CN105977468A - High-capacity lithium ion battery negative electrode material and preparation method thereof - Google Patents
High-capacity lithium ion battery negative electrode material and preparation method thereof Download PDFInfo
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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
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- 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
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H—ELECTRICITY
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- 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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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Abstract
The invention discloses a high-capacity lithium ion battery negative electrode material, and belongs to the field of new energy materials. The material comprises a copper foil, wherein the copper foil is coated with a coating, and the coating is mainly prepared from the following premixes in percentage by weight: 1%-1.5% of sodium carboxymethylcellulose, 1.5%-2% of butadiene styrene rubber, 0.95%-9.7% of nano diamond alkene and the balance of graphite. The invention further discloses a preparation method of the high-capacity lithium ion battery negative electrode material. The lithium ion battery negative electrode material is high in specific capacity, fine in charge-discharge property, low in discharge voltage, high in safety, cycle performance, heat dispersion and charge current and short in charge time, the specific capacity is improved from original 352mAh/g to about 408mAh/g by about 16%, and battery specific capacity and battery performance are stable.
Description
Technical field
The invention belongs to new energy materials field, be specifically related to a kind of cathode material for high capacity lithium ion battery and preparation thereof
Method.
Background technology
Since 21st century, along with the non-renewable resources such as coal, oil, natural gas constantly consume and burning brings
Environmental pollution, the sustainable development of the mankind is replaced passing by serious challenge, the new forms of energy in the urgent need to a kind of green non-pollution
The Fossil fuel of system.The most representative in novel energy is lithium ion battery, and lithium ion battery is a kind of secondary cell, and it is main
Lithium ion Li to be relied on+Movement between both positive and negative polarity carrys out work.In charge and discharge process, Li+Come and go embedding between two electrodes
Enter or deintercalation, during charging, Li+From positive pole deintercalation, embedding negative pole through electrolyte, negative pole is in rich lithium state, discharges the most contrary.
Have that running voltage is high, lightweight, volume is little, high-energy-density, high output voltage, memory-less effect and nonpollution environment etc. excellent
Point, has been used extensively on portable mobile apparatus, such as mobile phone, notebook computer, digital camera, IPAD etc.,
Electric car power supply and the energy storage device aspect such as wind energy, solar energy also have the biggest application potential.
In recent years, various electronic products are gradually toward intelligent, functional diversities development, and the performance of lithium ion battery is carried by this
Higher requirement, such as capacitance are gone out.In lithium ion battery general without lithium metal as negative pole because lithium metal is filling
Discharge process can produce Li dendrite, internal short-circuit of battery, the negative material master of current business-like lithium ion battery can be caused
Graphite type material to be, the theoretical specific capacity of graphite type material only has 372mAh/g, and actual value is about 352mAh/g, only gold
Belonging to about the 10% of lithium, capacitance is on the low side；Graphite layers is away from for 0.35nm, less than graphite lithium intercalation compound LixC6Crystal face interlayer
Away from 0.37nm, its deformation during the embedding and abjection of lithium ion is big, has released substantial amounts of heat in the process, to battery
Safety have a certain impact；Owing to the interlamellar spacing of graphite type material is little, in charging process, lithium ion cannot embed, and makes
The lithium concentration obtaining surface layer is more and more lower, affects the stability of its structure.Additionally lithium ion diffusion speed in graphite linings
Degree is relatively slow, and during high current charge-discharge, polarization is big, and resistance is big, and heating is many, the poor stability of battery, in electricity circulation and
In charge and discharge process, graphite layers, away from changing, easily causes graphite linings peeling, efflorescence, is very easy to cause structure collapses, leads
Cause cycle performance of battery worse and worse, affect the stability of its structure.
Summary of the invention
It is an object of the invention to provide a kind of cathode material for high capacity lithium ion battery and preparation method thereof.
