CN112429739A - Method for preparing silicon dioxide/nitrogen doped carbon nano tube with wave absorption performance - Google Patents

Method for preparing silicon dioxide/nitrogen doped carbon nano tube with wave absorption performance Download PDF

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CN112429739A
CN112429739A CN202011326913.4A CN202011326913A CN112429739A CN 112429739 A CN112429739 A CN 112429739A CN 202011326913 A CN202011326913 A CN 202011326913A CN 112429739 A CN112429739 A CN 112429739A
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coated
doped carbon
transition metal
nitrogen
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CN112429739B (en
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陈玉金
曹丰慧
朱春玲
闫峰
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Harbin Engineering University
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    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
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    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/158—Carbon nanotubes
    • C01B32/16—Preparation
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01Q—ANTENNAS, i.e. RADIO AERIALS
    • H01Q17/00—Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems
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    • H05K9/0073—Shielding materials
    • H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2202/00—Structure or properties of carbon nanotubes
    • C01B2202/20—Nanotubes characterized by their properties
    • C01B2202/34—Length
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    • C01B2202/00—Structure or properties of carbon nanotubes
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    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
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    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
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    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases

Abstract

The invention provides a method for preparing silicon dioxide/nitrogen doped carbon nano-tubes with wave absorption performance, which comprises the following steps: the method comprises the following steps: mixing SiO2Dispersing the spheres in an ethanol solution, adding transition metal nanoparticles, water and ammonia water, and carrying out ultrasonic treatment for 10 min; step two: sealing the mixture obtained in the step one in a conical flask, continuously stirring for 10h at 80 ℃, washing the precipitate with distilled water and ethanol, centrifuging and drying in a vacuum oven at 40 ℃ to obtain the SiO coated with the transition metal nanoparticles2(ii) a Step three: SiO to be coated with transition metal nanoparticles2And dicyandiamide were placed in a tube furnace, then annealed at 800 ℃ for 30min under an Ar atmosphere,and cooling to room temperature to obtain the silicon dioxide/nitrogen-doped carbon nanotube. The invention has the advantages of less required equipment, simple process flow, low cost, good impedance matching degree in electromagnetic wave absorption and high wave-absorbing performance.

