CN106532057B - A kind of lithium battery anode film for additive and preparation method - Google Patents
A kind of lithium battery anode film for additive and preparation method Download PDFInfo
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- CN106532057B CN106532057B CN201611126925.6A CN201611126925A CN106532057B CN 106532057 B CN106532057 B CN 106532057B CN 201611126925 A CN201611126925 A CN 201611126925A CN 106532057 B CN106532057 B CN 106532057B
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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
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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
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
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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
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Abstract
The present invention provides a kind of lithium battery anode film for additive, it is that one kind is wrapped by and amidated nano high purity silicon, positive electrode can be effectively inhibited for lithium battery anode to react with organic electrolyte, to prevent the generation of positive active material decaying, loss and gas, stability of active substances in cathode materials during circulating battery is improved.Preparation method is further provided for, by HIGH-PURITY SILICON, polyacrylamide, urea, surfactant by grinding cladding and amidated nano high purity silicon particle, as lithium battery anode film for additive, there is good dispersibility in anode material of lithium battery.
Description
Technical field
The present invention relates to battery material fields, and in particular to the improvement of lithium ion secondary battery anode material especially relates to
And a kind of lithium ion secondary battery anode material additive.
Background technique
The concept of lithium ion chargeable battery first by Armand in the 1980s by proposing, the positive and negative electrode of battery
Material carries out energy exchange using the material that can carry out ion storage and exchange, using the migration back and forth of ion when charge and discharge.
As energy crisis and problem of environmental pollution become increasingly conspicuous, hybrid electric vehicle market shows the booming impetus, this needs
Battery has that discharge current is larger, the higher performance characteristics of power.In addition, the electronic products such as some electric tools, model plane are also wanted
Ask battery can high-multiplying power discharge, therefore traditional small-sized, low-power lithium ion battery cannot fully meet the demand in market.
In recent years, there is ultra-thin, ultralight, high-energy density solid polymer lithium ion battery to be also developed in succession
Come and moves towards market.However, lithium ion battery can not fully meet existing use at present, anode especially in the prior art
For material due to its atomic structure etc., it is poor that there are thermal stability, leads to poor circulation under room temperature or high temperature, battery life
It is low, the problems such as safety is insufficient.Conventional lithium battery includes anode, cathode, the partition and lithium ion being inserted between these electrodes
Electric conductivity organic electrolyte.In the lithium secondary battery, using metal oxides such as lithium cobalt, lithium nickel, lithium manganese as positive electrode, to have
Solvent or organic polymer are as electrolyte, and in the long-term use, negative electrode material or positive electrode can be dissolved in electrolysis
It causes to be lost in liquid, so that battery capacity reduces.
For above situation, Chinese invention patent application number 201310006702.6 proposes a kind of lithium battery Malaysia acyl
Imines additive and corresponding lithium battery anode formula, the additive refer to using the modified span of cyanamide and melamine come
Acid imide, additive therefor form protective film in surface of positive electrode active material, can prevent positive electrode active materials in internal short-circuit
Cracking, so that battery is safer, while the safety protective film because having been formed in surface of positive electrode active material, improves lithium battery
Service life.But there is also certain defects for the technical solution: (1) cycle life of battery is relatively low；(2) though improving electricity
The service life in pond, but the self-discharge performance of battery is general.
Chinese invention patent application number 201610199779.3 proposes a kind of lithium battery anode additive, contains amino nitrile and ring
Shape alkali and the modified maleimide of cyclic annular acid composition modification, the battery being prepared into pass through lancing test, the results showed that big
The stability of gained battery anode active material is increased greatly, and improves the cycle life of battery.The invention additive therefor
Protective film is formd in surface of positive electrode active material, positive electrode active materials can be prevented to crack in internal short-circuit, so that battery is more pacified
Entirely, while the safety protective film because having been formed in surface of positive electrode active material, the service life of lithium battery is improved, is also improved
The cycle life and self-discharge performance of battery.However, cyanamide used by the technology etc. is extremely toxic substance, while lithium battery
Battery and battery storage performance are also without significantly improving.