Based on above-mentioned purpose, the present invention by the following technical solutions: a kind of cathode material for high capacity lithium ion battery, including
Copper Foil, Copper Foil is coated with coating, and described coating is mainly prepared from by the premix material of following weight percentage ratio: carboxymethyl cellulose
Element sodium 1% ~ 1.5%, butadiene-styrene rubber 1.5% ~ 2%, nanometer diamond alkene 0.95 ~ 9.7%, surplus is graphite.
Further, described nanometer diamond alkene by the nanometer diamond alkene of tri-kinds of particle diameters of 50nm, 200nm, 250nm according to quality
Mix than for (1 ~ 2) (3 ~ 4) (4 ~ 5).
Further, described graphite is (1 ~ 2) (3 ~ 4) by 10 μ, 20 μ, the graphite of 30 tri-kinds of particle diameters of μ according to mass ratio
(4 ~ 5) mix.
Above-mentioned cathode material for high capacity lithium ion battery uses following method to prepare, and step is:
(1) by graphite and nanometer diamond alkene according to mass ratio md/mg=1 (0.01 ~ 0.1) mixes, activates, dries to obtain premix material, stone
Consumption is the total consumption of graphite the 97.5% ~ 99.5% of ink；
(2) first being mixed with water by cmc (sodium carboxymethyl cellulose), the mass concentration of sodium carboxymethyl cellulose is 1.5% ~ 2%；Mend again
Enter electrically conductive graphite, stir 30min ~ 1h, stirring frequency 25 ~ 30Hz, add and mix, stir 3 ~ 5h, stirring frequency 20 ~
25Hz, adds a small amount of sbr (butadiene-styrene rubber), stirs 45min ~ 1h, stirring frequency 20 ~ 25Hz, according to practical situation, adds few
Amount water stirring, stirs 1h ~ 1.5h, stirring frequency 20 ~ 25Hz, by the viscosity adjustment of slurry to 2000 ~ 3000cp, is stirred for
30min ~ 1h, stirring frequency 5 ~ 10Hz, slurry just prepare, and basic proportioning is cmc:sp(graphite additional amount): sbr: premix
Material=(1 ~ 1.5) (0.5 ~ 2) (1.5 ~ 2) (94.5 ~ 97), solids content controls 40 ~ 50%.Wherein cmc and sbr acts primarily as
Flocculation adhesive effect；
(3) being coated on Copper Foil by the slurry prepared, one side surface density is 110 ~ 130g/m2,
(4) coated Copper Foil is dried.
Further, in step (1), activation process comprises the following steps: ultrasound wave alkali cleaning, ultrasound wave deionized water are clear
Wash, acid-wash activation, ultrasound wave deionized water clean.
Further, step (4) uses notch cuttype stoving process: after being warming up to 60 DEG C with the heating rate of 2 DEG C/min,
Insulation 30min ~ 1h；It is warming up to 80 DEG C of insulation 30min ~ 1h again；Then heat to 120 DEG C, be incubated 4 ~ 8h, finally naturally cool to
Room temperature.
Preparation method referenced patent CN2015107492073 of above-mentioned nanometer diamond alkene.
Compared with prior art, the invention have the advantages that
(1) specific capacity of negative electrode material of lithium ion battery that the present invention provides is high, original 352mAh/g bring up to about 408mAh/
G, increase rate about 16%；Having good charge-discharge performance, discharge voltage is low, and safety is high；Cycle performance is high, battery specific volume
Amount is stable；Heat dispersion is high, and battery performance is stable；Charging current is high, and the charging interval is short.
(2) owing to being mostly point cantact between electrode particle, therefore big big of the little resistance ratio particle diameter of particle diameter, but particle diameter is big
Granule in charge and discharge process dilation change substantially, the negative pole made after size particles is mixed by a certain percentage up to
To the contact area increased between granule, reduce contact resistance, increase capacitance.
