CN111082018A - LiVOPO4Preparation method of/C composite positive electrode material - Google Patents

LiVOPO4Preparation method of/C composite positive electrode material Download PDF

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CN111082018A
CN111082018A CN201911353621.7A CN201911353621A CN111082018A CN 111082018 A CN111082018 A CN 111082018A CN 201911353621 A CN201911353621 A CN 201911353621A CN 111082018 A CN111082018 A CN 111082018A
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livopo
preparation
carbon
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drying
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唐安平
付洋洋
陈核章
徐国荣
宋海申
汪靖伦
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Hunan University of Science and Technology
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • 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
    • H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract

The invention discloses LiVOPO4A preparation method of a/C composite positive electrode material. The method comprises the following steps: firstly, preparing carbon modified Li by pyrolysis of organic carbon sources such as citric acid, glucose and the like3V2(PO4)3‑V2O3the/C compound intermediate or precursor powder prepared by spray drying is mixed with carbon materials (acetylene black, Ketjen black, high specific surface carbon and the like) by ball milling, and then carbon-modified 2Li is obtained by high-temperature sintering3V2(PO4)3‑V2O3the/C compound intermediate is finally subjected to hydrothermal oxidation reaction to obtain LiVOPO4a/C composite material.Carbon modified not only to LiVOPO4Provides an excellent electron conduction network and effectively inhibits LiVOPO in the preparation process4Growth of the particles thereby significantly improving LiVOPO4The electrochemical performance of (2).

Description

LiVOPO4Preparation method of/C composite positive electrode material
Technical Field
The invention relates to a lithium ion battery LiVOPO4Preparation of anode material, in particular to LiVOPO4A preparation method of a/C composite positive electrode material.
Background
Vanadium is a transition metal element with rich valence, can be combined with lithium, phosphate radical and the like to generate a polyanion compound, can also be combined with oxygen firstly, and then is combined with lithium, phosphate radical and the like in the form of vanadium oxygen ions, so the polyanion positive electrode material of vanadium has a great research space. The currently reported vanadium-containing phosphate system positive electrode material with lithium storage performance mainly comprises LiVPO4F、Li3V2(PO4)3And VOPO4Or LiVOPO4And the like. Wherein LiVOPO4The existence of the P-O covalent bond not only can improve LiVOPO4The kinetic and thermodynamic stability of the compound, and can weaken the covalent bond of V-O (namely, induction effect) and reduce V4+/V5+Reverse key orbital energy, thereby increasing V4+/V5+Redox level of (a) so that LiVOPO4Has a ratio V2O5Higher discharge plateau (the former is about 3.9V vs Li/Li)+The latter being about 3.5V). Despite Li3V2(PO4)3The theoretical specific capacity of the nano-silver particles reaches 197 mAh.g-1However, a plurality of voltage platforms appear in the discharging process, which is not favorable for the practical application of the lithium ion battery; and the third electron has a de-intercalation potential of 4.5V or more, which is liable to cause the oxidative decomposition of the electrolyte. Thus, LiVOPO4The discharge plateau is desirable because it is not so high as to decompose the electrolyte, but not so low as to sacrifice energy density. Furthermore, although LiVOPO4Theoretical specific capacity (158mAh g)-1) Slightly lower than LiFePO4Theoretical specific capacity (170 mAh. g)-1) But it has a higher discharge plateau (3.9V vs Li/Li)+) And higher theoretical energy density (616Wh Kg. Kg)-1). Based on the above advantages, LiVOPO4The positive electrode material has attracted attention.
