CN109888223B - Preparation method and application of vanadium tetrasulfide @ reduced graphene oxide composite powder - Google Patents
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Abstract
A preparation method of vanadium tetrasulfide @ reduced graphene oxide composite powder comprises the steps of weighing 20-120 mg of graphene oxide, adding the graphene oxide into 58-62 ml of deionized water, and carrying out ultrasonic treatment to obtain a uniformly dispersed black solution A; weighing 0.9-1.1 g of sodium metavanadate and 3.5-3.7 g of thioacetamide, simultaneously adding the sodium metavanadate and the thioacetamide into the solution A, and magnetically stirring to obtain a solution B; pouring the solution B into a reaction inner liner, sealing, then placing the inner liner in an outer kettle, fixing, placing in a homogeneous reactor, and then reacting under the condition of rotating speed; after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, then taking out a cooled product after the reaction, and collecting the product after alternately cleaning with water and alcohol; and 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 and drying, and collecting the product to obtain the vanadium tetrasulfide @ reduced graphene oxide composite powder. The method has the characteristics of simple reaction process, low temperature, easy control and no need of large-scale equipment and harsh reaction conditions.
Description
Technical Field
The invention relates to the technical field of vanadium tetrasulfide @ reduced graphene oxide composite powder, in particular to a preparation method and application of vanadium tetrasulfide @ reduced graphene oxide composite powder.
Background
As a typical transition metal sulfide, VS4Has a one-dimensional chain structure. Wherein two S2 2-The group (four S) tightly surrounds V and expands in the c direction to form VS4Molecular chain, adjacent two VS4The molecular chains are connected through weak van der Waals force, and the chain spacing can reach
(Rout CS, Kim B-H, et al.J Am Chem Soc.2013,135: 8720-8725.). Similar to FeS2，VS4Derived from the natural mineral, chlorothiolite, and has a valence state of-1 for S and a valence state of +4 for V. The above structural characteristics make VS4The method is applied to the fields of photocatalysis, hydrofining reaction, lithium ion batteries, supercapacitors, aluminum ion batteries, magnesium ion batteries and the like. However, since 1970 VS due to the very oxophilic nature of V, the precise partial pressure of S required for the reaction process, and the presence of various non-stoichiometric ratios of vanadium sulfide4It was first reported that their synthesis was greatly hindered (Xu X, Jeong S, et al J Mater Chem A.2014,2:10847-10853.). And, for VS4The synthesis of (a) generally requires the introduction of a templating agent. Sun R et al prepared VS grown on the surface of reduced graphene by hydrothermal method4(Sun R, Wei Q, et al. ACS Appl Mater Inter.2015,7: 20902-20908.). Li S et al synthesized VS by a flexible hydrothermal method4Nanocomposites stacked on reduced graphene oxide (Li S, He W, et al. Mater Lett.2017,205: 52-55.). Pang Q et al prepared uniform graphene sheet anchored VS by CTAB cationic surfactant assisted hydrothermal method4Nanoparticles, followed by varying the amount of graphene sheets added, control VS4Size of nanoparticles (Pang Q, Zhao Y, et al. ChemSus chem.2018,11: 735-. Wang S et al prepared uniform cuboid VS by controlling the content of graphene oxide template using an in situ graphene oxide template hydrothermal method4Nanoparticles (Wang S, Gong F, et al. adv Funct Mater.2018,28: 1801806.). Rout CS et al successfully obtained oxidized graphene, carboxylated carbon nanotubes, pyrene rich in locking machine, perylene tetracarboxylic dianhydride, graphite and other carbon materials and VS in a hydrothermal system4The complex of (Rout CS, Kim B-H, et al.J Am Chem Soc.2013,135: 8720-8725.). However, in the above-described composite materials that have been reported, a part of VS4Not grown on the surface of the carbon material, but only VS4The other part of the composite with the carbon material grows on the surface of the carbon material, but the distribution is sparse and irregular, and VS is4The appearance of the alloy is also irregular and uniform. This inadequate and inefficient compounding causes VS4The high performance of (2) is not well performed.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method and application of vanadium tetrasulfide @ reduced graphene oxide composite powderZygotic growth of VS4The bent nanorod structure is simple in reaction process, low in temperature, easy to control, free of large-scale equipment and harsh reaction conditions, and capable of directly realizing VS in one reaction process4And in-situ growth on the surface of the reduced graphene oxide. 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.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of vanadium tetrasulfide @ reduced graphene oxide composite powder comprises the following steps;
the method comprises the following steps: weighing 20-120 mg of graphene oxide, adding the graphene oxide into 58-62 ml of deionized water, and carrying out ultrasonic treatment for 1.5-2.5 h to obtain a uniformly dispersed black solution A;
step two: weighing 0.9-1.1 g of sodium metavanadate and 3.5-3.7 g of thioacetamide, simultaneously adding the sodium metavanadate and the thioacetamide into the solution A, and magnetically stirring for 30-60 min to obtain a solution B;
step three: pouring the solution B 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 175-185 ℃ for 12-30 h under the condition of a rotating speed of 5-10 r/min;
step four: after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, taking out a cooled product after the reaction, and collecting the product after water and alcohol are alternately cleaned for 4-10 times;
step five: and 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 the vanadium tetrasulfide @ reduced graphene oxide composite powder.
