CN110282660B - Nano rod-shaped vanadium tetrasulfide powder and preparation method and application thereof - Google Patents
Nano rod-shaped vanadium tetrasulfide powder and preparation method and application thereof Download PDFInfo
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- H—ELECTRICITY
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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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Abstract
The invention discloses a method for preparing nano rod-shaped vanadium tetrasulfide powder, which comprises the following steps: (1) taking thioacetamide to dissolve in absolute ethyl alcohol, and stirring until the thioacetamide is completely dissolved to obtain a mixture A; (2) adding ammonium metavanadate into the mixture A, and stirring until the ammonium metavanadate is completely dissolved to obtain a mixture B; (3) dripping dilute hydrochloric acid into the mixture B under the stirring condition to form a transparent solution, so as to obtain a mixture C; (4) transferring the mixture C into a hydrothermal reaction kettle, and carrying out hydrothermal reaction for 24-25 h; (5) naturally cooling after the reaction is finished, centrifugally washing for a plurality of times, and drying in vacuum to obtain the nano rod-shaped vanadium tetrasulfide powder. The nano rod-shaped vanadium tetrasulfide prepared by the method has the advantages of higher specific capacity, excellent cycling stability, long service life and higher conductivity.
Description
Technical Field
The invention relates to the field of battery materials, in particular to nano rod-shaped vanadium tetrasulfide powder and a preparation method and application thereof.
Background
Currently, the main problem of the ion battery is still the research and design of the high-performance cathode material.
Graphite is widely applied to ion batteries as a negative electrode material, but the actual specific capacity of the graphite negative electrode material is relatively low, so that the ever-increasing energy storage requirement of people is difficult to meet.
In order to find suitable negative electrode materials for ion batteries, related researchers have extensively explored a range of compounds. Of these negative electrode materials, researchers generally consider metal sulfides with high theoretical capacity to be a very promising candidate, and the control of their nanostructure is a very important strategy to further improve their electrochemical performance.
Vanadium tetrasulfide has attracted the attention of many researchers due to its similar unique two-dimensional layered structure. Such a chalcogenide with a quasi-two-dimensional layered structure is typically a sandwich structure, i.e. a transition metal layer V is sandwiched between two S layers. In the crystal structure, each V atom in the S-V-S layer is in six coordination in an octahedron, covalent bonds are formed between the V-S atoms, and the layers are connected by Van der Waals force. This structure makes the compound have strong intra-layer bonding effect, and relatively weak interaction force between layers, and the gaps between the layers can allow the entry of foreign substances. The layered transition metal sulfide as the lithium/sodium ion negative electrode material has the greatest advantages of providing a good lithium/sodium ion diffusion channel, buffering the volume expansion generated during the process of lithium/sodium removal/insertion in the circulation process, and being one of the lithium/sodium ion battery negative electrode materials with a good development prospect.
Although vanadium tetrasulfide has higher theoretical capacity, excellent charge-discharge rate performance and cycle performance based on the above special physical characteristics, vanadium tetrasulfide also has some disadvantages, and the vanadium tetrasulfide has the characteristics of low conductivity and large volume change in the lithium ion intercalation/extraction process like other transition metal sulfides, thereby hindering VS4Becomes a high-performance electrode material, Three-dimensional VS4/graphene hierarchical architecture as high-capacity anode for lithium-ion batteries，Lithium reaction mechanism and high rate capability ofVS4The literature of graphene nanocomposites as an anode material for lithium batteries has been reported.
Therefore, how to provide VS with high conductivity and small volume change4Electrode materials are a technical problem that those skilled in the art need to solve.
Disclosure of Invention
In view of this, the invention provides a method for preparing nano rod-shaped vanadium tetrasulfide, and the prepared nano rod-shaped vanadium tetrasulfide has high specific capacity, excellent cycling stability, long service life and high conductivity.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing nano rod-shaped vanadium tetrasulfide powder comprises the following steps:
(1) taking thioacetamide to dissolve in absolute ethyl alcohol, and stirring until the thioacetamide is completely dissolved to obtain a mixture A;
(2) adding ammonium metavanadate into the mixture A, and stirring until the ammonium metavanadate is completely dissolved to obtain a mixture B;
(3) dripping dilute hydrochloric acid into the mixture B under the stirring condition to form a transparent solution, so as to obtain a mixture C;
(4) transferring the mixture C into a hydrothermal reaction kettle, and carrying out hydrothermal reaction for 24-25 h;
(5) naturally cooling after the reaction is finished, centrifugally washing for a plurality of times, and drying in vacuum to obtain the nano rod-shaped vanadium tetrasulfide powder.
