CN108075124A - A kind of microwave-hydrothermal method prepares Cu2V2O7The method of-CuO nano-complexes - Google Patents

A kind of microwave-hydrothermal method prepares Cu2V2O7The method of-CuO nano-complexes Download PDF

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CN108075124A
CN108075124A CN201711342607.8A CN201711342607A CN108075124A CN 108075124 A CN108075124 A CN 108075124A CN 201711342607 A CN201711342607 A CN 201711342607A CN 108075124 A CN108075124 A CN 108075124A
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complexes
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cuo nano
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CN108075124B (en
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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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    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
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Abstract

A kind of microwave-hydrothermal method prepares Cu2V2O7The method of CuO nano-complexes, by analytically pure V2O5Powder is scattered in CuCl2In aqueous solution；Under magnetic stirring, it is 7~9 to adjust pH value of solution, continues stirring and forms precursors；Precursors are poured into microwave hydrothermal reaction kettle, what is be equipped with is placed in microwave hydrothermal instrument, is reacted in 100~200 DEG C of microwave hydrothermals, and reaction terminates after instrument automatically cooling, and product separating, washing is drying to obtain Cu2V2O7CuO nano-complexes.The present invention prepares Cu with microwave-hydrothermal method2V2O7CuO nano-complexes, it is uniform using microwave heating, without heat transfer process, the advantages of firing rate is fast, Cu is prepared in a short period of time2V2O7CuO nano-complexes, product purity is high, good crystallinity, and appearance and size is homogeneous；The raw materials used in the present invention is easy to get, and short preparation period, low energy consumption, simple for process, and repeatability is high, and feasibility is strong.

