CN111704125A - WS (WS)2Preparation method of (N-styrene-butadiene-styrene)/CNTs (carbon nanotubes) hybrid wave-absorbing material - Google Patents
WS (WS)2Preparation method of (N-styrene-butadiene-styrene)/CNTs (carbon nanotubes) hybrid wave-absorbing material Download PDFInfo
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Abstract
The invention discloses a WS with electromagnetic wave absorption performance2-NS/CNTs hybrid material preparation method. In the invention, WS is successfully synthesized by adopting a one-step hydrothermal method2-NS/CNTs hybrid material, WS2NS grows uniformly on the 3D scaffold built from CNTs. The minimum reflection loss can reach-51.6 dB at 14.8GHz, the matching thickness is 1.95mm, and the maximum effective absorption bandwidth can reach 5.4 GHz. The invention improves a single WS2The problems of poor wave absorbing performance of NS and poor dispersity of CNTs. WS obtained by the present invention2The preparation method of the-NS/CNTs hybrid material is simple, low in cost, thin in thickness, wide in absorption band and excellent in electromagnetic wave absorption performance, and is mainly appliedIn the field of electromagnetic wave absorption.
Description
Technical Field
The invention belongs to the field of inorganic nano wave-absorbing materials, and particularly relates to a tungsten disulfide nanosheet (WS) with electromagnetic wave absorption performance2-NS)/Carbon Nanotubes (CNTs) hybrid materials (WS)2-NS/CNTs). Novel wave-absorbing material isThe technology requires strong absorption, light weight, wide frequency, infrared microwave absorption compatibility and good comprehensive performance. The development of inorganic nano composite wave-absorbing functional material by utilizing the special electromagnetic property of nano material and the excellent property of inorganic hybrid is an effective way for realizing the technical requirement.
Background
With the development of modern science and technology and the increasing improvement of the living standard of people, household appliances such as mobile phones, televisions, computers, microwave ovens and the like are more and more popular, and the environment pollution is more and more serious while the convenience is brought to the life of people. At airports, flights are delayed and cannot take off due to electromagnetic interference; in hospitals, mobile phones often interfere with the normal operation of various medical electronic instruments; more seriously, the ubiquitous electromagnetic wave can cause the human body to generate heat effect, non-heat effect, cumulative effect and the like, the human body is radiated by the electromagnetic wave again before the human body has self-repair, and the accumulated damage degree can cause permanent diseases, thereby affecting the normal work of body organs and even threatening the life. In the face of severe electromagnetic wave pollution, people are dedicated to research electromagnetic wave absorbing materials with strong absorption, wide absorption bandwidth, thin thickness and light weight.
WS2-NS is a typical Transition Metal Sulfide (TMDs) with a layered structure similar to graphite, belonging to the hexagonal system. The sandwich-like structure is provided, the sulfur atoms are connected with each other by strong covalent bonds, the bonding force between layers is Van der Waals force, the bonding force is weak, and the slippage between the layers is easy to occur to form a slippage surface. WS2The unique properties of-NS have been studied in different fields of catalytic hydrogen release, lithium batteries, energy storage, photocatalysis, thermoelectrics, etc. Notably, also for WS2The NS-based electromagnetic wave absorber was studied. In previous work, WS-based constructs were constructed by hybridization with rGO and NiO2-heterostructures of NS. Due to the higher specific surface area, the electromagnetic wave loss and the absorption performance of the composite material are greatly improved. And a single WS2Compared with NS, the heterostructure has more defects, more remarkable dipole polarization and interface polarization, easier charge conduction and better electromagnetic wave absorption performanceGood results are obtained.
The nanocarbon-based materials, particularly graphene and CNTs, are important absorbing or shielding materials due to their advantages of low density, high specific surface area, large aspect ratio, chemical stability, and the like. CNTs, a typical nanomaterial, have excellent electrical conductivity. The surface of the CNTs after acidification treatment has a plurality of oxygen-containing functional groups (-COOH, -OH) and defects, which are beneficial to the coupling of the CNTs with other substances so as to generate strong dielectric loss. However, the poor dispersibility of CNTs powders in matrix materials has led to their limited use in various technical fields. In general, well-dispersed CNTs can be used to prepare hybrid absorbent materials with excellent properties. It is therefore presumed that CNTs can be used as an essential component for the preparation of an electromagnetic wave absorbing material.