According to background above, the present invention provides a kind of lithium battery anode film for additive and preparation methods, pass through machinery
Amidated nano-scale particle is made with HIGH-PURITY SILICON, acrylamide, urea, surfactant, the nano particle in the mode of grinding
As lithium battery anode film for additive, and there is good dispersibility in anode material of lithium battery.When battery works, addition
The positive electrode active materials particle surface of film for additive forms protective layer, i.e., one layer stable SEI film (stationary electrolyte interface
Film, Solid Electrolyte Interface), it effectively hinders, positive electrode and organic electrolyte is inhibited to react,
To prevent positive active material decaying, loss, stability of positive active material during circulating battery is improved, is finally mentioned
High-lithium ion battery cycle life and high rate performance.
Summary of the invention
It is poor for the generally existing positive electrode thermal stability of current field of lithium ion secondary, while surface is easy shape
The dissolution for inhibiting ion in subsequent charge and discharge process at gaseous state film, leads to poor circulation, electricity under room temperature or high temperature
The problems such as pond service life is low, safety is insufficient, the present invention provides a kind of lithium battery anode film for additive, can effectively inhibit just
Pole material reacts with organic electrolyte, to prevent the generation of positive active material decaying, loss and gas, improves anode
Stability of material activity substance during circulating battery.
To solve the above problems, the invention adopts the following technical scheme:
A kind of preparation method of lithium battery anode film for additive, it is characterised in that the specific method is as follows:
(1) HIGH-PURITY SILICON, polyacrylamide, urea, surfactant are turned in a high speed mixer with 600-1200rpm
It is fast sufficiently to mix, disperse 10-30min, obtain pre-composition；The quality sum of pre-composition is in terms of 100% mass fraction, wherein high-purity
The mass fraction of silicon is 10 ~ 60%, and the mass fraction of polyacrylamide is 2-25%, and the mass fraction of surfactant is 5-10%
, the mass fraction of urea is 10-70%；
(2) pre-composition that step (1) obtains and abrasive sand are added to high speed star lapping machine in the ratio of 0.5 ~ 4:1
It grinds in tank body, grinding tank body is ground after carrying out vacuum sealing processing, is adjusted the revolving speed of master and is turned with 200-750rpm
Speed rotation, 0.5~6h of high speed grinding；
(3) so that step (2) is obtained particle, frosted mixture by sieve, remove frosted, air current classifying removes partial size > 0.1 μm
Coarse granule, obtain amidated nano particle, i.e. lithium battery anode film for additive.
The HIGH-PURITY SILICON is powdered silicon, and particle size distribution can be formed less than 10 μm by the grinding of high speed
The more uniform nano particle of granularity；
Preferably, the granularity of the high-purity powder shape silicon is to be conducive to for quickly forming nanoscale less than 1 μm
The instantaneous cladding of grain and polyacrylamide, ultimately forms amidation nano particles good dispersion and clad is more complete；
The surfactant includes isopropanol, pyridine, n-hexane, glycerine (glycerol), furans, 1,3- epoxy penta
At least two in alkane, chloroform, it can dissolve or disperse acrylamide and urea；
Preferably, the surfactant is made of isopropanol, glycerine and chloroform；
Preferably, the polyacrylamide, urea powder, surfactant can be in advance in the condition heating of isolation air
Melting；
Preferably, in the pre-composition that the HIGH-PURITY SILICON, polyacrylamide, urea, surfactant form, the matter of HIGH-PURITY SILICON
Measuring score is 50%, and the mass fraction of polyacrylamide is 15%, and the mass fraction of surfactant is 5%, the quality point of urea
Number is 30%；
Planetary-type grinding machine is mixing, fine grinding, nano material dispersion, the conventional machinery grinding dress for developing new and high technology material
It sets, is that mill tube also carries out rotation while revolution as principle, mill tube revolution revolving speed can be made to break through critical turn of general milling machine
The limitation of speed drives abrading-ball to do complicated movement, is hit, ground to material, the granularity of abrasive product can achieve nanometer
Grade and particle size distribution is more concentrated.HIGH-PURITY SILICON powder forms superfine nano particle under abrasive action, and fragmentation is formed disconnected
Broken face activity is high, and polyacrylamide, urea form stable combination in grinding system, and rear the two is made to be coated to nano particle
Surface.
