CN105140509B - Porous C oV2O6Nanometer sheet electrode material and its preparation method and application - Google Patents
Porous C oV2O6Nanometer sheet electrode material and its preparation method and application Download PDFInfo
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- CN105140509B CN105140509B CN201510565973.4A CN201510565973A CN105140509B CN 105140509 B CN105140509 B CN 105140509B CN 201510565973 A CN201510565973 A CN 201510565973A CN 105140509 B CN105140509 B CN 105140509B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention relates to porous C oV2O6Nanometer sheet electrode material and preparation method thereof, the nanometer sheet pattern is homogeneous, and size is 4 10 μm, and surface has obvious loose structure, and pore size is 10 50nm, and it is following preparation method products therefrom, is comprised the following steps:1) acetylene black is added to the water stirring it is subsequently adding cobalt acetate and stir together, acetylene black is completely immersed in water;2) ammonium metavanadate is added to deionized water, resulting solution is added dropwise to step 1 by water-bath dissolving) stir in resulting solution and at normal temperatures, obtain presoma;3) gained presoma is dried under water bath condition, is calcined under air conditionses after grinding, obtained final product.When the present invention is as lithium ion battery anode active material, high power capacity is shown, with extraordinary cyclical stability;Process is simple, feasibility is very strong, it is easy to amplificationization, the characteristics of meet Green Chemistry.
Description
Technical field
The invention belongs to nanometer material and electrochemical technology field, and in particular to porous C oV2O6Nanometer sheet electrode material and
Its preparation method and application the material can be used as lithium ion battery anode active material.
Background technology
Nowadays, with the fast development in the fields such as pure electric automobile, hybrid vehicle, extensive energy storage device,
Lithium ion battery has been widely used in the neck such as mobile phone, computer, electric automobile now as a kind of green energy resource memory device
Domain, thus research novel nano structure come obtain capacity higher, have a safety feature, lithium ion battery with low cost into
Forward position and focus for current research lithium ion battery.The capacity of the carbon-based negative material graphite of tradition is relatively low, and (theoretical capacity is
372mA h g-1).Cobalt/cobalt oxide because with capacity advantage high (>600mA h g-1) and be widely studied, and cobalt/cobalt oxide is just
It is wherein one of research object of hottest point.But cobalt/cobalt oxide electronic conductivity is not high, and its volume in charge and discharge process
Can expand many causes the destruction result to make the poor application for limiting it of cycle performance.
Research shows that loose structure has a series of excellent specific properties and obtained more and more in electrochemistry and energy field
Concern, the contact area that porous nanometer material can increase active material and electrolyte can thus increase the appearance of electrode material
Amount, while loose structure can provide space to prevent structure from destroying for expansion, while ion diffusion road can effectively be shortened
Footpath, improves the ionic conductivity of material.
The content of the invention
The technical problems to be solved by the invention are directed to above-mentioned prior art and propose a kind of process is simple, and feasibility is strong
Porous C o V2O6Nanometer sheet electrode material and preparation method thereof, can be used as lithium ion battery anode active material.
The present invention solves the technical scheme that is used of above-mentioned technical problem:Porous C oV2O6Nanometer sheet electrode material, it is described
Nanometer sheet pattern is homogeneous, and size is 4-10 μm, and surface has obvious loose structure, and pore size is 10-50nm, and it is following
Preparation method products therefrom, comprises the following steps:
1) acetylene black is added to the water stirring it is subsequently adding cobalt acetate and stir together, acetylene black is completely immersed in water
In;
2) ammonium metavanadate being added to deionized water, resulting solution is added dropwise to step 1 by water-bath dissolving) gained is molten
Stir in liquid and at normal temperatures, obtain presoma;
3) gained presoma is dried under water bath condition, is calcined under air conditionses after grinding, obtained final product porous
CoV2O6Nanometer sheet electrode material.
By such scheme, step 1) described in acetylene black consumption be 0.01-0.2g, cobalt acetate consumption be 0.1-2g.
By such scheme, step 2) described in ammonium metavanadate consumption be 0.1-2g.
By such scheme, step 3) drying temperature be 60-90 DEG C.
By such scheme, step 3) described in calcining heat be 300-700 DEG C, the time is 3-20h.
