CN114920294A - Double-layer structure V 2 O 5 Nano-belt electrode material and preparation method and application thereof - Google Patents

Double-layer structure V 2 O 5 Nano-belt electrode material and preparation method and application thereof Download PDF

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CN114920294A
CN114920294A CN202210525573.0A CN202210525573A CN114920294A CN 114920294 A CN114920294 A CN 114920294A CN 202210525573 A CN202210525573 A CN 202210525573A CN 114920294 A CN114920294 A CN 114920294A
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陈亚
封建邦
王龙君
姜源鹤
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Abstract

The invention relates to a double-layer structure V 2 O 5 A nano-belt electrode material and a preparation method and application thereof belong to the technical field of electrochemistry. The preparation method of the electrode material is that KVO is used for hydrothermal synthesis 3 The method comprises the steps of taking potassium dodecyl sulfate as a raw material, adjusting the pH value of a solution to be about 3.5, preparing a uniform solution, and then transferring the solution to a hydrothermal reaction kettle lined with polytetrafluoroethylene for hydrothermal synthesis at a certain temperature. Finally filtering, washing and drying to obtain a double-layer structure V 2 O 5 A nanoribbon. The invention is madeThe preparation process is simple, the conditions are mild, the preparation method is easy to realize, and the obtained material has good zinc storage performance.

Description

Double-layer structure V 2 O 5 Nano-band electrode material and preparation method and application thereof
Technical Field
The invention relates to a double-layer structure V 2 O 5 Nano-band electrode material and preparation method and application thereofBelonging to the technical field of electrochemistry.
Background
The rapid development of the current society has raised many problems related to resources, energy and environment, such as the demand for electricity rapidly increasing in people's lives and business activities. Therefore, the demand for various energy storage devices is increasing, and the water system zinc ion battery is receiving attention as a high-performance energy storage device. Since the research on such batteries has been receiving wide attention in recent years, the current research progress is in the early stage, and the performance of the batteries still needs to be improved. At present, the continuous research and development of the anode material with high structural stability and excellent electrochemical performance is the primary task of research.
Therefore, the continuous research and development of cathode materials with high structural stability and excellent electrochemical performance is a primary task of research. Vanadium pentoxide (V) 2 O 5 ) The anode material used as the anode material of the water system zinc ion battery has wide application prospect due to the characteristics of rich resources, low cost, high theoretical specific capacity and the like. But the poor conductivity and structural stability of the material lead to the fact that the actual measured specific capacity is far from the theoretical specific capacity, and the cycle performance is still to be improved, and the factors finally limit the V 2 O 5 The zinc oxide is practically applied as a positive electrode material of an aqueous zinc ion battery. Therefore, at present, there is still a need to find a V with mild conditions and simple operation 2 O 5 The preparation method of the nanobelt material expands the interlayer spacing of the crystal face of the material (001) and adopts Zn in charge-discharge reaction 2+ The de-intercalation in the positive electrode material provides a large interlayer spacing, thereby improving the zinc storage performance of the material.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a crystal face with the interlayer spacing of (001)
Figure BDA0003644309250000011
Double-layer structure V of 2 O 5 A nanoribbon electrode material.
The invention relates to a double-layer structure V 2 O 5 A nanoribbon electrode material, the double-layer structure V 2 O 5 Nano-band electrode materialIs KVO 3 And C 12 H 25 KO 4 S aqueous solution is synthesized under hydrothermal condition; in the obtained material, the interlayer spacing of the (001) crystal face is
Figure BDA0003644309250000012
The invention relates to a method for preparing a double-layer structure V 2 O 5 A method of preparing a nanoribbon electrode material, comprising the steps of:
step one
Adding KVO into deionized water 3 Stirring uniformly to obtain a mixed solution 1;
step two
Adding potassium dodecyl sulfate into deionized water, and uniformly stirring to obtain a mixed solution 2;
step three
Adding the mixed solution 2 formed in the step two into the mixed solution 1 formed in the step one, and uniformly stirring to obtain a mixed solution 3;
step four
Adding a pH regulator into the mixed solution 3 obtained in the step three until the pH of the mixed solution is 3.2-3.8 or 5.8-6.2, and uniformly stirring to obtain a mixed solution 4;
step five
Transferring the mixed solution 4 obtained in the step four to a hydrothermal reaction kettle lined with polytetrafluoroethylene for hydrothermal treatment; the temperature of the hydrothermal treatment is 175-205 ℃;
step six
After the reaction is finished, cooling, carrying out solid-liquid separation, washing and drying the obtained solid to obtain the double-layer structure V 2 O 5 A nanoribbon material.
