CN115332525A - Nb-shaped alloy 2 O 5 /GO/VS 2 Composite material and method for producing the same - Google Patents

Nb-shaped alloy 2 O 5 /GO/VS 2 Composite material and method for producing the same Download PDF

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CN115332525A
CN115332525A CN202211058050.6A CN202211058050A CN115332525A CN 115332525 A CN115332525 A CN 115332525A CN 202211058050 A CN202211058050 A CN 202211058050A CN 115332525 A CN115332525 A CN 115332525A
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composite material
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niobium
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黄剑锋
刘明鑫
王羽偲嘉
曹丽云
沈学涛
李嘉胤
严航
袁梦
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Shaanxi University of Science and Technology
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
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    • H—ELECTRICITY
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    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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Abstract

The invention belongs to the field of battery electrode materials, and relates to Nb 2 O 5 /GO/VS 2 Adding a niobium source into N and S doped graphene oxide solution, mixing, carrying out hydrothermal reaction, calcining a hydrothermal product to obtain N and S doped graphene niobium pentoxide composite material, adding a vanadium source and a sulfur source into the composite material, and carrying out solvothermal reaction to obtain Nb 2 O 5 /GO/VS 2 A composite material. Nb 2 O 5 Stores lithium ions through an intercalation mechanism, shows excellent structural stability, and can prevent VS 2 Dissolution of the intermediate, reducing the volume expansion accompanying the electrode reaction; VS 2 The capacity of the composite electrode material can be obviously improved; the introduction of doped graphene can improve Nb 2 O 5 The conductivity of the composite material can change the crystallization behavior of the transition metal sulfide to form a novel composite structure; and the volume expansion in the process of lithium ion intercalation and deintercalation can be relieved, the pulverization of the material is inhibited, and the circulation stability is improved.

Description

Nb-shaped steel 2 O 5 /GO/VS 2 Composite material and method for producing the same
Technical Field
The invention belongs to the field of battery electrode materials, and particularly relates to Nb 2 O 5 /GO/VS 2 Composite materials and methods for making the same.
Background
With the development of society, sustainable new energy is more and more concerned by people. Lithium ion batteries have attracted considerable attention over the past few decades as one of the most advanced rechargeable batteries. Lithium ion batteries are considered the power of the personal digital electronics revolution. As one may have noticed in everyday life, the increasing functionality of mobile electronic products requires better lithium ion batteries. Another important market expansion of lithium ion batteries is electric and hybrid vehicles, which require a new generation of lithium ion batteries, which not only have high power, high capacity, high charging rate, long life, but also require extremely high safety performance and as low cost as possible. Lithium ion batteries are very advanced in terms of weight and volumetric energy compared to other commercial rechargeable batteries. People are eager for high-power density and high-energy density power batteries, and research focuses on how to improve the specific capacity and rate capability of an electrode material. One important direction has been to develop materials that have a capacitive contribution in the battery capacity. This capacitive contribution is not only reflected in the increased capacity due to lithium ion intercalation, but more importantly in the greatly improved rate capability due to the short time response of the capacitive electrode process. Nb 2 O 5 As an embedded pseudocapacitance material, the lithium-extracting process occurs in a bulk phase, no phase change occurs,the material has short response time, is an electrode material capable of realizing quick charge and quick discharge, but has poor conductivity, can be compounded with a carbon material to provide a conductive network for the material so as to improve the conductivity, and has low battery capacity of niobium pentoxide.
Disclosure of Invention
The purpose of the present invention is to provide a Nb 2 O 5 /GO/VS 2 The composite material and the preparation method thereof solve the problem of low battery capacity of niobium pentoxide.
The invention is realized by the following technical scheme:
nb-shaped steel 2 O 5 /GO/VS 2 The preparation method of the composite material comprises the following steps:
step one, sequentially adding a nitrogen source, a sulfur source and a niobium source into graphene oxide dispersion liquid, mixing and stirring uniformly, and carrying out hydrothermal reaction to obtain a hydrothermal product;
the mass ratio of the graphene oxide to the nitrogen source to the sulfur source to the niobium source is 1: (0.1-1.2): (0.15-1.7): (2-8); the hydrothermal reaction time is 10-14h, and the hydrothermal temperature is 160-200 ℃;
step two, washing the hydrothermal product, heating to 600-700 ℃ in an inert atmosphere, and calcining to obtain N and S doped graphene niobium pentoxide black powder;
step three, adding the N-doped graphene niobium pentoxide black powder and the S-doped graphene niobium pentoxide black powder into ethanol, uniformly stirring, adding the vanadium source and the sulfur source which are the same as those in the step one under the stirring state, and carrying out a solvothermal reaction;
the mass ratio of the N and S doped graphene niobium pentoxide black powder to the vanadium source is 1: (0.8-1.2); the molar ratio of vanadium in the vanadium source to sulfur in the sulfur source is 1 (3-5);
step four, collecting the product, washing and drying to obtain the Nb 2 O 5 /GO/VS 2 A composite material.
