CN113912117A - Carbon bag V2O3Nano-rod composite material and preparation method and application thereof - Google Patents

Carbon bag V2O3Nano-rod composite material and preparation method and application thereof Download PDF

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CN113912117A
CN113912117A CN202111349095.4A CN202111349095A CN113912117A CN 113912117 A CN113912117 A CN 113912117A CN 202111349095 A CN202111349095 A CN 202111349095A CN 113912117 A CN113912117 A CN 113912117A
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composite material
carbon
coated
nano
rod
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谢阿明
陈佑剑
焦颖芝
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Shaoxing Daopu New Material Technology Co ltd
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Shaoxing Daopu New Material Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G31/00—Compounds of vanadium
    • C01G31/02—Oxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K9/00—Screening of apparatus or components against electric or magnetic fields
    • H05K9/0073—Shielding materials
    • H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • 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
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties

Abstract

The invention belongs to the field of material preparation, and particularly relates to a carbon-coated V2O3The nano-rod composite material takes pyrrole as a carbon source and V2O5Powder is a vanadium source, and V is subjected to reduction and carbon-coated reduction in a hydrothermal coating system in sequence2O5Reduction to V2O3Also provides a preparation method and application thereof in the field of electromagnetic wave absorption. The invention fills the blank of pure V-shaped oxide in the field of electromagnetic wave absorption, and the carbon layer is used for coating V2O3Effectively improving the environmental stabilityThe instability of the suboxide is avoided. Meanwhile, the material shows excellent electromagnetic wave absorption performance in a low-thickness system.

