CN114684805A - Carbon aerogel composite material and preparation method thereof - Google Patents
Carbon aerogel composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a carbon aerogel composite material and a preparation method thereof, wherein the composite material takes castor-based nano-cellulose carbon aerogel as a matrix and loads VS2The size of the nano flower ball-shaped particles is 200-1000nm, and VS is added in the preparation method2Dispersing the nano flower balls in castor-based nano cellulose colloidal solution, freeze-drying and calcining at high temperature to prepare VS2@ castor-based nanocellulose carbon aerogel composite. The composite material prepared by the invention not only solves the problem of single metal sulfide VS2Poor conductivity and insufficient wave-absorbing capacity, which can not be applied to wave-absorbing materials, and single carbon material lacks of the synergistic effect of multiple effective electromagnetic wave loss mechanisms, which can not meet the application requirements, and also realizes the impedance matching optimization within the frequency range of 2-18GHz, and shows thatThe material has the advantages of enhancing the attenuation capability of electromagnetic waves and being an ideal choice for novel light-weight high-efficiency microwave absorbing materials.
Description
Technical Field
The invention relates to a microwave absorbing material and a preparation method thereof, in particular to a carbon aerogel composite material and a preparation method thereof.
Background
The existing microwave absorbing material has the problems of weak absorbing capacity, single absorbing frequency band, large density, single structure and the like, and cannot meet the comprehensive requirements of the microwave absorbing material in a new period. Therefore, the development of microwave absorbing materials with high efficiency and excellent performance is urgent.
The metal sulfide is a novel microwave absorbing material, has a large specific surface area, a unique electronic structure and a heterogeneous structure which is easy to form and has special properties, and is proved to be an ideal low-frequency microwave absorbing material. Vanadium disulfide VS2As a transition metal sulfide, the transition metal sulfide not only retains the characteristics of the metal sulfide, but also enhances the magnetic loss and the dielectric loss due to the unique intrinsic ferromagnetism and the semiconductor property, enriches the microwave absorption mechanism, however, VS2The nano flower ball is not applied to the field of microwave absorption at present. VS2The low conductivity of the dielectric material leads to low conductive loss and influences the microwave absorption performance, so that the conductive loss can be enhanced, the conductivity of the material can be regulated and controlled by introducing other high-conductivity components, a proper dielectric constant can be obtained, the impedance matching optimization is realized, and meanwhile, the abundant interface structure is also beneficial to interface polarization consumption of electromagnetic waves.
The castor is a natural plant resource with strong adaptability and various soil qualities, and the castor-based nano-cellulose obtained by taking the castor as a raw material has wide availability. Meanwhile, the castor-based nano-cellulose has certain mechanical strength and nanoscale effect, and the castor-based nano-cellulose aerogel prepared from the castor-based nano-cellulose has high porosity and a three-dimensional pore network structure, so that the interface of the material is increased, and electromagnetic wave is favorably reflected and scattered for many times to cause electromagnetic attenuation. After carbonization, the carbon material with dielectric loss can be converted while the original porous structure is ensured, so that the carbon material is beneficial to dielectric loss and multiple reflection and scattering of electromagnetic waves, the conductivity is improved, and the conductive loss is enhanced. However, a single carbon material generally cannot meet impedance matching requirements, and needs to be compounded with other materials to improve dielectric loss and magnetic loss capabilities, and electromagnetic wave attenuation is enhanced through synergistic effects of multiple loss mechanisms.
Disclosure of Invention
The invention aims to: in order to solve the technical problems, the invention aims to provide a carbon aerogel composite material with excellent wave-absorbing performance, and the invention also provides a preparation method of the composite material.
The technical scheme is as follows: the carbon aerogel composite material comprises a castor-based nano-cellulose carbon aerogel matrix and VS2Nanospheres of the Nanoflava, said VS2The nanometer flower balls are loaded on the castor-oil plant-based nanometer cellulose carbon aerogel matrix.