Description

A kind of microwave-hydrothermal method prepares Cu2V2O7The method of-CuO nano-complexes
Technical field
The invention belongs to the electrode material technical fields of battery, and in particular to a kind of lithium ion battery electrode material microwave Hydro-thermal method prepares Cu2V2O7The method of-CuO nano-complexes.
Background technology
Copper vanadate (CuxVyOz) it is a kind of with layer structure, multistep can be carried out during insertion/deintercalate lithium ions Reduce (Cu2+/Cu+And Cu+/Cu0), it is considered to be there is the lithium ion battery electrode material of potential using value.Cu2V2O7For list Monoclinic phase, C2/c space groups have potential application value in negative expansion, magnetism, catalysis oxidation etc..
As a kind of semi-conducting material, Cu at present2V2O7Synthesis is generally sintered using solid phase method, and the reaction time is long, energy consumption Height, the Product size of synthesis is larger, and larger stress can be generated during circulating battery, influences the cyclical stability of battery.
The content of the invention
It is an object of the invention to provide a kind of synthesis temperature is low, the reaction time is short, and aggregate velocity is fast, prepared Cu2V2O7- CuO nano-complex uniform particle sizes, the microwave-hydrothermal method with preferable storage lithium performance prepare Cu2V2O7- CuO nanometers The method of compound.
In order to achieve the above object, the technical solution adopted by the present invention is as follows：
1) V is pressed5+And Cu2+Molar ratio be 1：(0.5~2), by analytically pure V2O5Powder is scattered in 0.1~1mol/L's CuCl2In aqueous solution；
2) it is 7~9 under magnetic stirring, to adjust pH value of solution, continues stirring and forms precursors；
3) precursors are poured into microwave hydrothermal reaction kettle, what is be equipped with is placed in microwave hydrothermal instrument, 100~ 200 DEG C of microwave hydrothermal reactions, reaction terminate after instrument automatically cooling, and product separating, washing is drying to obtain Cu2V2O7- CuO receives Rice compound.
The step 2) adjusts pH value using ammonium hydroxide.
Step 3) the microwave hydrothermal instrument power is 400W.
Step 3) the microwave hydrothermal reaction time is 1~2h.
Step 3) the separating, washing is dried：Decompression filters, and with deionized water and absolute ethyl alcohol respectively washing 3 times, is placed in In 250~300 DEG C of vacuum drying chamber, dry 0.5~2h.
Compared with prior art, the device have the advantages that：
The present invention prepares Cu with microwave-hydrothermal method2V2O7- CuO nano-complexes, it is uniform using microwave heating, it is passed without heat Process is led, the advantages of firing rate is fast, prepares Cu in a short period of time2V2O7- CuO nano-complexes, product purity is high, Good crystallinity, appearance and size are homogeneous；The raw materials used in the present invention is easy to get, and short preparation period, low energy consumption, simple for process, and repeatability is high, Feasibility is strong.
Description of the drawings
Fig. 1 prepares Cu for the present invention with microwave-hydrothermal method2V2O7The XRD diagram of-CuO nano-complexes.
Fig. 2 prepares Cu for the present invention with microwave-hydrothermal method2V2O7The SEM figures (x10.0k) of-CuO nano-complexes.
Fig. 3 prepares Cu for the present invention with microwave-hydrothermal method2V2O7The SEM figures (x50.0k) of-CuO nano-complexes.
Specific embodiment
Embodiment 1：
1) V is pressed5+And Cu2+Molar ratio be 1：0.5, by analytically pure V2O5Powder is scattered in the CuCl of 0.1mol/L2Water In solution；
2) ammonium hydroxide under magnetic stirring, is used to adjust pH value of solution as 7, continues stirring and forms precursors；
3) precursors are poured into microwave hydrothermal reaction kettle, what is be equipped with is placed on the microwave hydrothermal that power is 400W In instrument, 1h are reacted in 100 DEG C of microwave hydrothermals, reaction terminates after instrument automatically cooling, and decompression filters, with deionized water and anhydrous Ethyl alcohol respectively washing 3 times, are placed in 250 DEG C of vacuum drying chamber, and dry 2h is up to Cu2V2O7- CuO nano-complexes.
Embodiment 2：
1) V is pressed5+And Cu2+Molar ratio be 1：2, by analytically pure V2O5Powder is scattered in the CuCl of 0.5mol/L2It is water-soluble In liquid；
2) ammonium hydroxide under magnetic stirring, is used to adjust pH value of solution as 8, continues stirring and forms precursors；
3) precursors are poured into microwave hydrothermal reaction kettle, what is be equipped with is placed on the microwave hydrothermal that power is 400W In instrument, 2h are reacted in 150 DEG C of microwave hydrothermals, reaction terminates after instrument automatically cooling, and decompression filters, with deionized water and anhydrous Ethyl alcohol respectively washing 3 times, are placed in 300 DEG C of vacuum drying chamber, and dry 1h is up to Cu2V2O7- CuO nano-complexes.
Embodiment 3：
1) V is pressed5+And Cu2+Molar ratio be 1：1, by analytically pure V2O5Powder is scattered in the CuCl of 1mol/L2Aqueous solution In；
2) ammonium hydroxide under magnetic stirring, is used to adjust pH value of solution as 9, continues stirring and forms precursors；
3) precursors are poured into microwave hydrothermal reaction kettle, what is be equipped with is placed on the microwave hydrothermal that power is 400W In instrument, 1h are reacted in 200 DEG C of microwave hydrothermals, reaction terminates after instrument automatically cooling, and decompression filters, with deionized water and anhydrous Ethyl alcohol respectively washing 3 times, are placed in 300 DEG C of vacuum drying chamber, and dry 0.5h is up to Cu2V2O7- CuO nano-complexes.
Embodiment 4：
1) V is pressed5+And Cu2+Molar ratio be 1：1, by analytically pure V2O5Powder is scattered in the CuCl of 1mol/L2Aqueous solution In；
2) ammonium hydroxide under magnetic stirring, is used to adjust pH value of solution as 7, continues stirring and forms precursors；
3) precursors are poured into microwave hydrothermal reaction kettle, what is be equipped with is placed on the microwave hydrothermal that power is 400W In instrument, 2h are reacted in 150 DEG C of microwave hydrothermals, reaction terminates after instrument automatically cooling, and decompression filters, with deionized water and anhydrous Ethyl alcohol respectively washing 3 times, are placed in 300 DEG C of vacuum drying chamber, and dry 0.5h is up to Cu2V2O7- CuO nano-complexes.
Embodiment 5：
1) V is pressed5+And Cu2+Molar ratio be 1：1.5, by analytically pure V2O5Powder is scattered in the CuCl of 0.3mol/L2Water In solution；
2) ammonium hydroxide under magnetic stirring, is used to adjust pH value of solution as 8, continues stirring and forms precursors；
3) precursors are poured into microwave hydrothermal reaction kettle, what is be equipped with is placed on the microwave hydrothermal that power is 400W In instrument, 1.5h is reacted in 150 DEG C of microwave hydrothermals, reaction terminates after instrument automatically cooling, and decompression filters, with deionized water and nothing Water-ethanol respectively washing 3 times, are placed in 260 DEG C of vacuum drying chamber, and dry 1.5h is up to Cu2V2O7- CuO nano-complexes.
Embodiment 6：
1) V is pressed5+And Cu2+Molar ratio be 1：0.8, by analytically pure V2O5Powder is scattered in the CuCl of 0.8mol/L2Water In solution；
2) ammonium hydroxide under magnetic stirring, is used to adjust pH value of solution as 9, continues stirring and forms precursors；
3) precursors are poured into microwave hydrothermal reaction kettle, what is be equipped with is placed on the microwave hydrothermal that power is 400W In instrument, 1.5h is reacted in 180 DEG C of microwave hydrothermals, reaction terminates after instrument automatically cooling, and decompression filters, with deionized water and nothing Water-ethanol respectively washing 3 times, are placed in 280 DEG C of vacuum drying chamber, and dry 1h is up to Cu2V2O7- CuO nano-complexes.
Fig. 1 prepares Cu for the present invention with microwave-hydrothermal method2V2O7The XRD diagram of-CuO nano-complexes.It can from Fig. 1 Go out that product diffraction maximum peak shape is sharp, and crystallinity is preferable, product Cu2V2O7With CuO compound phases.Fig. 2 and Fig. 3 is the present invention with micro- Ripple hydro-thermal method prepares Cu2V2O7The SEM figures of-CuO nano-complexes.As can be seen that product morphology is diameter 600nm from Fig. 2,3 It is spherical, and ball is then assembled by the little particle of grain size 100nm.