The technical program novelty obtains amidation nano particle in the way of mechanical lapping, and mechanical lapping reaction can make
Reactant more fully mixes, improves the combination frequency of reactant, and the fluctuation of temperature and pressure will also be promoted in process of lapping
Reactivity makes reaction product be integrated to nano silicon particles surface to a greater degree.
A kind of lithium battery anode film for additive, it is characterized in that lithium battery anode prepared by the preparation method at
Film additive, one kind is wrapped by and amidated nano high purity silicon, for lithium battery anode can effectively inhibit positive electrode with
Organic electrolyte reacts, to prevent the generation of positive active material decaying, loss and gas, improves positive electrode activity
Stability of substance during circulating battery.
The present invention obtains amidated nano particle by the way of mechanical lapping, adds for anode material for lithium-ion batteries
Add agent, compared with prior art, the feature and excellent effect protruded is: (1) the technical program has been put forward for the first time amide
SiClx nanoparticle is as anode material for lithium-ion batteries additive；(2) the amidation nanoparticle of the technical program prepares work
Skill is simple and easy, low in cost, environment-protecting and non-poisonous, has significant market application value；(3) amidated nano particle dispersibility
Can be good, positive electrode active materials particle surface can be made to form protective layer, hinder, inhibit positive electrode and organic electrolyte generation anti-
It answers.
Specific embodiment
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
HIGH-PURITY SILICON, polyacrylamide, urea, surfactant (isopropanol, glycerine and chloroform) is mixed in high speed
It sufficiently mixed in conjunction machine with the revolving speed of 800rpm, disperse 15min, obtain pre-composition；The quality sum of pre-composition is with 100% mass
Score meter, the then wherein number of components of each raw material are as follows: the mass fraction of HIGH-PURITY SILICON is 55%, and the mass fraction of polyacrylamide is
22%, the mass fraction of surfactant is 8%, and the mass fraction of urea is 15%.Obtained pre-composition is ground with spherical corundum
It after frosted is in the ratio mixing of 4:1, is added in the grinding tank body of high speed star lapping machine, grinding tank body carries out at vacuum sealing
It is ground after reason.It adjusts the revolving speed of master to rotate with the revolving speed of 250rpm, high speed grinding reacts 2.5h, after the reaction was completed, will
Particle, frosted mixture are obtained by sub-sieve, the coarse granule of frosted and partial size > 0.1 μm is removed, obtains amidated nanometer
Grain.
Amidation particle will be obtained to be added in lithium ion cell anode material lithium cobaltate in 0.5% ratio, with PVDF, NMP
It is finely dispersed to arrive anode sizing agent, it is routinely prepared into battery anode slice, is tested, is recycled 1000 times at normal temperature, capacity
Conservation rate 86%；And 100 capacity retention ratios of battery cyclic that additive is not added are only 45%.Therefore, additive of the present invention
Positive electrode can be effectively inhibited to react with organic electrolyte, to prevent positive active material from decaying.