The size of the nanometer flower-shaped spherical particles is 200-1000 nm.
The preparation method of the carbon aerogel composite material comprises the following steps:
(1) dissolving vanadium salt, a sulfur-containing precursor and a surfactant in a solvent, uniformly stirring, carrying out solvothermal reaction, centrifuging, washing and drying the obtained product to obtain VS2Nano flower ball;
(2) adding castor fiber into solid acid, heating for melting, pre-hydrolyzing, shearing the pre-hydrolyzed castor fiber, centrifugally washing the obtained suspension, performing ultrasonic treatment, and stirring to obtain a castor-based nano cellulose colloidal solution;
(3) VS obtained in the step (1)2Dispersing the nano flower balls in the castor-based nano cellulose colloidal solution obtained in the step (2), and calcining and cooling the product obtained after ultrasonic and freeze drying at high temperature to obtain VS2@ castor-based nanocellulose carbon aerogel composite.
Further, in the step (1), the vanadium salt is one of ammonium metavanadate or sodium metavanadate, the sulfur-containing precursor is one of thioacetamide or thiourea, the surfactant is dodecyl trimethyl ammonium bromide, and the solvent is ethylene glycol.
Further, in the step (1), the mass ratio of the vanadium salt, the sulfur-containing precursor and the surfactant is 1:1:1-1:9: 3.
Further, the stirring time in the step (1) is 2-4h, and the conditions of the solvothermal reaction are as follows: the reaction temperature is 150 ℃ and 200 ℃, and the reaction time is 10-15 h.
Further, the solid acid in the step (2) is one of succinic acid or trichloroacetic acid.
Further, the mass ratio of the castor fiber to the solid acid in the step (2) is 1:20-1: 40.
Further, VS in the step (2)2The mass ratio of the nano flower ball to the castor-based nano cellulose is 1:100-1: 300.
Further, in the step (2), the heating temperature is 100-.
Further, the temperature and the vacuum degree of the freeze drying in the step (3) are constantly-50 ℃ and 15Pa, the time is 24-48h, the calcining temperature is 600-.
The invention principle is as follows: according to the invention, the natural plant castor is used as a raw material, the prepared castor-based nanocellulose has certain mechanical strength and nanoscale effect, the high porosity and three-dimensional pore network structure of the castor-based nanocellulose aerogel is beneficial to multiple reflection of electromagnetic waves to cause electromagnetic attenuation, the original structure of the aerogel is kept after carbonization, and meanwhile, the aerogel is converted into a carbon material with higher conductivity, so that the dielectric loss and multiple reflection and scattering of the electromagnetic waves are facilitated, the conductivity is improved, and the conductive loss is enhanced. And vanadium disulfide VS2Not only the characteristics of the metal sulfide are retained, but also the magnetic loss and the dielectric loss are enhanced due to the unique intrinsic ferromagnetism and the semiconductor property, and the microwave absorption mechanism is enriched. Therefore, the invention uses castor-based nano-cellulose carbon aerogel as a matrix to load VS obtained by the solvothermal reaction of metal vanadium salt2The nano flower ball and the prepared composite material solve the problem of single metal sulfide VS2Poor conductivity results in insufficient wave-absorbing capacity and single absorptionThe wave material is lack of the synergistic effect of a plurality of effective electromagnetic wave loss mechanisms, thereby realizing good impedance matching in the frequency range of 2-18GHz and effectively enhancing the attenuation capacity of electromagnetic waves, and being an ideal choice of a novel light high-efficiency microwave absorbing material.
