CN106186062B - A kind of homogeneous hydro-thermal method prepares flower-shaped Cu2V2O7The method of material and the Cu of preparation2V2O7Material - Google Patents
A kind of homogeneous hydro-thermal method prepares flower-shaped Cu2V2O7The method of material and the Cu of preparation2V2O7Material Download PDFInfo
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- CN106186062B CN106186062B CN201610511916.2A CN201610511916A CN106186062B CN 106186062 B CN106186062 B CN 106186062B CN 201610511916 A CN201610511916 A CN 201610511916A CN 106186062 B CN106186062 B CN 106186062B
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Abstract
A kind of homogeneous hydro-thermal method prepares flower-shaped Cu2V2O7The method of material and the Cu of preparation2V2O7Material, cuprous oxide is scattered in deionized water, and ammonium metavanadate is added after being uniformly dispersed, and obtains reaction precursor liquid；Body liquid is at 100~200 DEG C before reacting, after 5~48h of hydro-thermal reaction, is cooled to room temperature, and centrifuge washing precipitation will precipitate drying, obtain powder；Powder is sintered, flower-shaped Cu is obtained2V2O7Material.The present invention is using hard template reaction method in situ topological, especially by by Cu2O and NH4VO3Reaction precursor liquid is mixed with, then using hydro-thermal reaction, finally sintering removes the crystallization water, and negative electrode of lithium ion battery Cu has been made2V2O7Material, this method technique is simple, without complex device, material requested can be prepared at normal temperatures and pressures, the reaction time is short, and product purity is high, and reaction condition is easily controllable, can realize large-scale industrial production.
Description
Technical field
The invention belongs to the electrode material technical field of battery, it is related to a kind of Cu2V2O7Material and preparation method thereof, especially
It is related to a kind of homogeneous hydro-thermal method and prepares flower-shaped Cu2V2O7The method of material and the Cu of preparation2V2O7Material.
Background technology
Lithium ion has energy density height, power density is high, have extended cycle life, temperature in use scope is wide, memory-less effect
The advantages of, it is widely used in each field.But current commercialized lithium ion battery negative material is main based on graphite,
But its less theoretical capacity (372mAh/g), and also there is certain potential safety hazard in it, and these shortcomings limit answering for its
With.
Cu with layer structure2V2O7Multistep reduction (Cu can be carried out during insertion/deintercalate lithium ions2+/Cu+And
Cu+/Cu0), it is considered to be lithium ion battery negative material [Cheng F, Chen with potential using value
J.Transition metal vanadium oxides and vanadate materials for lithium
batteries[J].Journal of Materials Chemistry,2011,21(27):9841-9848.].Due to copper
Many single-step reductives, Cu2V2O7Higher energy density can be provided.
Cu2V2O7Synthetic method be mainly high temperature solid-state method [Hillel T, Ein-Eli Y.Copper vanadate
as promising high voltage cathodes for Li thermal batteries[J].Journal of
Power Sources,2013,229:112-116], [Guo Guanghui, Chen Shan, Liu Fangfang wait .Cu to sol-gal process2V2O7Synthesis
And chemical property [J] non-ferrous metals：Smelting Part, 2014 (2):57-60.] etc..High temperature solid-state method synthetic operation is simple, but
Long-time high-temperature process is needed, and product morphology is uncontrollable.Sol-gel method craft is complicated, severe reaction conditions, it is difficult to real
Existing large-scale industrial production, and further part needs also exist for high-temperature process.Both approaches are equal in commercial process
Cost can be sharply increased, while high temperature sintering also can produce influence to the chemical property of product.
The content of the invention
Flower-shaped Cu is prepared it is an object of the invention to provide a kind of homogeneous hydro-thermal method2V2O7The method of material, this method is used
Hydrothermal reaction at low temperature, by topological growing technology in situ, prepares the flower-shaped Cu with good chemical property2V2O7Material,
This method is simple to operate, and repeatability is high, and production cost is low, is adapted to industrialized production.
