CN109449394A - A kind of flower-shaped (NH4)2V3O8/ foam copper composite material and preparation method and application - Google Patents
A kind of flower-shaped (NH4)2V3O8/ foam copper composite material and preparation method and application Download PDFInfo
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- CN109449394A CN109449394A CN201811223043.0A CN201811223043A CN109449394A CN 109449394 A CN109449394 A CN 109449394A CN 201811223043 A CN201811223043 A CN 201811223043A CN 109449394 A CN109449394 A CN 109449394A
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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
- H01M4/362—Composites
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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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- 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
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- H—ELECTRICITY
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- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/626—Metals
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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
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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 invention discloses a kind of flower-shaped (NH4)2V3O8/ foam copper composite material and preparation method and application belong to nano material and electrochemical technology field.The following steps are included: 1) under agitation, ammonium metavanadate is dissolved in hot water, obtain colourless to light yellow transparent solution, i.e. ammonium metavanadate aqueous solution；2) clean foam copper is vertically put into ammonium metavanadate aqueous solution, and adjusted after pH value is 7~11, be placed in progress oil bath reaction in oil bath pan, take out be cooled to room temperature after reaction；3) by after the product cleaning of step 2), calcination processing, calcining terminates to be cooled to room temperature, and after products therefrom cleaning, drying, flower-shaped (NH is made4)2V3O8/ foam carbon/carbon-copper composite material.This method is easy to operate, is not necessarily to complex device, and process is environmentally protective；Through flower-shaped (NH made from this method4)2V3O8/ foam carbon/carbon-copper composite material has excellent chemical property, can be used as the negative electrode material of lithium ion and sodium-ion battery.
Description
Technical field
The invention belongs to nano material and electrochemical technology fields, are related to a kind of flower-shaped (NH4)2V3O8/ foam composite copper material
Material and its preparation method and application.
Background technique
As at present most prospect and obtain large-scale commercial application secondary cell, lithium ion battery with its work electricity
Pressure is high, and light weight small in size, specific energy is high, safety is good and memory-less effect and advantages of environment protection, in portable electronic
Equipment, electric car, the fields such as large-scale interactive mode energy storage device, have been widely used.
But currently used graphite cathode can no longer meet growing high capacity needs, negative in lithium ion battery
In the material of pole, transition metal oxide first circle irreversible capacity is big, and coulombic efficiency is low, and tinbase and silica-base material are in cyclic process
Serious volume expansion [[Scrosati B, Hassoun J, Sum Y K.Lithium-ion batteries.A can occur
Look into the future [J] .Energy&Environmental Science, 2011,4 (9): 3287-3295.]],
Cyclical stability is poor.Ammonium vanadate is as negative electrode material, the insertion reaction and transition metal oxide of the comprehensive graphite cathode of mechanism
Conversion reaction, have very big theoretical capacity.But ammonium vanadate electric conductivity is poor, and current negative electrode of lithium ion battery is being made
When standby, need to be added the materials such as binder and conductive agent.
Summary of the invention
In order to overcome the disadvantages of the above prior art, the purpose of the present invention is to provide a kind of flower-shaped (NH4)2V3O8/ foam
Carbon/carbon-copper composite material and its preparation method and application, this method is easy to operate, is not necessarily to complex device, and process is environmentally protective；Through the party
(NH flower-shaped made from method4)2V3O8/ foam carbon/carbon-copper composite material have excellent chemical property, can be used as lithium ion and sodium from
The negative electrode material of sub- battery.
In order to achieve the above object, the present invention is achieved by the following scheme:
The invention discloses a kind of flower-shaped (NH4)2V3O8The preparation method of/foam carbon/carbon-copper composite material, comprising the following steps:
1) under agitation, ammonium metavanadate is dissolved in hot water, is obtained colourless to light yellow transparent solution, i.e. metavanadic acid
Aqueous ammonium；
2) clean foam copper is vertically put into ammonium metavanadate aqueous solution, and adjusted after pH value is 7~11, be placed in oil bath
Oil bath reaction is carried out in pot, takes out be cooled to room temperature after reaction；
3) after cleaning the product deionized water and ethyl alcohol of step 2) repeatedly, calcination processing, calcining terminates to be cooled to
Flower-shaped (NH is made after products therefrom cleaning, drying in room temperature4)2V3O8/ foam carbon/carbon-copper composite material.
Preferably, in step 1), hot water temperature is 50~100 DEG C；The concentration of ammonium metavanadate aqueous solution be 0.01~
0.1mol/L。
Preferably, in step 1), stirring uses magnetic agitation, and the time is 10~60min.
Preferably, in step 2), oil bath reaction temperature is 50~100 DEG C, and the oil bath reaction time is 1~10h.
