CN115663169A - Vanadium oxide nanoflower and preparation method thereof - Google Patents
Vanadium oxide nanoflower and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of electrochemistry, and particularly relates to a vanadium oxide nanoflower and a preparation method thereof. The preparation method has the advantages of short production period, low cost, simple operation, mild reaction conditions and the like, and the vanadium oxide nanoflower can be widely applied to the field of electrochemistry.
Description
Technical Field
The invention relates to the technical field of electrochemistry, in particular to a vanadium oxide nanoflower and a preparation method thereof.
Background
The outermost electron arrangement of vanadium is 3d 3 4s 2 Therefore, the vanadium oxide crystal has rich oxidation valence, has larger theoretical specific capacity due to the special tunable layered structure, is very suitable to be used as an electrode host material to complete the embedding and the separation of ions, and is one of the electrode materials which people pay attention to.In addition, vanadium oxide is also known as "chemical bread" because vanadium oxide is one of the best catalysts in the chemical industry.
Researchers have used various manufacturing methods to prepare vanadium oxides, such as: sputtering, thermal evaporation, thermal decomposition, electrophoretic deposition, and many chemical methods (such as hydrothermal synthesis and sol-gel methods), and the like. It is reported that the chemical composition, crystal structure and crystallinity of vanadium oxides may play a key role in service and performance. More and more vanadium oxide electrochemical performance experimental results show that compared with bulk materials, the electrochemical performance of the nano material can be greatly improved. In the case of electrochemical lithium storage, some of the enhanced properties are reactivity to lithium, suppression of phase transitions to improve electrochemical reversibility, and the use of defects and high surface area to produce high capacity for lithium ion intercalation. In addition, short diffusion lengths in nanomaterials may also contribute to electrode rate capability. However, the morphology of the vanadium oxide is mainly spherical or rod-shaped at present, and the synthesis method is complex and time-consuming.
Disclosure of Invention
In order to solve the problems in the prior art, the invention mainly aims to provide the vanadium oxide nanoflower and the preparation method thereof, and the vanadium oxide nanoflower has the advantages of short production period, low cost, simplicity in operation, mild reaction conditions and the like, and can be widely applied to the field of electrochemistry.
To solve the above technical problem, according to an aspect of the present invention, the present invention provides the following technical solutions:
a vanadium oxide nanoflower is a carbon-coated vanadium oxide nanoflower and is assembled by vanadium oxide nanosheets, and the size of the vanadium oxide nanoflower is 100-500nm.
In order to solve the above technical problem, according to another aspect of the present invention, the present invention provides the following technical solutions:
a method for preparing vanadium oxide nanoflowers comprises the following steps:
s1, adding a vanadium oxide precursor into deionized water for ultrasonic dispersion to obtain a well-dispersed solution;
s2, adding ammonium molybdate and a carbon source into the solution, adding ethanol after the ammonium molybdate and the carbon source are completely dissolved, and stirring to obtain a solution before reaction; the solid-to-liquid ratio of the addition amount of the ammonium molybdate to the volume of the deionized water in the step S1 is 1 to 30; the solid-liquid ratio of the addition amount of the carbon source to the volume of the deionized water in the step S1 is 1 to 10;
s3, quickly injecting ammonia water into the solution before reaction, stirring, cleaning by adopting an ethanol solution, and centrifuging to obtain a reaction product;
and S4, grinding the powder obtained after the reaction product is dried, putting the powder into a tubular furnace filled with inert atmosphere for calcination treatment, and then cooling to room temperature to obtain the powder, thus obtaining the vanadium oxide nanoflower.
As a preferable scheme of the preparation method of the vanadium oxide nanoflower, the method comprises the following steps: in the step S1, the vanadium oxide is V 2 O 5 、VO 2 、V 2 O 3 And VO.
As a preferable scheme of the preparation method of the vanadium oxide nanoflower, the method comprises the following steps: in the step S1, the concentration of the solution is 1-10g/L.
As a preferable scheme of the preparation method of the vanadium oxide nanoflower, the method comprises the following steps: in the step S1, the ultrasonic dispersion time is 5 to 30min.
