CN112473577A - Preparation method of universal graphene aerogel with absorption performance - Google Patents
Preparation method of universal graphene aerogel with absorption performance Download PDFInfo
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- CN112473577A CN112473577A CN202011325214.8A CN202011325214A CN112473577A CN 112473577 A CN112473577 A CN 112473577A CN 202011325214 A CN202011325214 A CN 202011325214A CN 112473577 A CN112473577 A CN 112473577A
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Abstract
The invention provides a preparation method of universal graphene aerogel with absorption performance, which comprises the following steps: the method comprises the following steps: dispersing chitosan powder in acetic acid solution, stirring until the chitosan powder is completely dissolved, and marking as solution A; step two: dispersing graphite oxide and metal salt in water, and performing ultrasonic treatment until the graphite oxide and the metal salt are uniformly dispersed, wherein the solution is marked as a solution B; step three: mixing the solution A and the solution B, fully stirring and uniformly mixing; step four: transferring the mixed solution into a plastic freezing mold, starting freezing under the condition of liquid nitrogen refrigeration, after the upper surface of liquid in the plastic mold is frozen, finishing freezing, transferring the mixed solution into a freeze dryer with preset temperature until the mixed solution is completely freeze-dried to obtain dry gel; step five: and annealing the xerogel for 2h at 800 ℃ in Ar atmosphere to obtain the reduced graphene oxide aerogel of the nitrogen-doped 3D ordered pore channel embedded with the metal nanoparticles. The method has the advantages of simple required process flow, low cost and easy large-scale preparation.
Description
Technical Field
The invention relates to a preparation method of graphene aerogel, in particular to a preparation method of universal graphene aerogel with absorption performance.
Background
The rapid development of a high-frequency high-speed 5G communication technology and a high-integration, light and thin intelligent electronic product greatly facilitates the production and life of people, and simultaneously the severity of electromagnetic interference is also highlighted. Electromagnetic interference can cause negative effects such as signal interception, data loss and the like, and the performance and the normal operation of the electronic and electrical equipment are seriously influenced. The development of novel electromagnetic absorption materials is a key technology for solving the problem of electromagnetic pollution, and particularly relates to a high-performance electromagnetic absorption material which is light in weight and has excellent mechanical strength. Reduced graphene oxide is receiving attention as an electromagnetic wave absorbing material due to its low mass density, excellent chemical stability, and high specific surface area. Various 3D self-supporting reduced graphene oxide aerogels have been developed for electromagnetic wave absorption. However, the mechanical properties of the materials still need to be improved, and the practical application is limited. The invention provides a universal method for preparing nitrogen-doped reduced graphene oxide aerogel with embedded metal nanoparticles and 3D ordered pore channels and high wave absorption performance, wherein the mechanical property of the aerogel is obviously enhanced, and the application field of the aerogel can be expanded.
Disclosure of Invention
The invention aims to provide a preparation method of a universal graphene aerogel with absorption performance, which is simple and efficient to operate and suitable for mass industrial production.
The purpose of the invention is realized as follows:
a preparation method of universal graphene aerogel with absorption performance comprises the following steps:
the method comprises the following steps: dispersing chitosan powder in acetic acid solution, stirring until the chitosan powder is completely dissolved, and marking as solution A;
step two: dispersing graphite oxide and metal salt in water, and performing ultrasonic treatment until the graphite oxide and the metal salt are uniformly dispersed, wherein the solution is marked as a solution B;
step three: mixing the solution A and the solution B, fully stirring and uniformly mixing;
step four: transferring the mixed solution into a plastic freezing mold, starting freezing under the condition of liquid nitrogen refrigeration, after the upper surface of liquid in the plastic mold is frozen, finishing freezing, transferring the mixed solution into a freeze dryer with preset temperature until the mixed solution is completely freeze-dried to obtain dry gel;
step five: and annealing the xerogel for 2h at 800 ℃ in Ar atmosphere to obtain the reduced graphene oxide aerogel of the nitrogen-doped 3D ordered pore channel embedded with the metal nanoparticles.