The invention relates to a double-layer structure V 2 O 5 The method of preparing nano-belt electrode material includes the first step of mixing KVO 3 Dissolving in water to obtain potassium metavanadate water solution; KVO in the mixed solution 1 3 The salt concentration is 0.001 to 0.05mol/L, preferably 0.01 to 0.05 mol/L. In industrial application, in the step one, potassium metavanadate is added into deionized water and stirred uniformly at 30-60 ℃ to obtain potassium metavanadateAn aqueous solution.
The invention relates to a double-layer structure V 2 O 5 A method for preparing a nano-belt electrode material, in the second step, organic matter C is contained in the mixed solution 2 12 H 25 KO 4 The concentration of S is 0.001-0.05 mol/L, preferably 0.01-0.02 mol/L.
The invention relates to a double-layer structure V 2 O 5 The method of preparing nano-belt electrode material comprises the third step, in the mixed solution 3, KVO 3 And C 12 H 25 KO 4 The mass ratio of S is 50-1: 1, optimized to be 2.0-2.5: 1.
the invention relates to a double-layer structure V 2 O 5 In the fourth step, 1mol/L hydrochloric acid is used for adjusting the pH value, and preferably, in the mixed solution 3, the volume ratio of the mixed solution 3 to the hydrochloric acid is 10-100: 1, further optimized as 35: 1.
the invention relates to a double-layer structure V 2 O 5 The method of the nano-belt electrode material comprises the fifth step, wherein the hydrothermal temperature is 175-205 ℃, and preferably 180-200 ℃. If the hydrothermal temperature is too high, the polytetrafluoroethylene lining of the stainless steel hydrothermal reaction kettle can be softened, and the deformation of the polytetrafluoroethylene lining can cause the quality of a product to be rapidly reduced along with the increase of the temperature, so that a reaction system becomes complicated, and the generation of materials is not facilitated.
The invention relates to a double-layer structure V 2 O 5 In the sixth step, solid-liquid separation is carried out during the suction filtration treatment; washing with ethanol and/or pure water after solid-liquid separation, wherein the drying temperature is 50-120 ℃, and preferably 70-100 ℃. The drying time is 5 hours or more. Preferably 10 hours.
In the obtained material, the interlayer spacing of the (001) crystal face is
Figure BDA0003644309250000032
The invention relates to a double-layer structure V 2 O 5 Application of nano-band electrode material, and application of composite electrode material as water-based zinc ion batteryThe positive electrode material is prepared from 2mol/L zinc sulfate electrolyte, and the specific mass capacity of active substances is 300-420 mAh/g.
As a further preference, the present invention is a two-layer structure V 2 O 5 The application of the nano-belt electrode material is characterized in that the electrode material is used as an anode material of a water-based zinc ion battery, and the specific mass capacity is 400-430 mAh/g in a 2mol/L electrolyte system when the current density is 0.5A/g.
The invention relates to a double-layer structure V 2 O 5 The electrode material with the nano-belt has the following electrochemical test conditions:
weighing appropriate amount of the above-prepared double-layer structure V 2 O 5 The nano-band electrode material is an active material, acetylene black (conductive agent), PVDF (binder, solvent is N-methyl pyrrolidone), and the ratio of the active material to the solvent is 7: 2: 1, then uniformly coated on a Ti foil (polish, washed with alcohol and pure water, dried), and vacuum-dried at 70 ℃ for 10 hours. The invention relates to a double-layer structure V which is designed and prepared by using glass fiber as a diaphragm and a zinc sheet as a negative electrode 2 O 5 The working electrode is assembled into a CR2032 button cell, and the test of cyclic voltammetry and constant current charge and discharge is carried out, wherein the test potential is 0.2-1.6V.