Description

Carbon bag V2O3Nano-rod composite material and preparation method and application thereof
Technical Field
The invention belongs to the field of material preparation, and particularly relates to a carbon-coated V2O3A nano-rod composite material and a preparation method and application thereof.
Background
Electronic devices and related devices using electromagnetic waves as transmission media are continuously updated and widely used due to rapid development of information and technology. However, the electromagnetic radiation generated poses a serious threat to military safety and human health. To date, various advanced materials have been fully utilized to address the problems caused by harmful electromagnetic radiation. In order to provide a material with high electromagnetic wave absorption (EMA) performance, impedance matching should be considered first, which is a key parameter in determining how much electromagnetic wave energy enters the absorber. In addition, polarization loss is also an important factor for this consideration. It is well known that polarization tends to occur around heterointerfaces or structural defects where dipoles are easily formed. In this case, the electromagnetic wave will be attenuated by the dipole motion driven by the electromagnetic field. Therefore, constructing unique interfaces with efficient charge separation and fabricating polar defects is beneficial for high EMA performance.
Vanadium (V) oxide, a typical transition metal oxide, has received much attention due to its multivalency and open framework crystal structure, and has made great progress in various fields such as rechargeable zinc ion batteries, smart windows, and thermochromic smart coatings. However, in the EMA field, there are few reports on pure form V oxides.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a carbon bag V2O3The nano-rod composite material fills the blank of pure V-shaped oxide, and a carbon layer is used for coating V2O3The environment stability of the low-valence vanadium oxide is improved, the excellent electromagnetic wave absorption performance under low thickness is shown, and the material is simple and efficient to prepare and easy to produce in large quantities.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
carbon bag V2O3The preparation method of the nanorod composite material comprises the following steps:
step 1, mixing V2O5Dispersing the powder in water, and adding dilute hydrochloric acidAdjusting the pH to obtain an acidic suspension, wherein the pH is 1-2;
step 2, adding polypyrrole into the acidic suspension, stirring for 2h, reacting at constant temperature for 24h, naturally cooling to room temperature after the reaction is finished, washing and filtering by deionization, and drying at constant temperature overnight to obtain a polypyrrole-coated vanadium dioxide composite material, namely VO2@ C composite material; the polypyrrole and V2O5The mol ratio of the powder is 3:2, and the constant temperature reaction temperature is 130-200 ℃; the temperature for constant temperature overnight drying is 55 ℃;
step 3, putting the polypyrrole coated vanadium dioxide composite material into a tube furnace, and carrying out constant-temperature carbonization reaction for 2 hours in an argon atmosphere to obtain a carbon-coated V2O3Nanorod composites, i.e. V2O3@ C composite material; the temperature of the constant-temperature carbonization is 500-900 ℃, and the temperature rise speed of the constant-temperature carbonization is 3 ℃/min.
Carbon-coated V prepared according to method2O3Nanorod composites with V2O3The nano-rod is used as a wrapping core, the conductive carbon layer is used as a shell, and further, the carbon-coated V2O3 nano-rod composite material is in a twisted rod-shaped structure.
The carbon bag V2O3The nano-rod composite material is used in the field of electromagnetic wave absorption. Furthermore, the composite material still has excellent electromagnetic wave absorption performance under the condition of low thickness (1-5mm), wherein the Effective Absorption Bandwidth (EAB) is 7.21GHz when the thickness is 1.7mm, and the minimum reflection loss is-56 dB when the thickness is 2.5 mm.
From the above description, it can be seen that the present invention has the following advantages:
1. the invention fills the blank of pure V-shaped oxide in the field of electromagnetic wave absorption, and the carbon layer is used for coating V2O3The environmental stability is effectively improved, and the instability problem of the low-valence oxide is avoided.
2. The invention realizes the high valence state V in the polymerization process of pyrrole2O5The polypyrrole is utilized to be reduced to be matched with the wrapping system to reach an internal carbonization reduction system and reach V2O3Reduction of (2).
3. The invention is based on V2O3The conductivity and polarization behavior under the self-defect structure can realize the enhancement of EMA performance, the Effective Absorption Bandwidth (EAB) is 7.21GHz when the matching thickness is 1.7mm, the minimum reflection loss is-56 dB when the matching thickness is 2.5mm, and the excellent electromagnetic wave absorption performance under the low thickness is shown.
4. The method provided by the invention is simple and efficient, and is easy for mass production.
Drawings
FIG. 1 shows V in example 1 of the present invention2O5,VO2@ PPy and V2O3Transmission electron micrograph of @ C.
FIG. 2 shows V in example 1 of the present invention2O3@ C high resolution transmission electron microscopy image.
FIG. 3V in example 2 of the present invention2O5,VO2@ PPy and V2O3XRD pattern of @ C.
FIG. 4V in example 2 of the present invention2O5,VO2@ PPy and V2O3XRD pattern of @ C.
FIG. 5 VO in example 4 of the present invention2@PPy，V2O3@C，V2O3And the conductivity map of C.
FIG. 6 VO in example 5 of the present invention2@ PPy and V2O3Kore-Kore circle at @ C.
FIG. 7 shows V in example 5 of the present invention2O3The XRD pattern after 2 months of exposure to air @ C.
Detailed Description
A specific embodiment of the present invention will be described in detail with reference to fig. 1-7, but the present invention is not limited thereto.
Example 1
Will V2O5The powder (0.363g) was dispersed in water and the pH of the dispersion was adjusted to 1-2 with dilute hydrochloric acid. Pyrrole monomer (200. mu.L) was then added and stirred for 2 h. The reaction solution was transferred to a reaction vessel, heated to 130 ℃ and kept for 24 hours. When the reaction temperature is reduced to the chamberWarm, wash with deionized water, filter to obtain a dark green solid. Drying in a vacuum drying oven at 55 ℃ overnight to obtain VO2@ PPy composite. Placing the substance in a tube furnace in argon atmosphere, heating at a rate of 3 deg.C/min, and maintaining at 500 deg.C for 2h to obtain carbon-coated V2O3Nanorod composite material (V)2O3@C)。
