CN108726571B - VS (virtual switch)4nanorod/VS2Nano sheet three-dimensional self-assembly hollow rod-shaped composite powder and preparation method thereof - Google Patents

VS (virtual switch)4nanorod/VS2Nano sheet three-dimensional self-assembly hollow rod-shaped composite powder and preparation method thereof Download PDF

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CN108726571B
CN108726571B CN201810708733.9A CN201810708733A CN108726571B CN 108726571 B CN108726571 B CN 108726571B CN 201810708733 A CN201810708733 A CN 201810708733A CN 108726571 B CN108726571 B CN 108726571B
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黄剑锋
***
冯亮亮
曹丽云
何枢薇
王娜
范海鑫
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Shaanxi University of Science and Technology
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Abstract

VS (virtual switch)4nanorod/VS2The invention relates to a nano-sheet three-dimensional self-assembly hollow rod-shaped composite powder and a preparation method thereof, wherein ethanol is used as a solvent, sodium metavanadate and thioacetamide are respectively used as a vanadium source and a sulfur source, and the concentration and the proportion, the reaction temperature, the reaction time, the reaction pH value, the filling ratio and other parameters of the ethanol and the thioacetamide are cooperatively controlled, so that the uniform distribution VS is generated in situ by a one-step solvothermal method4VS of nanorods2The nano-sheet is self-assembled in a hollow rod-shaped structure. The method has the advantages of simple reaction process, low temperature, easy control, no need of large-scale equipment and harsh reaction conditions, and can simultaneously realize the structure that two substances are combined in a specific way in one reaction process. When the product is applied to a lithium/sodium ion battery negative electrode material and a photo/electro catalyst, the product can show excellent electrochemical performance and catalytic performance.

Description

VS (virtual switch)4nanorod/VS2Nano sheet three-dimensional self-assembly hollow rod-shaped composite powder and preparation method thereof
Technical Field
The invention relates to vanadium sulfide composite powder and a preparation method thereof, in particular to VS4nanorod/VS2A nano-sheet three-dimensional self-assembly hollow rod-shaped composite powder and a preparation method thereof.
Background
With large chain pitch
Figure BDA0001716187240000011
One-dimensional chain-like LVS with weak inter-chain interaction, high S content and low development cost4[Xu X,Jeong S,Rout CS,Oh P,Ko M,Kim H,et al.Lithium reaction mechanism and high rate capability of VS4-graphene nanocomposite as an anode material for lithium batteries.J Mater Chem A.2014；2:10847-53.]Are considered to have broad development prospects in the fields of energy storage and photo/electrocatalysis, and they have been in photocatalysis, supercapacitors, lithium/sodium ion electricityThe method is applied to the fields of pools and the like. Metallic VS possessing excellent conductivity2Has excellent electron transport properties and VS2With large spatial distances between layers
Figure BDA0001716187240000012
And weak van der Waals force connection to VS2Also becomes a very promising energy storage and photo/electro-catalytic material [ Jun F, Xu S, Changzheng W, et al. metallic few-layered VS2 ultrathin nanosheets:high two-dimensional conductivity for in-plane supercapacitors.[J].Journal of the American Chemical Society,2011,133(44):17832-17838]. If the two can be compounded efficiently, the respective advantages and the synergistic effect are fused, and the composite material has more excellent energy storage and photo/electro-catalytic performance. However, the known reports are mainly related to pure phase VS4And VS2The synthesis of (A) has not been reported to compound the two, let alone about VS4nanorod/VS2Report of the nano-sheet three-dimensional self-assembled hollow rod-shaped composite powder.
Disclosure of Invention
The invention aims to provide a VS4nanorod/VS2A nano-sheet three-dimensional self-assembly hollow rod-shaped composite powder and a preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
the method comprises the following steps: simultaneously adding 0.4-0.6 g of sodium metavanadate and 2.6-2.8 g of thioacetamide into 56-60 ml of absolute ethanol, and uniformly stirring to obtain a semi-clear solution A;
step two: pouring the solution A into a reaction inner liner, sealing, then placing the inner liner in an outer kettle, fixing, placing in a homogeneous reactor, and then reacting at 155-165 ℃ for 26-28 h at a rotating speed of 5-10 r/min;
step three: naturally cooling the reaction kettle to room temperature after the reaction is finished, then taking out the cooled product after the reaction, and collecting the product after washing with water and alcohol alternately;
step four: freeze drying the collected productFreezing in a cold well of the machine, then placing the frozen product in a tray, covering a sealing cover, vacuumizing to 10-20 Pa, drying for 12-18 h, and collecting the product to obtain VS4nanorod/VS2The nano-sheet three-dimensional self-assembly hollow rod-shaped composite powder.