In order to achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of homogeneous hydro-thermal method prepares flower-shaped Cu2V2O7The method of material, comprises the following steps：
1) cuprous oxide is scattered in deionized water, ammonium metavanadate powder is added after being uniformly dispersed, stirs, obtains
Reaction precursor liquid；Wherein, cuprous oxide and ammonium metavanadate ratio are 0.125g：0.102g；
2) body liquid is at 100~200 DEG C before reacting, and 5~48h of hydro-thermal reaction after question response terminates, is cooled to room temperature,
Washing precipitation is then centrifuged for, drying will be precipitated, obtain powder；
3) powder is sintered, sloughs the crystallization water, gained powder is flower-shaped Cu2V2O7Material.
Of the invention further improve be, described step 1) in ammonium metavanadate it is pure to analyze.
Of the invention further improve be, described step 1) in cuprous oxide and the ratio of deionized water be 0.125g：
80mL。
Of the invention further improve be, described step 1) in be uniformly dispersed and use magnetic agitation, stirring
Time is 0.5~5h.
Of the invention further improve be, described step 1) in mixing time be 1~5h.
Of the invention further improve be, described step 2) in hydro-thermal reaction when water heating kettle packing ratio be 30%
~70%.
Of the invention further improve be, described step 2) in the rotating speed of centrifuge washing be 8000 turns/min.
Of the invention further improve be, described step 2) in the temperature of drying be 50~100 DEG C, when dry
Between be 2~12h.
Of the invention further improve be, described step 3) in the temperature of calcining be 200 DEG C~500 DEG C, calcining
Time be 0.2h~5h.
A kind of Cu2V2O7Material, the Cu2V2O7Material shows the diameter being made up of thickness for 80~100nm nanometer sheet
For 1.0~1.2um floriform appearance.
Compared with prior art, the present invention has following beneficial technique effect：The present invention is using hard template-original position topology
Reaction method, especially by by Cu2O and NH4VO3Reaction precursor liquid is mixed with, then using hydro-thermal reaction, finally sintering is removed
The crystallization water, has been made negative electrode of lithium ion battery Cu2V2O7Material, the present invention prepares flower-shaped Cu2V2O7It is not used during material
Any surfactant.The present invention is due to using hydro-thermal reaction, so the temperature of reaction can be reduced, 5~48h of reaction time,
It is that the high temperature solid-state method reaction time is short relative to the material, and this method technique is simple, can be normal in normal temperature without complex device
Material requested is prepared in pressure, and the reaction time is short, and product purity is high, and reaction condition is easily controllable, can realize large-scale industry
Metaplasia is produced.Cu prepared by the present invention2V2O7Material show by thickness for 80~100nm nanometer sheet constitute a diameter of 1.0~
1.2um floriform appearance, the Cu2V2O7Material has good chemical property, because vanadic acid copper product prepared by the present invention is
Nanometer grade powder, floriform appearance makes the material have larger specific surface area, helps to shorten lithium ion in charge and discharge process
Diffusion path, improves its high rate performance and cycle performance.It can also effectively increase its contact area with electrolyte simultaneously, from
And with excellent chemical property.
Brief description of the drawings
The Cu that Fig. 1 is prepared for the present invention2V2O7The X-ray diffractogram of material；
The Cu that Fig. 2 is prepared for the present invention2V2O7The ESEM shape appearance figure of material；Wherein (a) is 50.0K；(b) it is 100K；
The Cu that Fig. 3 is prepared for the present invention2V2O7The cycle performance figure of electrode material.
Embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
1) the freshly prepd hexahedron cuprous oxide (Cu of 0.125g 20 are weighed2O) it is scattered in 80mL deionizations, magnetic force is stirred
0.5h is mixed, 0.102g ammonium metavanadates (NH is then added4VO3) powder, 2h is stirred, reaction precursor liquid is obtained；
2) body liquid before reaction is transferred in reactor, the packing ratio of reactor is 40%, then at 180 DEG C, hydro-thermal
12h is reacted, after question response terminates, room temperature is cooled to, washing precipitation is then centrifuged for, will be deposited at 60 DEG C and dry 10h, obtain powder
Body；
3) by dried powder, it is sintered at 300 DEG C, sloughs the crystallization water, and be incubated 0.5h；It is cold with stove afterwards
But, gained powder is the flower-shaped Cu of negative electrode of lithium ion battery2V2O7Material.
