CN106186062A - 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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Abstract
A kind of homogeneous hydro-thermal method prepares flower-shaped Cu2V2O7The method of material and the Cu of preparation2V2O7Material, is scattered in Red copper oxide in deionized water, adds ammonium metavanadate, obtain reaction precursor liquid after being uniformly dispersed；By front for reaction body liquid at 100～200 DEG C, after hydro-thermal reaction 5～48h, being cooled to room temperature, centrifuge washing precipitates, and precipitation is dried, obtains powder body；Powder body is sintered, obtains flower-shaped Cu2V2O7Material.The present invention uses hard template topology reaction method in situ, especially by by Cu2O and NH4VO3Being mixed with reaction precursor liquid, then use hydro-thermal reaction, finally sintering removes water of crystallization, has prepared lithium ion battery negative Cu2V2O7Material, the method technique is simple, it is not necessary to complex device, can prepare material requested at normal temperatures and pressures, and the response time is short, and product purity is high, and reaction condition is easily controllable, it is possible to realize large-scale industrial production.
Description
Technical field
The invention belongs to the electrode material technical field of battery, relate to a kind of Cu2V2O7Material and preparation method thereof, especially
Relate to a kind of homogeneous hydro-thermal method and prepare 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, use temperature range width, memory-less effect
Etc. advantage, it is widely used in each field.But current business-like lithium ion battery negative material is mainly based on graphite,
But its less theoretical capacity (372mAh/g), and it there is also certain potential safety hazard, and these shortcomings limit answering of its
With.
There is the Cu of layer structure2V2O7Multistep reduction (Cu can be carried out during embedding/deintercalate lithium ions2+/Cu+And
Cu+/Cu0) it is considered to be have lithium ion battery negative material [Cheng F, the Chen of 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 metal: Smelting Part, 2014 (2): 57-60.] etc..High temperature solid-state method synthetic operation is simple, but
Need long-time high-temperature process, and product morphology is uncontrollable.Sol-gel method craft is complicated, severe reaction conditions, it is difficult to real
Now large-scale industrial production, and further part needs also exist for high-temperature process.Both approaches is equal in commercial process
Cost can be made to sharply increase, and high temperature sintering also can produce impact to the chemical property of product simultaneously.
Summary of the invention
It is an object of the invention to provide a kind of homogeneous hydro-thermal method and prepare flower-shaped Cu2V2O7The method of material, the method uses
Hydrothermal reaction at low temperature, by topology growing technology in situ, prepares the flower-shaped Cu with good chemical property2V2O7Material, should
Method is simple to operate, and repeatability is high, and production cost is low, is suitable for industrialized production.
In order to achieve the above object, the technical solution used in 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) Red copper oxide is scattered in deionized water, adds ammonium metavanadate powder body after being uniformly dispersed, stir, obtain
Reaction precursor liquid；Wherein, Red copper oxide and ammonium metavanadate are than for 0.125g:0.102g；
2) by front for reaction body liquid at 100～200 DEG C, hydro-thermal reaction 5～48h, after question response terminates, it is cooled to room temperature,
It is then centrifuged for washing precipitation, precipitation is dried, obtains powder body；
3) being sintered by powder body, slough water of crystallization, gained powder body is flower-shaped Cu2V2O7Material.
The present invention is further improved by, described step 1) in ammonium metavanadate be analytical pure.
The present invention is further improved by, described step 1) in the ratio of Red copper oxide and deionized water be 0.125g:
80mL。
The present invention is further improved by, described step 1) in be uniformly dispersed employing use magnetic agitation, stirring
Time is 0.5～5h.
The present invention is further improved by, described step 1) in mixing time be 1～5h.
The present invention is further improved by, described step 2) in hydro-thermal reaction time water heating kettle packing ratio be 30%
～70%.
The present invention is further improved by, described step 2) in the rotating speed of centrifuge washing be 8000 turns/min.
The present invention is further improved by, described step 2) in be dried temperature be 50～100 DEG C, be dried time
Between be 2～12h.
The present invention is further improved by, 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, this Cu2V2O7Material presents the diameter being made up of the nanometer sheet that thickness is 80～100nm
It it is the floriform appearance of 1.0～1.2um.