Preferably, the thioacetamide: ammonium metavanadate: anhydrous ethanol: diluted hydrochloric acid (4-5) mmol: (0.5-1) mmol, (60-70) mL:1 mL.
Preferably, the thioacetamide: ammonium metavanadate: anhydrous ethanol: diluted hydrochloric acid ═ 5mmol:1 mmol: 70mL:1 mL.
Preferably, the dilute hydrochloric acid concentration is 20 wt%.
Preferably, the temperature of the hydrothermal reaction is controlled to be 180-190 ℃.
Preferably, the stirring in the step (1), the step (2) and the step (3) is magnetic stirring, the stirring speed is 300 r/min-400 r/min, the stirring time in the step (1) is 1-2 h, the stirring time in the step (2) is 1-2 h, and the stirring time in the step (3) is 0.5-1 h.
Preferably, the step (5) is specifically: and naturally cooling after the reaction is finished, centrifugally washing the reaction product for four times by using anhydrous absolute ethyl alcohol, centrifugally washing the reaction product for four times by using deionized water, and carrying out vacuum drying for 12-13 h.
A nano rod-shaped vanadium tetrasulfide powder is a nano rod-shaped structure with the diameter of 20-60 nm and the length of 1-2 um.
The application of the nano rod-shaped vanadium tetrasulfide powder prepared by the method is applied to the field of sodium/lithium/magnesium ion batteries or photocatalysis.
Compared with the prior art, the invention has the beneficial effects that:
1. the high sulfur content of vanadium tetrasulfide enables it to exhibit significant Li-S characteristics in lithium ion energy storage, and thus VS4The specific capacity is higher; the preparation method effectively inhibits the agglomeration problem of the nano rod-shaped vanadium tetrasulfide in the crystallization process by adding a certain amount of dilute hydrochloric acid. By adjusting the using amount of dilute hydrochloric acid, a certain amount of H is obtained+Thereby controlling VS4The more the amount of the dilute hydrochloric acid is, the less the agglomeration phenomenon is, and when 1mL of the dilute hydrochloric acid is reached, the agglomeration phenomenon basically disappears.
2. The change in solvent affects the shape of the material, e.g. echinoid VS4Octopus-like VS4Sea weed like VS4Flower-like VS4The shape difference is caused by different solvents, and the invention uses absolute ethyl alcohol as the solvent to prepare the rod-shaped VS for the first time4The absolute ethyl alcohol is used as a reaction solvent mainly for inhibiting the hydrolysis rate of vanadate, so that the growth rate can be effectively controlled.
3. The nano rod-shaped vanadium tetrasulfide is shown to have excellent cycling stability and longer service life through an electrochemical performance test; the smaller internal impedance also shows that the nano rod-shaped vanadium tetrasulfide anode material has higher conductivity, and promotes the excellent electrochemical performance of the nano rod-shaped vanadium tetrasulfide anode material.
4. The preparation of the whole solution is carried out under the condition of continuous stirring. VS prepared by the invention4Has larger specific surface area, can well relieve the self-agglomeration and pulverization of the vanadium tetrasulfide nano rod, and can effectively promote VS4The electrochemical performance of (2). Meanwhile, the method is simple to operate, can be obtained through one-step hydrothermal reaction, and has the advantages of low reaction temperature, short reaction period and capability of preparing VS4The chemical components are uniform and the purity is high.
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 embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is an SEM image of nanorod vanadium tetrasulfide prepared in example 1 of the present invention;
FIG. 2 is a diagram illustrating an electrochemical impedance spectrum of nanorod vanadium tetrasulfide prepared in example 1 of the present invention;
FIG. 3 is a diagram illustrating the electrochemical performance of nano-rod vanadium tetrasulfide prepared in example 1 of the present invention as a negative electrode material of a lithium ion battery;
FIG. 4 is an SEM photograph of nano rod-shaped vanadium tetrasulfide prepared in comparative example 1 according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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.
