CN113921805B - Preparation method of anion-doped vanadium trioxide positive electrode material for water-based zinc ion battery - Google Patents
Preparation method of anion-doped vanadium trioxide positive electrode material for water-based zinc ion battery Download PDFInfo
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Abstract
The invention discloses a preparation method of an anion doped vanadium trioxide anode material for a water system zinc ion battery, which comprises the following steps: will V 2 O 5 Adding the powder, an anion doping source reagent and a carbon-based reducing agent into a reaction solvent, and violently stirring to obtain a precursor mixed solution; then evaporating and drying the precursor mixed solution to a solid state and grinding the solid state into powder; finally, calcining the obtained powder in inert atmosphere to obtain the anion doped V 2 O 3 And (3) a positive electrode material. The preparation method has simple and easy process, can flexibly adjust the composition and the dosage of doped anions, simplifies the doping process and reduces the doping cost; successful anion doping promotes V 2 O 3 The conductivity reduces the diffusion potential barrier of zinc ions in the material, promotes the transmission of the zinc ions in the material structure, and effectively improves V 2 O 3 Capacity and rate performance of the material in an aqueous zinc ion battery.
Description
Technical Field
The invention belongs to the field of water-system zinc ion batteries, and particularly relates to a preparation method of an anion-doped vanadium trioxide positive electrode material for a water-system zinc ion battery.
Background
With the increasing exhaustion of fossil energy and the serious environmental problems caused by the exhaustion of fossil energy, the development of clean and renewable energy sources which are friendly to the environment is receiving more and more attention from people. Because renewable energy sources are difficult to stably and continuously provide energy sources, the development of high-performance energy storage materials and devices has important significance. Among various energy storage technologies, secondary batteries have attracted attention because of their relatively simple system and relatively high energy storage efficiency. Since the commercialization of lithium ion batteries, lithium ion batteries have been widely used in the fields of portable electronic devices, electric vehicles, energy storage, and the like. However, the lithium ion battery has problems of shortage and uneven distribution of lithium resources, poor safety, toxicity and environmental pollution caused by an organic system, and the like, so that the application of the lithium ion battery to the large-scale energy storage field is greatly restricted. Compared with batteries based on organic electrolyte, the water-based metal ion secondary battery, especially the water-based zinc ion battery, which adopts the water-based electrolyte, has the advantages of high safety, low cost, easy assembly and the like, has a plurality of advantages in a plurality of battery systems, and is considered to be one of novel electrochemical energy storage devices with the most potential and application prospect. However, the positive electrode material is still an important influencing factor for further development of the zinc ion battery.
V 2 O 3 The cathode material has an open tunnel structure, inherent metal property and good electron transfer capacity, and is a cathode material of an aqueous zinc ion battery with great potential. At present, V 2 O 3 The material is mainly prepared by a hydrothermal method or a solvothermal method, the yield is low, and the method is relatively complex. At the same time, pure V 2 O 3 The material has the problems of poor conductivity, high zinc ion repulsive force and the like, so that the ion transmission kinetic rate is slow, and the zinc storage capacity is limited. The construction of carbon-supported hollow/porous nanostructures is a common approach to solve this problem, but the complex preparation conditions limit its further development. Therefore, a simple positive electrode material V for zinc ion batteries is developed 2 O 3 The preparation and modification methods are necessary. At present, preparation of anion-doped V 2 O 3 Electrode materials have not been reported.
Disclosure of Invention
Aiming at the prior zinc ion battery anode material V 2 O 3 The invention provides a zinc ion battery anode material with V doped with anions 2 O 3 The simple preparation method effectively improves V 2 O 3 Capacity and rate capability of the positive electrode material in an aqueous zinc ion battery.