Preferably, in step 2), concentration is used to adjust pH value for the ammonium hydroxide of 2~4mol/L.
Preferably, in step 2), foam copper with a thickness of 0.1~3mm.
Preferably, in step 3), calcination temperature is 150~300 DEG C, and calcination time is 0.5~5h.
Preferably, in step 3), cleaning is successively to use products therefrom ethyl alcohol and deionized water repeated flushing to no powder
It falls off.
The invention also discloses using flower-shaped (NH made from above-mentioned preparation method4)2V3O8/ foam carbon/carbon-copper composite material.
The invention also discloses use above-mentioned flower-shaped (NH4)2V3O8/ foam carbon/carbon-copper composite material as lithium ion battery or
The application of anode material of lithium-ion battery.
Compared with prior art, the invention has the following advantages:
Of the invention prepares flower-shaped (NH4)2V3O8The method of/foam carbon/carbon-copper composite material has following outstanding feature:
(1) composite material prepared by the present invention can be directly used as battery cathode, save traditional coating, roll, at the pole pieces such as dry
Reason process；(2) in the present invention, foam copper serves not only as the transmission path of supporter and electronics, improves the electric conductivity of material, in turn
Its chemical property is promoted, also promotes (NH using its catalytic4)2V3O8Nucleating growth (3) by low temperature calcination, enhancing flower
Shape (NH4)2V3O8With the associativity of foam copper, the cyclical stability of electrode material is improved.(4) simple process, be easy to control and grasp
Make, safety and stability is good, Yi Shixian industrial-scale production.
Further, the present invention passes through control reaction condition, obtained (NH4)2V3O8/ foam carbon/carbon-copper composite material, has
Good chemical property and processing performance have potential application prospect.
Detailed description of the invention
Fig. 1 is that the embodiment of the present invention 6 prepares (NH4)2V3O8The XRD diagram of/foam carbon/carbon-copper composite material；
Fig. 2 is that the embodiment of the present invention 6 prepares (NH4)2V3O8The SEM of/foam carbon/carbon-copper composite material schemes；
Fig. 3 is that the embodiment of the present invention 6 prepares (NH4)2V3O8/ foam carbon/carbon-copper composite material is used as negative electrode of lithium ion battery
When cycle performance figure.
Specific embodiment
In order to enable those skilled in the art to better understand the solution of the present invention, below in conjunction in the embodiment of the present invention
Attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is only
The embodiment of a part of the invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill people
The model that the present invention protects all should belong in member's every other embodiment obtained without making creative work
It encloses.
In addition, term " includes " and " having " and their any deformation, it is intended that covering non-exclusive includes example
Such as, the process, method, system, product or equipment for containing a series of steps or units those of are not necessarily limited to be clearly listed
Step or unit, but may include being not clearly listed or intrinsic for these process, methods, product or equipment other
Step or unit.
The invention will be described in further detail below:
A kind of flower-shaped (NH4)2V3O8/ foam method of manufacturing carbon/carbon-copper composite material, comprising the following steps:
1) in magnetic agitation 10-60min, ammonium metavanadate is dissolved in 100 DEG C of hot water, obtaining concentration is 0.01-0.1mol/
The colourless of L arrives light yellow transparent solution, is denoted as solution A；
2) foam copper with a thickness of 0.1-3mm cleaned up is vertically put into solution A, is 1-4mol/L's with concentration
Ammonium hydroxide adjusts pH value to be placed in 50-100 DEG C of oil bath pan after 7-11, and 1-10h is reacted in oil bath, takes out cooling after reaction
To room temperature；
3) it after being cleaned the product of step 2) deionized water and ethyl alcohol repeatedly, is carried out at calcining in Muffle furnace
Reason, calcination temperature are 150-300 DEG C, time 0.5-5h.Calcining terminates to be cooled to room temperature, by gained foam copper sheet ethyl alcohol and
Deionized water repeated flushing to no powder falls off, and flower-shaped (NH can be obtained after dry4)2V3O8/ foam carbon/carbon-copper composite material.
Below with reference to embodiment, the invention will be described in further detail:
Embodiment 1
1) in magnetic agitation 10min, ammonium metavanadate is dissolved in 100 DEG C of hot water, obtaining concentration is the colourless of 0.01mol/L
To light yellow transparent solution, it is denoted as solution A；
2) foam copper with a thickness of 0.1mm cleaned up is vertically put into solution A, the ammonium hydroxide for being 4mol/L with concentration
It after adjusting pH value is 11, is placed in 50 DEG C of oil bath pan, 10h is reacted in oil bath, takes out be cooled to room temperature after reaction；
3) it after being cleaned the product of step 2) deionized water and ethyl alcohol repeatedly, is carried out at calcining in Muffle furnace
Reason, calcination temperature are 150 DEG C, time 5h.Calcining terminates to be cooled to room temperature, by gained foam copper sheet ethyl alcohol and deionized water
Repeated flushing to no powder falls off, and flower-shaped (NH can be obtained after dry4)2V3O8/ foam carbon/carbon-copper composite material.
