size of an inner cavity is 50 × 50 mm.
S4: and carbonizing the chitosan aerogel prepared in the step S3 in an argon atmosphere, controlling the heating rate to be 2 ℃/min, heating to 680 ℃ from room temperature, preserving heat for 1h, and naturally cooling to room temperature in the argon atmosphere to obtain the chitosan-based nitrogen-doped carbon aerogel wave-absorbing material.
As shown in fig. 1, an XPS total spectrum of the chitosan-based nitrogen-doped carbon aerogel wave-absorbing material is obtained. As can be seen from the figure, the wave-absorbing material mainly comprises C, N, O elements, wherein the existence of a nitrogen element diffraction peak indicates that the preparation method successfully realizes in-situ nitrogen doping under the condition of not using an externally doped nitrogen source.
As shown in fig. 2, is an SEM picture of the prepared chitosan-based nitrogen-doped carbon aerogel wave-absorbing material. As can be seen from the figure, the wave-absorbing material has a micron-scale cellular structure, which shows that the preparation method successfully realizes the construction of a three-dimensional network structure in a sample through a freeze casting-freeze drying process.
As shown in fig. 3, the reflection loss curve of the prepared chitosan-based nitrogen-doped carbon aerogel wave-absorbing material under different thickness conditions is shown. As can be seen from the figure, the wave-absorbing material has excellent electromagnetic wave absorption performance, the reflection loss value reaches-68.8 dB when the thickness is 5.1mm, and the effective absorption bandwidth covers the whole X wave band.
Example 2
This example uses the same preparation method as example 1, but differs from example 1 in that: in step S2, the amount of chitosan added was 2g, and the rest was the same as in example 1, specifically as follows:
s1: 1mL of glacial acetic acid is measured and added into 100mL of deionized water to prepare a dilute acetic acid solvent with the concentration of 1% (v/v).
S2: weighing 2g of chitosan, adding the chitosan into all the dilute acetic acid solvent prepared in S1, and mechanically stirring at the rotating speed of 400r/S at room temperature until the chitosan is fully dissolved to obtain a chitosan precursor solution.
S3: and (4) pouring 16g of the chitosan precursor solution prepared in the step S2 into an oriented cold casting mold for freezing casting, wherein the used cold source is a low-temperature test box, the cold casting temperature is-60 ℃, and the cold casting time is 3 hours. And transferring the mixture to a freeze drier after the cold casting is finished, and drying the mixture at a low temperature of-84 ℃ for 24 hours to obtain the chitosan aerogel.
S4: and carbonizing the chitosan aerogel prepared in the step S3 in an argon atmosphere, controlling the heating rate to be 2 ℃/min, heating to 680 ℃ from room temperature, preserving heat for 1h, and naturally cooling to room temperature in the argon atmosphere to obtain the chitosan-based nitrogen-doped carbon aerogel wave-absorbing material.
As a result, the wave-absorbing material prepared in this example is within the range of effective performance, but the chitosan precursor concentration is lower than that in example 1, and the sample obtained in this example has a reduced overall wave-absorbing agent content and a reduced structural macroscopic order degree.
Example 3
This example uses the same preparation method as example 1, but differs from example 1 in that: in step S3, the cooling source used is liquid nitrogen, the chill casting temperature is-196 ℃, and the other steps are the same as in example 1, specifically as follows:
s1: 1mL of glacial acetic acid is measured and added into 100mL of deionized water to prepare a dilute acetic acid solvent with the concentration of 1% (v/v).
S2: and 3g of chitosan is weighed and added into all the diluted acetic acid solvent prepared in the S1, and the mixture is mechanically stirred at the rotating speed of 400r/S at room temperature until the chitosan is fully dissolved, so that a chitosan precursor solution is obtained.
S3: and (4) pouring 16g of the chitosan precursor solution prepared in the step S2 into an oriented cold casting mold for freezing casting, wherein the used cold source is liquid nitrogen, the cold casting temperature is-196 ℃, and the cold casting time is 3 h. And transferring the mixture to a freeze drier after the cold casting is finished, and drying the mixture at a low temperature of-84 ℃ for 24 hours to obtain the chitosan aerogel.
S4: and carbonizing the chitosan aerogel prepared in the step S3 in an argon atmosphere, controlling the heating rate to be 2 ℃/min, heating to 680 ℃ from room temperature, preserving heat for 1h, and naturally cooling to room temperature in the argon atmosphere to obtain the chitosan-based nitrogen-doped carbon aerogel wave-absorbing material.
As a result, it is found that the wave-absorbing material prepared in this embodiment is also within the range of effective performance, but compared with example 1, the pore size of the micron-scale pore channel structure in the sample obtained in this embodiment is reduced.
Example 4
This example uses the same preparation method as example 1, but differs from example 1 in that: in step S4, the carbonization temperature was 700 ℃.
S1: 1mL of glacial acetic acid is measured and added into 100mL of deionized water to prepare a dilute acetic acid solvent with the concentration of 1% (v/v).
S2: and 3g of chitosan is weighed and added into all the diluted acetic acid solvent prepared in the S1, and the mixture is mechanically stirred at the rotating speed of 400r/S at room temperature until the chitosan is fully dissolved, so that a chitosan precursor solution is obtained.