In LiVOPO4Due to VO in the structure of6PO between octahedra4The tetrahedra restricts the variation of the lattice volume so that Li+The insertion/extraction movement of (A) is limited, resulting in LiVOPO4The material has low electronic conductivity and ion diffusion rate, so that the theoretical capacity of the material cannot be released to the maximum extent and the high-current discharge performance is not ideal. Aiming at the defect of low electronic conductivity, people mainly adopt the addition of a conductive agent to improve LiVOPO4Such as β -LiVOPO synthesized by Barker and the like by taking carbon black with high specific surface area as a carbon source4the/C composite material shows good cycle performance (Barker J, equivalent. electrochemical Properties of β -LiVOPO)4Prepared by Carbothermal Reduction, J Electrochem Soc,2004,151: 796-800). LiVOPO by Hameed et al4After high-energy ball milling with Super P carbon black, 103 mAh.g, 93 mAh.g, 73 mAh.g, 57 mAh.g are respectively obtained at the multiplying power of 0.1, 0.2, 0.5 and 1C-1The specific first discharge capacity (Dupr N, et al. phase Transition Induced by Lithium Insertion a. alpha.)I-andɑII-VOPO4JSOLID State Chem,2004,177: 2896-2902). Saravanan et al synthesized LiVOPO at 300 deg.C by solvothermal method4composite/C material (Saravanan K, et al. Hollow α -LiVOPO)4Sphere cathodos for HighEnergy Li-ion Battery application J Mater Chem,2011,21: 10042-; the results show that when the voltage range is 3.0-4.5V and the multiplying power is 0.1C and 1.7C, the specific discharge capacity is 130mAh/g and 61 mAh.g respectively-1Tang et al prepared α -LiVOPO by using acetylene black as a carbon source and using a sol-gel method4the/C composite material has good cycle Performance and rate capability (Tang AP, et al. electrochemical Performance of α -LiVOPO)4A β -LiVOPO was Synthesized by carbon composite Material Synthesized by Sol-gel method J Electrochem Soc,2013,161:10-13 Ren et al4/RuO2Composite material (Ren M, et al. LiVOPO)4:A CathodeMaterial for 4 V Lithium Ion Batteries.J Power Sources,2008,189:786-789)。RuO2The doping of the material not only increases the conductivity of the material, but also improves the electrochemical performance and the cycle performance of the material.
Carbon doping is one of the effective methods for increasing the electronic conductivity of materials, but LiVOPO4The carbon doping is usually performed by physical mixing (such as ball milling), which tends to result in non-uniform distribution of carbon or incomplete coating of the particle surface. Even in solvothermal synthesis of LiVOPO4The method of (1) has uniform distribution of surface carbon coating formed by cracking of organic carbon source, but in the high-temperature carbon coating process, V (IV) is easily reduced to V (III) by strong reducing atmosphere created by the presence of carbon, so LiVOPO4The carbon-coated synthesis temperature of (a) cannot be too high (e.g., 300 deg.c), thereby resulting in poor conductivity of the cracked carbon.
Disclosure of Invention
In view of the preparation of carbon-modified LiVOPO4In view of the above technical problems, the present invention provides a LiVOPO4A preparation method of a/C composite positive electrode material.
The purpose of the invention is realized by the following technical scheme:
LiVOPO4The preparation method of the/C composite positive electrode material comprises the following steps:
(1) dispersing oxalic acid, vanadium pentoxide or ammonium metavanadate, ammonium dihydrogen phosphate or diammonium hydrogen phosphate, lithium acetate or lithium hydroxide or lithium carbonate or lithium oxalate in distilled water according to a stoichiometric ratio and stirring to obtain a precursor solution;
(2) dissolving citric acid or glucose in the precursor solution obtained in the step (1), and then performing spray drying to obtain precursor powder; or directly spray-drying the precursor solution obtained in the step (1), and then ball-milling and mixing the precursor solution with a carbon material to prepare precursor powder;
(3) preserving the heat of the precursor powder obtained in the step (2) for 4-8 h at 600-800 ℃ in an inert atmosphere, and naturally cooling to room temperature along with a furnace body to obtain 2Li3V2(PO4)3-V2O3a/C intermediate;
(4) the intermediate powder obtained in the step (3) is mixedAdding the mixture into a reaction kettle, and adding H which is 15-30% excessive of the stoichiometric ratio2O2Carrying out solvothermal reaction by using the solution as an oxidant, filtering, washing, drying and collecting;
(5) sintering the powder collected in the step (4) in an inert atmosphere at 300-450 ℃ for 5-8 h, and naturally cooling to room temperature to obtain LiVOPO4a/C composite material.
Further, in the step (2), the molar ratio of vanadium pentoxide or ammonium metavanadate to citric acid or glucose is 1: 1-2, preferably 1: 1.
Further, in the step (2), the carbon material is one or more of acetylene black, ketjen black and high specific surface carbon.
Further, in the step (2), LiVOPO4The mass percentage content of the carbon material in the/C composite material is 1-19%.
Further, in the step (4), the solvent for the solvent thermal reaction is absolute ethyl alcohol or/and distilled water, and when the solvent is absolute ethyl alcohol and distilled water, the volume ratio of the absolute ethyl alcohol to the distilled water is 1: 1-1.1.
Further, in the step (4), H2O2The mass percentage of the solution is 20-30%, and more preferably 30%.
Further, in the step (4), the solvothermal reaction temperature is 150-180 ℃, and the reaction time is 12-15 hours.
Further, in the step (4), the drying is vacuum drying, the drying temperature is 70-120 ℃, and the drying time is 10-20 hours.