Described porous C oV2O6The preparation method of nanometer sheet electrode material, comprises the following steps:
1) acetylene black is added to the water stirring it is subsequently adding cobalt acetate and stir together, acetylene black is completely immersed in water
In;
2) ammonium metavanadate being added to deionized water, resulting solution is added dropwise to step 1 by water-bath dissolving) gained is molten
Stir in liquid and at normal temperatures, obtain presoma;
3) gained presoma is dried under water bath condition, is calcined under air conditionses after grinding, obtained final product porous
CoV2O6Nanometer sheet electrode material.
Described porous C oV2O6As the application of lithium ion battery anode active material.
Porous C oV prepared by the present invention2O6Nanometer sheet specific surface area is big, and its porous structure can increase solution with electrolysis
The contact area of matter, increases the capacity of electrode material, while loose structure can be expansion to improve space to prevent the broken of structure
It is bad, while ion diffusion path can also effectively be shortened, the ionic conductivity of material is improved, finally realize porous C oV2O6Receive
Rice plate electrode material in high power, the application of long-life electrode Material Field, so as to become the latent of lithium ion battery negative
In application material.Porous C oV2O6The drying with water bath combination solid sintering technology that nanometer sheet material is used is simple and easy to apply, by control
Sintering temperature can obtain porous pattern, and obtained material yield is high, pattern is homogeneous.
The present invention mainly prepares porous C oV by drying with water bath method combination solid sintering technology2O6Nanometer sheet material, its
During as lithium ion battery anode active material, show high power capacity, with extraordinary cyclical stability;Prepared by the present invention
Porous C oV2O6Its chemical property of nanometer sheet is 500mAh g in current density-1, its second circle capacity is 699mAh g-1, warp
Capacity still has 623mAh g after crossing 500 cycle charge-discharges-1, capability retention is up to 90%, and loose structure makes CoV2O6Receive
Rice piece has the potential application material that excellent cyclical stability is extended-life lithium ion battery;Present invention process is simple, feasible
Property it is very strong, it is easy to amplificationization, the characteristics of meet Green Chemistry, promoted beneficial to the marketization.
Brief description of the drawings
Fig. 1 is the porous C oV of the embodiment of the present invention 12O6The XRD of nanometer sheet material;
Fig. 2 is the porous C oV of the embodiment of the present invention 12O6The SEM figures of nanometer sheet material;
Fig. 3 is the porous C oV of the embodiment of the present invention 12O6The TEM figures of nanometer sheet material;
Fig. 4 is the porous C oV of the embodiment of the present invention 12O6Cycle performance of battery of the nanometer sheet material under low current density
Figure;
Fig. 5 is the porous C oV of the embodiment of the present invention 12O6Nanometer sheet material cycle performance of battery figure at higher current densities.
Specific embodiment
Technical scheme is further explained with reference to embodiment, but not as the limit to the scope of the present invention
System.
Embodiment 1
Mesoporous CoV2O6The preparation method of nanometer sheet, it comprises the following steps:
1) stirring in 0.08g acetylene blacks addition 20ml water is subsequently adding 0.9963g cobalt acetates first and stirs 2h together, made
Acetylene black can be completely immersed in water;
2) 0.9385g ammonium metavanadates are added in 20mL deionized waters, 85 DEG C of water-bath dissolvings dropwise add resulting solution
Enter step 1) in resulting solution, and stir 5h together at normal temperatures, obtain presoma;
3) gained presoma is dried under 85 DEG C of water bath conditions, after grinding under air conditionses 450 DEG C calcining 10h
Exactly finally give yellow porous C oV2O6Nanometer sheet electrode anode material.
With the present embodiment product porous C oV2O6As a example by nanometer sheet material, its structure is determined by X-ray diffractometer.The institute of accompanying drawing 1
Show that X ray diffracting spectrum (XRD) shows, porous C oV2O6It is the CoV of 01-077-1174 with card number2O6Standard sample is kissed substantially
Close, sample is monocline, and space group is C2.
SEM image shown in accompanying drawing 2 and TEM image shown in accompanying drawing 3 show the CoV prepared by us2O6It is porous nano-sheet knot
Structure, nanometer sheet pattern is homogeneous, and size is 4-10 μm, and pore size is 10-50nm.