The stirring in the step 1) is magnetic stirring or ultrasonic dispersion at normal temperature, and the rotating speed of the magnetic stirring is 400-600 r/min.
The filling ratio of the solution A poured into the reaction lining in the step 2) is 56-60%.
And in the step 3), suction filtration or centrifugal cleaning is adopted for water washing and alcohol washing.
The freezing conditions of the step 4) are as follows: freezing for 2-5 hours at-60 to-40 ℃.
And (3) before the product in the step 4) is placed into a tray for drying, sealing by using a preservative film, and pricking holes on the preservative film to ensure that the product is fully dried under a low-pressure condition.
VS prepared by the preparation method of the invention4nanorod/VS2The nano-sheet three-dimensional self-assembled hollow rod-shaped composite powder body is formed from irregular micrometer rod, and the interior of said micrometer rod is formed from VS2A hollow framework formed by overlapping nano sheets, wherein the thickness of the nano sheets is 10-20 nm, and VS distributed on the surfaces of the nano sheets is arranged outside the nano sheets4The diameter of the nanorod is 20-50 nm, and the nanosheet and the nanorod show single crystal characteristics.
VS prepared by the preparation method of the invention4nanorod/VS2The nano-sheet three-dimensional self-assembled hollow rod-shaped composite powder is applied to the field of lithium/sodium ion batteries or the field of photo/electro-catalysis.
The invention takes ethanol as a solvent, takes sodium metavanadate and thioacetamide as a vanadium source and a sulfur source respectively, and realizes the in-situ generation of uniformly distributed VS by a one-step solvothermal method by cooperatively controlling the concentration and the ratio of the vanadium source and the sulfur source, the reaction temperature, the reaction time, the reaction pH value, the filling ratio and other parameters4VS of nanorods2The nano-sheet is self-assembled in a hollow rod-shaped structure. The method has simple reaction process, low temperature, easy control, no need of large-scale equipment and harsh reaction conditions, and can realize one reactionThe structure that two substances are combined in a specific way is realized simultaneously in the reaction process. When the product is applied to a lithium/sodium ion battery negative electrode material and a photo/electro catalyst, the product can show excellent electrochemical performance and catalytic performance.
The method has the following specific beneficial effects:
(1) the invention adopts one-step solvothermal reaction to directly synthesize the final product, thereby having low synthesis temperature, simple synthesis path and no need of large-scale equipment and harsh reaction conditions;
(2) the vanadium source used in the method is sodium metavanadate, the sulfur source is thioacetamide, the two raw materials are common materials, and the method has the advantages of low price, easy obtainment, low cost, high yield, easy control of reaction, no need of post-treatment, environmental friendliness and suitability for large-scale production;
(3) when the product prepared by the method is used as a lithium/sodium ion battery negative electrode material and a photo/electro catalyst, excellent performance can be shown;
(4) the invention realizes the control of the existing state of vanadium and sulfur in the reaction by strictly and cooperatively controlling the concentration and the proportion of the vanadium source and the sulfur source, the reaction temperature, the reaction time, the reaction pH value, the filling ratio and other parameters, thereby preferentially controlling NaVO under the action of enabling the high-concentration sulfur source3Surface generation of VS on a micron rod4The nano rod is then treated with NaVO inside the micron rod under the action of low concentration sulfur source3Transition to VS2Nanosheets and making VS2The nano-sheets form an internal hollow structure in a self-assembly mode, and finally high-purity and uniform VS is realized4nanorod/VS2And (3) preparing the nano-sheet three-dimensional self-assembled hollow rod-shaped composite material. The reaction temperature plays a key role in the formation of the unique structure during the whole reaction process, and both too high and too low temperatures are unfavorable for the formation of the structure.
