CN108075124B - Microwave hydrothermal method for preparing Cu2V2O7Method of preparing-CuO nanocomposite - Google Patents

Microwave hydrothermal method for preparing Cu2V2O7Method of preparing-CuO nanocomposite Download PDF

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CN108075124B
CN108075124B CN201711342607.8A CN201711342607A CN108075124B CN 108075124 B CN108075124 B CN 108075124B CN 201711342607 A CN201711342607 A CN 201711342607A CN 108075124 B CN108075124 B CN 108075124B
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曹丽云
王勇
黄剑锋
寇领江
李嘉胤
冯亮亮
赵亚娟
许占位
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Shaanxi University of Science and Technology
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Abstract

Microwave hydrothermal method for preparing Cu2V2O7Method of CuO nanocomposites to analyze pure V2O5Dispersing the powder in CuCl2In an aqueous solution; under magnetic stirring, adjusting the pH value of the solution to 7-9, and continuously stirring to form a reaction precursor; pouring the reaction precursor into a microwave hydrothermal reaction kettle, placing the reaction precursor into a microwave hydrothermal instrument after the reaction is finished, carrying out microwave hydrothermal reaction at 100-200 ℃, separating, washing and drying the product after the instrument is automatically cooled after the reaction is finished, and obtaining the Cu2V2O7-CuO nanocomposites. The invention prepares Cu by a microwave hydrothermal method2V2O7the-CuO nano composite utilizes the advantages of uniform microwave heating, no need of heat conduction process and high heating speed to prepare Cu in a short time2V2O7the-CuO nano composite has high product purity, good crystallinity and uniform appearance and size; the method has the advantages of easily available raw materials, short preparation period, low energy consumption, simple process, high repeatability and strong feasibility.