Has the beneficial effects that: compared with the prior art, the invention has the following remarkable advantages:
(1) the invention selects VS for the first time2As a microwave absorbing material due to VS2The unique intrinsic ferromagnetism enhances the magnetic loss, the semiconductor property optimizes the dielectric loss, the wave absorption mechanism of the system is enriched, and VS is realized simultaneously2The nanometer flower spherical structure provides rich specific surface area and enhances interface polarization;
(2) according to the invention, through a direct carbonization method, castor fibers are calcined at high temperature in inert gas, volatile components are removed, the porous structure in the castor fibers is kept in a final product, the abundant pore structures can enable electromagnetic waves to be reflected and scattered for multiple times inside pores, so that the electromagnetic waves are attenuated, a natural fiber network structure is also kept, other methods are not needed, the high-temperature calcination causes the formation of graphitized carbon, C-C bonds are connected with one another along a graphite plane to form a two-dimensional plane, the movement of a large number of free electrons along the plane greatly improves the conductivity of the carbon material, and the conductive loss is enhanced;
(3) the invention takes castor-based nano-cellulose carbon aerogel as a matrix and loads VS2The addition of the nano-ball and the carbon material makes up for VS2Poor conductivity, increased conduction loss, VS of the composite material2The addition of the carbon material improves the defect of impedance mismatch of the carbon material, the advantages of the carbon material and the carbon material are complementary, loss mechanisms such as interface polarization, multiple reflection and the like are added, and the wave-absorbing performance of the composite material is further improved; compared with the traditional wave-absorbing material, the prepared composite material has the advantages of novel structure, small density and excellent wave-absorbing performance, and provides a certain technical reference and theoretical basis for realizing the novel wave-absorbing material with light weight, high efficiency and wide frequency;
(4) according to the invention, the carbon-based aerogel material is prepared by adopting renewable and ubiquitous castor fibers, so that the problems that expensive raw materials are needed for synthesizing carbon materials such as carbon nanotubes and graphene and a large amount of energy is consumed are solved, meanwhile, the cellulose nanofiber is extracted by adopting castor, the preparation method is simple and easy, the large-scale application is favorably realized, and the biomass castor fibers are sustainable and economic raw materials;
(5) the solid acid and the castor fiber used in the preparation process are harmless to the environment, easy to recover, reusable, free of waste liquid and green and environment-friendly, and the prepared castor-based cellulose nanofiber not only keeps the high strength and nano-size effect of cellulose, but also has good dispersion stability, surface functional groups and metal sulfide VS2The electrostatic interaction exists between the two components, so that the cellulose can be uniformly loaded on the surface of the cellulose.
Drawings
FIG. 1 is a schematic representation of VS prepared in example 2 of the present invention2SEM picture of the nanometer ball of flowers;
FIG. 2 is a schematic representation of VS prepared in example 2 of the present invention2SEM picture of @ castor-based nanocellulose carbon aerogel composite;
FIG. 3 is a chart showing VS prepared in example 2 of the present invention2The maximum reflection loss RL graph of the @ castor-oil plant based nano cellulose carbon aerogel composite material;
FIG. 4 is a chart of VS prepared in example 2 of the present invention2The effective absorption bandwidth EAB diagram of the @ castor-oil plant based nano-cellulose carbon aerogel composite material.
Detailed Description
The present invention will be further described with reference to the following specific embodiments and the accompanying drawings.
Example 1: VS according to the invention2The preparation method of the @ castor-based nano-cellulose carbon aerogel composite material comprises the following steps:
(1) sequentially dissolving 0.1g of ammonium metavanadate, 0.1g of thioacetamide and 0.1g of dodecyl trimethyl ammonium bromide in 15mL of ethylene glycol, stirring for 2 hours at the stirring speed of 300rpm, transferring the mixed solution into a hydrothermal kettle after stirring, carrying out solvothermal reaction for 10 hours at the temperature of 150 ℃, centrifuging the obtained product, washing each product by using distilled water and absolute ethyl alcohol for 3-5 times, and drying the product in vacuum at the temperature of 60 ℃ to obtain VS2Nano flower ball;
(2) adding 5g of castor into 100g of succinic acid, heating and melting for 30min at 100 ℃, fully infiltrating and pre-hydrolyzing, then adding castor cellulose obtained by pre-hydrolyzing into a shearing emulsifying machine for shearing for 30min, wherein the shearing rate is 5000rpm, adding water into the obtained suspension after centrifugal washing for ultrasonic treatment, and stirring at a high speed of 10000rpm for 4min to obtain castor carboxylated cellulose nano-fiber colloidal solution;
(3) 0.1g of VS obtained in step (1)2Dispersing the nano flower balls in 10g of castor carboxylated cellulose nano fiber colloidal solution obtained in the step (2), carrying out ultrasonic treatment for 30min, carrying out freeze drying at-50 ℃ and 15Pa for 24h, calcining the obtained product in a tubular furnace at the calcining temperature of 600 ℃, the heating rate of 3 ℃/min and the calcining time of 2h, cooling to room temperature, and taking out to obtain VS2@ castor-based nano-cellulose carbon aerogel composite material.