Description

Method for preparing silicon dioxide/nitrogen doped carbon nano tube with wave absorption performance
Technical Field
The invention relates to a method for universally doping a silicon dioxide/embedded transition metal nano particle nitrogen into a carbon nano tube with high wave absorption performance, belonging to a method for manufacturing a carbon nano tube composite material.
Background
Carbon nanotubes are receiving attention as electromagnetic wave absorbing materials due to their low mass density, excellent mechanical and chemical stability, and high specific surface area. Various magnetic transition metal nanoparticles embedded carbon nanotubes or nitrogen-doped carbon nanotubes have also been developed for electromagnetic wave absorption. However, both the magnetic nanoparticles and the carbon nanotubes have high conductivity, and if the filling ratio and the dispersibility of the magnetic nanoparticles and the carbon nanotubes in the non-conductive matrix are not precisely controlled, the impedance matching characteristics are insufficient. The invention provides a universal method for nitrogen-doped carbon nanotubes with silicon dioxide/embedded transition metal nanoparticles and high wave absorption performance, and can expand the application field of the nitrogen-doped carbon nanotubes.
Disclosure of Invention
The invention aims to provide a method for preparing a nitrogen-doped carbon nanotube composite material, which is simple to operate, high-efficiency and suitable for mass industrial production. The silicon dioxide/nitrogen-doped carbon nano tube with embedded transition metal nano particles 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:
a method for preparing silicon dioxide/nitrogen doped carbon nanotubes with wave absorption performance comprises the following steps:
The method comprises the following steps: mixing SiO2Dispersing the spheres in an ethanol solution, adding transition metal nanoparticles, water and ammonia water, and carrying out ultrasonic treatment for 10 min;
step two: sealing the mixture obtained in the step one in a conical flask, continuously stirring for 10h at 80 ℃, washing the precipitate with distilled water and ethanol, centrifuging and drying in a vacuum oven at 40 ℃ to obtain the SiO coated with the transition metal nanoparticles2；
Step three: SiO to be coated with transition metal nanoparticles2And dicyandiamide were placed in a tube furnace, then annealed at 800 ℃ for 30min under an Ar atmosphere,and cooling to room temperature to obtain the silicon dioxide/transition metal nanoparticle embedded nitrogen-doped carbon nanotube.
The invention also includes such features:
the transition metal nanoparticles in the first step are nickel acetate hexahydrate, nickel acetate or ferric acetylacetonate;
compared with the prior art, the invention has the beneficial effects that:
the required equipment is less, the process flow is simple, and the cost is low. The carbon nanotubes are about 1.5 μm in length and about 15nm in diameter. Meanwhile, the prepared silicon dioxide/nitrogen-doped carbon nano tube with embedded transition metal nano particles has good impedance matching degree in electromagnetic wave absorption and high wave-absorbing performance. The nitrogen-doped carbon nanotube embedded with the Ni nano particles is used as a wave-absorbing material, the adding percentage content is 30%, the effective absorption bandwidth is 4.14GHz, and the minimum reflection loss is-39.58 dB.
Drawings
FIG. 1 is a scanning and transmission electron microscope photomicrograph of nitrogen doping of embedded Ni nanoparticles of the present invention;
FIG. 2 is an XRD image of an embedded transition metal nanoparticle N-doped carbon nanotube of the present invention;
FIG. 3 is a reflection loss plot of the inventive embedded transition metal nanoparticle N-doped carbon nanotube.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
The purpose of the invention is realized as follows:
(1) a certain amount of SiO2Dispersing the spheres in an ethanol solution, adding a certain amount of nickel acetate hexahydrate, water and ammonia water into the mixture, and carrying out ultrasonic treatment for 10 min;
(2) the resulting mixture was sealed in an erlenmeyer flask and stirring was continued at 80 ℃ for 10 h. Washing the precipitate several times with distilled water and ethanol, centrifuging and drying in a vacuum oven at 40 deg.C to obtain SiO coated with nickel hydroxide2；
(3) SiO coated with nickel hydroxide2And dicyandiamideAnd (3) placing the carbon nano tube in a tube furnace, annealing the carbon nano tube at 800 ℃ for 30min in Ar atmosphere, and cooling the carbon nano tube to room temperature to obtain the nitrogen-doped carbon nano tube coated with the Ni nano particles.
Example 1:
(1) 216mg of SiO with a mean diameter of 400nm2The spheres were dispersed in 72mL of an ethanol solution, and 190mg of nickel acetate, 3.6mL of water, and 2.0mL of aqueous ammonia were added to the above mixture, and subjected to sonication for 10 minutes.
(2) The resulting mixture was sealed in an erlenmeyer flask and stirring was continued at 80 ℃ for 10 h. Washing the precipitate several times with distilled water and ethanol, centrifuging and drying in a vacuum oven at 40 deg.C to obtain SiO coated with nickel hydroxide2。
(3) Coating SiO with nickel hydroxide at the interval of 2.0cm2And placing dicyandiamide in a tube furnace, then annealing at 800 ℃ for 30min at the heating rate of 5 ℃/min in the Ar atmosphere, and cooling to room temperature to obtain the nitrogen-doped carbon nano tube coated with the Ni nano particles.
Example 2:
(1) 216mg of SiO with a mean diameter of 400nm2The spheres were dispersed in 72mL of an ethanol solution, and 270.5 of iron acetylacetonate, 3.6mL of water, and 2.0mL of aqueous ammonia were added to the above mixture, and subjected to sonication for 10 minutes.
(2) The resulting mixture was sealed in an erlenmeyer flask and stirring was continued at 80 ℃ for 10 h. Washing the precipitate several times with distilled water and ethanol, centrifuging and drying in a vacuum oven at 40 deg.C to obtain SiO coated with ferric hydroxide2。
(3) Coating SiO with 2.0cm spacing and coated with ferric hydroxide2And placing dicyandiamide in a tube furnace, then annealing at 800 ℃ for 30min at the heating rate of 5 ℃/min in the Ar atmosphere, and cooling to room temperature to obtain the Fe nanoparticle-coated nitrogen-doped carbon nanotube.
Example 3:
(1) 216mg of SiO with a mean diameter of 400nm2The spheres were dispersed in 72mL of an ethanol solution, and 190mg of cobalt acetylacetonate, 3.6mL of water, and 2.0mL of aqueous ammonia were added to the above mixture, and subjected to sonication for 10 minutes.
(2) The resulting mixture was sealed in an erlenmeyer flask and stirring was continued at 80 ℃ for 10 h. Washing the precipitate several times with distilled water and ethanol, centrifuging and drying in a vacuum oven at 40 deg.C to obtain SiO coated with cobalt hydroxide2。
(3) Coating cobalt hydroxide-coated SiO with a spacing of 2.0cm2And placing dicyandiamide in a tube furnace, then annealing at 800 ℃ for 30min at the heating rate of 5 ℃/min in the Ar atmosphere, and cooling to room temperature to obtain the nitrogen-doped carbon nano tube coated with the Co nano particles.