Description

Microwave hydrothermal method for preparing Cu2V2O7Method of preparing-CuO nanocomposite
Technical Field
The invention belongs to the technical field of electrode materials of batteries, and particularly relates to a microwave hydrothermal method for preparing Cu from an electrode material of a lithium ion battery2V2O7of-CuO nanocompositesA method.
Background
Copper vanadate (Cu)xVyOz) Is a layered structure, and can perform multi-step reduction (Cu) during the process of lithium ion intercalation/deintercalation2+/Cu+And Cu+/Cu0) And is considered to be an electrode material of a lithium ion battery with potential application value. Cu2V2O7The carbon nanotube is a monoclinic phase, and the C2/C space group has potential application values in the aspects of negative thermal expansibility, magnetism, catalytic oxidation and the like.
As a semiconductor material, Cu is currently used2V2O7The synthesis generally adopts a solid phase method for sintering, the reaction time is long, the energy consumption is high, the size of the synthesized product is large, and large stress can be generated in the battery circulation process to influence the circulation stability of the battery.
Disclosure of Invention
The invention aims to provide the Cu which is prepared by low synthesis temperature, short reaction time and high synthesis speed2V2O7Cu prepared by microwave hydrothermal method with uniform particle size of-CuO nano composite and good lithium storage performance2V2O7-a CuO nanocomposite.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
1) according to V5+And Cu2+In a molar ratio of 1: (0.5-2), analytically pure V2O5The powder is dispersed in 0.1-1 mol/L CuCl2In an aqueous solution;
2) under magnetic stirring, adjusting the pH value of the solution to 7-9, and continuously stirring to form a reaction precursor;
3) pouring the reaction precursor into a microwave hydrothermal reaction kettle, placing the reaction precursor into a microwave hydrothermal instrument after the reaction is finished, carrying out microwave hydrothermal reaction at 100-200 ℃, separating, washing and drying the product after the instrument is automatically cooled after the reaction is finished, and obtaining the Cu2V2O7-CuO nanocomposites.
And 2) adjusting the pH value by adopting ammonia water.
The power of the microwave water heat instrument in the step 3) is 400W.
The microwave hydrothermal reaction time in the step 3) is 1-2 h.
The step 3) of separating, washing and drying comprises the following steps: and (3) carrying out vacuum filtration, washing with deionized water and absolute ethyl alcohol for 3 times respectively, and drying in a vacuum drying oven at 250-300 ℃ for 0.5-2 h.
Compared with the prior art, the invention has the following beneficial effects:
the invention prepares Cu by a microwave hydrothermal method2V2O7the-CuO nano composite utilizes the advantages of uniform microwave heating, no need of heat conduction process and high heating speed to prepare Cu in a short time2V2O7the-CuO nano composite has high product purity, good crystallinity and uniform appearance and size; the method has the advantages of easily available raw materials, short preparation period, low energy consumption, simple process, high repeatability and strong feasibility.
Drawings
FIG. 1 shows the microwave hydrothermal method for preparing Cu according to the present invention2V2O7XRD pattern of CuO nanocomposite.
FIG. 2 shows the microwave hydrothermal method for preparing Cu according to the present invention2V2O7SEM image (x10.0k) of CuO nanocomposite.
FIG. 3 shows the microwave hydrothermal method for preparing Cu according to the present invention2V2O7SEM image (x50.0k) of CuO nanocomposite.
Detailed Description
Example 1:
1) according to V5+And Cu2+In a molar ratio of 1: 0.5, V will be analytically pure2O5The powder is dispersed in 0.1 mol/L CuCl2In an aqueous solution;
2) under magnetic stirring, adjusting the pH value of the solution to 7 by adopting ammonia water, and continuously stirring to form a reaction precursor;
3) pouring the reaction precursor into a microwave hydrothermal reaction kettle, placing the reaction precursor into a microwave hydrothermal instrument with the power of 400W after the reaction is finished, carrying out microwave hydrothermal reaction for 1h at the temperature of 100 ℃, carrying out reduced pressure suction filtration after the instrument is automatically cooled after the reaction is finished, and removing the productWashing the seed water and absolute ethyl alcohol for 3 times respectively, placing in a vacuum drying oven at 250 ℃, and drying for 2 hours to obtain Cu2V2O7-CuO nanocomposites.
Example 2:
1) according to V5+And Cu2+In a molar ratio of 1: 2, analytically pure V2O5The powder is dispersed in 0.5 mol/L CuCl2In an aqueous solution;
2) under magnetic stirring, adjusting the pH value of the solution to 8 by adopting ammonia water, and continuously stirring to form a reaction precursor;
3) pouring the reaction precursor into a microwave hydrothermal reaction kettle, placing the reaction precursor into a microwave hydrothermal instrument with the power of 400W after the reaction is finished, carrying out microwave hydrothermal reaction for 2h at the temperature of 150 ℃, carrying out reduced pressure suction filtration after the reaction is finished and the instrument is automatically cooled, washing the reaction product for 3 times by deionized water and absolute ethyl alcohol respectively, placing the reaction product in a vacuum drying box with the temperature of 300 ℃, and drying the reaction product for 1h to obtain the Cu2V2O7-CuO nanocomposites.
Example 3:
1) according to V5+And Cu2+In a molar ratio of 1: 1, analytically pure V2O5The powder is dispersed in 1 mol/L CuCl2In an aqueous solution;
2) under magnetic stirring, adjusting the pH value of the solution to 9 by adopting ammonia water, and continuously stirring to form a reaction precursor;
3) pouring the reaction precursor into a microwave hydrothermal reaction kettle, placing the reaction precursor into a microwave hydrothermal instrument with the power of 400W after the reaction is finished, carrying out microwave hydrothermal reaction for 1h at the temperature of 200 ℃, carrying out reduced pressure suction filtration after the reaction is finished and the instrument is automatically cooled, washing the reaction product for 3 times by deionized water and absolute ethyl alcohol respectively, placing the reaction product in a vacuum drying box with the temperature of 300 ℃, and drying the reaction product for 0.5h to obtain the Cu2V2O7-CuO nanocomposites.
Example 4:
1) according to V5+And Cu2+In a molar ratio of 1: 1, analytically pure V2O5The powder is dispersed in 1 mol/L CuCl2In an aqueous solution;
2) under magnetic stirring, adjusting the pH value of the solution to 7 by adopting ammonia water, and continuously stirring to form a reaction precursor;
3) pouring the reaction precursor into a microwave hydrothermal reaction kettle, placing the reaction precursor into a microwave hydrothermal instrument with the power of 400W after the reaction is finished, carrying out microwave hydrothermal reaction for 2h at the temperature of 150 ℃, carrying out reduced pressure suction filtration after the reaction is finished and the instrument is automatically cooled, washing the reaction product for 3 times by deionized water and absolute ethyl alcohol respectively, placing the reaction product in a vacuum drying box with the temperature of 300 ℃, and drying the reaction product for 0.5h to obtain the Cu2V2O7-CuO nanocomposites.
Example 5:
1) according to V5+And Cu2+In a molar ratio of 1: 1.5, analytically pure V2O5The powder is dispersed in 0.3 mol/L CuCl2In an aqueous solution;
2) under magnetic stirring, adjusting the pH value of the solution to 8 by adopting ammonia water, and continuously stirring to form a reaction precursor;
3) pouring the reaction precursor into a microwave hydrothermal reaction kettle, placing the reaction precursor into a microwave hydrothermal instrument with the power of 400W after the reaction is finished, carrying out microwave hydrothermal reaction for 1.5h at the temperature of 150 ℃, carrying out reduced pressure suction filtration after the reaction is finished and the instrument is automatically cooled, washing the reaction precursor for 3 times by using deionized water and absolute ethyl alcohol respectively, placing the reaction precursor in a vacuum drying box with the temperature of 260 ℃, and drying the reaction precursor for 1.5h to obtain the Cu2V2O7-CuO nanocomposites.
Example 6:
1) according to V5+And Cu2+In a molar ratio of 1: 0.8, V will be analytically pure2O5The powder is dispersed in 0.8 mol/L CuCl2In an aqueous solution;
2) under magnetic stirring, adjusting the pH value of the solution to 9 by adopting ammonia water, and continuously stirring to form a reaction precursor;
3) pouring the reaction precursor into a microwave hydrothermal reaction kettle, placing the reaction precursor into a microwave hydrothermal instrument with the power of 400W after the reaction is finished, carrying out microwave hydrothermal reaction for 1.5h at the temperature of 180 ℃, carrying out reduced pressure suction filtration after the reaction is finished and the instrument is automatically cooled, washing the reaction precursor for 3 times by using deionized water and absolute ethyl alcohol respectively, placing the reaction precursor in a vacuum drying box with the temperature of 280 ℃, and drying the reaction precursor for 1h to obtain the Cu2V2O7-CuO nanocomposites.
FIG. 1 shows the microwave hydrothermal method for preparing Cu according to the present invention2V2O7-CuXRD pattern of O nanocomposite. As can be seen from FIG. 1, the product has sharp diffraction peak shape and good crystallinity, and the product is Cu2V2O7And a CuO composite phase. FIGS. 2 and 3 show the microwave hydrothermal method for preparing Cu according to the present invention2V2O7SEM images of CuO nanocomposites. As can be seen from FIGS. 2 and 3, the morphology of the product is spherical with a diameter of 600nm, and the spheres are assembled by small particles with a particle size of 100 nm.