Compared with prior art, the present invention has following useful technique effect: the present invention uses hard template-original position topology
Reaction method, especially by by Cu2O and NH4VO3It is mixed with reaction precursor liquid, then uses hydro-thermal reaction, finally sinter removing
Water of crystallization, has prepared lithium ion battery negative Cu2V2O7Material, the present invention prepares flower-shaped Cu2V2O7Do not use during material
Any surfactant.Due to the fact that employing hydro-thermal reaction, it is possible to reduce the temperature of reaction, the response time 5～48h,
It is that the high temperature solid-state method response time is short relative to this material, and the method technique is simple, it is not necessary to complex device, can be normal at room temperature
Material requested is prepared in pressure, and the response time is short, and product purity is high, and reaction condition is easily controllable, it is possible to realize large-scale industry
Metaplasia is produced.Cu prepared by the present invention2V2O7Material present a diameter of 1.0 be made up of the nanometer sheet that thickness is 80～100nm～
The floriform appearance of 1.2um, this Cu2V2O7Material has good chemical property, and the copper vanadate material prepared due to the present invention is
Nanometer grade powder, floriform appearance makes this material have bigger specific surface area, contributes to shortening lithium ion in charge and discharge process
The evolving path, improves its high rate performance and cycle performance.Can also effectively increase the contact area of itself and electrolyte simultaneously, from
And there is the chemical property of excellence.
Accompanying drawing explanation
Fig. 1 is Cu prepared by the present invention2V2O7The X-ray diffractogram of material；
Fig. 2 is Cu prepared by the present invention2V2O7The scanning electron microscope shape appearance figure of material；Wherein (a) is 50.0K；B () is 100K；
Fig. 3 is Cu prepared by the present invention2V2O7The cycle performance figure of electrode material.
Detailed description of the invention
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
1) freshly prepd 0.125g 20 hexahedron Red copper oxide (Cu is weighed2O) being scattered in 80mL deionization, magnetic force stirs
Mix 0.5h, be subsequently adding 0.102g ammonium metavanadate (NH4VO3) powder body, stir 2h, obtain reaction precursor liquid；
2) being transferred in reactor by body liquid before reaction, the packing ratio of reactor is 40%, then at 180 DEG C, and hydro-thermal
Reaction 12h, after question response terminates, is cooled to room temperature, is then centrifuged for washing precipitation, will be deposited at 60 DEG C and be dried 10h, and obtain powder
Body；
3) by dried powder body, it is sintered at 300 DEG C, sloughs water of crystallization, and be incubated 0.5h；Cold with stove afterwards
But, gained powder body is the flower-shaped Cu of lithium ion battery negative2V2O7Material.
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.
From Fig. 2 (a) and Fig. 2 (b) it can be seen that prepared copper vanadate is by flower-like structure, thickness it is 80～100nm
Nanometer sheet constitute a diameter of 1.0～1.2um.
Fig. 3 is this copper vanadate material cycle performance figure at 0.1A/g, and 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) being scattered in deionized water by freshly prepared 20 hexahedron Red copper oxides, it is inclined that magnetic agitation 0.2h adds analytical pure
Ammonium vanadate powder body, magnetic agitation 5h, obtain reaction precursor liquid；Wherein, Red copper oxide and ammonium metavanadate and the ratio of deionized water
For 0.125g:0.102g:80mL；
2) being transferred in reactor by body liquid before reaction, the packing ratio of reactor is 70%, then at 100 DEG C, and hydro-thermal
Reaction 48h, after question response terminates, is cooled to room temperature, and then centrifuge washing precipitation under 8000 turns/min, will be deposited at 50 DEG C
It is dried 12h, obtains powder body；
3) at 500 DEG C, powder body being sintered 0.2h, slough water of crystallization, gained powder body is flower-shaped Cu2V2O7Material.
Embodiment 3
1) being scattered in deionized water by freshly prepared 20 hexahedron Red copper oxides, magnetic agitation 2h adds the inclined vanadium of analytical pure
Acid ammonium powder body, magnetic agitation 3h, obtain reaction precursor liquid；Wherein, the ratio of Red copper oxide and ammonium metavanadate and deionized water is
0.125g:0.102g:80mL
2) being transferred in reactor by body liquid before reaction, the packing ratio of reactor is 30%, then at 200 DEG C, and hydro-thermal
Reaction 5h, after question response terminates, is cooled to room temperature, and then centrifuge washing precipitation under 8000 turns/min, will be deposited at 100 DEG C
It is dried 2h, obtains powder body；
3) at 200 DEG C, powder body being sintered 5h, slough water of crystallization, gained powder body is flower-shaped Cu2V2O7Material.