The invention adopts the following technical scheme:
a preparation method of an anion doped vanadium trioxide anode material for a water system zinc ion battery is characterized by comprising the following steps: the doped anions are at least one of sulfur, fluorine, chlorine and bromine ions, and the capacity and rate performance of the obtained anion doped vanadium trioxide positive electrode material in the water system zinc ion battery are effectively improved. The method specifically comprises the following steps:
step 1: will be commercially available or homemade V 2 O 5 Adding the powder, the anion source reagent and the carbon-based reducing agent into a reaction solventStrongly stirring to obtain precursor mixed liquor;
step 2: evaporating and drying the precursor mixed solution to a solid state, and grinding into powder;
and 3, step 3: and calcining the obtained powder in an inert atmosphere to obtain the anion doped vanadium trioxide anode material.
Further, in step 1, the carbon-based reducing agent is at least one of glucose, sucrose, melamine, citric acid, oxalic acid and ascorbic acid.
Further, the anion source reagent is selected according to the anion to be doped, and comprises at least one of a sulfur source, a fluorine source, a chlorine source and a bromine source. The sulfur source is at least one of sulfur powder, thioacetamide and cysteine; the fluorine source is at least one of ammonium fluoride and polyvinylidene fluoride; the chlorine source is at least one of ammonium chloride and hexadecyl trimethyl ammonium chloride; the bromine source is at least one of ammonium bromide and hexadecyl trimethyl ammonium bromide.
Further, in step 1, said V 2 O 5 The molar ratio of the powder, the anion source reagent and the carbon-based reducing agent is 1:0.5 to 2:1.5 to 4.
Further, in step 1, the volume ratio of water to ethanol in the reaction solvent is 1:0 to 1 of water-ethanol mixed solution.
Further, in the step 1, the stirring time is 2-6 h.
Further, in the step 2, the temperature of the evaporation drying is 50-80 ℃, and the time is 8-12 h.
Further, in step 3, the inert atmosphere is N 2 Or Ar; the calcination treatment is to calcine at 300-350 ℃ for 0.5-2 h and then calcine at 500-800 ℃ for 2-4 h.
Compared with the prior art, the invention has the beneficial effects that:
the preparation method has simple and easy process, can flexibly adjust the composition and the dosage of doped anions, simplifies the doping process and reduces the doping cost; doping of anions raises V 2 O 3 Conductivity of (2) reduces zinc ionDiffusion potential barrier of the ions in the material promotes the transmission of zinc ions in the material structure, and effectively improves V 2 O 3 Capacity and rate performance of the material in an aqueous zinc ion battery.
Drawings
Fig. 1 is a structural morphology characterization of the cathode material obtained in example 1 and electrochemical performance of the aqueous zinc-ion battery: (a) The figure shows V before and after sulfur doping 2 O 3 XRD pattern of the material; (b) The figure is an enlarged view of the diffraction peak corresponding to the (104) crystal face; (c) Shown as sulfur doped V 2 O 3 SEM pictures of the material; (d) Shown as sulfur doped V 2 O 3 XPS plot of material; (e) The figure shows V before and after sulfur doping 2 O 3 A cycle performance profile of the material; (f) The figure shows V before and after sulfur doping 2 O 3 The charge-discharge curve of the material; (g) The figure shows V before and after sulfur doping 2 O 3 The rate performance of the material.
Fig. 2 is a structural morphology characterization of the cathode material obtained in example 2 and electrochemical performance of the aqueous zinc-ion battery: (a) The figure shows V before and after fluorine doping 2 O 3 XRD pattern of the material; (b) The figure is an enlarged view of the diffraction peak corresponding to the (104) crystal face; (c) Shown as fluorine doping V 2 O 3 SEM images of the material; (d) Shown as fluorine doping V 2 O 3 XPS plot of material; (e) The figure shows V before and after fluorine doping 2 O 3 A cycle performance profile of the material; (f) The figure shows V before and after fluorine doping 2 O 3 The charge-discharge curve of the material; (g) The figure shows V before and after fluorine doping 2 O 3 The rate performance of the material.