Further, the niobium source is niobium chloride, niobium oxalate hydrate or niobium oxalate.
Further, the nitrogen source is melamine or urea.
Further, the sulfur source is one or more of thioacetamide, thiourea and cysteine.
Further, the vanadium source comprises one or more of sodium vanadate, sodium metavanadate, vanadium chloride and vanadium acetylacetonate.
Further, in the first step and the third step, the stirring time is 0.5-4h.
Further, in the third step, the solvothermal reaction time is 16-24h, and the solvothermal reaction temperature is 160-200 ℃.
Further, in the second step, the calcination time is 2-4 hours, and the heating rate is 3-10 ℃/min.
The invention also discloses Nb prepared by the preparation method 2 O 5 /GO/VS 2 Composite material of said Nb 2 O 5 /GO/VS 2 The morphology of the composite material is that Nb is distributed on three-dimensional graphene 2 O 5 Particles and VS 2 And (3) particles.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention discloses a Nb 2 O 5 /GO/VS 2 The preparation method of the composite material comprises the steps of adding a niobium source into N and S doped graphene oxide solution, uniformly mixing, carrying out hydrothermal reaction, and calcining a hydrothermal product in a tubular furnace to obtain the N and S doped graphene niobium pentoxide composite material, namely the Nb-doped niobium pentoxide composite material with good crystallization property is prepared 2 O 5 /GO/VS 2 A composite material. The method has the advantages of mild reaction conditions, easy realization, easy process control, wide raw material sources and low preparation cost. The prepared product has the advantages of single component, high purity and the like. The hydrothermal reaction time is 10-14h, and Nb with high crystal phase can be prepared at the hydrothermal temperature of 160-200 DEG C 2 O 5 . The N and S-GO has good dispersibility in the composite material, and no serious agglomeration phenomenon occurs. The graphene has a three-dimensional structure in the composite material, and is not obviously stacked, which indicates that the nitrogen-sulfur doping is favorable for constructing the three-dimensional structure of the graphene, and the Nb is dispersed on the graphene lamellar layer 2 O 5 The particles can also be effectively inhibitedStacking of graphene sheets, which is advantageous for increasing the active area of the reaction and Li + Storage sites, thereby increasing capacity.
The invention discloses a Nb 2 O 5 /GO/VS 2 Composite material of the Nb 2 O 5 /GO/VS 2 The composite material can effectively and synergistically improve the electrochemical performance. Nb 2 O 5 Stores lithium ions through an intercalation mechanism, shows excellent structural stability, and can prevent VS 2 Dissolution of the intermediate, reducing the volume expansion accompanying the electrode reaction; VS 2 The capacity of the composite electrode material can be obviously improved. The introduction of doped graphene can improve Nb 2 O 5 The conductivity of the composite material can change the crystallization behavior of the transition metal sulfide to form a novel composite structure; the volume expansion in the process of lithium ion intercalation and deintercalation can be relieved, the pulverization of the material is inhibited, the circulation stability is improved, the defects of the two can be further compensated, and the electrochemical performance is improved.
Drawings
FIG. 1a shows Nb prepared in example 1 2 O 5 /GO/VS 2 Scanning Electron Micrographs (SEM) of the composite; FIG. 1a is an SEM image at 500nm and FIG. 1b is an SEM image at 200 nm;
FIG. 2 shows Nb prepared in example 1 2 O 5 /GO/VS 2 An X-ray diffraction (XRD) spectrum of the composite;
FIG. 3 shows Nb prepared in example 1 2 O 5 /GO/VS 2 Capacity voltage curve of the composite at 0.1A/g current density.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the following detailed description is made with reference to the accompanying drawings and embodiments. It should be understood that the detailed description and specific examples, while indicating the preferred embodiment of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
The components illustrated and described in the figures and embodiments of the present invention may be arranged and designed in a wide variety of different configurations, and accordingly, the detailed description of the embodiments of the present invention provided in the figures that follow is not intended to limit the scope of the invention, as claimed, but is merely representative of a selected embodiment of the invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the figures and embodiments of the present invention, belong to the scope of protection of the present invention.