The ultrasonic power in the first step is 400-600W, and the ultrasonic treatment is carried out at normal temperature.
And in the second step, the rotating speed of magnetic stirring is 400-600 r/min, and the stirring is carried out at normal temperature.
And in the third step, the filling ratio of the solution B poured into the reaction lining is 58-62%.
In the fourth step, water and alcohol are alternately cleaned mainly in a suction filtration or centrifugation mode, and the collection is also mainly performed in a suction filtration or centrifugation mode.
The refrigeration conditions of the step five are as follows: freezing for 2-5 h at-60 to-40 ℃.
And before the product obtained in the fifth step is placed into a tray for drying, sealing the product by using a preservative film, and pricking the preservative film to ensure that the product is sufficiently dried under a low-pressure condition.
The composite powder consists of irregular sheets, the interior of each sheet is a few layers (ultrathin 5-15 nm) of reduced graphene oxide, the surface of each sheet consists of uniform bent nanorods with the diameter of 20-50 nm and the length of 50-150 nm, and VS is arranged on each surface of each sheet4The bent nanorods have high crystallinity and orientation arrangement along the (110) crystal plane direction.
The combination of the vanadium tetrasulfide and the reduced graphene oxide is combined by chemical bonds, but not by physical bonds.
The vanadium tetrasulfide @ reduced graphene oxide composite powder can be applied to the field of lithium/sodium ion batteries and the field of photo/electrocatalysis, and can show excellent performance in the two fields.
The invention has the beneficial effects that:
(1) according to the invention, a final composite structure is directly synthesized by one-step template-free hydrothermal reaction, and the oxygen-containing functional group on the surface of the graphene oxide is taken as an active site in the whole in-situ growth process. Therefore, the method has the advantages of low synthesis temperature, simple synthesis path, easy control, high efficiency, low cost, no need of large-scale equipment and harsh reaction conditions;
(2) the vanadium source used in the invention is sodium metavanadate, the sulfur source is thioacetamide, the solvent is water, the three substances are common raw materials, the raw materials are cheap and easy to obtain, the cost is low, the whole reaction yield is high, easy to control and environment-friendly, the product does not need post-treatment, and the method is suitable 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) according to the invention, parameters such as the concentration and the proportion of a vanadium source and a sulfur source, reaction temperature, reaction time, filling ratio and the like are strictly and cooperatively controlled, and VS is realized by fully utilizing the abundant oxygen-containing crown energy groups on the surface of the graphene oxide4The graphene oxide is uniformly nucleated on the surface and grows by virtue of the nucleation, and meanwhile, the graphene oxide is reduced to reduced graphene oxide under hydrothermal conditions and becomes very thin, so that VS is formed4Bending the nano-rods to form a composite structure in which the nano-rods are laid on the surface of the reduced graphene oxide in situ;
(5) addition amount of graphene oxide for VS4The curved nanorod is evenly paved on the surface of reduced graphene oxide, so that the obtained structure has a key effect. Too much graphene oxide introduction can cause VS growth on the surface of the graphene oxide4The bent nano rod becomes very sparse, even the VS is not distributed on the surface of partial graphene oxide4And bending the nanorods. Too little graphene oxide introduction can cause VS growth on the graphene oxide surface4The nanorods became very dense, even partially VS4The bent nanorods cannot grow on the surface of graphene oxide;
(6) reaction time VS4The method has the key effect of obtaining the structure that the bent nanorod is evenly paved on the surface of the reduced graphene oxide, and VS is easy to appear in a reaction product due to too short reaction time2A nanoplate heterofacies;
(7)VS4in the process of in-situ growth on the surface of the reduced graphene oxide, the surface functional group of the reduced graphene oxide and the synergistic effect of a temperature field and a pressure field generated by hydrothermal reaction enable chemical bonding to be formed between vanadium tetrasulfide and the reduced graphene oxide;