(5) In the process of synthesizing the three-dimensional self-assembly structure, no template agent or surfactant is introduced, and the whole self-assembly process is based on a reaction starting material NaVO3The slightly soluble characteristic of the micron rod is controlled by the self-template action of the reaction raw materials, so that the whole reaction is simple, easy to control, high-efficiency andthe cost is low;
(6) the composite product prepared by the invention has a unique composite structure, wherein VS2The hollow structure formed by the nano sheets can well play a role in stabilizing the structure in the electrochemical reaction process, and can provide a large number of lithium/sodium ion storage sites. VS2VS at the surface of the nanoplatelets4A large number of lithium/sodium ion storage sites can be further provided, enabling the final composite to exhibit excellent cycling stability and rate capability as well as higher capacity. Furthermore, VS4Large amount of catalytic active sites and metal state VS on nano-rod surface2The excellent electrical conductivity allows the composite material to ultimately exhibit excellent catalytic performance.
Drawings
FIG. 1 is an X-ray diffraction pattern of the product prepared in example 1 of this invention.
FIG. 2 is a scanning electron micrograph of a product prepared according to example 1 of the present invention.
FIG. 3 is a high power scanning electron micrograph of the product prepared in example 1 of the present invention.
FIG. 4 is a super high power scanning electron micrograph of the product prepared in example 1 of the present invention.
FIG. 5 is a transmission electron micrograph of a product prepared in example 1 of the present invention.
FIG. 6 is a high resolution transmission electron microscope image of the outer nanorods of the product prepared in example 1 of the present invention.
FIG. 7 is a high-resolution transmission electron microscope image of nanosheets inside the product nanorods prepared in example 1 of the present invention.
FIG. 8 is a scanning electron micrograph of a product obtained by adjusting the reaction temperature to 120 ℃ in example 1 of the present invention (except for the same conditions as in example 1).
FIG. 9 is a scanning electron micrograph of a product obtained after the reaction temperature in example 1 of the present invention was set to 180 ℃ in full (other conditions were exactly the same as those in example 1).
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Example 1:
the method comprises the following steps: simultaneously adding 0.5g of sodium metavanadate and 2.6g of thioacetamide into 60ml of absolute ethyl alcohol, and magnetically stirring uniformly at normal temperature at 400r/min to obtain a semi-clear solution A;
step two: pouring the solution A into a reaction inner liner according to a filling ratio of 58%, sealing, then placing the inner liner into an outer kettle, fixing, placing into a homogeneous reactor, and then reacting at 155 ℃ for 26h at a rotating speed of 8 r/min;
step three: naturally cooling the reaction kettle to room temperature after the reaction is finished, then taking out the cooled product after the reaction, alternately cleaning for 3 times by adopting water and alcohol in a suction filtration mode, and collecting the product;
step four: placing the collected product in a cold well of a freeze dryer at-60 ℃, freezing for 2 hours, then placing the frozen product in a tray, sealing with a preservative film, pricking the preservative film to ensure that the preservative film is fully dried under a low-pressure condition, covering a sealing cover, vacuumizing to 15Pa, drying for 12 hours, and collecting the product to obtain VS4nanorod/VS2The nano-sheet three-dimensional self-assembly hollow rod-shaped composite powder.
It can be seen from FIG. 1 that VS occurs in the lower diffraction angle range4Shows a VS in a higher diffraction angle range2Diffraction Peak, indicating that the product synthesized by the preparation method provided in example 1 is VS4And VS2The complex of (1).
As can be seen from fig. 2, the resulting product is composed of an irregular rod-like three-dimensional structure, both in length and width on the order of microns.
As can be seen from FIG. 3, the resulting nanorods exhibited a hollow structure
As can be seen from FIG. 4, the interior of the resulting nanorods is indicated by VS2A hollow framework formed by overlapping nano sheets, wherein the thickness of the nano sheets is 10-20 nm, and VS distributed on the surfaces of the nano sheets is arranged outside the nano sheets4The diameter of the nanorod is 20-50 nm.
As can be seen from fig. 5, the nanorods exhibit a uniform hollow structure, and the size of the cavity is much larger than that of the wall.