As a preferable scheme of the preparation method of the vanadium oxide nanoflower, the method comprises the following steps: in the step S2, the carbon source is any one of dopamine hydrochloride, glucose, sucrose, fructose, and oleylamine.
As a preferable scheme of the preparation method of the vanadium oxide nanoflower, the method comprises the following steps: in the step S2, the stirring time is 2-10min.
As a preferable scheme of the preparation method of the vanadium oxide nanoflower, the method comprises the following steps: in the step S2, the volume ratio of the ethanol to the deionized water in the step S1 is 0.5-5.
As a preferable scheme of the preparation method of the vanadium oxide nanoflower, the method comprises the following steps: in the step S3, the volume ratio of the ammonia water to the deionized water in the step S1 is from 0.005 to 0.05.
As a preferable scheme of the preparation method of the vanadium oxide nanoflower, the method comprises the following steps: in the step S3, the stirring time is 30 to 200min.
As a preferable scheme of the preparation method of the vanadium oxide nanoflower, the method comprises the following steps: in the step S4, the inert atmosphere is filled with argon or nitrogen.
As a preferable scheme of the preparation method of the vanadium oxide nanoflower, the method comprises the following steps: in the step S4, the calcining temperature is 600 to 800 ℃, and the calcining time is 5 to 20h.
In order to solve the above technical problem, according to another aspect of the present invention, the present invention provides the following technical solutions:
an application of vanadium oxide nanoflower in the field of electrochemistry.
The invention has the following beneficial effects:
the invention provides a vanadium oxide nanoflower and a preparation method thereof, wherein the vanadium oxide nanoflower is synthesized by self-assembly at normal temperature, and then is calcined to carbonize a carbon source, so that the carbon-coated vanadium oxide nanoflower is obtained, the vanadium oxide nanoflower is assembled by vanadium oxide nanosheets, and the size of the vanadium oxide nanoflower is 100 to 500nm.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.
FIG. 1 is a FESEM image of a vanadium oxide precursor of examples 1-2 of the present invention;
FIG. 2 is an XRD pattern of vanadium oxide nanoflower of example 1 of the present invention;
FIG. 3 is a FESEM high magnification view of vanadium oxide nanoflowers according to example 1 of the present invention;
FIG. 4 is a FESEM micrograph of vanadium oxide nanoflower of example 1 according to the present invention;
fig. 5 is a TEM image of vanadium oxide nanoflowers of example 1 of the present invention.
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
The following will clearly and completely describe the technical solutions in the embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a vanadium oxide nanoflower and a preparation method thereof, wherein the vanadium oxide nanoflower is synthesized by self-assembly at normal temperature, then a carbon source is carbonized by calcination, and the carbon-coated vanadium oxide nanoflower is further obtained, and the vanadium oxide nanoflower is assembled by vanadium oxide nanosheets, and the size of the vanadium oxide nanoflower is 100-500nm. The preparation method has the advantages of short production period, low cost, simple operation, mild reaction conditions and the like, and the vanadium oxide nanoflower can be widely applied to the field of electrochemistry.
The invention provides a vanadium oxide nanoflower which is a carbon-coated vanadium oxide nanoflower and is formed by assembling vanadium oxide nanosheets, wherein the size of the vanadium oxide nanoflower is 100-500nm, and specifically, the size of the vanadium oxide nanoflower can be any one of or a range between any two of 100nm, 150nm, 200nm, 250nm, 300nm, 350nm, 400nm, 450nm and 500nm.