Claims (5)

1. a kind of microwave-hydrothermal method prepares Cu2V2O7The method of-CuO nano-complexes, it is characterised in that comprise the following steps：
1) V is pressed5+And Cu2+Molar ratio be 1：(0.5~2), by analytically pure V2O5Powder is scattered in the CuCl of 0.1~1mol/L2 In aqueous solution；
2) it is 7~9 under magnetic stirring, to adjust pH value of solution, continues stirring and forms precursors；
3) precursors are poured into microwave hydrothermal reaction kettle, what is be equipped with is placed in microwave hydrothermal instrument, 100~200 The reaction of DEG C microwave hydrothermal, reaction terminate after instrument automatically cooling, and product separating, washing is drying to obtain Cu2V2O7- CuO nanometers Compound.
2. microwave-hydrothermal method according to claim 1 prepares Cu2V2O7The method of-CuO nano-complexes, it is characterised in that： The step 2) adjusts pH value using ammonium hydroxide.
3. microwave-hydrothermal method according to claim 1 prepares Cu2V2O7The method of-CuO nano-complexes, it is characterised in that： Step 3) the microwave hydrothermal instrument power is 400W.
4. microwave-hydrothermal method according to claim 1 prepares Cu2V2O7The method of-CuO nano-complexes, it is characterised in that： Step 3) the microwave hydrothermal reaction time is 1~2h.
5. microwave-hydrothermal method according to claim 1 prepares Cu2V2O7The method of-CuO nano-complexes, it is characterised in that： Step 3) the separating, washing is dried：Decompression filters, and with deionized water and absolute ethyl alcohol respectively washing 3 times, is placed in 250~300 DEG C vacuum drying chamber in, dry 0.5~2h.
CN201711342607.8A 2017-12-14 2017-12-14 Microwave hydrothermal method for preparing Cu2V2O7Method of preparing-CuO nanocomposite Active CN108075124B (en)

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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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