(8) the products prepared by the present invention have a unique composite structure, wherein VS4The graphene oxide is loaded on the surface of the reduced graphene oxide in a flat-laid mode, crystal structures arranged along the (110) crystal plane orientation are fully exposed, and the (110) crystal plane has the largest crystal plane spacing and is used as a channel between a metal ion access chain, so that the metal ion VS is very facilitated4Inter-chain storage and transmission. The reduced graphene oxide can be used in the charge-discharge processProviding a good conductive network, but also VS4The volume change during the charge and discharge process provides a buffer space. VS4And the chemical bonding effect between the graphene oxide and the reduced graphene oxide can further stabilize the structure and accelerate the transmission of charges between the graphene oxide and the reduced graphene oxide. Under the synergistic effect of the structural advantages, the vanadium tetrasulfide @ reduced graphene oxide electrode can show excellent cycle performance and rate 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 in the thickness direction of a product prepared in example 1 of the present invention.
FIG. 4 is a planar super-scanning electron micrograph of a product prepared in example 1 of the present invention.
FIG. 5 is a high power transmission electron micrograph of the product prepared in example 1 of the present invention.
FIG. 6 is a high resolution TEM image of the product prepared in example 1 of the present invention.
FIG. 7 is a TEM-EDS profile of the product of example 1 according to the invention.
Fig. 8 is a scanning electron microscope image of a product obtained after the addition amount of graphene oxide in embodiment 1 of the present invention is reduced to 20 mg.
Fig. 9 is a scanning electron microscope image of a product obtained after increasing the addition amount of graphene oxide to 120mg in example 1 of the present invention.
FIG. 10 is a scanning electron micrograph of the product obtained after the reaction time in example 1 of the present invention was shortened to 6 hours.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1:
the method comprises the following steps: weighing 50mg of graphene oxide, adding the graphene oxide into 60ml of deionized water, and carrying out ultrasonic treatment for 2.0h at the ultrasonic power of 400-600W to obtain a uniformly dispersed black solution A.
Step two: and (3) weighing 1.0g of sodium metavanadate and 3.6g of thioacetamide, simultaneously adding the sodium metavanadate and the thioacetamide into the solution A, and magnetically stirring the solution A for 30min at the rotating speed of 500r/min to obtain a solution B.
Step three: pouring the solution B into a reaction inner liner, sealing, then placing the inner liner in an outer kettle, fixing, placing in a homogeneous reactor with a filling ratio of 60%, and then reacting at 180 ℃ for 24h under the condition of a rotation speed of 10 r/min.
Step four: and after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, taking out a cooled product after the reaction, and collecting the product after alternately cleaning water and alcohol for 6 times.
Step five: and (3) freezing the collected product in a cold well of a freeze dryer under the following freezing conditions: freezing for 4h at the temperature of minus 50 ℃, then placing the frozen product in a tray, covering a sealing cover, vacuumizing to 20Pa, drying for 18h, and collecting the product to obtain the vanadium tetrasulfide @ reduced graphene oxide composite powder.
Example 2:
the method comprises the following steps: weighing 20mg of graphene oxide, adding the graphene oxide into 58ml of deionized water, and carrying out ultrasonic treatment for 1.5h at the ultrasonic power of 400W to obtain a uniformly dispersed black solution A;
step two: weighing 0.9g of sodium metavanadate and 3.5g of thioacetamide, simultaneously adding the sodium metavanadate and the thioacetamide into the solution A, and magnetically stirring the solution A for 30-60 min at the rotating speed of 400r/min to obtain a solution B;
step three: pouring the solution B into a reaction inner liner, sealing, then placing the inner liner in an outer kettle, fixing, placing in a homogeneous reactor with a filling ratio of 58%, and then reacting at 175 ℃ for 12h under the condition of a rotating speed of 5 r/min;
step four: after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, then taking out a cooled product after the reaction, and collecting the product after washing the product with water and alcohol alternately for 4 times;
step five: and (3) freezing the collected product in a cold well of a freeze dryer under the following freezing conditions: freezing for 2h at minus 60 ℃, then placing the frozen product in a tray, covering a sealing cover, vacuumizing to 10Pa, drying for 12h, and collecting the product to obtain the vanadium tetrasulfide @ reduced graphene oxide composite powder.