The invention also provides a preparation method of the vanadium oxide nanoflower, which comprises the following steps:
s1, adding a vanadium oxide precursor into deionized water for ultrasonic dispersion to obtain a well-dispersed solution;
s2, adding ammonium molybdate and a carbon source into the solution, adding ethanol after the ammonium molybdate and the carbon source are completely dissolved, and stirring to obtain a solution before reaction; the solid-to-liquid ratio of the addition amount of the ammonium molybdate to the volume of the deionized water in the step S1 is 1 to 30; the solid-to-liquid ratio of the addition amount of the carbon source to the volume of the deionized water in the step S1 is 1 to 10; specifically, the solid-to-liquid ratio of the added amount of ammonium molybdate to the volume of deionized water in step S1 can be, for example, but not limited to, any one or a range between 1 mg/mL, 5 mg/mL, 10 mg/mL, 15 mg/mL, 20; the solid-to-liquid ratio of the added amount of the carbon source to the deionized water in step S1 can be, for example, but not limited to, any one or a range between 1;
s3, quickly injecting ammonia water into the solution before reaction, stirring, cleaning by adopting an ethanol solution, and centrifuging to obtain a reaction product; specifically, it may be centrifuged, for example, but not limited to, 2~3 times;
and S4, grinding the powder obtained after the reaction product is dried, putting the powder into a tubular furnace filled with inert atmosphere for calcination treatment, and then cooling to room temperature to obtain the powder, thus obtaining the vanadium oxide nanoflower.
Preferably, in step S1, the vanadium oxide precursor may be any commercially available material or micron-sized material synthesized by other methods, and the vanadium oxide is V 2 O 5 、VO 2 、V 2 O 3 And VO; the concentration of the solution is 1-10g/L; specifically, the concentration of the vanadium oxide precursor can be, for example, but not limited to, any one of 1g/L, 2g/L, 3g/L, 4g/L, 5g/L, 6g/L, 7g/L, 8g/L, 9g/L, 10g/L, or a range between any two; the ultrasonic dispersion time is 5 to 30min, and specifically, the ultrasonic dispersion time can be, for example and without limitation, 5min, 10min, 15min, 20min, 25min, 30min or a range between any two of the two;
preferably, in the step S2, the carbon source is any one of dopamine hydrochloride, glucose, sucrose, fructose and oleylamine; the stirring time is 2 to 10min, and specifically, the stirring time can be, for example, but not limited to, any one of 2min, 3min, 4min, 5min, 6min, 7min, 8min, 9min and 10min or a range between any two of the two; the volume ratio of the ethanol to the deionized water in the step S1 is 0.5 to 5, specifically, the volume ratio of the ethanol to the deionized water in the step S1 may be, for example, but not limited to, 0.5;
preferably, in the step S3, the volume ratio of the ammonia water to the deionized water in the step S1 is 0.005 to 0.05, and specifically, the volume ratio of the ammonia water to the deionized water in the step S1 may be, for example, but not limited to, any one or a range between 0.005; the stirring time is 30 to 200min, and specifically, the stirring time can be, for example and without limitation, 30min, 50min, 60min, 80min, 90min, 100min, 120min, 150min, 180min, 200min, or a range between any two of the two;
preferably, in the step S4, the inert atmosphere is filled with argon or nitrogen; the calcination temperature is 600 to 800 ℃, the calcination time is 5 to 20h, and specifically, the calcination temperature can be, for example, but is not limited to, 600 ℃, 620 ℃, 640 ℃, 660 ℃, 680 ℃, 700 ℃, 720 ℃, 740 ℃, 760 ℃, 780 ℃ and 800 ℃ or a range between any two of the temperatures; the calcination time may be, for example, but is not limited to, any one of 5h, 7h, 9h, 11h, 13h, 15h, 17h, 19h, 20h, or a range between any two;
in order to solve the above technical problem, according to another aspect of the present invention, the present invention provides the following technical solutions:
the vanadium oxide nanoflower can be applied to the fields of electrochemistry, such as electrochemical batteries and catalysis, and specifically can comprise but not limited to lithium ion batteries, sodium ion batteries, potassium ion batteries, zinc ion batteries, magnesium ion batteries, aluminum ion batteries, calcium ion batteries, hydrogen evolution catalysis (HER), and oxygen evolution catalysisChemo (OER), oxygen reduction catalysis (ORR), photocatalysis, carbon dioxide Catalysis (CO) 2 RR), etc.
The technical solution of the present invention is further illustrated by the following specific examples.