From FIG. 6, the regularly arranged lattice fringes, which correspond to VS, can be seen4The (110) crystal face of (A) proves that the nanorod is VS4On the other hand, VS is described4The nanorods exhibit single crystal properties.
From FIG. 7, it can be seen that the more regularly arranged lattice fringes, where the large pitch lattice fringes correspond to VS2With closely spaced lattice fringes corresponding to VS2The (011) crystal face of (A) proves that the nano sheet is VS2On the other hand, VS is also described2The nanosheets exhibit single crystal characteristics.
As can be seen from FIG. 8, the resulting product has a solid structure, meaning that the formation of hollow structure is not favored under the condition of excessively low reaction temperature.
It can be seen from FIG. 9 that the product had not been VS4Nanorod formation, meaning that VS is not favored at too high a reaction temperature4/VS2And (4) forming a composite product.
Example 2:
the method comprises the following steps: simultaneously adding 0.4g of sodium metavanadate and 2.7g of thioacetamide into 56ml of absolute ethyl alcohol, and magnetically stirring uniformly at normal temperature at 500r/min to obtain a semi-clear solution A;
step two: pouring the solution A into a reaction inner liner according to the filling ratio of 56%, sealing, then placing the inner liner into an outer kettle, fixing, placing into a homogeneous reactor, and then reacting for 27h at 160 ℃ at the rotating speed of 5 r/min;
step three: naturally cooling the reaction kettle to room temperature after the reaction is finished, then taking out the cooled product after the reaction, and collecting the product after cleaning for 4 times by adopting water and alcohol in a suction filtration mode;
step four: placing the collected product in a cold well of a freeze dryer at-50 ℃, freezing for 3 hours, then placing the frozen product in a tray, sealing with a preservative film, pricking the preservative film to ensure that the preservative film is fully dried under a low-pressure condition, covering a sealing cover, vacuumizing to 12Pa, drying for 16 hours, and collecting the product to obtain VS4nanorod/VS2Nano sheet three-dimensional self-assembly hollow rod-shaped compositeAnd (3) powder.
Example 3:
the method comprises the following steps: simultaneously adding 0.55g of sodium metavanadate and 2.8g of thioacetamide into 58ml of absolute ethyl alcohol, and uniformly stirring at normal temperature by magnetic force at 600r/min to obtain a semi-clear solution A;
step two: pouring the solution A into a reaction inner liner according to the filling ratio of 60%, sealing, then placing the inner liner into an outer kettle, fixing, placing into a homogeneous reactor, and then reacting at 165 ℃ for 28h at the rotating speed of 10 r/min;
step three: naturally cooling the reaction kettle to room temperature after the reaction is finished, then taking out the cooled product after the reaction, alternately cleaning for 5 times by adopting water and alcohol in a suction filtration mode, and collecting the product;
step four: placing the collected product in a cold well of a freeze dryer at-45 ℃, freezing for 4 hours, then placing the frozen product in a tray, sealing with a preservative film, pricking the preservative film to ensure that the preservative film is fully dried under a low-pressure condition, covering a sealing cover, vacuumizing to 18Pa, drying for 14 hours, and collecting the product to obtain VS4nanorod/VS2The nano-sheet three-dimensional self-assembly hollow rod-shaped composite powder.
Example 4:
the method comprises the following steps: simultaneously adding 0.45g of sodium metavanadate and 2.65g of thioacetamide into 57ml of absolute ethyl alcohol, and performing ultrasonic dispersion at normal temperature to obtain a semi-clear solution A;
step two: pouring the solution A into a reaction inner liner according to a filling ratio of 57%, sealing, then placing the inner liner into an outer kettle, fixing, placing into a homogeneous reactor, and then reacting at 158 ℃ for 28h at a rotating speed of 7 r/min;
step three: naturally cooling the reaction kettle to room temperature after the reaction is finished, taking out the cooled product after the reaction, alternately cleaning for 4 times by adopting water and alcohol in a centrifugal mode, and collecting the product;
step four: placing the collected product in a cold well of a freeze dryer, freezing for 4 hours at-55 ℃, then placing the frozen product in a tray, sealing with a preservative film, and pricking the preservative film to ensure that the preservative film is filled under a low-pressure conditionDrying, covering a sealing cover, vacuumizing to 10Pa, drying for 18h, and collecting the product to obtain VS4nanorod/VS2The nano-sheet three-dimensional self-assembly hollow rod-shaped composite powder.