It should be noted that: the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, element, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, element, method, article, or apparatus.
The features and properties of the present invention are further described in detail below with reference to examples.
Example 1
The invention discloses a Nb 2 O 5 /GO/VS 2 The preparation method of the composite material comprises the following steps:
step one, hydrothermal reaction
Dispersing 0.1g of graphene oxide in 25ml of deionized water, carrying out ultrasonic oscillation for 4 hours, centrifuging to obtain supernatant, and uniformly dispersing the graphene oxide to obtain a graphene oxide dispersion liquid;
adding 0.12g of melamine powder into the graphene oxide dispersion liquid, and stirring at 80 ℃ until the melamine powder is completely dissolved to obtain a solution A; dissolving 0.17g of trithiocyanuric acid in 25ml of ethanol to obtain solution B; slowly adding the solution B into the solution A, stirring for 10min at 70 ℃, adding 0.4g of niobium chloride, uniformly stirring, transferring into a reaction kettle with a polytetrafluoroethylene substrate, wherein the filling ratio is 50%, and placing into a homogeneous phase reactor for hydrothermal reaction at 180 ℃/12h; repeatedly washing and filtering the hydrothermal product with water and ethanol, and freeze-drying to obtain a hydrothermal product;
step two, high-temperature calcination
And (3) carrying out heat treatment on the hydrothermal product obtained in the step one, placing the hydrothermal product in a tube furnace under the protection of argon, and heating to 650 ℃ at the heating rate of 5 ℃/min and keeping the temperature for 2h. Grinding to obtain N and S doped graphene niobium pentoxide black powder.
Step three, solvothermal reaction
Adding 0.5g of the N and S doped graphene niobium pentoxide black powder obtained in the step two into a beaker containing 50ml of ethanol, uniformly stirring, adding 0.5g of sodium metavanadate and 1.8g of thioacetamide, stirring for one hour, transferring into a reaction kettle with a polytetrafluoroethylene substrate, wherein the filling ratio is 50%, and placing the reaction kettle in a homogeneous phase reactor for solvothermal reaction at 180 ℃ for 18 hours;
step four, repeatedly washing the solvent thermal product with water and ethanol, filtering, freezing and drying to obtain a final product, namely Nb 2 O 5 /GO/VS 2 A composite material.
FIG. 1a shows Nb prepared in example 1 2 O 5 /GO/VS 2 Scanning Electron Micrographs (SEM) of the composite; FIG. 1a is an SEM image at 500nm and FIG. 1b is an SEM image at 200 nm; the three-dimensional graphene structure can be seen from an SEM picture, and the rod-shaped structure is VS 2 Nanorods of about 200nm length and spheres of Nb 2 O 5 Nanoparticles, approximately 25nm 2 And Nb 2 O 5 Uniformly and crossly mixed together and loaded on the surface of the graphene.
As shown in FIG. 2, it can be seen from the XRD pattern that it corresponds to Nb of standard cards 28-0137 2 O 5 VS for Standard cards 36-1139 2 。
FIG. 3 shows Nb prepared in example 1, as shown in FIG. 3 2 O 5 /GO/VS 2 The capacity-voltage curve of the composite at a current density of 0.1A/g, the rising curve representing the charging process and the falling curve representing the discharging process. The first charge-discharge capacity is 667mAh/g and 873mAh/g respectively, the first coulombic efficiency is 76.4%, the second coulombic efficiency is 74.2%, and in the subsequent circulation, the coulombic efficiency is approximately maintained at 99.0%.
Example 2
The invention discloses a Nb 2 O 5 /GO/VS 2 The preparation method of the composite material comprises the following steps:
step one, hydrothermal reaction
Dispersing 0.1g of graphene oxide in 25ml of deionized water, performing ultrasonic oscillation for 4 hours, centrifuging to obtain supernatant, and uniformly dispersing the graphene oxide to obtain graphene oxide dispersion liquid;
adding 0.1g of melamine powder into the graphene oxide dispersion liquid, and stirring at 80 ℃ until the melamine powder is completely dissolved to obtain a solution A;
dissolving 0.15g of trithiocyanuric acid in 25ml of ethanol to obtain solution B; slowly adding the solution B into the solution A, stirring for 10min at 70 ℃, adding 0.2g of niobium chloride, uniformly stirring, transferring into a reaction kettle with a polytetrafluoroethylene substrate, wherein the filling ratio is 45%, and placing the reaction kettle in a homogeneous phase reactor for hydrothermal reaction at 180 ℃/12h;
repeatedly washing and filtering the hydrothermal product with water and ethanol, and freeze-drying to obtain a hydrothermal product;
step two, high-temperature calcination
And (3) carrying out heat treatment on the hydrothermal product obtained in the step one, placing the hydrothermal product in a tube furnace under the protection of argon, heating to 650 ℃ at a heating rate of 5 ℃/min, keeping the temperature for 2h, and grinding to obtain N and S doped graphene niobium pentoxide black powder.