Fig. 3 is a structural morphology characterization of the cathode material obtained in example 3 and electrochemical performance of an aqueous zinc ion battery: (a) The figure shows V before and after chlorine doping 2 O 3 XRD pattern of the material; (b) The figure is an enlarged view of the diffraction peak corresponding to the (104) crystal face; (c) Shown as chlorine doping V 2 O 3 SEM images of the material; (d) Shown as chlorine doping V 2 O 3 XPS plot of material; (e) The figure shows V before and after chlorine doping 2 O 3 A cycle performance map of the material; (f) The figure shows V before and after chlorine doping 2 O 3 The charge-discharge curve of the material; (g) The figure shows V before and after chlorine doping 2 O 3 Rate capability of materialEnergy diagram.
Fig. 4 is a structural morphology characterization of the cathode material obtained in example 4 and electrochemical performance of the aqueous zinc-ion battery: (a) Shown as V before and after bromine doping 2 O 3 XRD pattern of the material; (b) The figure is an enlarged view of the diffraction peak corresponding to the (104) crystal face; (c) Shown as bromine doped V 2 O 3 SEM images of the material; (d) Shown as bromine doped V 2 O 3 XPS plot of material; (e) The figure shows V before and after bromine doping 2 O 3 A cycle performance map of the material; (f) The figure shows V before and after bromine doping 2 O 3 The charge-discharge curve of the material; (g) The figure shows V before and after bromine doping 2 O 3 The rate performance of the material.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
The method for testing the electrochemical performance of the water-based zinc ion battery of the cathode material obtained in the embodiment comprises the following steps: mixing the positive electrode material obtained in each embodiment with acetylene black and PVDF according to a mass ratio of 7; the metal zinc foil is used as a negative electrode, the WHATMAN G/D glass fiber is used as a diaphragm, and the self-prepared 2M ZnSO 4 The aqueous solution is used as electrolyte and is assembled into a CR2032 type battery in the atmospheric environment.
Example 1
This example prepares sulfur doped V as follows 2 O 3 The positive electrode material:
1. 1mmol of commercially available V was weighed out 2 O 5 Added to 20mL of deionized water.
2. Weighing 1mmol of cysteine and 1.5mmol of citric acid, dissolving in 20mL of solution with the volume ratio of 1:1 in a water-ethanol mixture.
3. And (3) pouring the clear solution obtained in the step (2) into the orange dispersion obtained in the step (1), violently stirring at normal temperature for 4 hours, then evaporating and drying at 70 ℃ for 10 hours, and grinding into powder to obtain precursor powder.
4. Putting the precursor powder in the step 3 into N 2 Calcining treatment in atmosphere: firstly, heating to 300 ℃ at the heating rate of 5 ℃/min, and calcining for 1h; then, the mixture is calcined for 2 hours at the temperature of 5 ℃/min rising to 600 ℃; after calcining and sintering, furnace cooling to room temperature to obtain sulfur-doped V 2 O 3 And (3) a positive electrode material.
This example also produced undoped V 2 O 3 Sample for comparison, which was doped with V as described above 2 O 3 The preparation method of the cathode material is the same, and only the cysteine is not added.
Fig. 1 shows the structural morphology of the positive electrode material obtained in this example and the electrochemical performance of the aqueous zinc ion battery: (a) The figure shows V before and after sulfur doping 2 O 3 The XRD pattern of the material shows that the powder prepared can be indexed as V 2 O 3 (PDF # 34-0187) with no apparent impurities; (b) The figure is an enlarged view of a diffraction peak corresponding to a crystal face (104) of the crystal, and shows that the diffraction peak is shifted after the crystal is doped with the sulfide ions, and the success of doping is preliminarily explained; (c) Shown as sulfur doped with V 2 O 3 SEM images of the material, showing that the material consists mainly of nanoparticles between 50-200 nm; (d) Shown as sulfur doped V 2 O 3 An XPS diagram of the material shows a characteristic spectrum peak of sulfur, and further shows that the sulfur is successfully doped; (e) The figure shows V before and after sulfur doping 2 O 3 The cycle performance diagram of the material is that under the condition of large current density of 5A/g, after 50 cycles, V is doped by sulfur 2 O 3 The specific discharge capacity of the material reaches 307mAh/g, which is higher than that of undoped V 2 O 3 The material capacity is 269mAh/g; (f) The figure shows V before and after sulfur doping 2 O 3 The charge-discharge curves of the materials show that the voltage platforms of the charge-discharge curves of the materials are basically the same and have similar shapes; (g) The figure shows V before and after sulfur doping 2 O 3 The multiplying power performance of the material can be shown, and V doped with sulfur can be seen 2 O 3 The rate capability of the material is obviously superior to that of undoped V 2 O 3 A material. FIGS. (e) - (g) illustrate that V can be effectively raised after sulfur ion doping 2 O 3 The capacity and rate capability of the positive electrode material in the water-system zinc ion battery are not influenced 2 O 3 Operating voltage of material。
Example 2
This example prepares fluorine doped V as follows 2 O 3 The positive electrode material:
1. 1mmol of commercially available V was weighed 2 O 5 Added to 20mL of deionized water.