Principles and advantages
Principle of
The invention provides a method for preparing a double-layer structure V by a hydrothermal synthesis method 2 O 5 The nanometer electrode material is prepared through regulating pH value of solution and hydrothermal synthesis to decompose various matters in the liquid phase and to grow crystal, so as to produce V in homogeneous distribution under proper conditions 2 O 5 A nanoribbon. Meanwhile, the invention obtains the interlayer spacing of the (001) crystal face by selecting raw materials, controlling the dosage of each material, the reaction temperature and the pH value
Figure BDA0003644309250000033
Of a double-layer structure V 2 O 5 A nanoribbon electrode material.
The advantages are that:
compared with the prior preparation process, the preparation method has the following technical advantages:
(1) in the invention, a proper amount of potassium dodecyl sulfate is added as a buffering agent in the hydrothermal process, so that the morphology and the crystal structure of a generated product can be effectively regulated and controlled, and a double-layer structure V is generated 2 O 5 Nanoribbons and the resulting V 2 O 5 001) interplanar spacing of nanoribbons
Figure BDA0003644309250000031
(2) The invention can generate the double-layer structure V by using the hydrothermal condition with proper parameters 2 O 5 The nano-belt has larger interlayer spacing and is beneficial to Zn 2+ Is embedded and separated in the charging and discharging process, so that the double-layer structure V is formed 2 O 5 The nanobelt material shows good zinc storage performance.
(3) The electrode material is prepared by a one-step hydrothermal synthesis method, the process flow is simple, the operation is easy, the requirements on equipment and environment are low, and the time is saved.
Drawings
FIG. 1 shows a bilayer structure V prepared in example 1 2 O 5 Cyclic voltammograms of nanoribbon electrode materials.
FIG. 2 shows a two-layer structure V of example 1 2 O 5 The battery made of the nano-belt electrode material has a cycle performance diagram under different multiplying power (0.5A/g-10A/g).
FIG. 3 shows a double-layer structure V of example 1 2 O 5 XRD pattern of the nanoribbon electrode material.
FIG. 4 shows a two-layer structure V of example 1 2 O 5 SEM images of the nanobelt electrode material;
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specified, the reagents and materials used in the present invention are commercially available products or products obtained by a known method.
The specific implementation mode of the invention is as follows: the present invention is further illustrated by the specific examples.
Example 1
0.276g of KVO was weighed 3 Placed in pure water, and then magnetically stirred at 50 ℃ for 20 minutes to obtain a mixed solution 1. 0.11g of C was weighed 12 H 25 KO 4 S (potassium dodecyl sulfate) is put into pure water and stirred for 20 minutes by magnetic force. Then, the mixed solution 2 was poured into the mixed solution 1, and 1.5ml of hydrochloric acid was added to adjust the pH of the solution to about 3.5. And then transferring the prepared mixed solution to a stainless steel hydrothermal reaction kettle with polytetrafluoroethylene for hydrothermal treatment at 180 ℃ for 12 hours. After the reaction is finished, washing the reaction product by using ethanol and pure water, and drying the reaction product in vacuum at 70 ℃ for 12 hours to obtain a double-layer structure V 2 O 5 A nanoribbon; obtained V 2 O 5 001) interplanar spacing of nanoribbons
Figure BDA0003644309250000041
The obtained material is prepared into an electrode serving as a positive electrode material, a zinc sheet serving as a negative electrode and 2mol/LZnSO 4 And (3) assembling the electrolyte and the glass fiber diaphragm into a CR2032 button cell, and performing electrochemical test after activating for 12 hours. The test voltage window is 0.2-1.6V. The cyclic voltammogram of this electrode at a scan rate of 0.5mv/s is shown in FIG. 1. The mass specific capacity of the electrode material active substance prepared from the material is 425mAh/g when the current density is 0.5A/g through constant current charge-discharge test calculation, and the electrode material active substance has better rate capability as shown in figure 2.
To the double-layer structure V obtained by drying 2 O 5 XRD and SEM analysis of the material are shown in figures 3 and 4.
Comparative example 1:
the procedure and other conditions were the same as in the first experimental example, with the following different parameters:
the hydrothermal temperature is changed to 160 ℃;
the mass specific capacitance of the electrode active substance prepared by the material is 195mAh/g when the current density is 0.5A/g through constant current charge-discharge test.
