CN109037585A - The preparation method of negative electrode of lithium ion battery substrate - Google Patents
The preparation method of negative electrode of lithium ion battery substrate Download PDFInfo
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- CN109037585A CN109037585A CN201810874502.5A CN201810874502A CN109037585A CN 109037585 A CN109037585 A CN 109037585A CN 201810874502 A CN201810874502 A CN 201810874502A CN 109037585 A CN109037585 A CN 109037585A
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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
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0404—Methods of deposition of the material by coating on electrode collectors
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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
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
- H01M4/043—Processes of manufacture in general involving compressing or compaction
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
- H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
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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
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/661—Metal or alloys, e.g. alloy coatings
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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
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/663—Selection of materials containing carbon or carbonaceous materials as conductive part, e.g. graphite, carbon fibres
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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
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/665—Composites
- H01M4/667—Composites in the form of layers, e.g. coatings
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- 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
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Abstract
A kind of preparation method of negative electrode of lithium ion battery substrate provided by the invention, the preparation method is the following steps are included: graphene powder, graphene dispersion agent, solvent to be added in agitator tank with the ratio of mass ratio 5-8%:5-8%:84-90% and be stirred, it is uniformly mixed, obtains composite mortar；The composite mortar that will be stirred, is evenly applied to 6-8 μm of foil surface, and coating thickness is 2-3 μm；Foil after coating is compacted to 6-10 μm by roll squeezer；After compacting is completed, foil is toasted into 10-12h in vacuum oven, oven temperature is 40-50 DEG C to get arriving negative electrode of lithium ion battery substrate.The method of the present invention can greatly increase electric conductivity, reduce impedance, therefore also largely reduce the calorific value in battery use process.Meanwhile because the electric conductivity of graphene is higher than copper, copper foil foil thickness only needs the 60-80% of original thickness, can save the cost of 15-20%.
Description
Technical field
The present invention relates to graphene combination electrode material fields, more particularly to the preparation side of negative electrode of lithium ion battery substrate
Method.
Background technique
Lithium ion battery exists at present due to having many advantages, such as that discharge platform is high, energy density is big, having extended cycle life, environmental protection
Power supply has become Major Members in the market.As petroleum fuel gradually reduces, environmental pollution is got worse and people are to environmental protection
The enhancing of consciousness, people gradually attempt for lithium ion battery to be used for the fields such as pure electric automobile, hybrid-electric car.
However society above constantly spreads out of the message that lithium ion battery is on fire, explodes, and enables consumer to the peace of lithium ion battery
Full performance generates query, and cycle performance is also to be improved.In order to improve security performance, high rate performance and the matter of lithium ion battery
Specific energy is measured, scientific research personnel improves the performance of positive electrode by technologies such as doping, claddings, finds novel anode material to substitute
Graphite type material used by existing lithium ion battery attempts production ceramic diaphragm material to improve breakdown characteristics, and trial-production is each
Kind of high temperature resistant is not easily decomposed, the electrolyte of the characteristics such as overcharging resisting over-discharge, these technologies make lithium ion battery in safety and follow
There is large increase on ring, but researcher is less to collector concern.
In lithium ion battery production at present, anode, as collector, is made using the aluminium foil with a thickness of 4-10 μm in high current
With when, conveyance capacity will receive certain restrictions, and heat derives speed is general.
Summary of the invention
Technical problem: it is an object of the invention to solve prior art problem, a kind of negative electrode of lithium ion battery substrate is provided.
Technical solution: to achieve the above object, the invention provides the following technical scheme:
A kind of preparation method of negative electrode of lithium ion battery substrate of the invention, the preparation method the following steps are included:
Step 1: graphene powder, graphene dispersion agent, solvent are added with the ratio of mass ratio 5-8%:5-8%:84-90%
Enter and stirred into agitator tank, is uniformly mixed, obtains composite mortar；
Step 2: the composite mortar that will be stirred is evenly applied to 6-8 μm of foil surface, and coating thickness is 2-3 μm；
Step 3: the foil after step 2 is coated with is compacted to 6-10 μm by roll squeezer；
Step 4: after compacting is completed, toasting 10-12h for foil in vacuum oven, and oven temperature is 40-50 DEG C to get arriving
Negative electrode of lithium ion battery substrate.