Example 2
Will V2O5The powder (0.363g) was dispersed in water and the pH of the dispersion was adjusted to 1-2 with dilute hydrochloric acid. Pyrrole monomer (200. mu.L) was then added and stirred for 2 h. Transferring the reaction solution into a reaction kettle, heating to 150 ℃, and keeping for 24 hours. When the reaction temperature is reduced to room temperature, the mixture is washed by deionized water and filtered to obtain dark green solid. Drying in a vacuum drying oven at 55 ℃ overnight to obtain VO2@ PPy composite. Placing the substance in a tube furnace in argon atmosphere, heating at 3 deg.C/min for 2 hr at 700 deg.C to obtain carbon-coated V2O3Nanorod composite material (V)2O3@C)。
Example 3
Will V2O5The powder (0.363g) was dispersed in water and the pH of the dispersion was adjusted to 1-2 with dilute hydrochloric acid. Pyrrole monomer (200. mu.L) was then added and stirred for 2 h. Transferring the reaction solution into a reaction kettle, heating to 170 ℃, and keeping for 24 hours. When the reaction temperature is reduced to room temperature, the mixture is washed by deionized water and filtered to obtain dark green solid. Drying in a vacuum drying oven at 55 ℃ overnight to obtain VO2@ PPy composite. Placing the substance in a tube furnace in argon atmosphere, heating at a rate of 3 ℃/min, and maintaining at 800 ℃ for 2h to obtain carbon-coated V2O3Nanorod composite material (V)2O3@C)。
Example 4
Will V2O5The powder (0.363g) was dispersed in water and the pH of the dispersion was adjusted to 1-2 with dilute hydrochloric acid. Pyrrole monomer (200. mu.L) was then added and stirred for 2 h. Transferring the reaction solution into a reaction kettle, heating to 180 ℃, and keeping for 24 hours. Cooling to room temperature, washing with deionized water, and filtering to obtain the final productGreen solid. Drying in a vacuum drying oven at 55 ℃ overnight to obtain VO2@ PPy composite. Placing the substance in a tube furnace in argon atmosphere, heating at 3 deg.C/min and 900 deg.C for 2 hr to obtain carbon-coated V2O3Nanorod composite material (V)2O3@C)。
Example 5
Will V2O5The powder (0.363g) was dispersed in water and the pH of the dispersion was adjusted to 1-2 with dilute hydrochloric acid. Pyrrole monomer (200. mu.L) was then added and stirred for 2 h. Transferring the reaction solution into a reaction kettle, heating to 180 ℃, and keeping for 24 hours. When the reaction temperature is reduced to room temperature, the mixture is washed by deionized water and filtered to obtain dark green solid. Drying in a vacuum drying oven at 55 ℃ overnight to obtain VO2@ PPy composite. Placing the substance in a tube furnace in argon atmosphere, heating at 3 deg.C/min for 2 hr at 700 deg.C to obtain carbon-coated V2O3Nanorod composite material (V)2O3@C)。
Example 6
Will V2O5The powder (0.363g) was dispersed in water and the pH of the dispersion was adjusted to 1-2 with dilute hydrochloric acid. Pyrrole monomer (200. mu.L) was then added and stirred for 2 h. Transferring the reaction solution into a reaction kettle, heating to 200 ℃, and keeping for 24 hours. When the reaction temperature is reduced to room temperature, the mixture is washed by deionized water and filtered to obtain dark green solid. Drying in a vacuum drying oven at 55 ℃ overnight to obtain VO2@ PPy composite. Placing the substance in a tube furnace in argon atmosphere, heating at 3 deg.C/min for 2 hr at 700 deg.C to obtain carbon-coated V2O3Nanorod composite material (V)2O3@C)。
Performance detection
Electromagnetic parameters were tested in the 2-18GHz band using a network analyzer (VNA, N5245A, Agilent, usa). VO (vacuum vapor volume)2@PPy/V2O3The mass ratio of @ C to paraffin is 5: 5. All samples are pressed into the standard annulus by the same grinding toolin:3.04mm，Φout7.00mm) to maintain the certainty of the geometry. The thickness of all annuli was maintained at 2.5 mm. AnThe Jieren PNA software automatically outputs relevant electromagnetic parameters according to the Nicolson and Ross and Weir algorithm.
V used in example 12O5Hydrothermal product VO2@ PPy and high-temperature calcination product V2O3The transmissive mirror of @ C is presented in FIG. 1, and an irregular V can be seen2O5The nanometer material is changed into a regular nanometer belt after hydrothermal reaction with pyrrole, and is further carbonized at high temperature to be changed into a twisted nanometer rod structure. High-resolution transmission analysis was performed on the crystal, and as shown in FIG. 2, a carbon layer of 13.4nm was coated on the crystal surface. XRD spectrograms of the starting material and the product were analyzed (FIG. 3), and V was confirmed2O5Gradually reduced into VO through hydrothermal and high-temperature carbonization under the reduction action of pyrrole2And V2O3. FIG. 4 shows VO in example 32@ PPy and V2O3The wave absorbing property of @ C can be seen as being compatible with VO at low thickness2Comparison of @ PPy, V2O3@ C has a wide effective absorption width and small reflection losses. Description of V2O3@ C has excellent electromagnetic wave absorption properties. To further study the absorption mechanism, conduction loss and polarization loss are key factors for enhancing the absorption of electromagnetic waves. VO in example 42@PPy，V2O3@C，V2O3And conductivity of C as shown in FIG. 5, it can be seen that V2O3Conductivity ratio V of @ C2O3High because its surface is coated with a conductive carbon layer. Albeit V2O3The conductivity of @ C is VO-free2@ PPy is high, but V2O3@ C contains more of the Korl-Kohr circle (FIG. 6), illustrating V2O3@ C has a stronger polarization loss, resulting in a significant enhancement in its electromagnetic wave absorption properties. FIG. 7 shows V in example 52O3The XRD pattern after 2 months of exposure to air at @ C still has significant V2O3Characteristic peak of crystal, indicating carbon packet V2O3Is beneficial to the environmental stability. Carbon-coated V prepared by the invention2O3The nano-rod composite material has good stability and low thicknessHas excellent electromagnetic wave absorption performance.
It should be understood that the detailed description of the invention is merely illustrative of the invention and is not intended to limit the invention to the specific embodiments described. It will be appreciated by those skilled in the art that the present invention may be modified or substituted equally as well to achieve the same technical result; as long as the use requirements are met, the method is within the protection scope of the invention.