Claims (5)

1. A method for preparing silicon dioxide/nitrogen doped carbon nano-tubes with wave absorption performance is characterized by comprising the following steps:
the method comprises the following steps: mixing SiO2Dispersing the spheres in an ethanol solution, adding transition metal nanoparticles, water and ammonia water, and carrying out ultrasonic treatment for 10 min;
step two: sealing the mixture obtained in the step one in a conical flask, continuously stirring for 10h at 80 ℃, washing the precipitate with distilled water and ethanol, centrifuging and drying in a vacuum oven at 40 ℃ to obtain the SiO coated with the transition metal nanoparticles 2；
Step three: SiO to be coated with transition metal nanoparticles2And placing dicyandiamide in a tube furnace, then annealing for 30min at 800 ℃ in Ar atmosphere, and cooling to room temperature to obtain the silicon dioxide/transition metal nanoparticle-embedded nitrogen-doped carbon nanotube.
2. The method of claim 1, wherein the transition metal nanoparticles in the first step are nickel acetate hexahydrate, nickel acetate or iron acetylacetonate.
3. The method of claim 1, comprising the steps of:
(1) 216mg of SiO with a mean diameter of 400nm2The spheres were dispersed in 72mL of ethanol solutionTo the mixture, 190mg of nickel acetate, 3.6mL of water, and 2.0mL of aqueous ammonia were added, and ultrasonic treatment was performed for 10 minutes;
(2) the resulting mixture was sealed in an erlenmeyer flask and stirring was continued at 80 ℃ for 10 h. Washing the precipitate several times with distilled water and ethanol, centrifuging and drying in a vacuum oven at 40 deg.C to obtain SiO coated with nickel hydroxide2；
(3) Coating SiO with nickel hydroxide at the interval of 2.0cm2And placing dicyandiamide in a tube furnace, then annealing at 800 ℃ for 30min at the heating rate of 5 ℃/min in the Ar atmosphere, and cooling to room temperature to obtain the nitrogen-doped carbon nano tube coated with the Ni nano particles.
4. The method of claim 1, comprising the steps of:
(1) 216mg of SiO with a mean diameter of 400nm2Dispersing the spheres in 72mL of ethanol solution, adding 270.5 parts of ferric acetylacetonate, 3.6mL of water and 2.0mL of ammonia water to the mixture, and performing ultrasonic treatment for 10 minutes;
(2) the resulting mixture was sealed in an erlenmeyer flask and stirring was continued at 80 ℃ for 10 h. Washing the precipitate several times with distilled water and ethanol, centrifuging and drying in a vacuum oven at 40 deg.C to obtain SiO coated with ferric hydroxide2；
(3) Coating SiO with 2.0cm spacing and coated with ferric hydroxide2And placing dicyandiamide in a tube furnace, then annealing at 800 ℃ for 30min at the heating rate of 5 ℃/min in the Ar atmosphere, and cooling to room temperature to obtain the Fe nanoparticle-coated nitrogen-doped carbon nanotube.
5. The method of claim 1, comprising the steps of:
(1) 216mg of SiO with a mean diameter of 400nm2Dispersing the spheres in 72mL of ethanol solution, adding 190mg of cobalt acetylacetonate, 3.6mL of water and 2.0mL of ammonia water to the mixture, and performing ultrasonic treatment for 10 minutes;
(2) The resulting mixture was sealed in an erlenmeyer flask and stirring was continued at 80 ℃ for 10 h. Washing the precipitate several times with distilled water and ethanol, centrifuging and drying in a vacuum oven at 40 deg.C to obtain SiO coated with cobalt hydroxide2；
(3) Coating cobalt hydroxide-coated SiO with a spacing of 2.0cm2And placing dicyandiamide in a tube furnace, then annealing at 800 ℃ for 30min at the heating rate of 5 ℃/min in the Ar atmosphere, and cooling to room temperature to obtain the nitrogen-doped carbon nano tube coated with the Co nano particles.
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CN113265223A (en) * 2021-05-24 2021-08-17 西北工业大学 Nitrogen-doped iron-carbon composite wave-absorbing material and preparation method and application thereof
CN113318767A (en) * 2021-06-22 2021-08-31 邯郸市赵都精细化工有限公司 Catalyst for preparing amino acid by ammoniating carbonyl acid and preparation method and application thereof
CN114641200A (en) * 2022-04-02 2022-06-17 四川农业大学 Nitrogen-doped microwave absorbing material and preparation method thereof

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113265223A (en) * 2021-05-24 2021-08-17 西北工业大学 Nitrogen-doped iron-carbon composite wave-absorbing material and preparation method and application thereof
CN113318767A (en) * 2021-06-22 2021-08-31 邯郸市赵都精细化工有限公司 Catalyst for preparing amino acid by ammoniating carbonyl acid and preparation method and application thereof
CN114641200A (en) * 2022-04-02 2022-06-17 四川农业大学 Nitrogen-doped microwave absorbing material and preparation method thereof

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