The microwave absorption performance of the obtained composite material is tested by a vector network analyzer, when the filler amount is 5-10 wt% and the coating thickness is 2.3-2.5mm, the optimal reflection loss of the material in an electromagnetic band of 2-18GHz reaches-30 dB to-45 dB, and the effective absorption broadband can reach 5.5-8.5 GHz.
Example 2: the VS2The preparation method of the @ castor-based nano-cellulose carbon aerogel composite material comprises the following steps:
(1) sequentially dissolving 0.1g of ammonium metavanadate, 0.3g of thiourea and 0.2g of dodecyl trimethyl ammonium bromide in 20mL of ethylene glycol, stirring for 3 hours at the stirring speed of 400rpm, transferring the mixed solution into a hydrothermal kettle after stirring, carrying out solvothermal reaction for 12 hours at 160 ℃, centrifuging the obtained product, washing each product by using distilled water and absolute ethyl alcohol for 3-5 times in a centrifugal manner, and drying the product in vacuum at 60 ℃ to obtain VS2Nano flower ball;
(2) adding 6g of castor into 150g of succinic acid, heating and melting for 45min at 120 ℃, fully infiltrating and pre-hydrolyzing, then adding castor cellulose obtained by pre-hydrolyzing into a shearing emulsifying machine for shearing for 45min, wherein the shearing rate is 7000rpm, adding water into the obtained suspension after centrifugal washing for ultrasonic treatment, and stirring at 12000rpm for 5min to obtain castor carboxylated cellulose nanofiber colloidal solution;
(3) 0.15g of VS obtained in step (1)2Dispersing the nano flower balls in 18g of castor carboxylated cellulose nano fiber colloidal solution obtained in the step (2), carrying out ultrasonic treatment for 30min, carrying out freeze drying at-50 ℃ and 15Pa for 36h, calcining the obtained product in a tubular furnace at the calcining temperature of 650 ℃, the heating rate of 4 ℃/min and the calcining time of 3h, cooling to room temperature, and taking out to obtain VS2@ castor-based nanocellulose carbon aerogel composite;
the microwave absorption performance of the obtained composite material is tested by a vector network analyzer, when the filler amount is 5-10 wt% and the coating thickness is 2.5-3.0mm, the optimal reflection loss of the material in an electromagnetic band of 2-18GHz reaches-35 to-50 dB, and the effective absorption broadband can reach 6.5-9.5 GHz.