The invention provides a WS with electromagnetic wave absorption performance2The preparation method of the (E) -NS/CNTs hybrid material adopts WCl6Thioacetamide and CNTs as starting materials, by a one-step hydrothermal process at a suitable temperature2-NS/CNTs hybrid material. The method improves single WS2The CNTs have poor wave-absorbing performance and the CNTs have poor dispersibility, a novel electromagnetic wave absorbent is synthesized by a simple preparation method, and a new way is opened up for developing wave-absorbing materials with light weight, thin thickness, wider absorption band and excellent electromagnetic wave absorption performance.
Disclosure of Invention
The invention relates to a WS with electromagnetic wave absorption performance2-NS/CNTs hybrid material preparation method, for single WS2The problem of poor wave absorbing performance of NS, and a proper amount of CNTs is introduced into a system to improve the conductive performance and the dielectric performance of a wave absorbing agent, so that WS is enabled to have poor wave absorbing performance2the-NS/CNTs hybrid material has excellent electromagnetic wave absorption performance. The invention uses WCl6Thioacetamide and CNTs are used as raw materials, the CNTs are pretreated by acidification, and then the WS is prepared by the steps of stirring, heating, centrifuging, washing, drying and the like2-NS/CNTs hybrid material.
The invention relates to a WS with electromagnetic wave absorption performance2-NS/CNTs hybrid material preparation method, characterized by: firstly, the methodAnd carrying out ultrasonic treatment on the acidified CNTs for 30min to uniformly disperse the CNTs in deionized water. Subsequently, a dispersion containing 0.94% by weight of CNTs was added to a reactor (75mL) with 1.0g of WCl6And 2.0g of thioacetamide (WS)2The molar ratio of NS to CNTs is 9: 1-11: 1), and then 60mL of deionized water is added into the mixture. Stirring the mixed solution for 30min, transferring the mixed solution into a reactor, and heating the mixed solution at 205-215 ℃ for 24 h. After the reaction is finished, after the reactor is gradually cooled to room temperature, black precipitates are extracted by a centrifugal method and washed for 2 times by deionized water and absolute ethyl alcohol. Finally, it was dried in vacuum at 60 ℃ for 20h to give a black solid powder as WS2-NS/CNTs hybrid material. The method has the advantage of providing a simple one-step hydrothermal method for preparing the WS with good dispersity and appearance2The NS/CNTs hybrid material has excellent wave-absorbing performance, and provides a new idea for the research and development of subsequent wave-absorbing materials.
The invention designs the following technical scheme for realizing the aim of the invention:
(1) a certain amount of CNTs is weighed into a 75mL reactor, and concentrated sulfuric acid and concentrated nitric acid are added thereto in a ratio of 3:1 to acidify the CNTs.
(2) The reactor was set to 80 ℃ with constant stirring for 2 h.
(3) After the reactor was cooled to room temperature, the acidified CNTs were repeatedly washed with deionized water until the pH showed neutral.
(4) Dispersing CNTs in deionized water to prepare 0.94 wt% of dispersion liquid, and storing the dispersion liquid in a reagent bottle;
(5) and (3) placing the reagent bottle filled with the acidified CNTs in an ultrasonic device for ultrasonic treatment for 30min to uniformly disperse the reagent bottle in deionized water.
(6) Weighing 1.0g of WCl6And 2.0g of thioacetamide were added to the reactor, and then 0.5g of CNTs dispersion liquid and 60mL of deionized water were added thereto.
(7) The mixed solution was stirred for 30min to be thoroughly mixed.
(8) The reactor temperature was set to 210 ℃ and the reaction was continued with stirring for 24 h.
(9) After the reactor was gradually cooled to room temperature, the black precipitate was extracted by centrifugation and washed 2 times with deionized water and absolute ethanol.