Claims (5)

1. Microwave hydrothermal method for preparing Cu2V2O7-a method of CuO nanocomposites, characterized by comprising the steps of:
1) according to V5+And Cu2+In a molar ratio of 1: (0.5-2), analytically pure V2O5The powder is dispersed in 0.1-1 mol/L CuCl2In an aqueous solution;
2) under magnetic stirring, adjusting the pH value of the solution to 7-9, and continuously stirring to form a reaction precursor;
3) pouring the reaction precursor into a microwave hydrothermal reaction kettle, placing the reaction precursor into a microwave hydrothermal instrument after the reaction is finished, carrying out microwave hydrothermal reaction at 100-200 ℃, separating, washing and drying the product after the instrument is automatically cooled after the reaction is finished, and obtaining the Cu2V2O7-CuO nanocomposites.
2. The microwave hydrothermal method for preparing Cu according to claim 12V2O7-a method of CuO nanocomposite characterized in that: and 2) adjusting the pH value by adopting ammonia water.
3. The microwave hydrothermal method for preparing Cu according to claim 12V2O7-a method of CuO nanocomposite characterized in that: the power of the microwave water heat instrument in the step 3) is 400W.
4. The microwave hydrothermal method for preparing Cu according to claim 12V2O7-a method of CuO nanocomposite characterized in that: the step 3) of microwave hydrothermal reactionThe reaction time is 1-2 h.
5. The microwave hydrothermal method for preparing Cu according to claim 12V2O7-a method of CuO nanocomposite characterized in that: the step 3) of separating, washing and drying comprises the following steps: and (3) carrying out vacuum filtration, washing with deionized water and absolute ethyl alcohol for 3 times respectively, and drying in a vacuum drying oven at 250-300 ℃ for 0.5-2 h.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101920993A (en) * 2010-08-03 2010-12-22 复旦大学 Preparation method and application of copper vanadate electrode material
WO2016148441A1 (en) * 2015-03-13 2016-09-22 주식회사 엘지화학 Lithium metal oxide, and negative electrode active material for lithium secondary battery having same, and manufaturing method therefor
CN106099092A (en) * 2016-07-01 2016-11-09 陕西科技大学 A kind of preparation method of the copper vanadate for lithium ion battery negative material
CN106186062A (en) * 2016-07-01 2016-12-07 陕西科技大学 A kind of homogeneous hydro-thermal method prepares flower-shaped Cu2v2o7the method of material and the Cu of preparation2v2o7material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101920993A (en) * 2010-08-03 2010-12-22 复旦大学 Preparation method and application of copper vanadate electrode material
WO2016148441A1 (en) * 2015-03-13 2016-09-22 주식회사 엘지화학 Lithium metal oxide, and negative electrode active material for lithium secondary battery having same, and manufaturing method therefor
CN106099092A (en) * 2016-07-01 2016-11-09 陕西科技大学 A kind of preparation method of the copper vanadate for lithium ion battery negative material
CN106186062A (en) * 2016-07-01 2016-12-07 陕西科技大学 A kind of homogeneous hydro-thermal method prepares flower-shaped Cu2v2o7the method of material and the Cu of preparation2v2o7material

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