CN107104235A - Preparation method for the graphene nano carbon/carbon-copper composite material of lithium ion battery negative material - Google Patents
Preparation method for the graphene nano carbon/carbon-copper composite material of lithium ion battery negative material Download PDFInfo
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- CN107104235A CN107104235A CN201710284011.0A CN201710284011A CN107104235A CN 107104235 A CN107104235 A CN 107104235A CN 201710284011 A CN201710284011 A CN 201710284011A CN 107104235 A CN107104235 A CN 107104235A
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- carbon
- lithium ion
- copper
- ion battery
- cellulose
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- 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
- H01M2004/026—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 preparation method of the graphene nano carbon/carbon-copper composite material for lithium ion battery negative material, comprise the following steps：A, prepare glue：Cellulose glue is made by cellulose is soluble in water；It is prepared by B, metal paste：Glue in copper powder and step A is mixed and made into paste；It is prepared by C, composite：Cupric oxide powder is added in step B paste and cuprous oxide powder is well mixed, hybrid particles thing is obtained；D, calcining：Hybrid particles thing made from step C is subjected to reduction calcining, the composite of graphene and nanometer copper ball is obtained.The present invention is exactly to prepare a kind of conductive material of 3 D stereo by the way that nanometer copper ball and graphene are combined, and uses it for aiding in the conductive field of lithium ion battery active material.
Description
Technical field
The present invention relates to a kind of lithium ion battery negative material, more particularly to it is a kind of for lithium ion battery negative material
The preparation method of graphene nano carbon/carbon-copper composite material.
Background technology
Lithium ion battery：It is a kind of secondary cell (rechargeable battery), it relies primarily on lithium ion between a positive electrode and a negative electrode
Movement carrys out work.In charge and discharge process, Li+ comes and goes insertion and deintercalation between two electrodes：During charging, Li+ is de- from positive pole
It is embedding, negative pole is embedded in by electrolyte, negative pole is in rich lithium state；It is then opposite during electric discharge.Battery, which is typically used, contains elemental lithium
Material, as electrode, is the representative of modern high performance battery.
The negative pole of lithium ion battery is by carbon element or non-carbon material, adhesive and additive mixing system
Copper foil both sides are uniformly applied into pasty state adhesive, are formed through drying, rolling.It is made lithium ion battery success, it is crucial
It is to prepare the negative material of reversibly de-/embedding lithium ion.
In general, a kind of good negative material is selected to follow following principle：Specific energy is high；With respect to the electrode of lithium electrode
Current potential is low；Discharge and recharge reaction good reversibility；It is compatible good with electrolyte and binding agent；Specific surface area it is small (<10m2/g), it is very close
Degree height (>2.0g/cm3)；Size and good mechanical stability in process of intercalation；Aboundresources, it is cheap；Stable in the air,
Have no toxic side effect.At present, the negative material typically all carbon materials of lithium ion battery has been actually used in, such as graphite, soft carbon are (such as
Coke etc.), hard carbon etc..
Although existing carbon materials has higher electronic conductivity high in itself, because graphite isoreactivity material is general
It is micron-sized material, therefore needs also exist for adding a certain proportion of conductive agent face is changed into a contact filling space and connect
Touch, the conductive agent being currently mainly used is nano carbon black.But because the electric conductivity of nano carbon black ought even be not so good as stone with graphite-phase
Ink, therefore by as conductive bottleneck in the case of high-power discharge and recharge.And graphene is to generally acknowledge that two-dimentional electric conductivity is best
Material, the electric conductivity of copper also is difficult to lithium ion diffusion coefficient greatly, and layer structure Volume Changes before and after embedding lithium are small, embedding lithium capacity
Height, the low advantage of intercalation potential.But the shortcoming of graphite cathode is：It is poor with compatibility of electrolyte, first charge-discharge reversible capacity
It is low, be not suitable for high current charge-discharge, cycle performance is poor.
Existing lithium alloy negative material, although energy density is high, but cyclical stability is poor.The theory of silicon based anode material
Capacity is high, but Volume Changes are big, cause the efflorescence of alloy, capacity drastically declines.Material structure after the storage lithium of tin base cathode material
There is no significant change, good cycle with volume, but store lithium finite capacity.