Preferably, the graphene powder is made of sublevel graphene, and the sublevel graphene is by multilayer chip graphene
Formed with diamond, the diamond is located between adjacent two layers of multilayer chip graphene, the diamond with it is described
The carbon atom of multilayer chip graphene corresponds.
Preferably, the weight ratio of the multilayer chip graphene and the diamond is 18-19:1.
Preferably, the multilayer chip graphene is 3-5 lamellar graphene, every layer of the multilayer chip graphene
With a thickness of 0.2-0.5nm；The interlamellar spacing of the adjacent two layers of the multilayer chip graphene is 0.2-0.4nm.
Preferably, the graphene dispersion agent is Emulsifier EL-60.
Preferably, solvent is deionized water.
Preferably, the foil is copper foil or aluminium foil.
Preferably, in the step 1, stirring condition are as follows: under vacuum conditions, temperature is 30-50 DEG C, and mixing speed is
50rpm, mixing time 8-10h.
The utility model has the advantages that compared with prior art, the beneficial effects of the present invention are:
The present invention applies one layer of graphene on foil surface in advance, and grapheme material has good electric conductivity and a thermal conductivity, and copper foil
It is very harsh to conduction requirement as battery cathode collector, by adding graphene, electric conductivity can be greatly increased, is reduced
Impedance, therefore also largely reduce the calorific value in battery use process.Meanwhile because the electric conductivity of graphene is higher than
Copper can save the cost of 15-20% so copper thickness only needs the 60-80% of original thickness.
Detailed description of the invention
Fig. 1 is the nominal 8Ah battery core 5C charge and discharge cycles figure (500 weeks) of embodiment 1.
Fig. 2 is the nominal 8Ah battery core 5C charge and discharge discharge of electricity of embodiment 1 and temperature profile.
Fig. 3 is other battery core Life Cycle figures in the case of common material.
Specific embodiment
The embodiment of the present invention addressed below.The elements and features described in one embodiment of the invention can be with
The elements and features shown in one or more other embodiments combine.It should be noted that for purposes of clarity, saying
The expression and description of component unrelated to the invention, known to persons of ordinary skill in the art and processing are omitted in bright.
Heretofore described graphene powder is made of sublevel graphene, and the sublevel graphene is by multilayer chip graphene
Formed with diamond, the diamond is located between adjacent two layers of multilayer chip graphene, the diamond with it is described
The carbon atom of multilayer chip graphene corresponds；The weight ratio of the multilayer chip graphene and the diamond is 18-19:
1；The multilayer chip graphene is 3-5 lamellar graphene, every layer of the multilayer chip graphene with a thickness of 0.2-
0.5nm；The interlamellar spacing of the adjacent two layers of the multilayer chip graphene is 0.2-0.4nm；The diamond is Spherical Carbon, and institute
The partial size for stating Spherical Carbon is 0.7-1.6nm.
Graphene powder used in the present invention, preparation method carry out in accordance with the following steps:
Step 1: preparing multilayer chip graphene using chemical deposition: being deposited with cathode-ray on silica substrate surface
One layer of nickel metal layer.Cannot be other substrates, the nickel metal layer with a thickness of 200-400nm.
Step 2: be passed through in 950-1150 DEG C of temperature of tube furnace methane, hydrogen and ammonia composition gaseous mixture and
Common graphite powder, and it is cooled to room temperature within the 100ms time, obtain multilayer chip graphene, multilayer chip graphite described herein
The number of plies of alkene is 3-12 layers.
Step 3:, by being removed after electron microscope observation with molecular knife, being screened under 100,000 grades or more cleanliness environment
3-5 lamellar graphene out.
Step 4: the 3-5 lamellar graphene that step 3 filters out is mixed in proportion with diamond, it is evacuated to 100-
200MPa, temperature are controlled in 600-800 DEG C of stirring 36h, are prepared into graphene powder.
A kind of preparation method of negative electrode of lithium ion battery substrate of the invention, the preparation method the following steps are included:
Step 1: graphene powder, graphene dispersion agent, solvent are added with the ratio of mass ratio 5-8%:5-8%:84-90%
Enter and stirred into agitator tank, is uniformly mixed, obtains composite mortar；
Step 2: the composite mortar that will be stirred is evenly applied to 6-8 μm of foil surface, and coating thickness is 2-3 μm；
Step 3: the foil after step 2 is coated with is compacted to 6-10 μm by roll squeezer；
Step 4: after compacting is completed, toasting 10-12h for foil in vacuum oven, and oven temperature is 40-50 DEG C to get arriving
Negative electrode of lithium ion battery substrate.