2. Weighing 1mmol of ammonium fluoride and 2mmol of ascorbic acid, dissolving in 20mL of solution with the volume ratio of 1:0.3 of water-ethanol mixture.
3. Pouring the clear solution obtained in the step 2 into the orange dispersion liquid obtained in the step 1, violently stirring at normal temperature for 2 hours, then evaporating and drying at 60 ℃ for 12 hours, and grinding into powder to obtain precursor powder;
4. putting the precursor powder in the step 3 into N 2 Calcining treatment in atmosphere: firstly, heating to 350 ℃ at the heating rate of 5 ℃/min, and calcining for 1.5h; then, the mixture is calcined for 4 hours at the temperature of 5 ℃/min rising to 600 ℃; after calcining and sintering, furnace cooling to room temperature to obtain the fluorine-doped V 2 O 3 And (3) a positive electrode material.
This example also produced undoped V 2 O 3 Sample for comparison, which was doped with V as described above 2 O 3 The positive electrode material was prepared in the same manner except that ammonium fluoride was not added.
Fig. 2 shows the structural morphology of the positive electrode material obtained in this example and the electrochemical performance of the aqueous zinc ion battery: (a) The figure shows V before and after fluorine doping 2 O 3 The XRD pattern of the material shows that the powder prepared can be indexed as V 2 O 3 (PDF # 34-0187) with no apparent impurities; (b) The figure is an enlarged view of the diffraction peak corresponding to the (104) crystal face, and the diffraction peak shifts after doping fluorine ions, which preliminarily shows that the doping is successful; (c) Shown as fluorine doping V 2 O 3 SEM image of the material, it can be seen that the material is mainly composed of nanoparticles of 50-200 nm; (d) Shown as fluorine doping V 2 O 3 XPS graph of the material shows characteristic spectrum peak of fluorine, further indicates the success of doping; (e) Is shown as V 2 O 3 And fluorine doping of V 2 O 3 The cycle performance diagram of the material is that after 50 cycles of circulation under the high current density of 5A/g, V is doped by fluorine 2 O 3 The specific discharge capacity of the material reaches 315mAh/g, which is higher than that of undoped V 2 O 3 The material capacity is 269mAh/g; (f) The figure shows V before and after fluorine doping 2 O 3 The charge-discharge curves of the materials show that the voltage platforms of the charge-discharge curves of the materials are basically the same and have similar shapes; (g) The figure shows V before and after fluorine doping 2 O 3 The multiplying power performance of the material can be seen, and fluorine doping V can be seen 2 O 3 The rate capability of the material is superior to that of the undoped V 2 O 3 A material. FIGS. e to g show that V can be effectively raised after fluorine ion doping 2 O 3 The capacity and rate capability of the positive electrode material in the water-system zinc ion battery are not influenced 2 O 3 The operating voltage of the material.
Example 3
This example prepares chlorine doped V as follows 2 O 3 The preparation method of the cathode material comprises the following steps:
1. 1mmol of commercially available V was weighed 2 O 5 Added to 20mL of deionized water.