The invention has the beneficial effects that:
the invention firstly prepares the carbon modified 2Li3V2(PO4)3-V2O3the/C compound intermediate is subjected to solvent thermal oxidation reaction at low temperature to obtain carbon-modified LiVOPO4The carbon modified is not only LiVOPO4Provides an excellent electron conduction network and effectively inhibits LiVOPO in the preparation process4Growth of the particles thereby significantly improving LiVOPO4The electrochemical performance of (2).
Drawings
FIG. 1 is an X-ray diffraction pattern of a sample of example 1 of the present invention.
FIG. 2 is a scanning electron micrograph of a sample of example 1 of the present invention.
FIG. 3 is a plot of the first 3 charge and discharge cycles of a sample of example 1 of the present invention; the charging and discharging system is room temperature, C/20 constant current charging and discharging, and the voltage interval is 2.5V-4.5V.
FIG. 4 is a graph of the cycling performance of the samples of example 1 of the present invention; the charging and discharging system is room temperature, C/10 constant current charging and discharging, and the voltage interval is 2.5V-4.5V.
FIG. 5 is an X-ray diffraction pattern of a sample of example 3 of the present invention.
Detailed Description
For a better understanding of the present invention, the present invention will be further described with reference to the following examples and drawings, but the scope of the present invention is not limited to the examples shown.
Example 1
LiVOPO4The preparation method of the/C composite material comprises the following steps:
(1) 3.6363g V are weighed according to the stoichiometric ratio2O5，7.5653g H2C2O4·2H2O was dispersed in 400ml of secondary water, magnetically stirred at 70 ℃ to obtain a solution, and 5.2831g of (NH) was added4)2HPO4And 4.0817g CH3COOLi, and continuously stirring, dissolving, and spray drying to obtain powder. Then 2.5000g of powder and 0.4500g of Ketjen black are weighed and ball-milled for 6h to obtain precursor powder.
(2) Keeping the precursor powder in the step (1) at 750 ℃ for 6h in Ar atmosphere, and naturally cooling to room temperature along with the furnace body to obtain 2Li3V2(PO4)3-V2O3C intermediate powder.
(3) Adding 0.9000g of the intermediate powder obtained in the step (2) into a polytetrafluoroethylene-lined reaction kettle, adding 70mL of absolute ethyl alcohol as a solvent, and adding 0.27mL of H2O2The solution (30 wt%) was reacted at 180 ℃ with constant stirring for 15h, washed, filtered, dried under vacuum at 80 ℃ for 12h and collected.
(4) Preserving the heat of the black powder collected in the step (3) for 8 hours at 450 ℃ in an Ar atmosphere tubular furnace, and naturally cooling to room temperature to obtain LiVOPO4a/C (residual carbon content 19.0 wt%) composite material.
The sample of example 1 was measured using an X-ray diffractometer model Brucker D8 Advance. The XRD spectrum is shown in figure 1. As can be seen from FIG. 1, the intermediate powder of the sample of example 1 has characteristic X-ray diffraction peaks corresponding to Li3V2(PO4)3Standard cards of (80-1515) and V2O3The standard cards (74-0325) are consistent, and the target product LiVOPO4The characteristic peak of X-ray diffraction of the/C is consistent with that of a standard card (47-064,) which shows that the intermediate 2Li is obtained after hydrothermal reaction and sintering3V2(PO4)3-V2O3the/C compound is completely converted into the triclinic system LiVOPO4a/C complex. While V is absent in the figure2O5、VO2、Li3PO4、Li2VPO6And waiting for impurity peaks, which indicates that the prepared compound has high purity. As can be seen from FIG. 2, the sample particles are uniformly distributed, and the particle size is between 100 nm and 200 nm.
The charge and discharge test and the cycle performance test were performed on the sample of example 1, and the results are shown in fig. 3 and 4, respectively. As can be seen from FIG. 3, LiVOPO4The discharge specific capacities of the first circle, the second circle and the third circle of the/C composite positive electrode material are 151.4, 157.7 and 156.6 mAh.g respectively under the set charge-discharge system-1Extremely close to 158mAh g-1The theoretical specific capacity of (a). As can be seen from FIG. 4, LiVOPO4After 30 cycles of the/C composite positive electrode material, the capacity is 133.8 mAh.g-1The capacity retention rate reaches 100 percent. The above results show that the LiVOPO prepared by the present invention4the/C composite positive electrode material not only has high discharge specific capacity, but also shows excellent cycle performance.