Embodiment 2
1) in magnetic agitation 20min, ammonium metavanadate is dissolved in 80 DEG C of hot water, obtaining concentration is the colourless of 0.02mol/L
To light yellow transparent solution, it is denoted as solution A；
2) foam copper with a thickness of 0.3mm cleaned up is vertically put into solution A, the ammonium hydroxide for being 3mol/L with concentration
It after adjusting pH value is 10, is placed in 60 DEG C of oil bath pan, 5h is reacted in oil bath, takes out be cooled to room temperature after reaction；
3) it after being cleaned the product of step 2) deionized water and ethyl alcohol repeatedly, is carried out at calcining in Muffle furnace
Reason, calcination temperature are 200 DEG C, time 3h.Calcining terminates to be cooled to room temperature, by gained foam copper sheet ethyl alcohol and deionized water
Repeated flushing to no powder falls off, and flower-shaped (NH can be obtained after dry4)2V3O8/ foam carbon/carbon-copper composite material.
Embodiment 3
1) in magnetic agitation 40min, ammonium metavanadate is dissolved in 60 DEG C of hot water, obtaining concentration is the colourless of 0.05mol/L
To light yellow transparent solution, it is denoted as solution A；
2) foam copper with a thickness of 1mm cleaned up is vertically put into solution A, the ammonium hydroxide tune for being 2mol/L with concentration
It after section pH value is 9, is placed in 80 DEG C of oil bath pan, 3h is reacted in oil bath, takes out be cooled to room temperature after reaction；
3) it after being cleaned the product of step 2) deionized water and ethyl alcohol repeatedly, is carried out at calcining in Muffle furnace
Reason, calcination temperature are 250 DEG C, time 1h.Calcining terminates to be cooled to room temperature, by gained foam copper sheet ethyl alcohol and deionized water
Repeated flushing to no powder falls off, and flower-shaped (NH can be obtained after dry4)2V3O8/ foam carbon/carbon-copper composite material.
Embodiment 4
1) in magnetic agitation 60min, ammonium metavanadate is dissolved in 50-100 DEG C of hot water, obtains the nothing that concentration is 0.1mol/L
Color is denoted as solution A to light yellow transparent solution；
2) foam copper with a thickness of 3mm cleaned up is vertically put into solution A, the ammonium hydroxide tune for being 1mol/L with concentration
It after section pH value is 8, is placed in 100 DEG C of oil bath pan, 1h is reacted in oil bath, takes out be cooled to room temperature after reaction；
3) it after being cleaned the product of step 2) deionized water and ethyl alcohol repeatedly, is carried out at calcining in Muffle furnace
Reason, calcination temperature are 300 DEG C, time 0.5h.Calcining terminates to be cooled to room temperature, by gained foam copper sheet ethyl alcohol and deionization
Water repeated flushing to no powder falls off, and flower-shaped (NH can be obtained after dry4)2V3O8/ foam carbon/carbon-copper composite material.
Embodiment 5
1) in magnetic agitation 10min, ammonium metavanadate is dissolved in 80 DEG C of hot water, obtaining concentration is the colourless of 0.02mol/L
To light yellow transparent solution, it is denoted as solution A；
2) foam copper with a thickness of 2mm cleaned up is vertically put into solution A, the ammonium hydroxide tune for being 1mol/L with concentration
It after section pH value is 7, is placed in 80 DEG C of oil bath pan, 5h is reacted in oil bath, takes out be cooled to room temperature after reaction；
3) it after being cleaned the product of step 2) deionized water and ethyl alcohol repeatedly, is carried out at calcining in Muffle furnace
Reason, calcination temperature are 250 DEG C, time 1h.Calcining terminates to be cooled to room temperature, by gained foam copper sheet ethyl alcohol and deionized water
Repeated flushing to no powder falls off, and flower-shaped (NH can be obtained after dry4)2V3O8/ foam carbon/carbon-copper composite material.