Example 3: the VS2The preparation method of the @ castor-based nano-cellulose carbon aerogel composite material comprises the following steps:
(1) sequentially dissolving 0.2g of ammonium metavanadate, 0.6g of thioacetamide and 0.3g of dodecyl trimethyl ammonium bromide in 25mL of ethylene glycol, stirring for 2 hours at the stirring speed of 300rpm, transferring the mixed solution into a hydrothermal kettle after stirring, carrying out solvothermal reaction for 15 hours at the temperature of 150 ℃, centrifuging the obtained product, washing each product by using distilled water and absolute ethyl alcohol for 3-5 times, and drying the product in vacuum at the temperature of 60 ℃ to obtain VS2Nano flower ball;
(2) adding 8g of castor into 240g of trichloroacetic acid, heating and melting for 30min at 100 ℃, fully infiltrating and pre-hydrolyzing, then adding pre-hydrolyzed castor cellulose into a shearing emulsifying machine for shearing for 50min, wherein the shearing rate is 6000rpm, adding water into the obtained suspension after centrifugal washing for ultrasonic treatment, and stirring at 12000rpm for 5min to obtain castor carboxylated cellulose nanofiber colloidal solution;
(3) 0.2g of VS obtained in step (1)2Dispersing the nano flower balls in 40g of castor carboxylated cellulose nano fiber colloidal solution obtained in the step (2), carrying out ultrasonic treatment for 30min, carrying out freeze drying at-50 ℃ and 15Pa for 24h, calcining the obtained product in a tubular furnace at the calcining temperature of 700 ℃, the heating rate of 4 ℃/min and the calcining time of 2.5h, cooling to room temperature, and taking out to obtain VS2@ castor-based nanofiberA plain carbon aerogel composite wave-absorbing material;
the microwave absorption performance of the obtained composite material is tested by a vector network analyzer, when the filler amount is 10-15 wt% and the coating thickness is 2.5-3.4mm, the optimal reflection loss of the material in an electromagnetic band of 2-18GHz reaches-45 dB to-55 dB, and the effective absorption broadband can reach 7.5-8.0 GHz.
Example 4: the VS2The preparation method of the @ castor-based nano-cellulose carbon aerogel composite material comprises the following steps:
(1) sequentially dissolving 0.1g of sodium metavanadate, 0.9g of thiourea and 0.3g of dodecyl trimethyl ammonium bromide in 30mL of ethylene glycol, stirring for 4 hours at the stirring speed of 300rpm, transferring the mixed solution into a hydrothermal kettle after stirring, carrying out solvothermal reaction for 15 hours at the temperature of 200 ℃, centrifuging the obtained product, washing each product for 3-5 times by using distilled water and absolute ethyl alcohol in a centrifugal manner, and drying the product in vacuum at the temperature of 60 ℃ to obtain VS2Nano flower ball;
(2) adding 8g of castor into 320g of succinic acid, heating and melting for 60min at 150 ℃, fully infiltrating and pre-hydrolyzing, then adding pre-hydrolyzed castor cellulose into a shearing emulsifying machine for shearing for 50min, wherein the shearing rate is 10000rpm, adding water into the obtained suspension after centrifugal washing for ultrasonic treatment, and stirring at a high speed of 15000rpm for 6min to obtain castor carboxylated cellulose nanofiber colloidal solution;
(3) 0.2g of VS obtained in step (1)2And (3) dispersing the nano flower balls in 60g of castor carboxylated cellulose nano fiber colloidal solution obtained in the step (2), carrying out ultrasonic treatment for 30min, carrying out freeze drying at-50 ℃ and 15Pa for 24h, and then calcining the obtained product in a tubular furnace, wherein the calcining temperature is 800 ℃, the heating rate is 5 ℃/min, and the calcining time is 4 h. Cooling to room temperature and taking out to obtain VS2@ castor-based nanocellulose carbon aerogel composite;
the microwave absorption performance of the obtained composite material is tested by a vector network analyzer, when the filler amount is 15-20 wt% and the coating thickness is 3.5-4.4mm, the optimal reflection loss of the material in an electromagnetic band of 2-18GHz reaches-40 dB to-50 dB, and the effective absorption broadband can reach 4.5-5.5 GHz.
Comparative example 1: the VS2The preparation method comprises the following steps: sequentially dissolving 0.2g of sodium metavanadate, 0.8g of thioacetamide and 0.2g of dodecyl trimethyl ammonium bromide in 30mL of ethylene glycol, stirring for 2 hours at the stirring speed of 300rpm, transferring the mixed solution into a hydrothermal kettle after stirring, carrying out solvothermal reaction for 12 hours at 180 ℃, centrifuging the obtained product, washing each product by using distilled water and absolute ethyl alcohol for 3-5 times in a centrifugal manner, and drying the product in vacuum at 60 ℃ to obtain VS2Nano flower ball;
the microwave absorption performance of the obtained composite material is tested by a vector network analyzer, when the filler amount is 15-20 wt% and the coating thickness is 3.5-4.4mm, the optimal reflection loss of the material in an electromagnetic band of 2-18GHz is only-10 to-20 dB, and the effective absorption broadband can reach 1.5-2.5 GHz.