The invention also includes such features:
and in the fourth step, the Fe metal block is placed in liquid nitrogen, after the metal is refrigerated, the plastic mould is placed on the Fe metal block, a temperature gradient from bottom to top is formed in the plastic mould, and the icicles grow along the bottom to top direction.
Compared with the prior art, the invention has the beneficial effects that:
the method has the advantages of simple required process flow, low cost and easy large-scale preparation. The reduced graphene oxide aerogel with the formed 3D ordered pore channels has the diameter of about 40 μm and the density is low (about 15mg cm)-3) And has certain compression resistance in the longitudinal direction and the transverse direction. Meanwhile, the prepared nitrogen-doped reduced graphene oxide aerogel with the 3D ordered pore channels embedded with the metal nanoparticles has good impedance matching degree in electromagnetic wave absorption and high wave absorption performance, the adding percentage content is 30%, the effective absorption bandwidth is 4.02GHz, and the minimum reflection loss is-45.02 dB.
Drawings
Fig. 1 is (a) a photograph of nitrogen-doped reduced graphene oxide aerogel with embedded metal nanoparticles and 3D ordered channels according to the present invention, (b) a photograph of low density, and (C) a photograph of compressive resistance;
fig. 2 is an XRD spectrum of the nitrogen-doped reduced graphene oxide aerogel with embedded metal nanoparticles 3D ordered channels according to the present invention;
fig. 3 is a scanning and transmission electron microscope photomicrograph of a nitrogen-doped reduced graphene oxide aerogel with embedded nanoparticles 3D ordered channels of the present invention;
fig. 4 is a wave-absorbing performance diagram of the nitrogen-doped reduced graphene oxide aerogel with the embedded metal nanoparticles and 3D ordered pore channels.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
The invention relates to a preparation method of a universal nitrogen-doped reduced graphene oxide aerogel with metal nano particles embedded in 3D ordered pore channels and electromagnetic wave absorption performance. The prepared aerogel has stronger mechanical property and good electrical conductivity, and belongs to a simple preparation method of the reduced graphene oxide aerogel with certain mechanical property.
The invention aims to provide a method for reducing graphene oxide aerogel with nitrogen-doped embedded metal nano particles 3D ordered pore channels, which is simple and efficient to operate and suitable for mass industrial production. The reduced graphene oxide aerogel with the nitrogen-doped 3D ordered pore channels embedded with the metal nanoparticles, which is prepared by the method, has good impedance matching degree in electromagnetic wave absorption and high wave-absorbing performance.
The purpose of the invention is realized as follows:
(1) a quantity of Chitosan (CS) powder was dispersed in acetic Acid (AC) solution and stirred until completely dissolved, labeled as solution a.
(2) Dispersing a certain amount of Graphite Oxide (GO) and a certain amount of metal salt in water, and performing ultrasonic treatment until the graphite oxide and the metal salt are uniformly dispersed, wherein the mark is solution B.
(3) And mixing the solution A and the solution B, fully stirring and uniformly mixing.
(4) And transferring the mixed solution into a plastic freezing mold (the Fe metal block is placed in liquid nitrogen, after the metal is refrigerated, the plastic mold is placed on the Fe metal block, a temperature gradient from bottom to top is formed in the plastic mold, and icicles grow along the bottom to top), starting freezing under the condition of refrigerating by the liquid nitrogen, after the upper surface of liquid in the plastic mold is frozen, finishing freezing, transferring to a freeze dryer with preset temperature, and completely freezing to obtain dried gel.
And annealing the xerogel for 2h at 800 ℃ in Ar atmosphere to obtain the reduced graphene oxide aerogel of the nitrogen-doped 3D ordered pore channel embedded with the metal nanoparticles.
Example 1:
(1) dissolving 200mg of CS powder and 240. mu.L of AC in 6mL of DI, and stirring for 2 hours to prepare a CS solution; 50mg GO and 0.5mmol FeCl3·6H2Dissolving O in 4mL of DI by ultrasonic to prepare a GO solution; and then mixing the CS solution and the GO solution, and stirring for 5 hours to obtain a uniform precursor.