Embodiment 1
By 0.2g Graphene powder, 0.2g Emulsifier EL-60,2.4g deionized water is added in agitator tank；In vacuum condition
Under, temperature is 30 DEG C, mixing speed 50rpm, mixing time 8h.The slurry that will be stirred uniformly is applied to 6 μm of copper foil tables
Face, 3 μm of coating thickness；8 μm are compacted to by roll squeezer after the completion of coating；After compacting is completed, toasted in vacuum oven
50 DEG C of oven temperature, negative electrode of lithium ion battery substrate of the invention can be obtained in 10h.It is prepared into cylindrical LiFePO4 8Ah electricity
Core.
Embodiment 2
By 0.6g Graphene powder, 0.6g Emulsifier EL-60,7.2g deionized water is added in agitator tank；In vacuum condition
Under, temperature is 50 DEG C, mixing speed 50rpm, mixing time 8h.The slurry that will be stirred uniformly is applied to 8 μm of copper foil tables
Face, 3 μm of coating thickness；10 μm are compacted to by roll squeezer after the completion of coating；After compacting is completed, toasted in vacuum oven
50 DEG C of oven temperature, negative electrode of lithium ion battery substrate of the invention can be obtained in 10h.It is prepared into cylindrical LiFePO4 21Ah
Battery core.
Embodiment 3
By 0.06g Graphene powder, 0.06g Emulsifier EL-60,0.72g deionized water is added in agitator tank；In vacuum item
Under part, temperature is 50 DEG C, mixing speed 50rpm, mixing time 10h.The slurry that will be stirred uniformly is applied to 8 μm of copper
Foil surface, 2 μm of coating thickness；9 μm are compacted to by roll squeezer after the completion of coating；After compacting is completed, in vacuum oven
10h is toasted, 50 DEG C of oven temperature, negative electrode of lithium ion battery substrate of the invention can be obtained.It is prepared into cylindrical ternary 2.2Ah
Battery core.
Charge and discharge cycles test analysis:
It is depressed in a normal atmosphere, in room temperature environment, carries out charge and discharge cycles test analysis to cylindrical battery core is prepared into.
Test battery core specification: 3.2V8Ah.
1: with 5C multiplying power (40A) constant-current charge to 3.65V, switching constant pressure 3.65V charges to electric current and is reduced to 0.01C
(0.08A)；2: standing 30 minutes；3: 2.5V is discharged to 5C multiplying power (40A)；4: standing 30 minutes；5: repeating step 1-4.
Test result is as follows for charge and discharge cycles:
As shown in Figure 1, being the nominal 8Ah battery core of embodiment 1,5C charge and discharge cycles figure (500 weeks), as can be seen from Figure in addition green wood
After material, cycle life decaying is faint, and charge conservation rate is powerful.
As shown in Fig. 2, being the nominal 8Ah battery core single charge and discharge of embodiment 1 and temperature curve, adding newly as can be seen from Figure
After material, the more conventional battery core of temperature change is good many in the case of high power charging-discharging.
As shown in figure 3, being other common material battery core charge and discharge cycles figures, as can be seen from Figure, the positive material of same system
In the case of material, service life decline is obvious after 1C charge and discharge, and produces irreversible damage after multiple circulation.
Graphene dispersion agent uses Emulsifier EL-60 in the present invention, can stable dispersion graphene, graphene leads
Electrically also it is greatly improved.
The present invention applies one layer of graphene on foil surface in advance, and grapheme material has good electric conductivity and thermal conductivity, and
Copper foil requires conduction very harsh as battery cathode collector, by adding graphene, can greatly increase electric conductivity,
Impedance is reduced, therefore also largely reduces the calorific value in battery use process.Meanwhile because graphene electric conductivity
The cost of 15-20% can be saved so copper foil foil thickness only needs the 60-80% of original thickness higher than copper.