Comparative example 2: the preparation method of the castor-based nano-cellulose carbon aerogel comprises the following steps:
(1) adding 10g of castor into 350g of succinic acid, heating and melting for 30min at 150 ℃, fully infiltrating and pre-hydrolyzing, then adding pre-hydrolyzed castor cellulose into a shearing emulsifying machine for shearing for 30min, wherein the shearing rate is 5000rpm, adding water into the obtained suspension after centrifugal washing for ultrasonic treatment, and stirring at 10000rpm for 5min at a high speed to obtain castor carboxylated cellulose nanofiber colloidal solution;
(2) freezing and drying 50g of the castor carboxylated cellulose nanofiber colloidal solution obtained in the step (2) at-50 ℃ and 15Pa for 24h, calcining the obtained product in a tubular furnace at the calcining temperature of 800 ℃, at the heating rate of 5 ℃/min and for 4h, cooling to room temperature, and taking out to obtain the castor-based nano cellulose carbon aerogel;
the microwave absorption performance of the obtained composite material is tested by a vector network analyzer, when the filler amount is 20-25 wt% and the coating thickness is 3.5-4.4mm, the optimal reflection loss of the material in an electromagnetic band of 2-18GHz reaches-5 to-15 dB, and the effective absorption broadband can reach 1.0-2.0 GHz.
Claims (9)
1. A carbon aerogel composite, comprising: comprising a castor-based nanocellulose carbon aerogel matrix and VS2Nanospheres of the Nanoflava, said VS2Castor-based nano-cellulose carbon loaded with nano flower ballsOn an aerogel matrix.
2. The carbon aerogel composite of claim 1, wherein: the size of the nanometer flower-shaped spherical particles is 200-1000 nm.
3. A method of preparing the carbon aerogel composite of claim 1, characterized in that: the method comprises the following steps:
(1) dissolving vanadium salt, a sulfur-containing precursor and a surfactant in a solvent, uniformly stirring, carrying out solvothermal reaction, centrifuging, washing and drying the obtained product to obtain VS2Nano flower ball;
(2) adding castor fiber into solid acid, heating to melt and prehydrolyze, shearing the prehydrolyzed castor fiber, and centrifugally washing, ultrasonically treating and stirring the obtained suspension to obtain a castor-based nano cellulose colloidal solution;
(3) VS obtained in the step (1)2Dispersing the nano flower balls in the castor-based nano cellulose colloidal solution obtained in the step (2), and calcining and cooling the product obtained after ultrasonic and freeze drying at high temperature to obtain VS2@ castor-based nano-cellulose carbon aerogel composite material.
4. The production method according to claim 3, characterized in that: in the step (1), the vanadium salt is one of ammonium metavanadate or sodium metavanadate, and the sulfur-containing precursor is one of thioacetamide or thiourea.
5. The production method according to claim 3, characterized in that: the mass ratio of the vanadium salt to the sulfur-containing precursor in the step (1) is 1:1-1: 9.
6. The production method according to claim 3, characterized in that: and (3) in the step (2), the solid acid is one of succinic acid or trichloroacetic acid.
7. The production method according to claim 3, characterized in that: the mass ratio of the castor fiber to the solid acid in the step (2) is 1:20-1: 40.
8. The production method according to claim 3, characterized in that: VS in the step (3)2The mass ratio of the nano flower ball to the castor-based nano cellulose is 1:100-1: 300.
9. The production method according to claim 3, characterized in that: the calcination temperature in the step (3) is 600-800 ℃, and the calcination time is 2-4 h.
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