Embodiment 6
1) in magnetic agitation 20min, ammonium metavanadate is dissolved in 80 DEG C of hot water, obtaining concentration is the colourless of 0.02mol/L
To light yellow transparent solution, it is denoted as solution A；
2) foam copper with a thickness of 1mm cleaned up is vertically put into solution A, the ammonium hydroxide tune for being 2mol/L with concentration
It after section pH value is 8, is placed in 70 DEG C of oil bath pan, 5h is reacted in oil bath, takes out be cooled to room temperature after reaction；
3) it after being cleaned the product of step 2) deionized water and ethyl alcohol repeatedly, is carried out at calcining in Muffle furnace
Reason, calcination temperature are 250 DEG C, time 1h.Calcining terminates to be cooled to room temperature, by gained foam copper sheet ethyl alcohol and deionized water
Repeated flushing to no powder falls off, and flower-shaped (NH can be obtained after dry4)2V3O8/ foam carbon/carbon-copper composite material.
It can be seen from figure 1 that prepared material meets (NH well4)2V3O8The standard card of/Cu, illustrates (NH4)2V3O8/ Cu is pure phase, no other impurities.As can be seen from Figure 2, (NH4)2V3O8The pattern of/Cu is the flower-like structure that diameter is 1um, should
Structure has biggish specific surface, can increase the contact area with electrolyte, reduces ion diffusion path.As can be seen from Figure 3, exist
100mAg-1When, discharge capacity is 1365mAh g for the first time-1, 1050mAh g is remained at after recycling 45 times-1, flower-shaped (NH4)2V3O8Foam copper shows excellent chemical property.
The above content is merely illustrative of the invention's technical idea, and this does not limit the scope of protection of the present invention, all to press
According to technical idea proposed by the present invention, any changes made on the basis of the technical scheme each falls within claims of the present invention
Protection scope within.
Claims (10)
1. a kind of flower-shaped (NH4)2V3O8The preparation method of/foam carbon/carbon-copper composite material, which comprises the following steps:
1) under agitation, ammonium metavanadate is dissolved in hot water, is obtained colourless to light yellow transparent solution, i.e. ammonium metavanadate water
Solution；
2) clean foam copper is vertically put into ammonium metavanadate aqueous solution, and adjusted after pH value is 7~11, is placed in oil bath pan
Oil bath reaction is carried out, takes out be cooled to room temperature after reaction；
3) by after the product cleaning of step 2), calcination processing, calcining terminates to be cooled to room temperature, and products therefrom is cleaned, is dry
Afterwards, flower-shaped (NH is made4)2V3O8/ foam carbon/carbon-copper composite material.
2. flower-shaped (NH according to claim 14)2V3O8The preparation method of/foam carbon/carbon-copper composite material, which is characterized in that step
It is rapid 1) in, hot water temperature be 50~100 DEG C；The concentration of ammonium metavanadate aqueous solution is 0.01~0.1mol/L.
3. flower-shaped (NH according to claim 14)2V3O8The preparation method of/foam carbon/carbon-copper composite material, which is characterized in that step
It is rapid 1) in, stirring use magnetic agitation, the time be 10~60min.
4. flower-shaped (NH according to claim 14)2V3O8The preparation method of/foam carbon/carbon-copper composite material, which is characterized in that step
It is rapid 2) in, oil bath reaction temperature be 50~100 DEG C, the oil bath reaction time be 1~10h.
5. flower-shaped (NH according to claim 14)2V3O8The preparation method of/foam carbon/carbon-copper composite material, which is characterized in that step
It is rapid 2) in, use concentration for 2~4mol/L ammonium hydroxide adjust pH value.
6. flower-shaped (NH according to claim 14)2V3O8The preparation method of/foam carbon/carbon-copper composite material, which is characterized in that step
It is rapid 2) in, foam copper with a thickness of 0.1~3mm.
7. flower-shaped (NH according to claim 14)2V3O8The preparation method of/foam carbon/carbon-copper composite material, which is characterized in that step
It is rapid 3) in, calcination temperature be 150~300 DEG C, calcination time be 0.5~5h.
8. flower-shaped (NH according to claim 14)2V3O8The preparation method of/foam carbon/carbon-copper composite material, which is characterized in that step
It is rapid 3) in, cleaning is that products therefrom is successively fallen off with ethyl alcohol and deionized water repeated flushing to no powder.
9. using flower-shaped (NH made from preparation method described in any one of claim 1~84)2V3O8/ foam composite copper material
Material.
10. flower-shaped (NH as claimed in claim 94)2V3O8/ foam carbon/carbon-copper composite material is negative as lithium ion battery or sodium-ion battery
The application of pole material.
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Cited By (1)
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|---|---|---|---|---|
| CN113206253A (en) * | 2021-04-29 | 2021-08-03 | 陕西科技大学 | Foam copper potassium ion battery material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113206253A (en) * | 2021-04-29 | 2021-08-03 | 陕西科技大学 | Foam copper potassium ion battery material and preparation method thereof |
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