Example 1
5mmol Thioacetamide (TAA) was added to 70mL absolute ethanol, followed by magnetic stirring for 1hIt is completely dissolved; then adding 1mmol of ammonium metavanadate under magnetic stirring, and continuing stirring for 1 hour to completely dissolve the ammonium metavanadate; adding 1mL of dilute hydrochloric acid under continuous stirring, and stirring for 0.5h to form a transparent solution; the stirring speed is 300 r/min-400 r/min, the obtained mixed solution is transferred to a polytetrafluoroethylene lining of a 100mL stainless steel high-pressure reaction kettle, the stainless steel high-pressure reaction kettle is sealed and put into a forced air drying oven to react for 24 hours at 180 ℃; naturally cooling to room temperature, centrifugally washing the obtained product four times by using anhydrous absolute ethyl alcohol, centrifugally washing the obtained product four times by using deionized water, and vacuum drying for 12 hours to obtain the nano rod-shaped vanadium tetrasulfide powder. Fig. 1 is an SEM image of the nanorod-shaped vanadium tetrasulfide prepared in this example. Confirms VS prepared in this example4Has the advantages of regular appearance, high purity and crystallinity and basically no disordered stacking phenomenon.
In order to further show the beneficial effects of the invention, the nano rod-shaped vanadium tetrasulfide prepared in example 1 is used as a lithium ion battery negative electrode material to carry out conductivity and electrochemical performance tests:
firstly, dissolving nano rod-shaped vanadium tetrasulfide, acetylene black and polyvinylidene fluoride in N-methyl pyrrolidone according to the mass fraction ratio of 8:1:1, stirring into uniform slurry, coating the uniform slurry on copper foil, drying in air at 80 ℃ for 0.5h, drying in vacuum at 110 ℃ for 12h, and then slicing and compacting to be used as a working electrode of a lithium ion battery; CR2032 button cells were assembled in a pure argon atmosphere using a lithium sheet as the counter electrode, a polypropylene membrane (Celgard 2400) as the separator, 1.0M lithium hexafluorophosphate ethylene carbonate/diethyl carbonate/dimethyl carbonate (volume ratio 1:1:1) as the electrolyte; and testing the ion battery on a LAND test system, wherein the charging and discharging voltage range is 0.01V-3V, and the charging and discharging current density of the lithium ion battery is 200 mA/g.
FIG. 2 is an electrochemical impedance spectrum, the frequency range of the test is 0.01 Hz-100 KHz, the charge transfer impedance (Rct) is represented by the semi-circle diameter of the high frequency region, and the relative size of the Warburg impedance (Zw) is represented by the slope of the low frequency region straight line. Demonstrates the nanorod-like VS prepared by the invention4The negative electrode has a small Rct value of about 100ohm and a small Zw value, which meansIs flavored with nano-rod-shaped VS4The negative electrode has good conductivity and high rate performance.
FIG. 3 is a diagram of the electrochemical performance of nano-rod vanadium tetrasulfide as a negative electrode material of a lithium ion battery. Demonstrates the nanorod-like VS prepared using the present invention4The first discharge specific capacity of the manufactured lithium ion battery reaches 574.3mAh g under the current density of 200mA/g-1After long circulation for 120 circles, reversible residual specific capacity can still be reserved to 439.3mAh g-1Still, the volume of the negative electrode material can account for 76.5% of the first specific capacity, and the volume change of the negative electrode material is small and the cycle life of the battery is long as can be seen from fig. 3.
Example 2
4mmol Thioacetamide (TAA) is added into 60mL absolute ethyl alcohol, and then the mixture is stirred by magnetic force for 2 hours to be completely dissolved; then adding 0.5mmol of ammonium metavanadate under magnetic stirring, and continuously stirring for 2 hours to completely dissolve the ammonium metavanadate; adding 1mL of dilute hydrochloric acid under continuous stirring, and stirring for 1h to form a transparent solution; the stirring speed is 300 r/min-400 r/min, the obtained mixed solution is transferred to a polytetrafluoroethylene lining of a 100mL stainless steel high-pressure reaction kettle, the stainless steel high-pressure reaction kettle is sealed and put into an air-blast drying oven to react for 23 hours at 190 ℃; naturally cooling to room temperature, centrifugally washing the obtained product four times by using anhydrous absolute ethyl alcohol, centrifugally washing the obtained product four times by using deionized water, and vacuum drying for 12 hours to obtain the nano rod-shaped vanadium tetrasulfide powder.