Example 2:
the operation process and other conditions were the same as in the experimental example one, and the different condition parameters were as follows:
the hydrothermal temperature is changed to 200 ℃; obtained V 2 O 5 The (001) interplanar spacing of the nanoribbons is about
Figure BDA0003644309250000051
The mass specific capacitance of the electrode active substance prepared by the material is 340mAh/g when the current density is 0.5A/g through constant current charge-discharge test.
Comparative example 2:
the procedure and other conditions were the same as in the first experimental example, with the following different parameters:
the hydrothermal temperature is changed to 220 ℃; obtained V 2 O 5 001) interplanar spacing of nanoribbons
Figure BDA0003644309250000052
The mass specific capacitance of the electrode active substance prepared by the material is 255mAh/g when the current density is 0.5A/g through constant current charge-discharge test.
Comparative example 3
The operation process and other conditions were the same as in the experimental example one, and the different condition parameters were as follows:
the material is prepared by hydrothermal synthesis without adding potassium dodecyl sulfate. The obtained material is prepared into an electrode, and the mass specific capacitance of the electrode active substance prepared from the material is 240mAh/g when the current density is 0.5A/g through constant current charge-discharge test.
Example 3
The other conditions were the same as in example 1, except that: adding 0.31g of potassium dodecyl sulfate; (ii) a Obtained V 2 O 5 The (001) interplanar spacing of the nanoribbons was about
Figure BDA0003644309250000053
The mass specific capacity of the active material of the electrode material prepared by the material is 310mAh/g when the current density is 0.5A/g through constant current charge-discharge test.
Comparative example 4
The other conditions were the same as in example 1 except that: adding 0.05g of potassium dodecyl sulfate; (ii) a Obtained V 2 O 5 001) interplanar spacing of nanoribbons
Figure BDA0003644309250000061
The mass specific capacity of the electrode material active substance prepared from the material is 210mAh/g when the current density is 0.5A/g through constant current charge-discharge test.
Comparative example 5
The other conditions were the same as in example 1 except that: using 0.362gV 2 O 5 Alternative KVO in example 1 3 (ii) a Hydrothermal treatment at 180 ℃ for 10 hours. Obtained V 2 O 5 001) interplanar spacing of nanoribbons
Figure BDA0003644309250000062
The mass specific capacity of the active material of the electrode material prepared by the material is 330mAh/g when the current density is 0.5A/g through constant current charge-discharge test.
Comparative example 6
The other conditions were the same as in example 1 except that: then, the mixed solution 2 is poured into the mixed solution 1, and hydrochloric acid is added to adjust the pH of the solution to about 2. The obtained material is a tunnel structure K 0.51 V 2 O 5 。
The mass specific capacity of the electrode material active substance prepared from the material is calculated to be 305mAh/g when the current density is 0.5A/g through constant current charge-discharge test.
Comparative example 7
The other conditions were the same as in example 1 except that: then, the mixed solution 2 is poured into the mixed solution 1, and hydrochloric acid is added to adjust the pH of the solution to about 5. The resulting materialFor tunnel construction K 0.51 V 2 O 5 。
The mass specific capacity of the electrode material active substance prepared by the material is 155mAh/g when the current density is 0.5A/g through constant current charge-discharge test.
Comparative example 8
The other conditions were the same as in example 1 except that: the mixed solution 2 was then poured into the mixed solution 1, and hydrochloric acid was added to adjust the pH of the solution to 6. The obtained material is a tunnel structure K 2 V 8 O 16 。
The mass specific capacity of the active substance of the electrode material prepared by the material is 355mAh/g when the current density is 0.5A/g through constant current charge-discharge test.
Comparative example 9
The other conditions were the same as in example 1, except that: 0.242g of NaVO was weighed out 3 Placed in pure water, and then magnetically stirred at 50 ℃ for 20 minutes to obtain a mixed solution 1. 0.576g of C are weighed 12 H 25 NaO 4 S (sodium dodecyl sulfate) was placed in pure water and stirred magnetically for 20 minutes.
The mass specific capacity of the active material of the electrode material prepared by the material is 365mAh/g when the current density is 0.5A/g through constant current charge-discharge test.