(10) Drying the collected black precipitate in a vacuum drying oven at 60 deg.C for 20h to obtain black solid powder WS2-NS/CNTs hybrid material.
The invention relates to a WS with electromagnetic wave absorption performance2The preparation method of the-NS/CNTs hybrid material has the advantages that: the raw materials selected by the invention are universal and have low price, and the use amount of the raw materials in the experimental process is small; the CNTs can be pretreated by acidification, so that the dispersibility of the CNTs can be improved; the raw materials are simple in proportion, the electromagnetic wave-absorbing performance of the hybrid material can be regulated and controlled by controlling the using amount of the CNTs, and the granularity and the morphology of the product are controlled. The method adopts a one-step hydrothermal method, is simple and convenient to operate, has no other byproducts, and is green and environment-friendly. The hybrid material prepared by the invention has the advantages of light weight, thin thickness, wider absorption band and excellent electromagnetic wave absorption performance.
Drawings
FIG. 1: WS in the invention2TEM image of the NS/CNTs hybrid material sample S1.
FIG. 2: WS under 2-18 GHz2The NS/CNTs hybrid material sample S1 corresponds to reflection loss values of different thicknesses.
Detailed Description
Example 1
(1) A certain amount of CNTs is weighed into a 75mL reactor, and concentrated sulfuric acid and concentrated nitric acid are added thereto in a ratio of 3:1 to acidify the CNTs.
(2) The reactor was set to 80 ℃ with constant stirring for 2 h.
(3) After the reactor was cooled to room temperature, the acidified CNTs were repeatedly washed with deionized water until the pH showed neutral.
(4) CNTs are dispersed in deionized water and prepared into 0.94 wt% of dispersion liquid to be stored in a reagent bottle.
(5) And (3) placing the reagent bottle filled with the acidified CNTs in an ultrasonic device for ultrasonic treatment for 30min to uniformly disperse the reagent bottle in deionized water.
(6) Weighing 1.0g of WCl6And 2.0g of thioacetamide were added to the reactor, and then 0.5g of CNTs dispersion liquid and 60mL of deionized water were added thereto.
(7) The mixed solution was stirred for 30min to be thoroughly mixed.
(8) The reactor temperature was set to 210 ℃ and the reaction was continued with stirring for 24 h.
(9) After the reactor was gradually cooled to room temperature, the black precipitate was extracted by centrifugation and washed 2 times with deionized water and absolute ethanol.
(10) Drying the collected black precipitate in a vacuum drying oven at 60 deg.C for 20h to obtain black solid powder WS2-NS/CNTs hybrid material, WS2-NS to CNTs molar ratio is about 10: 1. For simplicity, the product is represented as sample S1.
As shown in FIG. 1, WS2-NS/CNTs hybrid materials from large amounts of WS2-NS and CNTs of different lengths. WS2The NS is in a lamellar disordered petal structure, and the acidified CNTs are mutually crossed to form a 3D framework. The product is distributed uniformly in the system, and a large amount of WS2NS is stacked in clusters with a radius of about 500 nm.
FIG. 2 shows the WS at 2-18 GHz2The integrated thickness of the NS/CNTs hybrid material is about 1.70-2.15 mm; at 14.8GHz, WS2The wave absorbing performance of the-NS/CNTs hybrid material can reach-51.6 dB, the matching thickness is only 1.95mm, and the effective bandwidth is about 5.4GHz
As shown by curve ⑥.
Example 2
(1) A certain amount of CNTs is weighed into a 75mL reactor, and concentrated sulfuric acid and concentrated nitric acid are added thereto in a ratio of 3:1 to acidify the CNTs.
(2) The reactor was set to 80 ℃ with constant stirring for 2 h.
(3) After the reactor was cooled to room temperature, the acidified CNTs were repeatedly washed with deionized water until the pH showed neutral.
(4) CNTs are dispersed in deionized water and prepared into 0.94 wt% of dispersion liquid to be stored in a reagent bottle.