Example 3:
the method comprises the following steps: weighing 120mg of graphene oxide, adding the graphene oxide into 62ml of deionized water, and carrying out ultrasonic treatment for 2.5h with the ultrasonic power of 600W to obtain a uniformly dispersed black solution A;
step two: weighing 1.1g of sodium metavanadate and 3.7g of thioacetamide, simultaneously adding the sodium metavanadate and the thioacetamide into the solution A, and magnetically stirring the solution A for 60min at the rotating speed of 600r/min to obtain a solution B;
step three: pouring the solution B into a reaction inner liner, sealing, then placing the inner liner in an outer kettle, fixing, placing in a homogeneous reactor with a filling ratio of 62%, and then reacting at 185 ℃ for 30h under the condition of a rotating speed of 10 r/min;
step four: after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, then taking out a cooled product after the reaction, and collecting the product after water and alcohol are alternately cleaned for 10 times;
step five: and (3) freezing the collected product in a cold well of a freeze dryer under the following freezing conditions: freezing for 5h at minus 40 ℃, then placing the frozen product in a tray, covering a sealing cover, vacuumizing to 20Pa, drying for 18h, and collecting the product to obtain the vanadium tetrasulfide @ reduced graphene oxide composite powder.
Example 4:
the method comprises the following steps: weighing 70mg of graphene oxide, adding the graphene oxide into 60ml of deionized water, and carrying out ultrasonic treatment for 2 hours at the ultrasonic power of 500W to obtain a uniformly dispersed black solution A;
step two: weighing 1g of sodium metavanadate and 3.6g of thioacetamide, simultaneously adding the sodium metavanadate and the thioacetamide into the solution A, and magnetically stirring the mixture for 45min at the rotating speed of 500r/min to obtain a solution B;
step three: pouring the solution B into a reaction inner liner, sealing, then placing the inner liner in an outer kettle, fixing, placing in a homogeneous reactor with a filling ratio of 60%, and then reacting at 180 ℃ for 20h under the condition of a rotating speed of 7 r/min;
step four: after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, then taking out a cooled product after the reaction, and collecting the product after water and alcohol are alternately cleaned for 7 times;
step five: and (3) freezing the collected product in a cold well of a freeze dryer under the following freezing conditions: freezing at the temperature of minus 50 ℃ for 3h, then placing the frozen product in a tray, covering a sealing cover, vacuumizing to 15Pa, drying for 15h, and collecting the product to obtain the vanadium tetrasulfide @ reduced graphene oxide composite powder.
As shown in FIG. 1, all diffraction peaks are substantially well matched to VS4Standard card PDF # 72-1294. The diffraction peak of the reduced graphene oxide cannot be observed in fig. 1 because the content of the reduced graphene oxide is small and the crystallinity is low.
As shown in FIG. 2, the composite powder is composed of irregular nano-sheets, reduced graphene oxide is arranged in the nano-sheets, and VS is arranged on the surface of the nano-sheets4And bending the nanorods.
As shown in FIG. 3, the thickness of the reduced graphene oxide inside the nanosheets is 5-15 nm.
As shown in FIG. 4, VS4The bent nanorods are uniformly distributed on the surface of the reduced graphene oxide in a tiled mode, and VS4The bent nanorod has a diameter of 20-50 nm and a length of 50-150 nm.
As shown in FIG. 5, VS4The bent nanorods are uniformly distributed on the surface of the reduced graphene oxide in a tiled mode, and the reduced graphene oxide has an ultrathin structure.
As shown in fig. 6. The normalized VS is clearly seen in the figure4(110) The lattice fringes of the lattice were distributed over the entire nanorod, indicating VS4The nanorods have high crystallinity and are arranged along the (110) crystal plane orientation.
As shown in fig. 7. From the figure, we can see that the C, V and S elements are uniformly distributed in the sample region, further confirming VS4The bent nanorods are uniformly distributed on the surface of the reduced graphene oxide in a tiled mode.
As shown in fig. 8. From the figure, a more dense VS can be observed4The flexible nanorod is loaded on the surface of the reduced graphene oxide.