In addition, in the prior art using graphene as negative material, graphene is a kind of two-dimensional material, in two dimensional surface
Electric conductivity on it is very outstanding, but Z-direction conduction just have certain shortcoming.
The content of the invention
The technical problem to be solved in the present invention is, for the defect of prior art, there is provided a kind of three dimensional conductive is excellent
Graphene nano copper composite conducting agent material preparation method.
The technical solution adopted for the present invention to solve the technical problems is：
A kind of preparation method of graphene nano carbon/carbon-copper composite material for lithium ion battery negative material, including following step
Suddenly：
A, prepare glue：Cellulose glue is made by cellulose is soluble in water；
It is prepared by B, metal paste：Glue in copper powder and step A is mixed and made into paste；
It is prepared by C, composite：Cupric oxide powder is added in step B paste and cuprous oxide powder is well mixed, is obtained
To hybrid particles thing；
D, calcining：Hybrid particles thing made from step C is subjected to reduction calcining, the compound of graphene and nanometer copper ball is obtained
Material.
In the described preparation method for the graphene nano carbon/carbon-copper composite material of lithium ion battery negative material, preferred institute
State in step A, cellulose is ethyl cellulose or methylcellulose, and the weight ratio of cellulose and water is 1:100-3:100.
In the described preparation method for the graphene nano carbon/carbon-copper composite material of lithium ion battery negative material, preferred institute
State in step A, cellulose is added to the water, high-speed stirred is dispersed in water cellulose, cellulose glue is made.
In the described preparation method for the graphene nano carbon/carbon-copper composite material of lithium ion battery negative material, preferred institute
State in step B, the water atomization copper powder of the mesh of the mesh of copper powder use -150~-400, the weight ratio of the copper powder and glue is 45:
100-85:100。
In the described preparation method for the graphene nano carbon/carbon-copper composite material of lithium ion battery negative material, preferred institute
State in step C, the weight ratio of the cupric oxide powder and paste is 0.05:100-0.1:100, the cuprous oxide powder and paste
The weight ratio of thing is 0.05:100-0.01:100.
In the described preparation method for the graphene nano carbon/carbon-copper composite material of lithium ion battery negative material, preferred institute
State in step D, step C hybrid particles thing is put into hydrogen reducing furnace and calcined, wherein calcining heating rate is 10 DEG C/min,
Dew point of hydrogen is 5 DEG C -15 DEG C, and calcining heat is 1085 DEG C -1150 DEG C, and calcination time is 10-25min.
Beneficial effects of the present invention are：The theoretical resistivity of graphite is 8 × 10-6Ω m, the resistivity of carbon black is then more than 10-5
Ω m, and the theoretical resistivity of copper is 1.67 × 10-8Ω m, the theoretical resistivity of graphene is 1 × 10-8Ωm.The present invention is used
Graphene and nanometer copper ball are combined, form graphene nano carbon/carbon-copper composite material, and material significant increase lithium ion battery is in XYZ
The electric conductivity in three directions.
Brief description of the drawings
Below in conjunction with drawings and Examples, the invention will be further described, in accompanying drawing：
Fig. 1 is the Scanning Electron microphotograph of composite.
Embodiment
In order to which technical characteristic, purpose and effect to the present invention are more clearly understood from, now compare accompanying drawing and describe in detail
The embodiment of the present invention.
A kind of preparation method of graphene nano carbon/carbon-copper composite material for lithium ion battery negative material, including following step
Suddenly：
A, prepare glue：Cellulose glue is made by cellulose is soluble in water；
It is prepared by B, metal paste：Glue in copper powder and step A is mixed and made into paste；
It is prepared by C, composite：Cupric oxide powder is added in step B paste and cuprous oxide powder is well mixed, is obtained
To hybrid particles thing；
D, calcining：Hybrid particles thing made from step C is subjected to reduction calcining, the compound of graphene and nanometer copper ball is obtained
Material.
In the described preparation method for the graphene nano carbon/carbon-copper composite material of lithium ion battery negative material, preferred institute
State in step A, cellulose is ethyl cellulose or methylcellulose, and the weight ratio of cellulose and water is 1:100-3:100.
In the described preparation method for the graphene nano carbon/carbon-copper composite material of lithium ion battery negative material, preferred institute
State in step A, cellulose is added to the water, high-speed stirred is dispersed in water cellulose, cellulose glue is made.