Embodiment 4
1) being scattered in deionized water by freshly prepared 20 hexahedron Red copper oxides, magnetic agitation 5h adds the inclined vanadium of analytical pure
Acid ammonium powder body, magnetic agitation 1h, obtain reaction precursor liquid；Wherein, the ratio of Red copper oxide and ammonium metavanadate and deionized water is
0.125g:0.102g:80mL
2) being transferred in reactor by body liquid before reaction, the packing ratio of reactor is 60%, then at 120 DEG C, and hydro-thermal
Reaction 36h, after question response terminates, is cooled to room temperature, and then centrifuge washing precipitation under 8000 turns/min, will be deposited at 70 DEG C
It is dried 8h, obtains powder body；
3) at 400 DEG C, powder body being sintered 3h, slough water of crystallization, gained powder body is flower-shaped Cu2V2O7Material.
Embodiment 5
1) being scattered in deionized water by freshly prepared 20 hexahedron Red copper oxides, magnetic agitation 1h adds the inclined vanadium of analytical pure
Acid ammonium powder body, magnetic agitation 10h, obtain reaction precursor liquid；Wherein, the ratio of Red copper oxide and ammonium metavanadate and deionized water is
0.125g:0.102g:80mL
2) being transferred in reactor by body liquid before reaction, the packing ratio of reactor is 50%, then at 150 DEG C, and hydro-thermal
Reaction 24h, after question response terminates, is cooled to room temperature, and then centrifuge washing precipitation under 8000 turns/min, will be deposited at 80 DEG C
It is dried 6h, obtains powder body；
3) at 350 DEG C, powder body being sintered 3h, slough water of crystallization, gained powder body is flower-shaped Cu2V2O7Material.
Flower-shaped Cu prepared by the present invention2V2O7Material presents be made up of the nanometer sheet that thickness is 80～100nm a diameter of
The floriform appearance of 1.0～1.2um.
Claims (10)
1. a homogeneous hydro-thermal method prepares flower-shaped Cu2V2O7The method of material, it is characterised in that comprise the following steps:
1) Red copper oxide is scattered in deionized water, adds ammonium metavanadate powder body after being uniformly dispersed, stir, reacted
Precursor liquid；Wherein, Red copper oxide and ammonium metavanadate are than for 0.125g:0.102g；
2) by front for reaction body liquid at 100～200 DEG C, hydro-thermal reaction 5～48h, after question response terminates, it is cooled to room temperature, then
Centrifuge washing precipitates, and precipitation is dried, obtains powder body；
3) being sintered by powder body, slough water of crystallization, gained powder body is flower-shaped Cu2V2O7Material.
Homogeneous hydro-thermal method the most according to claim 1 prepares flower-shaped Cu2V2O7The method of material, it is characterised in that described
Step 1) in ammonium metavanadate be analytical pure.
Homogeneous hydro-thermal method the most according to claim 1 prepares flower-shaped Cu2V2O7The method of material, it is characterised in that described
Step 1) in the ratio of Red copper oxide and deionized water be 0.125g:80mL.
Homogeneous hydro-thermal method the most according to claim 1 prepares flower-shaped Cu2V2O7The method of material, it is characterised in that described
Step 1) in be uniformly dispersed employing use magnetic agitation, the time of stirring is 0.5～5h.
Homogeneous hydro-thermal method the most 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.
Homogeneous hydro-thermal method the most according to claim 1 prepares flower-shaped Cu2V2O7The method of material, it is characterised in that described
Step 2) in hydro-thermal reaction time water heating kettle packing ratio be 30%～70%.
Homogeneous hydro-thermal method the most according to claim 1 prepares flower-shaped Cu2V2O7The method of material, it is characterised in that described
Step 2) in the rotating speed of centrifuge washing be 8000 turns/min.
Homogeneous hydro-thermal method the most according to claim 1 prepares flower-shaped Cu2V2O7The method of material, it is characterised in that described
Step 2) in be dried temperature be 50～100 DEG C, be dried time be 2～12h.