Claims (9)

1. Carbon bag V2O3The preparation method of the nano-rod composite material is characterized by comprising the following steps: the method comprises the following steps:
step 1, mixing V2O5Dispersing the powder into water, and adding dilute hydrochloric acid to adjust the pH value to obtain an acidic suspension;
step 2, adding polypyrrole into the acidic suspension, stirring for 2h, reacting at constant temperature for 24h, naturally cooling to room temperature after the reaction is finished, washing and filtering by deionization, and drying at constant temperature overnight to obtain a polypyrrole-coated vanadium dioxide composite material, namely VO2@ C composite material;
step 3, putting the polypyrrole coated vanadium dioxide composite material into a tube furnace, and carrying out constant-temperature carbonization reaction for 2 hours in an argon atmosphere to obtain a carbon-coated V2O3Nanorod composites, i.e. V2O3@ C composite material.
2. Carbon-coated V according to claim 12O3The preparation method of the nano-rod composite material is characterized by comprising the following steps: the pH value in the step 1 is 1-2.
3. Carbon-coated V according to claim 12O3The preparation method of the nano-rod composite material is characterized by comprising the following steps: the temperature of the constant temperature reaction in the step 2 is 130-200 ℃; the temperature for the constant temperature overnight drying was 55 ℃.
4. Carbon-coated V according to claim 12O3Method for preparing nano-rod composite material, and nano-rod composite materialIs characterized in that: the temperature of the constant temperature carbonization in the step 3 is 500-900 ℃, and the temperature rise speed of the constant temperature carbonization is 3 ℃/min.
5. A carbon coated V prepared by the method of any one of claims 1 to 42O3The nano-rod composite material is characterized in that: the material is represented by V2O3The nano-rod is used as a coating inner core, and the conductive carbon layer is used as the outer layer.
6. Carbon-coated V according to claim 52O3The nano-rod composite material is characterized in that: the carbon-coated V2O3 nanorod composite material is of a twisted rod-shaped structure.
7. Carbon-coated V according to claim 52O3The nano-rod composite material is characterized in that: the carbon bag V2O3The nano-rod composite material is used in the field of electromagnetic wave absorption.
8. Carbon-coated V according to claim 52O3The nano-rod composite material is characterized in that: the composite material still has excellent electromagnetic wave absorption performance under low thickness.
9. Carbon-coated V according to claim 82O3The nano-rod composite material is characterized in that: the low thickness is 1-5 mm.
CN202111349095.4A 2021-11-15 2021-11-15 Carbon bag V2O3Nano-rod composite material and preparation method and application thereof Pending CN113912117A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040065619A1 (en) * 2002-10-04 2004-04-08 Klabunde Kenneth J. Carbon-coated metal oxide nanoparticles
CN102517639A (en) * 2011-11-18 2012-06-27 武汉大学 Preparation method of ribbon carbon-enwrapped V2O3, VO2 and VC core-shell material
CN106025276A (en) * 2016-08-18 2016-10-12 南京航空航天大学 Carbon-coated vanadium trioxide nano material preparing method and lithium ion batteries
CN110021746A (en) * 2019-04-24 2019-07-16 青海民族大学 A kind of preparation method and lithium ion battery of carbon coating vanadium trioxide

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040065619A1 (en) * 2002-10-04 2004-04-08 Klabunde Kenneth J. Carbon-coated metal oxide nanoparticles
CN102517639A (en) * 2011-11-18 2012-06-27 武汉大学 Preparation method of ribbon carbon-enwrapped V2O3, VO2 and VC core-shell material
CN106025276A (en) * 2016-08-18 2016-10-12 南京航空航天大学 Carbon-coated vanadium trioxide nano material preparing method and lithium ion batteries
CN110021746A (en) * 2019-04-24 2019-07-16 青海民族大学 A kind of preparation method and lithium ion battery of carbon coating vanadium trioxide

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