In the described preparation method for the graphene nano carbon/carbon-copper composite material of lithium ion battery negative material, preferred institute
State in step B, the water atomization copper powder of the mesh of copper powder use -270~-280, the weight ratio of the copper powder and glue is 45:
100-85:100。
In the described preparation method for the graphene nano carbon/carbon-copper composite material of lithium ion battery negative material, preferred institute
State in step C, the weight ratio of the cupric oxide powder and paste is 0.05:100-0.1:100, the cuprous oxide powder and paste
The weight ratio of thing is 0.05:100-0.01:100.
In the described preparation method for the graphene nano carbon/carbon-copper composite material of lithium ion battery negative material, preferred institute
State in step D, step C hybrid particles thing is put into hydrogen reducing furnace and calcined, wherein calcining heating rate is 10 DEG C/min,
Dew point of hydrogen is 5 DEG C -15 DEG C, and calcining heat is 1085 DEG C -1150 DEG C, and calcination time is 10-25min.
It is described in detail below by way of embodiment：
Embodiment 1, a kind of preparation method of graphene nano carbon/carbon-copper composite material for lithium ion battery negative material, bag
Include following steps：
A, prepare glue：Cellulose is added in deionized water, high-speed stirred is dispersed in water cellulose, and fiber is made
Plain glue.Cellulose selects ethyl cellulose or methylcellulose, and the wherein weight ratio of cellulose and water is 1:100.
It is prepared by B, metal paste：Glue in copper powder and step A is mixed and made into paste；The copper powder use -275
Purpose water atomization copper powder, the weight ratio of the copper powder and glue is 45:100.
It is prepared by C, composite：Cupric oxide powder is added in step B paste and cuprous oxide powder is well mixed, is obtained
To hybrid particles thing；The weight ratio of cupric oxide powder and paste is 0.05:100, the weight of the cuprous oxide powder and paste
Than for 0.05:100.
D, calcining：Step C hybrid particles thing is put into hydrogen reducing furnace and calcined, wherein calcining heating rate is 10
DEG C/min, dew point of hydrogen is 5 DEG C DEG C, and calcining heat is 1085 DEG C, and calcination time is 25min, obtains graphene and nanometer copper ball
Composite.
As shown in figure 1, being the Scanning Electron microphotograph of composite, it can be seen that from photo：In graphene
Some nano level copper balls of Surface Creation.Copper ball realizes the conduction of Z-direction, compensate for the defect of graphene so that this
The negative material of invention can have fabulous electric conductivity in tri- directions of XYZ.
Embodiment 2, a kind of preparation method of graphene nano carbon/carbon-copper composite material for lithium ion battery negative material, bag
Include following steps：
A, prepare glue：Cellulose is added in deionized water, high-speed stirred is dispersed in water cellulose, and fiber is made
Plain glue.Cellulose selects ethyl cellulose or methylcellulose, and the wherein weight ratio of cellulose and water is 2:100.
It is prepared by B, metal paste：Glue in copper powder and step A is mixed and made into paste；The copper powder use -100
Purpose water atomization copper powder, the weight ratio of the copper powder and glue is 65:100.
It is prepared by C, composite：Cupric oxide powder is added in step B paste and cuprous oxide powder is well mixed, is obtained
To hybrid particles thing；The weight ratio of cupric oxide powder and paste is 0.08:100, the weight of the cuprous oxide powder and paste
Than for 0.08:100.
D, calcining：Step C hybrid particles thing is put into hydrogen reducing furnace and calcined, wherein calcining heating rate is 10
DEG C/min, dew point of hydrogen is 10 DEG C, and calcining heat is 1100 DEG C, and calcination time is 15min, obtains graphene and nanometer copper ball
Composite.
Embodiment 3, a kind of preparation method of graphene nano carbon/carbon-copper composite material for lithium ion battery negative material, bag
Include following steps：
A, prepare glue：Cellulose is added in deionized water, high-speed stirred is dispersed in water cellulose, and fiber is made
Plain glue.Cellulose selects ethyl cellulose or methylcellulose, and the wherein weight ratio of cellulose and water is 3:100.
It is prepared by B, metal paste：Glue in copper powder and step A is mixed and made into paste；The copper powder use -400
Purpose water atomization copper powder, the weight ratio of the copper powder and glue is 85:100.