Homogeneous hydro-thermal method the most according to claim 1 prepares flower-shaped Cu2V2O7The method of material, it is characterised in that described
Step 3) in the temperature of calcining be 200 DEG C～500 DEG C, the time of calcining is 0.2h～5h.
10. the Cu that prepared by a method according to claim 12V2O7Material, it is characterised in that this Cu2V2O7Material in
Reveal a diameter of 1.0～the floriform appearance of 1.2um being made up of the nanometer sheet that thickness is 80～100nm.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108075124A (en) * | 2017-12-14 | 2018-05-25 | 陕西科技大学 | A kind of microwave-hydrothermal method prepares Cu2V2O7The method of-CuO nano-complexes |
| CN108075123A (en) * | 2017-12-14 | 2018-05-25 | 陕西科技大学 | A kind of solvent-thermal method prepares flower-shaped Cu2V2O7The method of-CuO nano-complexes |
| CN108101108A (en) * | 2017-12-14 | 2018-06-01 | 陕西科技大学 | A kind of β-Cu2V2O7Raw powder's production technology |
| CN108117098A (en) * | 2017-12-14 | 2018-06-05 | 陕西科技大学 | A kind of coralliform α-Cu2V2O7Raw powder's production technology |
| CN108134058A (en) * | 2017-12-14 | 2018-06-08 | 陕西科技大学 | A kind of Cu5V2O10The preparation method of-CuO composite granules |
| CN110120520A (en) * | 2019-03-08 | 2019-08-13 | 北京化工大学 | Conductive carrier self-supporting flower shape Co3V2O8Lithium ion battery negative material and preparation |
| CN113371758A (en) * | 2021-07-01 | 2021-09-10 | 陕西理工大学 | Short rod self-assembly coralliform Cu11O2(VO4)6Preparation method of flower ball |
| CN115064680A (en) * | 2022-06-29 | 2022-09-16 | 上海空间电源研究所 | Cu for thermal battery 2 V 2 O 7 Nano cage-shaped conductive substrate composite positive electrode material and preparation method thereof |
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Cited By (13)
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|---|---|---|---|---|
| CN108101108B (en) * | 2017-12-14 | 2020-02-21 | 陕西科技大学 | β -Cu2V2O7Method for preparing powder |
| CN108075123A (en) * | 2017-12-14 | 2018-05-25 | 陕西科技大学 | A kind of solvent-thermal method prepares flower-shaped Cu2V2O7The method of-CuO nano-complexes |
| CN108101108A (en) * | 2017-12-14 | 2018-06-01 | 陕西科技大学 | A kind of β-Cu2V2O7Raw powder's production technology |
| CN108117098A (en) * | 2017-12-14 | 2018-06-05 | 陕西科技大学 | A kind of coralliform α-Cu2V2O7Raw powder's production technology |
| CN108134058A (en) * | 2017-12-14 | 2018-06-08 | 陕西科技大学 | A kind of Cu5V2O10The preparation method of-CuO composite granules |
| CN108075124A (en) * | 2017-12-14 | 2018-05-25 | 陕西科技大学 | A kind of microwave-hydrothermal method prepares Cu2V2O7The method of-CuO nano-complexes |
| CN108117098B (en) * | 2017-12-14 | 2020-02-21 | 陕西科技大学 | Coralliform α -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 |
| CN108075124B (en) * | 2017-12-14 | 2020-07-28 | 陕西科技大学 | Microwave hydrothermal method for preparing Cu2V2O7Method of preparing-CuO nanocomposite |
| CN110120520A (en) * | 2019-03-08 | 2019-08-13 | 北京化工大学 | Conductive carrier self-supporting flower shape Co3V2O8Lithium ion battery negative material and preparation |
| CN113371758A (en) * | 2021-07-01 | 2021-09-10 | 陕西理工大学 | Short rod self-assembly coralliform Cu11O2(VO4)6Preparation method of flower ball |
| CN115064680A (en) * | 2022-06-29 | 2022-09-16 | 上海空间电源研究所 | Cu for thermal battery 2 V 2 O 7 Nano cage-shaped conductive substrate composite positive electrode material and preparation method thereof |
| 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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