Accompanying drawing explanation
Fig. 1 is the influence curve of the anticathode material electric conductivity of different nanometer diamond alkene addition；
Fig. 2 is the influence curve of the anticathode material specific capacity of different nanometer diamond alkene addition, and wherein (a) does not contains nanometer diamond
Alkene, (b) md/mg=0.05。
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in detail.
The preparation of the different nanometer diamond alkene addition premix material of embodiment 1
The preparation process of premix material is:
(a) respectively by graphite and nanometer diamond alkene according to mass ratio md/mg=0、0.01、0.02、0.03、0.04、0.05、0.06、
0.07,0.08,0.09,0.1 mixing, obtains compound；Nanometer diamond alkene is bored by the nanometer of tri-kinds of particle diameters of 50nm, 200nm, 250nm
Stone alkene mixes for (1 ~ 2) (3 ~ 4) (4 ~ 5) according to mass ratio；Graphite by 10 μ, 20 μ, 30 tri-kinds of particle diameters of μ graphite according to
Mass ratio mixes for (1 ~ 2) (3 ~ 4) (4 ~ 5).
B above-mentioned compound is activated by (), activation step is:
1), ultrasound wave alkali cleaning: compound is put in alkaline bath, be provided with supersonic generator, ultrasound wave frequency bottom alkaline bath
Rate is 35-40KHz, is the NaOH solution of 10%-12% for concentration in alkali cleaning pond, and alkali wash water temperature controls between 50-60 ° of C,
And Stirring, rotary rpm controls at 20-30rpm, and scavenging period controls at 20-30min；
2), ultrasonic waves for cleaning: ultrasonic frequency is 35-40KHz, and cleanout fluid is deionized water, and compound is put in cleanout fluid
And Stirring, rotary rpm controls at 10-20rpm, and mixing time controls at 15-20min, measures supernatant pH value, instead
Multiple clean until pH=7；
3), acid-wash activation: pickle be concentration be the dilution heat of sulfuric acid of 10%-30%, temperature is room temperature, and compound is put into pickling
In solution and stir, rotary rpm controls at 5-10rpm, and mixing time controls at 5-10min, reaches to activate mix surface
Purpose；
4), ultrasonic wave water washing: ultrasonic wave water washing is that room temperature cleans, and ultrasonic frequency is 35-40KHz, and water lotion is deionization
Water.Being entered by compound in deionized water and Stirring, rotary rpm controls at 10-20rpm, and mixing time, at 5-10min, is surveyed
Amount supernatant pH value, cleans repeatedly until pH=7.
C () uses staged baking process to dry: heating rate is 2 DEG C/min, and room temperature is warming up to 60 DEG C, and constant temperature is incubated
30min, then it is warming up to 80 DEG C, constant temperature insulation 30min, then heat to 120 DEG C, constant temperature insulation 60min, finally it is warming up to 280
DEG C, constant temperature insulation 2h, naturally cool to room temperature, obtain premix material.
The preparation of embodiment 2 cathode material for high capacity lithium ion battery
Cathode material for high capacity lithium ion battery uses following method to prepare, and step is:
(1) being mixed with 1100ml water by 16.5 g cmc (sodium carboxymethyl cellulose), the mass concentration of sodium carboxymethyl cellulose is
1.5%；Fill into 22g electrically conductive graphite again, stir 30min ~ 1h, stirring frequency 25 ~ 30Hz, then gained solution is divided into 11
Part.
(2) in above-mentioned 11 parts of solution, it is separately added into the premix material 95g of embodiment 1 preparation, stirs 3 ~ 5h, stirring frequency 20
~ 25Hz, then it is separately added into 1.5g butadiene-styrene rubber, stir 45min ~ 1h, stirring frequency 20 ~ 25Hz, the viscosity of the regulation slurry that adds water
Being adjusted to 2000 ~ 3000cp, be stirred for 30min ~ 1h, stirring frequency 5 ~ 10Hz, slurry has just been prepared
(3) being coated on Copper Foil by the slurry prepared, one side coats its surface density and controls at 110-130g/m2, dual coating
Surface density is multiplied by 2.