It will be seen from figure 1 that the copper vanadate prepared by embodiment 1 is α-Cu2V2O7, its diffraction maximum and Cu2V2O7
(JCPDSNo.26-0569) base peak matches, without obvious impurity.
It is 80~100nm by thickness from Fig. 2 (a) and Fig. 2 (b) as can be seen that prepared copper vanadate is by flower-like structure
A diameter of 1.0~1.2um for constituting of nanometer sheet.
Fig. 3 be the vanadic acid copper product in 0.1A/g cycle performance figure, its initial discharge capacity reaches 760mAh/g, through 30
After circle circulation, specific capacity remains at 469mAh/g, shows good cycle performance.
Embodiment 2
1) freshly prepared 20 hexahedron cuprous oxide is scattered in deionized water, it is pure partially that magnetic agitation 0.2h adds analysis
Ammonium vanadate powder, magnetic agitation 5h obtains reaction precursor liquid；Wherein, cuprous oxide and ammonium metavanadate and the ratio of deionized water
For 0.125g：0.102g：80mL；
2) body liquid before reaction is transferred in reactor, the packing ratio of reactor is 70%, then at 100 DEG C, hydro-thermal
48h is reacted, after question response terminates, room temperature is cooled to, then centrifuge washing is precipitated under 8000 turns/min, will be deposited at 50 DEG C
12h is dried, powder is obtained；
3) powder is sintered into 0.2h at 500 DEG C, sloughs the crystallization water, gained powder is flower-shaped Cu2V2O7Material.
Embodiment 3
1) freshly prepared 20 hexahedron cuprous oxide is scattered in deionized water, magnetic agitation 2h adds the pure inclined vanadium of analysis
Sour ammonium powder, magnetic agitation 3h obtains reaction precursor liquid；Wherein, cuprous oxide and ammonium metavanadate and the ratio of deionized water are
0.125g：0.102g：80mL
2) body liquid before reaction is transferred in reactor, the packing ratio of reactor is 30%, then at 200 DEG C, hydro-thermal
5h is reacted, after question response terminates, room temperature is cooled to, then centrifuge washing is precipitated under 8000 turns/min, will be deposited at 100 DEG C
2h is dried, powder is obtained；
3) powder is sintered into 5h at 200 DEG C, sloughs the crystallization water, gained powder is flower-shaped Cu2V2O7Material.
Embodiment 4
1) freshly prepared 20 hexahedron cuprous oxide is scattered in deionized water, magnetic agitation 5h adds the pure inclined vanadium of analysis
Sour ammonium powder, magnetic agitation 1h obtains reaction precursor liquid；Wherein, cuprous oxide and ammonium metavanadate and the ratio of deionized water are
0.125g：0.102g：80mL
2) body liquid before reaction is transferred in reactor, the packing ratio of reactor is 60%, then at 120 DEG C, hydro-thermal
36h is reacted, after question response terminates, room temperature is cooled to, then centrifuge washing is precipitated under 8000 turns/min, will be deposited at 70 DEG C
8h is dried, powder is obtained；
3) powder is sintered into 3h at 400 DEG C, sloughs the crystallization water, gained powder is flower-shaped Cu2V2O7Material.
Embodiment 5
1) freshly prepared 20 hexahedron cuprous oxide is scattered in deionized water, magnetic agitation 1h adds the pure inclined vanadium of analysis
Sour ammonium powder, magnetic agitation 10h obtains reaction precursor liquid；Wherein, cuprous oxide and ammonium metavanadate and the ratio of deionized water are
0.125g：0.102g：80mL
2) body liquid before reaction is transferred in reactor, the packing ratio of reactor is 50%, then at 150 DEG C, hydro-thermal
24h is reacted, after question response terminates, room temperature is cooled to, then centrifuge washing is precipitated under 8000 turns/min, will be deposited at 80 DEG C
6h is dried, powder is obtained；
3) powder is sintered into 3h at 350 DEG C, sloughs the crystallization water, gained powder is flower-shaped Cu2V2O7Material.
Flower-shaped Cu prepared by the present invention2V2O7Material show by thickness for 80~100nm nanometer sheet constitute it is a diameter of
1.0~1.2um floriform appearance.