Step three, solvothermal reaction
Adding 0.3g of the N and S doped graphene niobium pentoxide black powder obtained in the second step into a beaker containing 50ml of ethanol, uniformly stirring, adding 0.3g of sodium vanadate and 1.2g of thioacetamide, stirring for one hour, transferring into a reaction kettle with a polytetrafluoroethylene substrate, wherein the filling ratio is 55%, and placing the reaction kettle in a homogeneous reactor for solvothermal reaction at 180 ℃ for 16 hours;
step four, repeatedly washing and filtering the solvent thermal product by using water and ethanol, and freeze-drying to obtain a final product, namely Nb 2 O 5 /GO/VS 2 A composite material.
Example 3
The invention discloses a Nb 2 O 5 /GO/VS 2 The preparation method of the composite material comprises the following steps:
step one, hydrothermal reaction
Dispersing 0.2g of graphene oxide in 25ml of deionized water, carrying out ultrasonic oscillation for 4 hours, centrifuging to obtain supernatant, and uniformly dispersing the graphene oxide to obtain a graphene oxide dispersion liquid;
adding 0.04g of melamine powder into the graphene oxide dispersion liquid, and stirring at 80 ℃ until the melamine powder is completely dissolved to obtain a solution A;
dissolving 0.1g of trithiocyanuric acid in 25ml of ethanol to obtain solution B; slowly adding the solution B into the solution A, stirring for 10min at 70 ℃, adding 0.4g of niobium chloride, uniformly stirring, transferring into a reaction kettle with a polytetrafluoroethylene substrate, filling the reaction kettle with the niobium chloride at a filling ratio of 45%, and placing the reaction kettle in a homogeneous phase reactor for hydrothermal reaction at 200 ℃/14h; repeatedly washing and filtering the hydrothermal product with water and ethanol, and freeze-drying to obtain a hydrothermal product;
step two, high-temperature calcination
And (3) carrying out heat treatment on the hydrothermal product obtained in the step one, placing the hydrothermal product in a tube furnace under the protection of argon, and heating to 660 ℃ at the heating rate of 6 ℃/min and keeping the temperature for 2h. Grinding to obtain the N and S doped graphene niobium pentoxide black powder.
Step three, solvothermal reaction
Adding 0.6g of the N and S doped graphene niobium pentoxide black powder obtained in the second step into a beaker containing 50ml of ethanol, uniformly stirring, adding 0.6g of sodium metavanadate and 2.0g of thioacetamide, stirring for one hour, transferring into a reaction kettle with a polytetrafluoroethylene substrate, wherein the filling ratio is 50%, and placing the reaction kettle in a homogeneous phase reactor for solvothermal reaction at 180 ℃/20h; repeatedly washing the solvent thermal product with water and ethanol, filtering, and freeze drying to obtain the final product, namely Nb 2 O 5 /GO/VS 2 A composite material.
Example 4
The invention discloses a Nb 2 O 5 /GO/VS 2 The preparation method of the composite material comprises the following steps:
step one, hydrothermal reaction
Dispersing 0.2g of graphene oxide in 25ml of deionized water, carrying out ultrasonic oscillation for 4 hours, centrifuging to obtain supernatant, and uniformly dispersing the graphene oxide to obtain a graphene oxide dispersion liquid;
adding 0.08g of melamine powder into the graphene oxide dispersion liquid, and stirring at 80 ℃ until the melamine powder is completely dissolved to obtain a solution A;
dissolving 0.14g of trithiocyanuric acid in 25ml of ethanol to obtain solution B; slowly adding the solution B into the solution A, stirring for 10min at 70 ℃, adding 0.4g of niobium chloride, uniformly stirring, transferring into a reaction kettle with a polytetrafluoroethylene substrate, wherein the filling ratio is 50%, and placing into a homogeneous phase reactor for hydrothermal reaction at 180 ℃/14h; repeatedly washing and filtering the hydrothermal product with water and ethanol, and freeze-drying to obtain a hydrothermal product;
step two, high-temperature calcination
And (3) carrying out heat treatment on the hydrothermal product obtained in the first step, placing the hydrothermal product in a tube furnace under the protection of argon, and heating to 660 ℃ at the heating rate of 6 ℃/min for heat preservation for 2h. Grinding to obtain the N and S doped graphene niobium pentoxide black powder.