Comparative example 1
Adding 5mmol Thioacetamide (TAA) into 70mL absolute ethyl alcohol, and then stirring by magnetic force for 1h to completely dissolve the thioacetamide; then adding 1mmol of ammonium metavanadate under magnetic stirring, and continuing stirring for 1 hour to completely dissolve the ammonium metavanadate; adding 0.75mL of dilute hydrochloric acid under continuous stirring, and stirring for 0.5h to form a transparent solution; transferring the obtained mixed solution into a polytetrafluoroethylene lining of a 100mL stainless steel high-pressure reaction kettle, sealing the stainless steel high-pressure reaction kettle, and putting the stainless steel high-pressure reaction kettle into an air-blast drying oven to react for 24 hours at 180 ℃; naturally cooling to room temperature, centrifugally washing the obtained product four times by using anhydrous absolute ethyl alcohol, centrifugally washing the obtained product four times by using deionized water, and vacuum drying for 12 hours to obtain the nano rod-shaped vanadium tetrasulfide powder. FIG. 4 is a comparative example preparationSEM image of nanorod-like vanadium tetrasulfide of (a). Confirm that the part of the nano-rod VS prepared by the comparative example4Both bending growth and dimensional non-uniformity appear, which affects VS to some extent4The crystallinity of (a).
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (6)
1. A method for preparing nano rod-shaped vanadium tetrasulfide powder is characterized by comprising the following steps:
(1) taking thioacetamide to dissolve in absolute ethyl alcohol, and stirring until the thioacetamide is completely dissolved to obtain a mixture A;
(2) adding ammonium metavanadate into the mixture A, and stirring until the ammonium metavanadate is completely dissolved to obtain a mixture B;
(3) dripping dilute hydrochloric acid into the mixture B under the stirring condition to form a transparent solution, so as to obtain a mixture C;
(4) transferring the mixture C into a hydrothermal reaction kettle, and carrying out hydrothermal reaction for 24-25 h;
(5) naturally cooling after the reaction is finished, centrifugally washing for a plurality of times, and drying in vacuum to obtain nano rod-shaped vanadium tetrasulfide powder;
the thioacetamide: ammonium metavanadate: anhydrous ethanol: diluted hydrochloric acid (4-5) mmol: (0.5-1) mmol, (60-70) mL:1 mL; the concentration of the dilute hydrochloric acid is 20 wt%;
the temperature of the hydrothermal reaction is controlled to be 180-190 ℃.
2. The method for preparing nanorod vanadium tetrasulfide powder according to claim 1, wherein the thioacetamide: ammonium metavanadate: anhydrous ethanol: diluted hydrochloric acid ═ 5mmol:1 mmol: 70mL of: 1 mL.
3. The method for preparing nanorod vanadium tetrasulfide powder according to claim 1, wherein the stirring in the step (1), the step (2) and the step (3) is magnetic stirring, the stirring speed is 300r/min to 400r/min, the stirring time in the step (1) is 1 to 2 hours, the stirring time in the step (2) is 1 to 2 hours, and the stirring time in the step (3) is 0.5 to 1 hour.
4. The method for preparing nanorod-shaped vanadium tetrasulfide powder according to claim 3, wherein the step (5) specifically comprises: and naturally cooling after the reaction is finished, centrifugally washing the reaction product for four times by using absolute ethyl alcohol, centrifugally washing the reaction product for four times by using deionized water, and carrying out vacuum drying for 12-13 h.
5. The nanorod-shaped vanadium tetrasulfide powder prepared by the preparation method of any one of claims 1 to 4, wherein the nanorod-shaped vanadium tetrasulfide powder is of a nanorod-shaped structure with the diameter of 20-60 nm and the length of 1-2 um.
6. The use of the nano rod-shaped vanadium tetrasulfide powder according to claim 5 in the preparation of sodium ion batteries, lithium ion batteries, magnesium ion batteries or photocatalysts.
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| CN108726571A (en) * | 2018-07-02 | 2018-11-02 | 陕西科技大学 | A kind of VS4Nanometer rods/VS2Nanometer sheet three-dimensional self assembly hollow rod-shape composite granule and preparation method thereof |
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