The vanadium oxide precursors of examples 1-2 of the present invention were prepared as follows, and examples 3-5 used commercial vanadium oxide precursors.
The vanadium oxide precursor of example 1-2 was prepared as follows:
0.6g of commercial V are stirred vigorously at 80 ℃ under stirring 2 O 5 And 9.89mmol of H 2 C 2 O 4 Dissolved in 20mL of deionized water for 5h, and then 6mL of the prepared solution was added to a 100mL Teflon container previously charged with 60mL of isopropanol. After stirring for 20min, the vessel was sealed in a steel autoclave and kept in an electric oven at 200 ℃ for 2.5h. After natural cooling, the precipitate was collected by centrifugation and washed three times with pure ethanol to give V 2 O 3 Vanadium oxide precursor, as shown in fig. 1.
Example 1
A method for preparing vanadium oxide nanoflowers comprises the following steps:
s1, mixing V of 40mg 2 O 3 Adding the vanadium oxide precursor into 10mL of deionized water, and performing ultrasonic dispersion for 20min to obtain a well-dispersed solution;
s2, adding 100mg of ammonium molybdate and 25mg of dopamine hydrochloride into the solution, adding ethanol after the ammonium molybdate and the dopamine hydrochloride are completely dissolved, and stirring for 5min to obtain a solution before reaction;
s3, quickly injecting 0.15mL of ammonia water into the solution before reaction, stirring for 120min, cleaning by using an ethanol solution, and centrifuging for 2 times to obtain a reaction product;
s4, grinding the powder obtained after the reaction product is dried, putting the powder into a tubular furnace filled with nitrogen atmosphere, calcining for 16h at 750 ℃, cooling to room temperature, taking out the powder, and finally obtaining the carbon-coated vanadium oxide nanoflower, wherein the size of the nanoflower is about 200nm, and the phase and the morphology of the nanoflower are shown in figures 2-5.
Example 2
A method for preparing vanadium oxide nanoflowers comprises the following steps:
s1, 20mg of V 2 O 3 Adding the vanadium oxide precursor into 10mL of deionized water, and performing ultrasonic dispersion for 30min to obtain a well-dispersed solution;
s2, adding 150mg of ammonium molybdate and 50mg of dopamine hydrochloride into the solution, adding ethanol after the ammonium molybdate and the dopamine hydrochloride are completely dissolved, and stirring for 10min to obtain a solution before reaction;
s3, quickly injecting 0.25mL of ammonia water into the solution before reaction, stirring for 60min, cleaning by using an ethanol solution, and centrifuging for 3 times to obtain a reaction product;
s4, grinding the powder obtained after the reaction product is dried, then placing the powder into a tubular furnace filled with nitrogen atmosphere to calcine for 10 hours at 600 ℃, and then taking out the powder when the temperature is cooled to room temperature to finally obtain the carbon-coated vanadium oxide nanoflower.
Example 3
A method for preparing vanadium oxide nanoflowers comprises the following steps:
s1, 30mg of commercial V 2 O 5 Adding the precursor into 10mL deionized water, and performing ultrasonic dispersion for 25min to obtain a well-dispersed solution;
s2, adding 50mg of ammonium molybdate and 20mg of dopamine hydrochloride into the solution, adding ethanol after the ammonium molybdate and the dopamine hydrochloride are completely dissolved, and stirring for 5min to obtain a solution before reaction;
s3, quickly injecting 0.20mL of ammonia water into the solution before reaction, stirring for 20min, cleaning by using an ethanol solution, and centrifuging for 2 times to obtain a reaction product;
s4, grinding the powder obtained after the reaction product is dried, putting the powder into a tubular furnace filled with nitrogen atmosphere, calcining the powder for 6 hours at 800 ℃, cooling the powder to room temperature, and taking out the powder to finally obtain the carbon-coated vanadium oxide nanoflower.