Step three, solvothermal reaction
Adding 0.6g of the N and S doped graphene niobium pentoxide black powder obtained in the second step into a beaker containing 50ml of ethanol, uniformly stirring, adding 0.72g of sodium metavanadate and 2.16g of thioacetamide, stirring for one hour, transferring into a reaction kettle with a polytetrafluoroethylene substrate, wherein the filling ratio is 50%, and placing the reaction kettle in a homogeneous phase reactor for solvothermal reaction at 180 ℃/20h; repeatedly washing the solvent thermal product with water and ethanol, filtering, and freeze drying to obtain the final product, namely Nb 2 O 5 /GO/VS 2 A composite material.
Example 5
The invention discloses a Nb 2 O 5 /GO/VS 2 The preparation method of the composite material comprises the following steps:
step one, hydrothermal reaction
Dispersing 0.4g of graphene oxide in 25ml of deionized water, carrying out ultrasonic oscillation for 4 hours, centrifuging to obtain supernatant, and uniformly dispersing the graphene oxide to obtain a graphene oxide dispersion liquid;
adding 0.24g of melamine powder into the graphene oxide dispersion liquid, and stirring at 80 ℃ until the melamine powder is completely dissolved to obtain a solution A;
dissolving 0.36g of trithiocyanuric acid in 25ml of ethanol to obtain solution B; slowly adding the solution B into the solution A, stirring for 10min at 70 ℃, adding 2.4 niobium chloride, uniformly stirring, transferring into a reaction kettle with a polytetrafluoroethylene substrate, wherein the filling ratio is 50%, and placing into a homogeneous phase reactor for hydrothermal reaction at 200 ℃/14h; repeatedly washing and filtering the hydrothermal product with water and ethanol, and freeze-drying to obtain a hydrothermal product;
step two, high-temperature calcination
And (3) carrying out heat treatment on the hydrothermal product obtained in the step one, placing the hydrothermal product in a tube furnace under the protection of argon, and heating to 680 ℃ at a heating rate of 8 ℃/min and preserving heat for 4h. Grinding to obtain N and S doped graphene niobium pentoxide black powder.
Step three, solvothermal reaction
Adding 1.2g of the N-doped and S-doped graphene niobium pentoxide black powder obtained in the step two into a beaker containing 50ml of ethanol, uniformly stirring, adding 1.30g of sodium metavanadate and 5.28g of thioacetamide, stirring for one hour, transferring into a reaction kettle with a polytetrafluoroethylene substrate, wherein the filling ratio is 50%, and placing into a homogeneous reactor for solvothermal reaction at 200 ℃/22h; repeatedly washing the solvent thermal product with water and ethanol, filtering, and freeze drying to obtain the final product, namely Nb 2 O 5 /GO/VS 2 A composite material.
Example 6
The invention discloses a Nb 2 O 5 /GO/VS 2 The preparation method of the composite material comprises the following steps:
step one, hydrothermal reaction
Dispersing 0.4g of graphene oxide in 25ml of deionized water, carrying out ultrasonic oscillation for 4 hours, centrifuging to obtain supernatant, and uniformly dispersing the graphene oxide to obtain a graphene oxide dispersion liquid;
adding 0.32g of melamine powder into the graphene oxide dispersion liquid, and stirring at 80 ℃ until the melamine powder is completely dissolved to obtain a solution A;
dissolving 0.44g of trithiocyanuric acid in 25ml of ethanol to obtain solution B; slowly adding the solution B into the solution A, stirring for 10min at 70 ℃, adding 3.2g of niobium chloride, uniformly stirring, transferring into a reaction kettle with a polytetrafluoroethylene substrate, filling the reaction kettle with the niobium chloride at a filling ratio of 55%, and placing the reaction kettle in a homogeneous phase reactor for hydrothermal reaction at 200 ℃/14h; repeatedly washing and filtering the hydrothermal product with water and ethanol, and freeze-drying to obtain a hydrothermal product;
step two, high-temperature calcination
And (3) carrying out heat treatment on the hydrothermal product obtained in the step one, placing the hydrothermal product in a tube furnace under the protection of argon, and heating to 680 ℃ at a heating rate of 8 ℃/min and preserving heat for 4h. Grinding to obtain the N and S doped graphene niobium pentoxide black powder.