(5) And (3) placing the reagent bottle filled with the acidified CNTs in an ultrasonic device for ultrasonic treatment for 30min to uniformly disperse the reagent bottle in deionized water.
(6) Weighing 1.0g of WCl6And 2.0g of thioacetamide were added to the reactor, and then 0.6g of CNTs dispersion liquid and 60mL of deionized water were added thereto.
(7) The mixed solution was stirred for 30min to be thoroughly mixed.
(8) The reactor temperature was set to 205 ℃ and the reaction was continued with stirring for 24 h.
(9) After the reactor was gradually cooled to room temperature, the black precipitate was extracted by centrifugation and washed 2 times with deionized water and absolute ethanol.
(10) Drying the collected black precipitate in a vacuum drying oven at 60 deg.C for 20h to obtain black solid powder WS2-NS/CNTs hybrid material, WS2The molar ratio of-NS to CNTs is about 9: 1. For simplicity, the product is represented as sample S2.
Example 3
(1) A certain amount of CNTs is weighed into a 75mL reactor, and concentrated sulfuric acid and concentrated nitric acid are added thereto in a ratio of 3:1 to acidify the CNTs.
(2) The reactor was set to 80 ℃ with constant stirring for 2 h.
(3) After the reactor was cooled to room temperature, the acidified CNTs were repeatedly washed with deionized water until the pH showed neutral.
(4) CNTs are dispersed in deionized water and prepared into 0.94 wt% of dispersion liquid to be stored in a reagent bottle.
(5) And (3) placing the reagent bottle filled with the acidified CNTs in an ultrasonic device for ultrasonic treatment for 30min to uniformly disperse the reagent bottle in deionized water.
(6) Weighing 1.0g of WCl6And 2.0g of thioacetamide were added to the reactor, and then 0.4g of CNTs dispersion liquid and 60mL of deionized water were added thereto.
(7) The mixed solution was stirred for 30min to be thoroughly mixed.
(8) The reactor temperature was set to 215 ℃ and the reaction was continued with stirring for 24 h.
(9) After the reactor is gradually cooled to room temperature, black precipitate is extracted by a centrifugal method and repeatedly washed by deionized water and absolute ethyl alcohol.
(10) Drying the collected black precipitate in a vacuum drying oven at 60 deg.C for 20h to obtain black solid powder WS2-NS/CNTs hybrid material, WS2The molar ratio of-NS to CNTs is about 11: 1. For simplicity, the product is represented as sample S3.
Claims (2)
1. WS with electromagnetic wave absorption performance2-method for the preparation of a hybrid NS/CNTs material, characterized in that it is carried out according to the following experimental method:
firstly, the acidified CNTs are subjected to ultrasonic treatment for 30min, so that the CNTs are uniformly dispersed in deionized water. The dispersion containing 0.94% by weight of CNTs was added to a hydrothermal reactor having a capacity of 75mL, and 1.0g of WCl6And 2.0g of thioacetamide, and then 60mL of deionized water was added thereto. Stirring the mixed solution for 30min, transferring the mixed solution into a hydrothermal reactor, and heating the mixed solution at 205-215 ℃ for 24 h; naturally cooling the hydrothermal reactor to room temperature, opening the hydrothermal reactor, taking out reaction liquid, and separating by a centrifugal method to obtain black precipitate; the black precipitate was washed with deionized water and absolute ethanol 2 times and centrifuged. Finally, the centrifuged precipitate was dried in vacuum at 60 ℃ for 20 hours to obtain a black solid powder WS2-NS/CNTs hybrid material.
2. WCl of claim 16WS prepared by hydrothermal reaction of thioacetamide2The mol ratio of-NS to acidified CNTs is controlled to be 9: 1-11: 1.
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| CN112919544A (en) * | 2021-01-25 | 2021-06-08 | 齐齐哈尔大学 | Low-frequency-band electromagnetic wave absorption WS2/TiO2Method for preparing hybrid material |
| CN114804218A (en) * | 2022-05-19 | 2022-07-29 | 郑州大学 | Microwave absorbing material with multilevel heterostructure and preparation method thereof |
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