The above is merely a preferred embodiment of the present invention, it is noted that for those skilled in the art
For, under the premise of not departing from core of the invention technology, improvements and modifications can also be made, these improvements and modifications are also answered
Belong to scope of patent protection of the invention.With any change in the comparable meaning and scope of claims of the present invention, all
It is considered as being included within the scope of the claims.
Claims (8)
1. a kind of preparation method of negative electrode of lithium ion battery substrate, which is characterized in that the preparation method the following steps are included:
Step 1: graphene powder, graphene dispersion agent, solvent are added to the ratio of mass ratio 5-8%:5-8%:84-90%
It is stirred in agitator tank, is uniformly mixed, obtains composite mortar；
Step 2: the composite mortar that will be stirred is evenly applied to 6-8 μm of foil surface, and coating thickness is 2-3 μm；
Step 3: the foil after step 2 is coated with is compacted to 6-10 μm by roll squeezer；
Step 4: after compacting is completed, toasting 10-12h for foil in vacuum oven, and oven temperature is 40-50 DEG C to get arriving
Negative electrode of lithium ion battery substrate.
2. the preparation method of negative electrode of lithium ion battery substrate according to claim 1, which is characterized in that the Graphene powder
End is made of sublevel graphene, and the sublevel graphene is made of multilayer chip graphene and diamond, and the diamond is located at
Between adjacent two layers of multilayer chip graphene, the carbon atom one of the diamond and the multilayer chip graphene is a pair of
It answers.
3. the preparation method of negative electrode of lithium ion battery substrate according to claim 2, which is characterized in that the multilayer chip
The weight ratio of graphene and the diamond is 18-19:1.
4. the preparation method of negative electrode of lithium ion battery substrate according to claim 1, which is characterized in that the multilayer chip
Graphene is 3-5 lamellar graphene, every layer of the multilayer chip graphene with a thickness of 0.2-0.5nm；The multilayer tablet
The interlamellar spacing of the adjacent two layers of shape graphene is 0.2-0.4nm.
5. the preparation method of negative electrode of lithium ion battery substrate according to claim 1, which is characterized in that the graphene point
Powder is Emulsifier EL-60.
6. the preparation method of negative electrode of lithium ion battery substrate according to claim 1, which is characterized in that solvent is deionization
Water.
7. the preparation method of negative electrode of lithium ion battery substrate according to claim 1, which is characterized in that the foil is copper
Foil or aluminium foil.
8. the preparation method of negative electrode of lithium ion battery substrate according to claim 1, which is characterized in that the step 1
In, stirring condition are as follows: under vacuum conditions, temperature is 30-50 DEG C, mixing speed 50rpm, mixing time 8-10h.
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| CN201810874502.5A CN109037585A (en) | 2018-08-03 | 2018-08-03 | The preparation method of negative electrode of lithium ion battery substrate |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103187576A (en) * | 2011-12-28 | 2013-07-03 | 清华大学 | Current collector, electrochemical battery electrode and electrochemical battery |
| CN103725046A (en) * | 2012-10-12 | 2014-04-16 | 东丽先端材料研究开发（中国）有限公司 | Graphene dispersion liquid and preparation method thereof |
| CN105322178A (en) * | 2015-10-16 | 2016-02-10 | 广东烛光新能源科技有限公司 | Electrochemical battery electrode, electrochemical battery containing same and preparation method thereof |
| CN107445146A (en) * | 2017-07-21 | 2017-12-08 | 昆山正国新能源动力电池有限公司 | Lithium ion battery time layer graphene and preparation method |
-
2018
- 2018-08-03 CN CN201810874502.5A patent/CN109037585A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103187576A (en) * | 2011-12-28 | 2013-07-03 | 清华大学 | Current collector, electrochemical battery electrode and electrochemical battery |
| CN103725046A (en) * | 2012-10-12 | 2014-04-16 | 东丽先端材料研究开发（中国）有限公司 | Graphene dispersion liquid and preparation method thereof |
| CN105322178A (en) * | 2015-10-16 | 2016-02-10 | 广东烛光新能源科技有限公司 | Electrochemical battery electrode, electrochemical battery containing same and preparation method thereof |
| CN107445146A (en) * | 2017-07-21 | 2017-12-08 | 昆山正国新能源动力电池有限公司 | Lithium ion battery time layer graphene and preparation method |
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