2. Weighing 1mmol of hexadecyl trimethyl ammonium chloride and 4mmol of oxalic acid, dissolving in 20mL of solution with the volume ratio of 1:1 in a water-ethanol mixture.
3. And (3) pouring the clear solution obtained in the step (2) into the orange dispersion obtained in the step (1), violently stirring at normal temperature for 4 hours, then evaporating and drying at 70 ℃ for 10 hours, and grinding into powder to obtain precursor powder.
4. Putting the precursor powder in the step 3 into N 2 Calcining treatment in atmosphere: firstly, raising the temperature to 330 ℃ at a heating rate of 5 ℃/min, and calcining for 2h; then calcining for 2h at the temperature of 5 ℃/min rising to 700 ℃; after calcination and sintering, the mixture is cooled to room temperature along with the furnace to obtain the chlorine-doped V 2 O 3 And (3) a positive electrode material.
This example also produced undoped V 2 O 3 Sample for comparison, which was doped with chlorine V as described above 2 O 3 The positive electrode material was prepared in the same manner except that cetyltrimethylammonium chloride was not added.
Fig. 3 shows the structural morphology of the positive electrode material obtained in this example and the electrochemical performance of the aqueous zinc ion battery: (a) FIG. is a diagram of chlorine dopingHetero front and back V 2 O 3 The XRD pattern of the material shows that the prepared powder can be indexed to V 2 O 3 (PDF # 34-0187) with no apparent impurities; (b) The figure is an enlarged view of the diffraction peak corresponding to the (104) crystal face, and the diffraction peak is shifted after the chloride ions are doped, which preliminarily shows that the doping is successful; (c) Shown as chlorine doping V 2 O 3 SEM image of the material, it can be seen that the material is mainly composed of nanoparticles of 50-100 nm; (d) Shown as chlorine doped V 2 O 3 XPS picture of the material, the characteristic energy spectrum peak of chlorine appears, further illustrate the success of doping; (e) The figure shows V before and after chlorine doping 2 O 3 The cycle performance diagram of the material is that under the condition of large current density of 5A/g, after 50 cycles, the chlorine is doped with V 2 O 3 The specific discharge capacity of the material reaches 343mAh/g, which is higher than that of undoped V 2 O 3 The material capacity is 269mAh/g; (f) The figure shows V before and after chlorine doping 2 O 3 The charge-discharge curves of the materials show that the voltage platforms of the charge-discharge curves of the materials are basically the same and have similar shapes; (g) The figure shows V before and after chlorine doping 2 O 3 The multiplying power performance of the material can be seen, and the chlorine doping V can be seen 2 O 3 The rate capability of the material is superior to that of the undoped V 2 O 3 A material. FIGS. e to g show that V can be effectively increased after chloride ion doping 2 O 3 The capacity and rate performance of the material in the water-based zinc ion battery are not influenced 2 O 3 The operating voltage of the material.
Example 4
This example prepares bromine-doped V as follows 2 O 3 The preparation method of the cathode material comprises the following steps:
1. 1mmol of commercially available V was weighed 2 O 5 Added to 20mL of deionized water.
2. Weighing 1mmol of hexadecyl trimethyl ammonium bromide and 2mmol of glucose, dissolving in 20mL of a solution with the volume ratio of 1:1 in a water-ethanol mixture.
3. And (3) pouring the clear solution obtained in the step (2) into the orange dispersion obtained in the step (1), violently stirring at normal temperature for 6 hours, then evaporating and drying at 80 ℃ for 8 hours, and grinding into powder to obtain precursor powder.
4. Putting the precursor powder in the step 3 into N 2 Calcining treatment in atmosphere: firstly, heating to 350 ℃ at the heating rate of 5 ℃/min, and calcining for 0.5h; then calcining for 2h at the temperature of 5 ℃/min rising to 800 ℃; after calcining and sintering, furnace cooling to room temperature to obtain the bromine-doped V 2 O 3 And (3) a positive electrode material.