The present embodiment gained porous C oV2O6Nanometer sheet material is as follows as the application of lithium ion battery anode active material:
The preparation process of negative plate uses porous C oV2O6, used as active material, acetylene black is used as conductive agent, 1.5wt% marine algas for nanometer sheet
Used as binding agent, active material, acetylene black, the mass ratio of sodium alginate are 70 to acid sodium aqueous solution:20:10;By active material with
After acetylene black is sufficiently mixed in proportion, the sodium alginate aqueous solution of respective amount is added, grinding is uniform, and gained mixed solution is applied to
On the Copper Foil of about 10 μ m-thicks.Taken out after electrode slice after coating to be placed in 80 DEG C of oven drying 24h, be made into a diameter of 14
μm electrode slice it is standby.With the LiPF of 1M6It is dissolved in vinyl carbonate (EC) and dimethyl carbonate (DMC) as electrolyte,
Lithium piece is negative pole, and Celgard2325 is barrier film, and CR2016 types stainless steel is assembled into fastening lithium ionic cell for battery case.Lithium
Remaining step of the preparation method of ion battery is identical with common preparation method.
Shown in accompanying drawing 3, transmission electron microscope (TEM) and SEAD (SAED) test show that the nano wire has monocrystalline
Structure.Accompanying drawing 4 is porous C oV2O6Nanometer sheet material is 500mAh g in current density-1Its second circle capacity is 699mAh g-1
Still there are 623mAh g by capacity after 500 cycle charge-discharges-1, capability retention is up to 90% and illustrates excellent electrochemistry
Performance.Accompanying drawing 5 is porous C oV2O6Nanometer sheet material is 5000mAh g in current density-1High current density under, material just
Beginning discharge capacity is 910mAh/g, and the second circle capacity is 440mAh g-1The discharge capacity after 1000 times is circulated still up to 441mAh/
g.Even if under the high current density of 10A/g, specific capacity of the material after circulating 200 times is still 307mAh/g.Above-mentioned performance table
It is bright, porous C oV2O6Nanometer sheet material has very excellent chemical property, is a kind of potential lithium ion battery negative material
Material.
Embodiment 2
1) stirring in 0.15g acetylene blacks addition 20ml water is subsequently adding 0.9963g cobalt acetates first and stirs 2h together, made
Acetylene black can be completely immersed in water;
2) 0.9385g ammonium metavanadates are added in 20mL deionized waters, 85 DEG C of water-bath dissolvings dropwise add resulting solution
Enter step 1) in resulting solution, and stir 5h together at normal temperatures, obtain presoma;
3) gained presoma is dried under 85 DEG C of water bath conditions, after grinding under air conditionses 450 DEG C calcining 10h
Exactly finally give yellow porous C oV2O6Nanometer sheet electrode anode material.
With the porous C oV obtained by the present embodiment2O6As a example by nanometer sheet material, under the current density of 5A/g, material it is initial
Discharge capacity is 690mAh/g, circulates the discharge capacity after 500 times still up to 399mAh/g, and capability retention is 57.8%.
Embodiment 3
1) stirring in 0.08g acetylene blacks addition 20ml water is subsequently adding 2g cobalt acetates first and stirs 2h together, make acetylene
It is black to be completely immersed in water;
2) 2g ammonium metavanadates are added in 20mL deionized waters, resulting solution is added dropwise over step by 85 DEG C of water-bath dissolvings
In rapid 1) resulting solution, and stir 5h together at normal temperatures, obtain presoma;
3) gained presoma is dried under 85 DEG C of water bath conditions, after grinding under air conditionses 450 DEG C calcining 10h
Exactly finally give yellow porous C oV2O6Nanometer sheet electrode anode material.
With the porous C oV obtained by the present embodiment2O6As a example by nanometer sheet material, under the current density of 5A/g, material it is initial
Discharge capacity is 589mAh/g, circulates the discharge capacity after 500 times still up to 302mAh/g, and capability retention is 51.2%.
Embodiment 4
1) stirring in 0.08g acetylene blacks addition 20ml water is subsequently adding 0.9963g cobalt acetates first and stirs 2h together, made
Acetylene black can be completely immersed in water;
2) 0.9385g ammonium metavanadates are added in 20mL deionized waters, 85 DEG C of water-bath dissolvings dropwise add resulting solution
Enter step 1) in resulting solution, and stir 5h together at normal temperatures, obtain presoma;
3) gained presoma is dried under 85 DEG C of water bath conditions, after grinding under air conditionses 600 DEG C calcining 10h
Exactly finally give yellow porous C oV2O6Nanometer sheet electrode anode material.