(4) notch cuttype stoving process is used to be dried by coated Copper Foil: to be warming up to 60 DEG C with the heating rate of 2 DEG C/min
After, it is incubated 30min ~ 1h；It is warming up to 80 DEG C of insulation 30min ~ 1h again；Then heat to 120 DEG C, be incubated 4 ~ 8h, the coldest
But room temperature is arrived.
The preparation of embodiment 3 cathode material for high capacity lithium ion battery
(1) being mixed with 100ml water by 1.0gcmc (sodium carboxymethyl cellulose), the mass concentration of sodium carboxymethyl cellulose is 1.5%；
Fill into 0.5g electrically conductive graphite again, stir 30min ~ 1h, stirring frequency 25 ~ 30Hz.
(2) in above-mentioned solution, m in embodiment 1 is addedd/mg=The premix material 96.5g prepared when 0.05, stirs 3 ~ 5h, stirs
Mixing frequency 20 ~ 25Hz, then be separately added into 2g butadiene-styrene rubber, stir 45min ~ 1h, stirring frequency 20 ~ 25Hz, add water regulation slurry
Viscosity adjustment to 2000 ~ 3000cp, be stirred for 30min ~ 1h, stirring frequency 5 ~ 10Hz, slurry has just been prepared
(3) being coated on Copper Foil by the slurry prepared, one side coats its surface density and controls at 110-130g/m2, dual coating
Surface density is multiplied by 2.
(4) notch cuttype stoving process is used to be dried by coated Copper Foil: to be warming up to 60 DEG C with the heating rate of 2 DEG C/min
After, it is incubated 30min ~ 1h；It is warming up to 80 DEG C of insulation 30min ~ 1h again；Then heat to 120 DEG C, be incubated 4 ~ 8h, the coldest
But room temperature is arrived.
Embodiment 4 performance test
Electrical conductivity: weigh the major parameter of negative pole raw material electric conductivity.
Specific capacity: refer generally to weight ratio capacity, refers to the electricity that the battery of Unit Weight is released, unit mAh/g, is to weigh
One important symbol of battery performance quality.
Cycle performance: refer to, under a certain electric current density, battery is carried out discharge and recharge, see the impact on specific capacity of the charge and discharge number of times.
4.1 conductance measurement
The material using FT-310 conductivity of graphite tester to prepare embodiment 2 is tested, and uses four end methods of testing to carry out
Test, test result is shown in Fig. 1.
Knowable to the result of Fig. 1, the nanometer diamond alkene of Different adding amount is different on the impact of its negative material electric conductivity
, along with the raising of nanometer diamond alkene content, the electric conductivity of anode material is gradually reduced, (m within limitsD/
mG≤ 0.05), the impact on its electric conductivity of adding of nanometer diamond alkene is more weak, and electric conductivity is barely affected, but
Being as the further raising of nanometer diamond alkene content, the electric conductivity of anode material is decreased obviously, and electric conductivity is turned by quantitative change
Become qualitative change, it can be seen that nanometer diamond alkene must just can ensure that the conduction of composite negative pole material in certain content
Property.
4.2 specific capacities measure
Test object: with m in embodiment 2d/mg=0 (a) and md/mg=The material prepared time 0.05 (b), as experimental subject, is surveyed
Test result part Fig. 2.
Specific capacity test condition: electrolyte: 1M-LiPF6, EC/DMC/EMC=1:1:1
To electrode: lithium sheet
Discharge and recharge: 1, constant-current discharge: 0.1C, 0.01V
2, constant-current charge: 0.2C, 2.0V
From figure 2 it can be seen that adding after a certain amount of nanometer diamond alkene, specific capacity has had and has improved significantly, by original
352mAh/g brings up to about 408mAh/g, increase rate about 16%, and this is for improving the lithium ion with Delanium as cathode material
Battery capacity is the most significant, and this composite negative pole material has good charge-discharge performance, and this composite negative pole material is put
Piezoelectric voltage, at below 1V, has relatively low discharge voltage, suitably as the cathode material of lithium ion battery.