Comparative example 10
The other conditions were identical to those of example 1 except that: 0.362gV instead of potassium dodecyl sulfate and potassium metavanadate 2 O 5 The powder was dissolved in 50ml of pure water and 5ml of hydrogen peroxide (30%) was added. Obtained V 2 O 5 The (001) interplanar spacing of the nanoribbons is about
Figure BDA0003644309250000071
The mass specific capacity of the active substance of the electrode material prepared by the material is 350mAh/g when the current density is 0.5A/g through constant current charge-discharge test.

Claims (10)

1. Bilayer structure V 2 O 5 The nano-band electrode material is prepared by the following steps,the method is characterized in that: the double-layer structure V 2 O 5 The nano-band electrode material is KVO 3 And C 12 H 25 KO 4 S aqueous solution is synthesized under hydrothermal condition; in the obtained material, the distance between (001) crystal plane layers is
Figure FDA0003644309240000011
2. A method for preparing the double-layer structure V2O5 nanobelt electrode material of claim 1, characterized by comprising the steps of:
step one
Adding KVO into deionized water 3 Stirring uniformly to obtain a mixed solution 1;
step two
Adding potassium dodecyl sulfate into deionized water, and uniformly stirring to obtain a mixed solution 2;
step three
Adding the mixed solution 2 formed in the step two into the mixed solution 1 formed in the step one, and uniformly stirring to obtain a mixed solution 3;
step four
Adding a pH regulator into the mixed solution 3 obtained in the step three until the pH of the mixed solution is 3.2-3.8, and uniformly stirring to obtain a mixed solution 4;
step five
Transferring the mixed solution 4 obtained in the step four to a hydrothermal reaction kettle lined with polytetrafluoroethylene for hydrothermal treatment; the temperature of the hydrothermal treatment is 175-205 ℃;
step six
After the reaction is finished, cooling, carrying out solid-liquid separation, washing and drying the obtained solid to obtain the double-layer structure V 2 O 5 A nanoribbon material.
3. A method of preparing a bilayer structure V according to claim 2 2 O 5 A method of producing a nanoribbon electrode material, comprising: KVO in the mixed solution 1 3 The concentration of (b) is 0.001-0.05 mol/L.
4. A method of preparing a bilayer structure V according to claim 2 2 O 5 A method of producing a nanoribbon electrode material, comprising: in step two, C 12 H 25 KO 4 C in S mixed solution 12 H 25 KO 4 The concentration of S is 0.01-0.05 mol/L.
5. A method of preparing a bilayer structure V according to claim 2 2 O 5 A method of producing a nanoribbon electrode material, comprising: KVO3 and C in step three 12 H 25 KO 4 The mass ratio of S is 50-1: 1.
6. a method of preparing a bilayer structure V according to claim 2 2 O 5 A method for preparing a nano-belt electrode material, which is characterized by comprising the following steps: in the fourth step, 1mol/L hydrochloric acid is used for adjusting the pH value.
7. A method of preparing a bilayer structure V according to claim 2 2 O 5 A method for preparing a nano-belt electrode material, which is characterized by comprising the following steps: and fifthly, the hydrothermal temperature is 180-200 ℃, and the hydrothermal time is 12-24 hours.
8. A method of preparing a bilayer structure V according to claim 2 2 O 5 A method of producing a nanoribbon electrode material, comprising: in the sixth step, solid-liquid separation is realized through suction filtration; after solid-liquid separation, washing with ethanol and/or pure water, and drying at 50-120 deg.C for more than 5 hr.
9. A method of preparing a bilayer structure V according to claim 1 2 O 5 The application of the nano-belt electrode material is characterized in that: the electrode material is used as a positive electrode material of a water-based zinc ion battery, and the specific mass capacity of an active substance in a 2mol/L electrolyte system is 300-430 mAh/g.
10. The method of claim 1Preparation of double-layer structure V 2 O 5 The application of the nano-belt electrode material is characterized in that: the electrode material is used as an anode material of an aqueous zinc ion battery, and the specific mass capacity is 400-430 mAh/g when the current density is 0.5A/g in a 2mol/L electrolyte system.
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