S3: and (4) pouring 16g of the chitosan precursor solution prepared in the step S2 into an oriented cold casting mold for freezing casting, wherein the used cold source is a low-temperature test box, the cold casting temperature is-60 ℃, and the cold casting time is 3 hours. And transferring the mixture to a freeze drier after the cold casting is finished, and drying the mixture at a low temperature of-84 ℃ for 24 hours to obtain the chitosan aerogel.
S4: and carbonizing the chitosan aerogel prepared in the step S3 in an argon atmosphere, controlling the heating rate to be 2 ℃/min, heating from the room temperature to 700 ℃, preserving the heat for 1h, and naturally cooling to the room temperature in the argon atmosphere to obtain the chitosan-based nitrogen-doped carbon aerogel wave-absorbing material.
As a result, the wave-absorbing material prepared in this example is within the range of effective performance, but compared with example 1, the sample obtained in this example has an improved carbonization degree, and more nano graphite crystallite structures exist in the sample.
The wave-absorbing properties of the chitosan-based nitrogen-doped carbon aerogels prepared in example 1, example 2, example 3 and example 4 were investigated by comparatively analyzing the reflection loss curves of the chitosan-based nitrogen-doped carbon aerogels prepared in example 1, example 2, example 3 and example 4. As shown in fig. 4, compared with examples 2, 3, and 4, the wave-absorbing performance of the chitosan-based nitrogen-doped carbon aerogel prepared in example 1 is significantly improved, which indicates that the multi-scale structure control has an important meaning for the optimization of the wave-absorbing performance of the material.
Therefore, the chitosan-based nitrogen-doped carbon aerogel prepared by the invention has the performance characteristics of low density, high reflection loss and wide band absorption, is simple in preparation method and controllable in structure, meets the requirements of practical application, and has great application potential in the technical field of microwave absorption materials.
The above-described embodiments are merely preferred embodiments of the present invention, which should not be construed as limiting the invention. Various changes and modifications may be made by one of ordinary skill in the pertinent art without departing from the spirit and scope of the present invention. Therefore, the technical scheme obtained by adopting the mode of equivalent replacement or equivalent transformation is within the protection scope of the invention.
Claims (10)
1. A preparation method of a chitosan-based nitrogen-doped carbon aerogel wave-absorbing material is characterized by comprising the following steps:
s1: adding chitosan into a dilute acetic acid solvent, and stirring until the chitosan is fully dissolved to obtain a chitosan precursor solution;
s2: performing freeze casting on the chitosan precursor solution, and then performing freeze drying to obtain chitosan aerogel;
s3: and carbonizing the chitosan aerogel in an inert atmosphere, and cooling to obtain the chitosan-based nitrogen-doped carbon aerogel wave-absorbing material.
2. The method for preparing a chitosan-based nitrogen-doped carbon aerogel wave-absorbing material as claimed in claim 1, wherein in S1, the concentration of dilute acetic acid solvent is 1% v/v, and glacial acetic acid is added into water to prepare the chitosan-based nitrogen-doped carbon aerogel wave-absorbing material.
3. The preparation method of the chitosan-based nitrogen-doped carbon aerogel wave-absorbing material according to claim 1, wherein the addition amount of chitosan in S1 is 1-4 g.
4. The method for preparing a chitosan-based nitrogen-doped carbon aerogel wave-absorbing material according to claim 1, wherein in S1, the stirring speed is 400 r/S.
5. The method for preparing a chitosan-based nitrogen-doped carbon aerogel wave-absorbing material according to claim 1, wherein in S2, the chitosan precursor solution is poured into an oriented chill casting mold for freeze casting; the directional chill casting mold comprises a copper base for realizing temperature conduction between a chitosan precursor solution and a cold source and a polytetrafluoroethylene square tube for containing the chitosan precursor solution.
6. The preparation method of the chitosan-based nitrogen-doped carbon aerogel wave-absorbing material as claimed in claim 1, wherein in S2, the temperature of freeze casting is-20 ℃ to-196 ℃, and the time is 3 h.
7. The method for preparing a chitosan-based nitrogen-doped carbon aerogel wave-absorbing material according to claim 1, wherein in the step S2, the freeze drying is performed in a freeze dryer at-84 ℃, and the freeze drying time is 24 h.
8. The method for preparing a chitosan-based nitrogen-doped carbon aerogel wave-absorbing material according to claim 1, wherein in S3, the carbonization treatment is specifically as follows:
heating from room temperature to 650-700 ℃ at the heating rate of 2 ℃/min, preserving heat for 1h, and then naturally cooling to room temperature.
9. The method for preparing a chitosan-based nitrogen-doped carbon aerogel wave-absorbing material as claimed in claim 1, wherein the amount of chitosan added in S1 is 3g, the cold source used in the freeze casting in S2 is a low-temperature test box, the cold casting temperature is-60 ℃, and the temperature is raised to 680 ℃ during the carbonization treatment in S3.
10. The chitosan-based nitrogen-doped carbon aerogel wave-absorbing material prepared by the preparation method according to any one of claims 1 to 9.
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