4.3 cycle performance tests
With m in embodiment 2d/mg=The material prepared when 0.05 as experimental subject,
Test condition: constant current is tested, tests electric current 0.3C, and test result is shown in Table 1.
From table 1 it follows that after repeatedly circulation, its specific capacity is basicly stable, and amplitude of variation is little, coulombic efficiency
Height, has good chemical property.
Charge efficiency is also one of major parameter weighing battery performance.The charging interval of lithium ion battery is longer at present,
As a example by electric motor car, being typically filled with electricity at least needs 8 hours, and the charging interval is long.The charging current one of lithium ion battery at present
As be 0.5C, if improve charging current, then inside battery negative response can be made to increase, produce substantial amounts of heat, following of battery
Ring performance reduces, and shortens the service life of battery.And this composite negative pole material is owing to the addition of nanometer diamond alkene, nanometer diamond
Alkene has good heat conductivility, it is possible to increase charging current, the charging current of battery can be brought up to 0.55-0.6C, thus
Shorten the charging interval.
Claims (6)
1. a cathode material for high capacity lithium ion battery, including Copper Foil, Copper Foil is coated with coating, it is characterised in that described
Coating is mainly prepared from by the premix material of following weight percentage ratio: sodium carboxymethyl cellulose 1% ~ 1.5%, butadiene-styrene rubber 1.5% ~
2%, nanometer diamond alkene 0.95% ~ 9.7%, surplus is graphite.
Cathode material for high capacity lithium ion battery the most according to claim 1, it is characterised in that described nanometer diamond alkene by
The nanometer diamond alkene of tri-kinds of particle diameters of 50nm, 200nm, 250nm mixes for (1 ~ 2) (3 ~ 4) (4 ~ 5) according to mass ratio.
Cathode material for high capacity lithium ion battery the most according to claim 1, it is characterised in that described graphite by 10 μ, 20
μ, the graphite of 30 tri-kinds of particle diameters of μ mix for (1 ~ 2) (3 ~ 4) (4 ~ 5) according to mass ratio.
4. the preparation method of the arbitrary described cathode material for high capacity lithium ion battery of claim 1 ~ 3, it is characterised in that step
For:
(1) graphite is mixed with nanometer diamond alkene according to mass ratio 1 (0.01 ~ 0.1), activate, dries to obtain premix material, graphite
Consumption is the 97.5% ~ 99.5% of the total consumption of graphite；
(2) under agitation, sodium carboxymethyl cellulose being mixed with water, the mass concentration of sodium carboxymethyl cellulose is 1.5% ~
2%, add residue graphite；It is subsequently adding the premix material of step (1) gained, adds butadiene-styrene rubber and prepare slurry, regulation slurry
Viscosity adjustment is to 2000 ~ 3000cp；
(3) being coated on Copper Foil by the slurry prepared, one side surface density is 110 ~ 130g/m2；
(4) coated Copper Foil is dried.
The preparation method of cathode material for high capacity lithium ion battery the most according to claim 4, it is characterised in that step
(1), in, activation process comprises the following steps: ultrasound wave alkali cleaning, the cleaning of ultrasound wave deionized water, acid-wash activation, ultrasound wave go from
Sub-water cleans.
The preparation method of cathode material for high capacity lithium ion battery the most according to claim 4, it is characterised in that step
(4) use notch cuttype stoving process in: after being warming up to 60 DEG C with the heating rate of 2 DEG C/min, be incubated 30min ~ 1h；It is warming up to again
80 DEG C of insulation 30min ~ 1h；Then heat to 120 DEG C, be incubated 4 ~ 8h, finally naturally cool to room temperature.
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Application publication date: 20160928 |