Example 2
(1) 1.8182g V are weighed according to the stoichiometric ratio2O5，3.7827g H2C2O4·2H2Dispersing O in 300ml of secondary water, and magnetically stirring at 70 DEG CAfter the solution had formed, 2.3012g of NH were added4H2PO4，0.9557g Li2C2O4，4.2028gC6H8O7·H2And O (citric acid) and continuously stirring for 1h, and spray drying to obtain precursor powder.
(2) Preserving the heat of the precursor powder in the step (1) for 6h at 750 ℃ in Ar atmosphere, and naturally cooling to room temperature along with the furnace body to obtain the 2Li3V2(PO4)3-V2O3C intermediate powder.
(3) Adding 0.8000g of the intermediate powder obtained in the step (2) into a polytetrafluoroethylene lining reaction kettle, taking a mixed solution of 35mL of water and 35mL of ethanol as a solvent, and adding 0.24mL of H2O2The solution (30 wt%) was reacted at 160 ℃ with constant stirring for 14h, washed, filtered, dried under vacuum at 80 ℃ for 12h and collected.
(4) Preserving the heat of the black powder collected in the step (3) for 6 hours at 400 ℃ in a nitrogen atmosphere, and naturally cooling to room temperature to obtain LiVOPO4a/C (residual carbon content 16.7 wt%) composite material.
Example 3
(1) 2.3401g of NH were weighed out in stoichiometric proportions4VO3，2.5214g H2C2O4·2H2O is dispersed in 200ml of secondary water and stirred magnetically at 70 ℃ to form a solution, 2.3009g of NH are added4H2PO4，0.4792g LiOH，3.9614gC6H12O6·H2And O (glucose) and continuously stirring for 1h, and spray drying to obtain precursor powder.
(2) Preserving the heat of the precursor powder in the step (1) for 6h at 750 ℃ in Ar atmosphere, and naturally cooling to room temperature along with the furnace body to obtain the 2Li3V2(PO4)3-V2O3C intermediate powder.
(3) Adding 1.0000g of intermediate powder obtained in the step (2) into a polytetrafluoroethylene-lined reaction kettle, taking 70mL of distilled water as a solvent, and adding 0.3mL of H2O2Stirring the solution (30 wt%) at 150 deg.C for 12 hr, washing, filtering, and heating to 80 deg.CDried under vacuum for 12h and collected.
(4) Preserving the heat of the black powder collected in the step (3) for 8 hours at 300 ℃ in Ar atmosphere, and naturally cooling to room temperature to obtain LiVOPO4a/C (residual carbon content 18.5 wt%) composite.
The XRD spectrum of the sample of example 3 is shown in fig. 5. As can be seen from fig. 5, the X-ray powder diffraction characteristic peak and α of the sample of example 4 are1-LiVOPO4Has extremely high matching degree and no V in the spectrogram2O5、Li2VPO6And impurity peaks are obtained, which indicates that the sample has high purity.
Example 4
LiVOPO4The preparation method of the/C composite material comprises the following steps:
(1) 3.6363g V are weighed accurately according to the stoichiometric ratio2O5，7.5653g H2C2O4·2H2O was dispersed in 400ml of secondary water, magnetically stirred at 70 ℃ to obtain a solution, and 4.5996g of NH was added4H2PO4And 1.4773g Li2CO3And after stirring for 1h, a powder was obtained by spray drying. Then, 2.5000g of precursor powder and 0.1150g of acetylene black are weighed and ball-milled for 6 hours to obtain precursor powder.
(2) Preserving the heat of the precursor powder in the step (1) for 6h at 750 ℃ in Ar atmosphere, and naturally cooling to room temperature along with the furnace body to obtain the 2Li3V2(PO4)3-V2O3C intermediate powder.
(3) Taking 0.9000g of the intermediate powder obtained in the step (2), adding the intermediate powder into a polytetrafluoroethylene-lined reaction kettle, taking 70mL of absolute ethyl alcohol as a solvent, and adding 0.27mL of H2O2The solution (30 wt%) was reacted at 180 ℃ with constant stirring for 12h, washed, filtered, dried under vacuum at 80 ℃ for 12h and collected.
(4) Preserving the heat of the black powder collected in the step (3) for 5 hours at 450 ℃ in Ar atmosphere, and naturally cooling to room temperature to obtain LiVOPO4a/C (residual carbon content 4.5 wt%) composite material.
Example 5
LiVOPO4The preparation method of the/C composite material comprises the following steps:
(1) 3.6363g V are weighed accurately according to the stoichiometric ratio2O5，7.5653g H2C2O4·2H2O was dispersed in 400ml of secondary water, magnetically stirred at 70 ℃ to obtain a solution, and 4.5996g of NH was added4H2PO4And 4.0817g CH3After continued stirring for 1h with COOLi, a powder was obtained by spray drying. Then, 2.5000g of precursor powder and 0.0220g of carbon ball mill with high specific surface area are weighed for 6 hours to obtain precursor powder.