With the porous C oV obtained by the present embodiment2O6As a example by nanometer sheet material, under the current density of 5A/g, material it is initial
Discharge capacity is 489mAh/g, circulates the discharge capacity after 500 times still up to 340mAh/g, and capability retention is 69.5%.
Embodiment 5
1) stirring in 0.08g acetylene blacks addition 20ml water is subsequently adding 0.9963g cobalt acetates first and stirs 2h together, made
Acetylene black can be completely immersed in water;
2) 0.9385g ammonium metavanadates are added in 20mL deionized waters, 85 DEG C of water-bath dissolvings dropwise add resulting solution
Enter step 1) in resulting solution, and stir 5h together at normal temperatures, obtain presoma;
3) gained presoma is dried under 85 DEG C of water bath conditions, after grinding under air conditionses 450 DEG C calcining 3h
Exactly finally give yellow porous C oV2O6Nanometer sheet electrode anode material.
With the porous C oV obtained by the present embodiment2O6As a example by nanometer sheet material, under the current density of 5A/g, material it is initial
Discharge capacity is 489mAh/g, circulates the discharge capacity after 900 times still up to 320mAh/g, and capability retention is 65.4%.
Claims (11)
1. porous C oV2O6Nanometer sheet electrode material, the nanometer sheet pattern is homogeneous, and size is 4-10 μm, and surface has obvious
Loose structure, pore size is 10-50nm, and it is following preparation method products therefrom, is comprised the following steps:
1) acetylene black is added to the water stirring it is subsequently adding cobalt acetate and stir together, acetylene black is completely immersed in water;
2) ammonium metavanadate is added to deionized water, resulting solution is added dropwise to step 1 by water-bath dissolving) in resulting solution
And stir at normal temperatures, obtain presoma;
3) gained presoma is dried under water bath condition, is calcined under air conditionses after grinding, obtained final product porous C oV2O6Receive
Rice plate electrode material.
2. porous C oV as claimed in claim 12O6Nanometer sheet electrode material, it is characterised in that step 1) described in acetylene black
Consumption be 0.01-0.2g, cobalt acetate consumption be 0.1-2g.
3. porous C oV as claimed in claim 12O6Nanometer sheet electrode material, it is characterised in that step 2) described in metavanadic acid
Ammonium consumption is 0.1-2g.
4. porous C oV as claimed in claim 12O6Nanometer sheet electrode material, it is characterised in that step 3) drying temperature be 60-
90℃。
5. porous C oV as claimed in claim 12O6Nanometer sheet electrode material, it is characterised in that step 3) described in calcining temperature
It is 300-700 DEG C to spend, and the time is 3-20h.
6. the porous C oV described in claim 12O6The preparation method of nanometer sheet electrode material, comprises the following steps:
1) acetylene black is added to the water stirring it is subsequently adding cobalt acetate and stir together, acetylene black is completely immersed in water;
2) ammonium metavanadate is added to deionized water, resulting solution is added dropwise to step 1 by water-bath dissolving) in resulting solution
And stir at normal temperatures, obtain presoma;
3) gained presoma is dried under water bath condition, is calcined under air conditionses after grinding, obtained final product porous C oV2O6Receive
Rice plate electrode material.
7. porous C oV as claimed in claim 62O6The preparation method of nanometer sheet electrode material, it is characterised in that step 1) institute
The consumption of the acetylene black stated is 0.01-0.2g, and cobalt acetate consumption is 0.1-2g.
8. porous C oV as claimed in claim 62O6The preparation method of nanometer sheet electrode material, it is characterised in that step 2) institute
The ammonium metavanadate consumption stated is 0.1-2g.
9. porous C oV as claimed in claim 62O6The preparation method of nanometer sheet electrode material, it is characterised in that step 3) dry
Dry temperature is 60-90 DEG C.
10. porous C oV as claimed in claim 62O6The preparation method of nanometer sheet electrode material, it is characterised in that step 3) institute
The calcining heat stated is 300-700 DEG C, and the time is 3-20h.
Porous C oV described in 11. claims 12O6Nanometer sheet electrode material should as lithium ion battery anode active material
With.
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CN108117103B (en) * | 2017-12-25 | 2022-06-21 | 青岛科技大学 | Cobalt vanadate compound and preparation method and application thereof |
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Facile Synthesis of Cobalt Vanadium Oxides and Their Applications in Lithium Batteries;Yan Tang等;《Int. J. Electrochem. Sci》;20130101;第8卷;第1138-1145页 * |
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