A solvothermal method for preparation of flower-like Cu 2 v 2 o 7 -cuo nanocomposite approach

Abstract

The invention discloses a method for preparing a flower-like Cu2V2O7-CuO nanocomposite according to a solvothermal method. The method comprises the following steps: dissolving analytically pure V2O5 powder into an aqueous hydrogen peroxide solution to obtain a solution A; adding the solution A into an ethanol solution of Cu(CH3COO)2 under a magnetic stirring condition; adjusting the pH value of the solution to 7-9, and continuing stirring to form a reaction precursor; pouring the reaction precursor into a reaction kettle, placing in a homogeneous hydrothermal instrument after mounting, performing a hydrothermal reaction at 100-200 DEG C. After the reaction is completed, the apparatus is cooled automatically, and separating, washing and drying a product after completion of the reaction andautomatic cooling of the instrument so as to obtain the flower-like Cu2V2O7-CuO nanocomposite. The solvothermal method is used for preparing the flower-like Cu2V2O7-CuO nanocomposite, and compared with a solid-phase reaction method, the solvothermal method has the advantages as follows: the solvothermal method is cheaper, more convenient and more effective, and the preparation time of theCu2V2O7-CuO nanocomposite is relatively short. The prepared product has high purity, good crystallinity, uniform morphology and size and complete flower-like morphology; the raw materials are easy to obtain, the preparation cycle is short, the energy consumption is low, the process is simple, the repeatability is high, and the feasibility is strong; the prepared flower-like Cu2V2O7-CuO nanocomposite has avery good lithium storage property.

Description

technical field

[0001] The invention belongs to the technical field of electrode materials for batteries, and in particular relates to a lithium-ion battery electrode material prepared by a solvothermal method to prepare flower-shaped Cu 2 V 2 o 7 - Method for CuO nanocomposites. Background technique

[0002] Copper vanadate (Cu x V y o z ) is a layered structure that can undergo multi-step reduction during intercalation / deintercalation of lithium ions (Cu 2+ / Cu + and Cu + / Cu 0 ), considered to be a lithium-ion battery electrode material with potential application value. Cu 2 V 2 o 7 It is monoclinic phase, C2 / c space group, and has potential application value in negative thermal expansion, magnetism, catalytic oxidation, etc.

[0003] As a semiconductor material, Cu 2 V 2 o 7 The synthesis generally adopts the solid-state sintering method, which has a long reaction time, high energy consumption, and the size of the synthesized product is large, which will ...

Examples

Embodiment 1

[0020] 1) will analytically pure V 2 o 5 The powder is dissolved in an aqueous hydrogen peroxide solution with a mass fraction of 15% to obtain V 5+ The concentration is 0.5mol / l brownish red transparent solution A;

[0021] 2) Under magnetic stirring, press V 5+ and Cu 2+ The molar ratio is 1:0.5 Add solution A to the concentration of 0.1mol / L Cu(CH 3 COO) 2 in ethanol solution;

[0022] 3) Use analytically pure sodium hydroxide to adjust the pH value of the solution to 7, and continue to stir to form a reaction precursor;

[0023] 4) Pour the reaction precursor into the reaction kettle, put it in a homogeneous hydrothermal instrument after the equipment is ready, and carry out the hydrothermal reaction at 100°C for 48 hours. Centrifuge and wash with water and ethanol three times respectively, and dry in an electric blast drying oven at 250°C for 2 hours to obtain flower-shaped Cu 2 V 2 o 7 -CuO nanocomposites.

Embodiment 2

[0025] 1) will analytically pure V 2 o 5 The powder is dissolved in an aqueous hydrogen peroxide solution with a mass fraction of 15% to obtain V 5+ The concentration is 0.3mol / l brownish red transparent solution A;

[0026] 2) Under magnetic stirring, press V 5+ and Cu 2+ The molar ratio is 1:1. Solution A is added to the concentration of 0.5mol / L Cu(CH 3 COO) 2 in ethanol solution;

[0027] 3) Use analytically pure sodium hydroxide to adjust the pH value of the solution to 8, and continue to stir to form a reaction precursor;

[0028] 4) Pour the reaction precursor into the reaction kettle, put it in the homogeneous hydrothermal instrument after the equipment is ready, and carry out the hydrothermal reaction at 150°C for 24 hours. Water and ethanol were washed by centrifugation for 3 times respectively, and dried in an electric blast drying oven at 300°C for 3 hours to obtain flower-shaped Cu 2 V 2 o 7 -CuO nanocomposites.