Example 4
A method for preparing vanadium oxide nanoflowers comprises the following steps:
s1, 50mg of commercial VO 2 Adding the precursor into 10mL deionized water, and performing ultrasonic dispersion for 35min to obtain a well-dispersed solution;
s2, adding 80mg of ammonium molybdate and 30mg of dopamine hydrochloride into the solution, adding ethanol after the ammonium molybdate and the dopamine hydrochloride are completely dissolved, and stirring for 5min to obtain a solution before reaction;
s3, quickly injecting 0.10mL of ammonia water into the solution before reaction, stirring for 30min, cleaning by using an ethanol solution, and centrifuging for 2 times to obtain a reaction product;
s4, grinding the dried powder, and then placing the powder in a tubular furnace filled with nitrogen atmosphere to calcine for 8 hours at 700 ℃; and taking out the powder when the temperature is completely cooled to the room temperature, and finally obtaining the carbon-coated vanadium oxide nanoflower.
Example 5
A preparation method of a vanadium oxide nanoflower material comprises the following steps:
s1.45mg of commercial VO precursor is added into 10mL of deionized water for ultrasonic dispersion for 30min to obtain a well-dispersed solution;
s2, adding 50mg of ammonium molybdate and 20mg of dopamine hydrochloride into the solution, adding ethanol after the ammonium molybdate and the dopamine hydrochloride are completely dissolved, and stirring for 5min to obtain a solution before reaction;
s3, quickly injecting 0.15mL of ammonia water into the solution before reaction, stirring for 20min, cleaning by using an ethanol solution, and centrifuging for 2-3 times to obtain a reaction product;
s4, grinding the powder after the reaction product is dried, and then calcining the powder in a tubular furnace filled with nitrogen atmosphere at 800 ℃ for 10 hours; and then cooling to room temperature, and taking out the powder to finally obtain the carbon-coated vanadium oxide nanoflower.
The above description is only a preferred embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which are made by the present specification and directly/indirectly applied to other related technical fields within the spirit of the present invention are included in the scope of the present invention.
Claims (10)
1. The vanadium oxide nanoflower is characterized by being a carbon-coated vanadium oxide nanoflower which is assembled by vanadium oxide nanosheets, and the size of the vanadium oxide nanoflower is 100-500nm.
2. A method for preparing vanadium oxide nanoflowers according to claim 1, comprising the steps of:
s1, adding a vanadium oxide precursor into deionized water for ultrasonic dispersion to obtain a well-dispersed solution;
s2, adding ammonium molybdate and a carbon source into the solution, adding ethanol after the ammonium molybdate and the carbon source are completely dissolved, and stirring to obtain a solution before reaction; the solid-to-liquid ratio of the addition amount of the ammonium molybdate to the deionized water in the step S1 is 1 to 30; the solid-to-liquid ratio of the addition amount of the carbon source to the deionized water in the step S1 is 1 to 10;
s3, quickly injecting ammonia water into the solution before reaction, stirring, cleaning by adopting an ethanol solution, and centrifuging to obtain a reaction product;
and S4, grinding the powder obtained after the reaction product is dried, putting the powder into a tubular furnace filled with inert atmosphere for calcination treatment, and then cooling to room temperature to obtain the powder, thus obtaining the vanadium oxide nanoflower.
3. The method according to claim 2, wherein in step S1, the vanadium oxide is V 2 O 5 、VO 2 、V 2 O 3 And VO.
4. The method according to claim 2, wherein the concentration of the solution in step S1 is 1 to 10g/L.
5. The method according to claim 2, wherein the carbon source in step S1 is any one of dopamine hydrochloride, glucose, sucrose, fructose, and oleylamine.
6. The preparation method according to claim 2, wherein in step S2, the volume ratio of ethanol to deionized water in step S1 is 0.5 to 5.
7. The method according to claim 2, wherein in step S3, the volume ratio of the ammonia water to the deionized water in step S1 is 0.005 to 0.05.
8. The method according to claim 2, wherein in step S4, the inert gas atmosphere is filled with argon gas or nitrogen gas.
9. The method according to claim 2, wherein the calcining temperature is 600 to 800 ℃ and the calcining time is 5 to 20h in the step S4.
10. Use of the vanadium oxide nanoflower according to claim 1 in the field of electrochemistry.
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