(2) Preserving the heat of the precursor powder in the step (1) for 6h at 750 ℃ in Ar atmosphere, and naturally cooling to room temperature along with the furnace body to obtain the 2Li3V2(PO4)3-V2O3C intermediate powder.
(3) Adding 0.9000g of the intermediate powder obtained in the step (2) into a polytetrafluoroethylene-lined reaction kettle, adding 70mL of absolute ethyl alcohol as a solvent, and adding 0.27mL of H2O2The solution (30 wt%) was reacted at 180 ℃ with stirring for 13h, washed, filtered, dried under vacuum at 80 ℃ for 12h and collected.
(4) Preserving the heat of the black powder collected in the step (3) for 8 hours at 350 ℃ in Ar atmosphere, and naturally cooling to room temperature to obtain LiVOPO4a/C (residual carbon content 1.0 wt%) composite material.
The above is only a preferred embodiment of the present invention, and various modifications and changes can be made by those skilled in the art based on the above concept of the present invention, for example, combinations and changes of the ratio and the process conditions within the scope of the ratio and the process conditions given in the present invention, and such changes and modifications are within the spirit of the present invention.

Claims (8)

1. LiVOPO4The preparation method of the/C composite material comprises the following steps:
(1) dispersing oxalic acid, vanadium pentoxide or ammonium metavanadate, ammonium dihydrogen phosphate or diammonium hydrogen phosphate, lithium acetate or lithium hydroxide or lithium carbonate or lithium oxalate in distilled water according to a stoichiometric ratio and stirring to prepare a precursor solution;
(2) dissolving citric acid or glucose in the precursor solution obtained in the step (1), and then performing spray drying to obtain precursor powder; or directly spray-drying the precursor solution obtained in the step (1), and then ball-milling and mixing the precursor solution with a carbon material to prepare precursor powder;
(3) preserving the precursor powder obtained in the step (2) at the temperature of 600-800 ℃ for 4-8 h in an inert atmosphere, and naturally cooling to room temperature along with a furnace body to obtain 2Li3V2(PO4)3-V2O3a/C intermediate.
(4) Transferring the intermediate powder obtained in the step (3) into a reaction kettle, and adding H which is 15-30% of stoichiometric excess2O2Carrying out solvothermal reaction by using the solution as an oxidant, then filtering, washing, drying and collecting powder;
(5) sintering the powder obtained in the step (4) for 5-8 hours at 300-450 ℃ in an inert atmosphere, and naturally cooling to room temperature to obtain LiVOPO4a/C composite material.
2. LiVOPO according to claim 14The preparation method of the/C composite cathode material is characterized in that in the step (2), the molar ratio of vanadium pentoxide or ammonium metavanadate to citric acid or glucose is 1: 1-2.
3. LiVOPO according to claim 14The preparation method of the/C composite cathode material is characterized in that in the step (2), the carbon material is one or more than two of acetylene black, Ketjen black and high specific surface carbon.
4. LiVOPO according to claim 14The preparation method of the/C composite cathode material is characterized in that in the step (2), LiVOPO4The mass percentage content of the carbon material in the/C composite material is 1-19%.
5. LiVOPO according to claim 14A preparation method of a/C composite anode material is characterized in that,in the step (4), the solvent for the solvothermal reaction is absolute ethyl alcohol or/and distilled water, and when the solvent is absolute ethyl alcohol and distilled water, the volume ratio of the absolute ethyl alcohol to the distilled water is 1: 1-1.1.
6. LiVOPO according to claim 14The preparation method of the/C composite cathode material is characterized in that in the step (4), the solvothermal reaction temperature is 150-180 ℃, and the reaction time is 12-15 hours.
7. LiVOPO according to claim 14The preparation method of the/C composite cathode material is characterized in that in the step (4), H2O2The mass percentage of the solution is 20-30%.
8. LiVOPO according to claim 14The preparation method of the/C composite cathode material is characterized in that in the step (4), the drying is vacuum drying, the drying temperature is 70-120 ℃, and the drying time is 10-20 hours.
CN201911353621.7A 2019-12-24 2019-12-24 LiVOPO4Preparation method of/C composite positive electrode material Pending CN111082018A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113526552A (en) * 2021-07-19 2021-10-22 湖南科技大学 Composite positive electrode active material of lithium ion battery and preparation method thereof

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Application publication date: 20200428