Claims (7)
1. a kind of homogeneous hydro-thermal method prepares flower-shaped Cu2V2O7The method of material, it is characterised in that comprise the following steps：
1) freshly prepd cuprous oxide is scattered in deionized water, analytically pure ammonium metavanadate powder is added after being uniformly dispersed,
Stir, obtain reaction precursor liquid；Wherein, cuprous oxide and ammonium metavanadate ratio are 0.125g：0.102g；
2) body liquid is at 100~200 DEG C before reacting, and 5~48h of hydro-thermal reaction after question response terminates, is cooled to room temperature, then
Centrifuge washing is precipitated, and will be precipitated drying, is obtained powder；
3) powder is sintered, sloughs the crystallization water, gained powder is flower-shaped Cu2V2O7Material；
Step 1) in cuprous oxide and the ratio of deionized water be 0.125g：80mL；
Step 3) in the temperature of calcining be 200 DEG C~500 DEG C, time of calcining is 0.2h~5h.
2. homogeneous hydro-thermal method according to claim 1 prepares flower-shaped Cu2V2O7The method of material, it is characterised in that described
Step 1) in be uniformly dispersed and use magnetic agitation, the time of stirring is 0.5~5h.
3. homogeneous hydro-thermal method according to claim 1 prepares flower-shaped Cu2V2O7The method of material, it is characterised in that described
Step 1) in mixing time be 1~5h.
4. homogeneous hydro-thermal method according to claim 1 prepares flower-shaped Cu2V2O7The method of material, it is characterised in that described
Step 2) in hydro-thermal reaction when water heating kettle packing ratio be 30%~70%.
5. homogeneous hydro-thermal method according to claim 1 prepares flower-shaped Cu2V2O7The method of material, it is characterised in that described
Step 2) in centrifuge washing rotating speed be 8000 turns/min.
6. homogeneous hydro-thermal method according to claim 1 prepares flower-shaped Cu2V2O7The method of material, it is characterised in that described
Step 2) in the temperature of drying be 50~100 DEG C, dry time is 2~12h.
7. a kind of Cu prepared according to the method described in claim 12V2O7Material, it is characterised in that the Cu2V2O7Material is presented
Go out a diameter of 1.0~1.2 μm of floriform appearance being made up of thickness for 80~100nm nanometer sheet.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108075124B (en) * | 2017-12-14 | 2020-07-28 | 陕西科技大学 | Microwave hydrothermal method for preparing Cu2V2O7Method of preparing-CuO nanocomposite |
| CN108101108B (en) * | 2017-12-14 | 2020-02-21 | 陕西科技大学 | β -Cu2V2O7Method for preparing powder |
| CN108075123B (en) * | 2017-12-14 | 2020-07-28 | 陕西科技大学 | Method for preparing flower-shaped Cu by solvothermal method2V2O7Method of preparing-CuO nanocomposite |
| CN108134058B (en) * | 2017-12-14 | 2020-08-04 | 陕西科技大学 | Cu5V2O10Preparation method of-CuO composite powder |
| CN108117098B (en) * | 2017-12-14 | 2020-02-21 | 陕西科技大学 | Coralliform α -Cu2V2O7Method for preparing powder |
| CN110120520B (en) * | 2019-03-08 | 2020-09-22 | 北京化工大学 | Self-supporting flower-shaped Co of conductive carrier3V2O8Lithium ion battery cathode material and preparation |
| CN113371758B (en) * | 2021-07-01 | 2023-02-17 | 陕西理工大学 | Short rod self-assembly coralliform Cu 11 O 2 (VO 4 ) 6 Preparation method of flower ball |
| CN115064680B (en) * | 2022-06-29 | 2024-04-30 | 上海空间电源研究所 | Cu for thermal battery2V2O7Composite positive electrode material of nano cage-shaped conductive substrate and preparation method thereof |
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| JPS58172868A (en) * | 1982-04-05 | 1983-10-11 | Nippon Telegr & Teleph Corp <Ntt> | Lithium battery |
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| CN105576206A (en) * | 2016-01-07 | 2016-05-11 | 陕西科技大学 | Preparation method of Cu<2>V<2>O<7>-graphene composite material for negative electrode of lithium-ion battery |
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