It is prepared by C, composite：Cupric oxide powder is added in step B paste and cuprous oxide powder is well mixed, is obtained
To hybrid particles thing；The weight ratio of cupric oxide powder and paste is 0.1:100, the weight ratio of the cuprous oxide powder and paste
For 0.01:100.
D, calcining：Step C hybrid particles thing is put into hydrogen reducing furnace and calcined, wherein calcining heating rate is 10
DEG C/min, dew point of hydrogen is 15 DEG C, and calcining heat is 1150 DEG C, and calcination time is that 10min obtains graphene and nanometer copper ball
Composite.
Product test：Graphene nano composite copper material prepared by the inventive method is new for manufacturing negative electrode of lithium ion battery
Type conduction agent material, and material property is carried out to test as follows：
Test condition：
1. anode formula：LCO:PVDF:Conductive black=100:1.2:1.5
2. electrolyte prescription：EC:DEC:EMC=3：3：3, Vc 1%, PS 1%
Negative pole A group of formula (embodiment of the present invention)：Graphite:CMC:SBR:Graphene nano copper=100:1.4:1.9:0.5
Negative pole B group of formula (comparative example)：Graphite:CMC:SBR:Conductive black=100:1.4:1.9:1；
Method of testing：Resultant battery, different times of test are produced using identical technique and auxiliary material by above-mentioned formula
The dynamic performance of rate charging negative pole (i.e. whether negative pole the precipitation of lithium metal occurs)
Test result：
Following result is the test result that charges under the conditions of 2C constant current constant voltages：
It can be seen that from above test result：Lithium ion battery negative material is used as using graphene nano carbon/carbon-copper composite material
Conductive agent can with larger proportion lifting lithium ion battery constant-current charge ratio, and negative pole do not occur because polarize it is excessive
The analysis lithium phenomenon of (large current charge causes), therefore illustrate that the conductive agent material can largely lift the conduction of electrode in itself
Performance and chemical kinetics performance.
Claims (6)
1. a kind of preparation method of graphene nano carbon/carbon-copper composite material for lithium ion battery negative material, it is characterised in that
Comprise the following steps：
A, prepare glue：Cellulose glue is made by cellulose is soluble in water；
It is prepared by B, metal paste：Glue in copper powder and step A is mixed and made into paste；
It is prepared by C, composite：Cupric oxide powder is added in step B paste and cuprous oxide powder is well mixed, is mixed
Close particulate matter；
D, calcining：Hybrid particles thing made from step C is subjected to reduction calcining, the composite wood of graphene and nanometer copper ball is obtained
Material.
2. the preparation side of the graphene nano carbon/carbon-copper composite material according to claim 1 for lithium ion battery negative material
Method, it is characterised in that in the step A, cellulose is ethyl cellulose or methylcellulose, and the weight ratio of cellulose and water is
1:100-3:100。
3. the preparation side of the graphene nano carbon/carbon-copper composite material according to claim 1 for lithium ion battery negative material
Method, it is characterised in that in the step A, cellulose is added to the water, high-speed stirred is dispersed in water cellulose, fibre is made
The plain glue of dimension.
4. the preparation side of the graphene nano carbon/carbon-copper composite material according to claim 1 for lithium ion battery negative material
Method, it is characterised in that in the step B, the water atomization copper powder of the mesh of the mesh of copper powder use -150~-400, the copper powder and glue
The weight ratio of water is 45:100-85:100.
5. the preparation side of the graphene nano carbon/carbon-copper composite material according to claim 1 for lithium ion battery negative material
Method, it is characterised in that in the step C, the weight ratio of the cupric oxide powder and paste is 0.05:100-0.1:100, it is described
The weight ratio of cuprous oxide powder and paste is 0.05:100-0.01:100.
6. the preparation side of the graphene nano carbon/carbon-copper composite material according to claim 1 for lithium ion battery negative material
Method, it is characterised in that in the step D, step C hybrid particles thing is put into hydrogen reducing furnace and calcined, wherein calcining rises
Warm speed is 10 DEG C/min, and dew point of hydrogen is 5 DEG C -15 DEG C, and calcining heat is 1085 DEG C -1150 DEG C, and calcination time is 10-
25min。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113860351A (en) * | 2021-08-23 | 2021-12-31 | 中南大学 | Preparation method and application of CuO-graphite composite material prepared from waste graphite |
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