(2) The precursor is moved into a plastic mold (35mm multiplied by 35mm), and is frozen on a frozen iron block from bottom to top through an ice template in a one-way and rapid mode until the upper surface of the solution is frozen in a self-made device (the iron block soaked in liquid nitrogen). And finally, drying for 48 hours by using a freeze dryer to obtain Fe/CG xerogel.
(3) Annealing Fe/CG xerogel at 500 ℃ for 1h and at 2 ℃ for min-1. Finally, in N2At 5 deg.C for min under atmosphere-1Next, Fe @ C/CG aerogels were prepared at 800 ℃ respectively.
Example 2:
(1) dissolving 200mg of CS powder and 240 μ L of acetic acid AC in 6mL of DI, and stirring for 2h to prepare a CS solution; 50mg GO and 0.5mmol Co (AC)2·4H2Dissolving O in 4mL of DI by ultrasonic to prepare a GO solution; and then mixing the CS solution and the GO solution, and stirring for 5 hours to obtain a uniform precursor.
(2) The precursor is moved into a plastic mold (35mm multiplied by 35mm), and is frozen on a frozen iron block from bottom to top through an ice template in a one-way and rapid mode until the upper surface of the solution is frozen in a self-made device (the iron block soaked in liquid nitrogen). And finally, drying for 48 hours by using a freeze dryer to obtain Co/CG xerogel.
(3) Annealing Co/CG xerogel at 500 ℃ for 1h and at 2 ℃ for min-1. Finally, in N2At 5 deg.C for min under atmosphere-1Next, Co @ C/CG aerogels were prepared at 800 ℃ respectively.
Example 3:
(1) dissolving 200mg of CS powder and 240 μ L of acetic acid AC in 6mL of DI, and stirring for 2h to prepare a CS solution; 50mg GO and 0.5mmol Ni (AC)2·4H2Dissolving O in 4mL of DI by ultrasonic to prepare a GO solution; and then mixing the CS solution and the GO solution, and stirring for 5 hours to obtain a uniform precursor.
(2) The precursor is moved into a plastic mold (35mm multiplied by 35mm), and is frozen on a frozen iron block from bottom to top through an ice template in a one-way and rapid mode until the upper surface of the solution is frozen in a self-made device (the iron block soaked in liquid nitrogen). Finally, drying for 48h by a freeze dryer to obtain Ni/CG xerogel.
(3) Annealing Ni/CG xerogel at 500 ℃ for 1h and at 2 ℃ for min-1. Finally, in N2At 5 deg.C for min under atmosphere-1Next, Ni @ C/CG aerogels were prepared at 800 ℃ respectively.
Claims (2)
1. A preparation method of universal graphene aerogel with absorption performance is characterized by comprising the following steps:
the method comprises the following steps: dispersing chitosan powder in acetic acid solution, stirring until the chitosan powder is completely dissolved, and marking as solution A;
step two: dispersing graphite oxide and metal salt in water, and performing ultrasonic treatment until the graphite oxide and the metal salt are uniformly dispersed, wherein the solution is marked as a solution B;
step three: mixing the solution A and the solution B, fully stirring and uniformly mixing;
step four: transferring the mixed solution into a plastic freezing mold, starting freezing under the condition of liquid nitrogen refrigeration, after the upper surface of liquid in the plastic mold is frozen, finishing freezing, transferring the mixed solution into a freeze dryer with preset temperature until the mixed solution is completely freeze-dried to obtain dry gel;
step five: and annealing the xerogel for 2h at 800 ℃ in Ar atmosphere to obtain the reduced graphene oxide aerogel of the nitrogen-doped 3D ordered pore channel embedded with the metal nanoparticles.
2. The method for preparing the universal graphene aerogel with the absorption performance as claimed in claim 1, wherein in the fourth step, the Fe metal block is placed in liquid nitrogen, after the metal is cooled, the plastic mold is placed on the Fe metal block, a temperature gradient from bottom to top is formed in the plastic mold, and the icicles grow along the bottom to top direction.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113617303A (en) * | 2021-08-27 | 2021-11-09 | 青岛科技大学 | Preparation method of chitosan/reduced graphene oxide aerogel |
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| CN113617303A (en) * | 2021-08-27 | 2021-11-09 | 青岛科技大学 | Preparation method of chitosan/reduced graphene oxide aerogel |
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