Example 5:
the method comprises the following steps: simultaneously adding 0.6g of sodium metavanadate and 2.75g of thioacetamide into 59ml of absolute ethyl alcohol, and performing ultrasonic dispersion at normal temperature to obtain a semi-clear solution A;
step two: pouring the solution A into a reaction inner liner according to a filling ratio of 59%, sealing, then placing the inner liner into an outer kettle, fixing, placing into a homogeneous reactor, and then reacting at 162 ℃ for 26h at a rotating speed of 9 r/min;
step three: naturally cooling the reaction kettle to room temperature after the reaction is finished, taking out the cooled product after the reaction, alternately cleaning the product for 5 times by adopting water and alcohol in a centrifugal mode, and collecting the product;
step four: placing the collected product in a cold well of a freeze dryer at-40 ℃, freezing for 5 hours, then placing the frozen product in a tray, sealing with a preservative film, pricking the preservative film to ensure that the preservative film is fully dried under a low-pressure condition, covering a sealing cover, vacuumizing to 20Pa, drying for 15 hours, and collecting the product to obtain VS4nanorod/VS2The nano-sheet three-dimensional self-assembly hollow rod-shaped composite powder.

Claims (4)

1. VS (virtual switch)4nanorod/VS2The preparation method of the nano-sheet three-dimensional self-assembly hollow rod-shaped composite powder is characterized by comprising the following steps:
the method comprises the following steps: simultaneously adding 0.4-0.6 g of sodium metavanadate and 2.6-2.8 g of thioacetamide into 56-60 ml of absolute ethanol, and uniformly stirring to obtain a semi-clear solution A;
step two: pouring the solution A into a reaction inner liner, sealing, then placing the inner liner in an outer kettle, fixing, placing in a homogeneous reactor, and then reacting at 155-165 ℃ for 26-28 h at a rotating speed of 5-10 r/min;
step three: naturally cooling the reaction kettle to room temperature after the reaction is finished, then taking out the cooled product after the reaction, and collecting the product after washing with water and alcohol alternately;
step four: placing the collected product in a cold well of a freeze dryer for freezing, then placing the frozen product in a tray, covering a sealing cover, vacuumizing to 10-20 Pa, drying for 12-18 h, and collecting the product to obtain VS4nanorod/VS2Nano-sheet three-dimensional self-assembled hollow rod-shaped composite powder;
the filling ratio of the solution A poured into the reaction lining in the step 2) is 56-60%;
the freezing conditions of the step 4) are as follows: freezing for 2-5 hours at the temperature of minus 60-minus 40 ℃;
the stirring in the step 1) is magnetic stirring or ultrasonic dispersion at normal temperature, and the rotating speed of the magnetic stirring is 400-600 r/min;
and in the step 3), suction filtration or centrifugal cleaning is adopted for water washing and alcohol washing.
2. VS according to claim 14nanorod/VS2The preparation method of the nano-sheet three-dimensional self-assembly hollow rod-shaped composite powder is characterized by comprising the following steps: and (3) before the product in the step 4) is placed into a tray for drying, sealing by using a preservative film, and pricking holes on the preservative film to ensure that the product is fully dried under a low-pressure condition.
3. VS prepared by the preparation method according to claim 14nanorod/VS2The nano-sheet three-dimensional self-assembly hollow rod-shaped composite powder is characterized in that: the composite powder consists of irregular micron rods, and VS is arranged inside the micron rods2A hollow framework formed by overlapping nano sheets, wherein the thickness of the nano sheets is 10-20 nm, and VS is distributed on the surfaces of the nano sheets4The diameter of the nanorod is 20-50 nm, and the nanosheet and the nanorod show single crystal characteristics.
4. VS prepared by the preparation method according to claim 14nanorod/VS2The nano-sheet three-dimensional self-assembly hollow rod-shaped composite powder is characterized in that: VS4nanorod/VS2Three-dimensional self-assembly of nanosheetsThe hollow rod-shaped composite powder is applied to the field of lithium/sodium ion batteries or the field of photo/electro-catalysis.
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