This example also produced undoped V 2 O 3 Sample for comparison, which is doped with bromine V as described above 2 O 3 The preparation method of the cathode material is the same, except that cetyl trimethyl ammonium bromide is not added.
Fig. 4 shows the structural morphology characterization of the cathode material obtained in this example and the electrochemical performance of the aqueous zinc ion battery: (a) The figure shows V before and after bromine doping 2 O 3 The XRD pattern of the material shows that the prepared powder can be indexed to V 2 O 3 (PDF # 34-0187) with no apparent impurities; (b) The figure is an enlarged view of the diffraction peak corresponding to the (104) crystal face, and the diffraction peak is shifted after the bromide ion doping, which preliminarily shows the success of the doping; (c) Shown as bromine doped V 2 O 3 SEM image of the material, it can be seen that the material is mainly composed of nanoparticles of 200-500 nm; (d) Shown as bromine doped V 2 O 3 XPS picture of the material, the characteristic spectrum peak of bromine appears, further illustrate the success of doping; (e) The figure shows V before and after bromine doping 2 O 3 The cycle performance of the material is shown in the figure, after 50 cycles of circulation under the high current density of 5A/g, the bromine is doped with V 2 O 3 The specific discharge capacity of the material reaches 365mAh/g, which is higher than that of undoped V 2 O 3 The material capacity is 269mAh/g; (f) Shown as V before and after bromine doping 2 O 3 The charge-discharge curves of the materials show that the voltage platforms of the charge-discharge curves of the materials are basically the same and have similar shapes; (g) The figure shows V before and after doping 2 O 3 The multiplying power performance of the material can be seen, and bromine doped V can be seen 2 O 3 The rate capability of the material is superior to that of the undoped V 2 O 3 A material. FIGS. e to g show that V can be effectively raised after bromide ion doping 2 O 3 The capacity and rate performance of the material in the water-based zinc ion battery are not influenced 2 O 3 The operating voltage of the material.
The present invention is not limited to the above exemplary embodiments, and any modifications, equivalent replacements, and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A preparation method of an anion doped vanadium trioxide positive electrode material for a water system zinc ion battery is characterized by comprising the following steps:
step 1: will V 2 O 5 The powder, the anion source reagent and the carbon-based reducing agent are mixed according to the mol ratio of 1:0.5 to 2: 1.5-4, adding the mixture into a reaction solvent, and stirring to obtain a precursor mixed solution; the anion source reagent is selected according to the required doped anions and comprises at least one of a sulfur source, a fluorine source, a chlorine source and a bromine source;
the carbon-based reducing agent is at least one of glucose, sucrose, melamine, citric acid, oxalic acid and ascorbic acid;
step 2: evaporating and drying the precursor mixed solution to a solid state, and grinding the solid state into powder;
and step 3: placing the obtained powder in an inert atmosphere N 2 Or calcining under Ar to obtain the anion-doped vanadium trioxide cathode material, wherein the doped anions are at least one of sulfur, fluorine, chlorine and bromide ions; the calcination treatment is to calcine at 300-350 ℃ for 0.5-2 h and then calcine at 500-800 ℃ for 2-4 h.
2. The method of claim 1, wherein: the sulfur source is at least one of sulfur powder, thioacetamide and cysteine; the fluorine source is at least one of ammonium fluoride and polyvinylidene fluoride; the chlorine source is at least one of ammonium chloride and hexadecyl trimethyl ammonium chloride; the bromine source is at least one of ammonium bromide and hexadecyl trimethyl ammonium bromide.
3. The production method according to claim 1, characterized in that: in the step 1, the reaction solvent is a mixture of water and ethanol with a volume ratio of 1:0 to 1 of water-ethanol mixed solution.
4. The method of claim 1, wherein: in the step 1, the stirring time is 2-6 h.
5. The method of claim 1, wherein: in the step 2, the temperature of the evaporation drying is 50-80 ℃, and the time is 8-12 h.
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