Embodiment 3

[0030] 1) will analytically pure V 2 o 5 The powder is dissolved in an aqueous hydrogen peroxide solution with a mass fraction of 15% to obtain V 5+ The concentration is 0.8mol / l brownish red transparent solution A;

[0031] 2) Under magnetic stirring, press V 5+ and Cu 2+ The molar ratio is 1:2. Solution A is added to the concentration of 1mol / L Cu(CH 3 COO) 2 in ethanol solution;

[0032] 3) Use analytically pure sodium hydroxide to adjust the pH value of the solution to 9, and continue to stir to form a reaction precursor;

[0033] 4) Pour the reaction precursor into the reaction kettle, put it in the homogeneous hydrothermal instrument after the equipment is ready, and carry out the hydrothermal reaction at 200°C for 8 hours. Centrifuge and wash with water and ethanol three times respectively, and dry in an electric blast drying oven at 300°C for 4 hours to obtain flower-shaped Cu 2 V 2 o 7 -CuO nanocomposites.

technical field

[0001] The invention belongs to the technical field of electrode materials for batteries, and in particular relates to a lithium-ion battery electrode material prepared by a solvothermal method to prepare flower-shaped Cu 2 V 2 o 7 - Method for CuO nanocomposites. Background technique

[0002] Copper vanadate (Cu x V y o z ) is a layered structure that can undergo multi-step reduction during intercalation / deintercalation of lithium ions (Cu 2+ / Cu + and Cu + / Cu 0 ), considered to be a lithium-ion battery electrode material with potential application value. Cu 2 V 2 o 7 It is monoclinic phase, C2 / c space group, and has potential application value in negative thermal expansion, magnetism, catalytic oxidation, etc.

[0003] As a semiconductor material, Cu 2 V 2 o 7 The synthesis generally adopts the solid-state sintering method, which has a long reaction time, high energy consumption, and the size of the synthesized product is large, which will ...

Examples

Embodiment 1

[0020] 1) will analytically pure V 2 o 5 The powder is dissolved in an aqueous hydrogen peroxide solution with a mass fraction of 15% to obtain V 5+ The concentration is 0.5mol / l brownish red transparent solution A;

[0021] 2) Under magnetic stirring, press V 5+ and Cu 2+ The molar ratio is 1:0.5 Add solution A to the concentration of 0.1mol / L Cu(CH 3 COO) 2 in ethanol solution;

[0022] 3) Use analytically pure sodium hydroxide to adjust the pH value of the solution to 7, and continue to stir to form a reaction precursor;

[0023] 4) Pour the reaction precursor into the reaction kettle, put it in a homogeneous hydrothermal instrument after the equipment is ready, and carry out the hydrothermal reaction at 100°C for 48 hours. Centrifuge and wash with water and ethanol three times respectively, and dry in an electric blast drying oven at 250°C for 2 hours to obtain flower-shaped Cu 2 V 2 o 7 -CuO nanocomposites.

Embodiment 2

[0025] 1) will analytically pure V 2 o 5 The powder is dissolved in an aqueous hydrogen peroxide solution with a mass fraction of 15% to obtain V 5+ The concentration is 0.3mol / l brownish red transparent solution A;

[0026] 2) Under magnetic stirring, press V 5+ and Cu 2+ The molar ratio is 1:1. Solution A is added to the concentration of 0.5mol / L Cu(CH 3 COO) 2 in ethanol solution;

[0027] 3) Use analytically pure sodium hydroxide to adjust the pH value of the solution to 8, and continue to stir to form a reaction precursor;

[0028] 4) Pour the reaction precursor into the reaction kettle, put it in the homogeneous hydrothermal instrument after the equipment is ready, and carry out the hydrothermal reaction at 150°C for 24 hours. Water and ethanol were washed by centrifugation for 3 times respectively, and dried in an electric blast drying oven at 300°C for 3 hours to obtain flower-shaped Cu 2 V 2 o 7 -CuO nanocomposites.

Embodiment 3

[0030] 1) will analytically pure V 2 o 5 The powder is dissolved in an aqueous hydrogen peroxide solution with a mass fraction of 15% to obtain V 5+ The concentration is 0.8mol / l brownish red transparent solution A;

[0031] 2) Under magnetic stirring, press V 5+ and Cu 2+ The molar ratio is 1:2. Solution A is added to the concentration of 1mol / L Cu(CH 3 COO) 2 in ethanol solution;

[0032] 3) Use analytically pure sodium hydroxide to adjust the pH value of the solution to 9, and continue to stir to form a reaction precursor;

[0033] 4) Pour the reaction precursor into the reaction kettle, put it in the homogeneous hydrothermal instrument after the equipment is ready, and carry out the hydrothermal reaction at 200°C for 8 hours. Centrifuge and wash with water and ethanol three times respectively, and dry in an electric blast drying oven at 300°C for 4 hours to obtain flower-shaped Cu 2 V 2 o 7 -CuO nanocomposites.

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