Step three, solvothermal reaction
Adding 1.5g of the N-S doped graphene niobium pentoxide black powder obtained in the second step into a beaker containing 50ml of ethanol, uniformly stirring, adding 1.5g of sodium metavanadate and 6.0g of thioacetamide, stirring for one hour, transferring into a reaction kettle with a polytetrafluoroethylene substrate, wherein the filling ratio is 50%, and placing the reaction kettle in a homogeneous phase reactor for solvothermal reaction at 200 ℃/22h; repeatedly washing the solvent thermal product with water and ethanol, filtering, and freeze drying to obtain the final product, i.e. Nb 2 O 5 /GO/VS 2 A composite material.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the above embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the embodiments of the invention without departing from the spirit and scope of the invention, which is to be covered by the claims.

Claims (9)

1. Nb-shaped alloy 2 O 5 /GO/VS 2 The preparation method of the composite material is characterized by comprising the following steps:
step one, sequentially adding a nitrogen source, a sulfur source and a niobium source into a graphene oxide dispersion liquid, mixing and stirring uniformly, and carrying out hydrothermal reaction to obtain a hydrothermal product;
the mass ratio of the graphene oxide to the nitrogen source to the sulfur source to the niobium source is 1: (0.1-1.2): (0.15-1.7): (2-8); the hydrothermal reaction time is 10-14h, and the hydrothermal temperature is 160-200 ℃;
step two, washing the hydrothermal product, heating to 600-700 ℃ in an inert atmosphere, and calcining to obtain N and S doped graphene niobium pentoxide black powder;
step three, adding the N-doped graphene niobium pentoxide black powder and the S-doped graphene niobium pentoxide black powder into ethanol, uniformly stirring, adding the vanadium source and the sulfur source which are the same as those in the step one under the stirring state, and carrying out a solvothermal reaction;
the mass ratio of the N-doped graphene niobium pentoxide black powder to the vanadium source is 1: (0.8-1.2); the molar ratio of vanadium in the vanadium source to sulfur in the sulfur source is 1 (3-5);
step four, collecting the product, washing and drying to obtain the Nb 2 O 5 /GO/VS 2 A composite material.
2. An Nb in accordance with claim 1 2 O 5 /GO/VS 2 The preparation method of the composite material is characterized in that the niobium source is niobium chloride, niobium oxalate hydrate or niobium oxalate.
3. An Nb in accordance with claim 1 2 O 5 /GO/VS 2 The preparation method of the composite material is characterized in that the nitrogen source is melamine or urea.
4. An Nb in accordance with claim 1 2 O 5 /GO/VS 2 The preparation method of the composite material is characterized in that the sulfur source is one or more of thioacetamide, thiourea and cysteine.
5. An Nb in accordance with claim 1 2 O 5 /GO/VS 2 The preparation method of the composite material is characterized in that the vanadium source comprises one or more of sodium vanadate, sodium metavanadate, vanadium chloride and vanadium acetylacetonate.
6. An Nb in accordance with claim 1 2 O 5 /GO/VS 2 A method for preparing a composite material is characterized in that,in the first step and the third step, the stirring time is 0.5-4h.
7. An Nb in accordance with claim 1 2 O 5 /GO/VS 2 The preparation method of the composite material is characterized in that in the third step, the solvothermal reaction time is 16-24h, and the solvothermal reaction temperature is 160-200 ℃.
8. An Nb in accordance with claim 1 2 O 5 /GO/VS 2 The preparation method of the composite material is characterized in that in the second step, the calcination time is 2-4 hours, and the heating rate is 3-10 ℃/min.
9. Nb produced by the production method according to any one of claims 1 to 8 2 O 5 /GO/VS 2 Composite material, characterized in that said Nb 2 O 5 /GO/VS 2 The morphology of the composite material is that Nb is distributed on three-dimensional graphene 2 O 5 Particles and VS 2 And (3) granules.
CN202211058050.6A 2022-08-30 2022-08-30 Nb-shaped alloy 2 O 5 /GO/VS 2 Composite material and method for producing the same Pending CN115332525A (en)

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