As shown in fig. 9. VS loaded on the surface of the reduced graphene oxide can be observed from the figure4The bent nanorods become less.
As shown in fig. 10. As can be seen from the figure, VS appeared in the product2Heterofacies of the nanoplatelets.
Claims (8)
1. A preparation method of vanadium tetrasulfide @ reduced graphene oxide composite powder is characterized by comprising the following steps of;
the method comprises the following steps: weighing 20-120 mg of graphene oxide, adding the graphene oxide into 58-62 ml of deionized water, and carrying out ultrasonic treatment for 1.5-2.5 h to obtain a uniformly dispersed black solution A;
step two: weighing 0.9-1.1 g of sodium metavanadate and 3.5-3.7 g of thioacetamide, simultaneously adding the sodium metavanadate and the thioacetamide into the solution A, and magnetically stirring for 30-60 min to obtain a solution B;
step three: pouring the solution B 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 175-185 ℃ for 12-30 h under the condition of a rotating speed of 5-10 r/min;
step four: after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, taking out a cooled product after the reaction, and collecting the product after water and alcohol are alternately cleaned for 4-10 times;
step five: 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 vanadium tetrasulfide @ reduced graphene oxide composite powder;
the composite powder consists of irregular sheets, the reduced graphene oxide with few layers is arranged inside the sheets, the surfaces of the sheets consist of uniform bent nanorods with the diameters of 20-50 nm and the lengths of 50-150 nm, and VS is arranged on the surfaces of the sheets4The bent nanorods have high crystallinity and orientation arrangement along the (110) crystal plane direction.
2. The preparation method of vanadium tetrasulfide @ reduced graphene oxide composite powder according to claim 1, wherein in the first step, the ultrasonic power is 400-600W, and the preparation method is performed at normal temperature.
3. The preparation method of vanadium tetrasulfide @ reduced graphene oxide composite powder according to claim 1, wherein the rotation speed of magnetic stirring in the second step is 400-600 r/min, and the magnetic stirring is performed at normal temperature.
4. The preparation method of vanadium tetrasulfide @ reduced graphene oxide composite powder according to claim 1, wherein the filling ratio of the solution B poured into the reaction lining in the third step is 58-62%.
5. The preparation method of vanadium tetrasulfide @ reduced graphene oxide composite powder according to claim 1, wherein water and alcohol are alternately cleaned in the step four by suction filtration or centrifugation, and collection is performed by suction filtration or centrifugation.
6. The preparation method of vanadium tetrasulfide @ reduced graphene oxide composite powder according to claim 1, wherein the freezing conditions in the fifth step are as follows: freezing for 2-5 h at-60 to-40 ℃.
7. The preparation method of vanadium tetrasulfide @ reduced graphene oxide composite powder according to claim 1, wherein the product obtained in the fifth step is sealed by a preservative film before being placed in a tray for drying, and the preservative film is perforated to ensure sufficient drying under a low pressure condition.
8. The vanadium tetrasulfide @ reduced graphene oxide composite powder obtained by the preparation method of any one of claims 1 to 7 is applied to the field of lithium ion batteries or sodium ion batteries or the field of photocatalysis or electrocatalysis.
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| CN110247050A (en) * | 2019-06-21 | 2019-09-17 | 东北大学 | A method of four vanadic sulfides/graphene composite material is prepared using containing vanadium leachate |
| CN111354931A (en) * | 2020-03-09 | 2020-06-30 | 天津师范大学 | Lithium-sulfur battery positive electrode composite material with high active substance content and preparation method and application thereof |
| CN111874950B (en) * | 2020-07-31 | 2022-07-29 | 陕西科技大学 | Vanadium-doped tungsten disulfide/graphene oxide composite electrode material and preparation method and application thereof |
| CN112490438B (en) * | 2020-11-27 | 2022-03-11 | 青岛科技大学 | Mo-VS4Positive electrode material of/N-GNTs magnesium ion battery |
| CN113247949B (en) * | 2021-04-30 | 2023-04-14 | 哈尔滨理工大学 | Preparation and application of three-dimensional rosette vanadium sulfide nanosheet sphere-reduced graphene oxide composite material |
| CN114162874B (en) * | 2021-12-09 | 2023-03-10 | 中国科学技术大学 | Preparation method of composite metal sulfide loaded mixed carbon material serving as sulfur main body material of lithium-sulfur battery |
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