Embodiment 2
By HIGH-PURITY SILICON, polyacrylamide, urea, surfactant (50% glycerine and 50% chloroform) in mixed at high speed
It sufficiently mixed in machine with the revolving speed of 1000rpm, disperse 15min, obtain pre-composition；The quality sum of pre-composition is with 100% mass
Score meter, the then wherein number of components of each raw material are as follows: the mass fraction of HIGH-PURITY SILICON is 10%, and the mass fraction of polyacrylamide is
12%, the mass fraction of surfactant is 8%, and the mass fraction of urea is 70%.Obtained pre-composition is ground with spherical corundum
It after frosted is in the ratio mixing of 1:1, is added in the grinding tank body of high speed star lapping machine, grinding tank body carries out at vacuum sealing
It is ground after reason.It adjusts the revolving speed of master to rotate with the revolving speed of 550rpm, high speed grinding reacts 5.5h, after the reaction was completed, will
Particle, frosted mixture are obtained by sub-sieve, the coarse granule of frosted and partial size > 0.1 μm is removed, obtains amidated nanometer
Grain.
Amidation particle will be obtained to be added in anode material for lithium-ion batteries in 0.8% ratio, carried out pair with group is not added
Than discovery is discharged by the gas of the battery after addition nano particle in the circulating cycle to be significantly reduced.It effectively prevent positive electrode
Decaying, more not additivated battery pack, which improves, uses time 1000h or more.
Embodiment 3
By HIGH-PURITY SILICON, polyacrylamide, urea, surfactant (isopropanol and furans respectively account for 50%), after melting, in height
It sufficiently mixed in fast mixing machine with the revolving speed of 600rpm, disperse 25min, obtain pre-composition；The quality sum of pre-composition is with 100%
Mass fraction meter, the then wherein number of components of each raw material are as follows: the mass fraction of HIGH-PURITY SILICON is 50%, the mass fraction of polyacrylamide
It is 15%, the mass fraction of surfactant is 5%, and the mass fraction of urea is 30%；By obtained pre-composition and spherical corundum
It after abrasive sand is in the ratio mixing of 2:1, is added in the grinding tank body of high speed star lapping machine, grinding tank body carries out vacuum sealing
It is ground after processing.The revolving speed of master is adjusted to rotate with the revolving speed of 450rpm, high speed grinding reacts 2.5h, after the reaction was completed,
Particle, frosted mixture will be obtained by sub-sieve, the coarse granule of frosted and partial size > 0.1 μm is removed, obtain amidated nanometer
Grain.
Amidation particle will be obtained to be added in anode material for lithium-ion batteries in 0.8% ratio, carried out pair with group is not added
Than by the battery after addition nano particle, temperature is stablized at 45 DEG C or less at work for discovery.
Embodiment 4
By HIGH-PURITY SILICON, polyacrylamide, urea, surfactant (pyridine, n-hexane, glycerol, furans) in mixed at high speed
It sufficiently mixed in machine with the revolving speed of 1200rpm, disperse 10min, obtain pre-composition；The quality sum of pre-composition is with 100% mass
Score meter, the then wherein number of components of each raw material are as follows: the mass fraction of HIGH-PURITY SILICON is 31%, and the mass fraction of polyacrylamide is 9%,
The mass fraction of surfactant is 10%, and the mass fraction of urea is 50%.By obtained pre-composition and spherical corundum abrasive sand
It after the ratio mixing of 0.5:1, is added in the grinding tank body of high speed star lapping machine, grinding tank body carries out vacuum sealing processing
After ground.It adjusts the revolving speed of master to rotate with the revolving speed of 700rpm, high speed grinding reaction 1.5h will be obtained after the reaction was completed
Particle, frosted mixture are obtained by sub-sieve, the coarse granule of frosted and partial size > 0.1 μm is removed, obtains amidated nano particle.
Embodiment 5
By HIGH-PURITY SILICON, polyacrylamide, urea, surfactant (glycerine, 1,3- epoxypentane) in high-speed mixer
In sufficiently mixed with the revolving speed of 900rpm, disperse 30min, obtain pre-composition；The quality sum of pre-composition is with 100% mass fraction
Meter, the then wherein number of components of each raw material are as follows: the mass fraction of HIGH-PURITY SILICON is 45%, and the mass fraction of acrylamide is 15%, surface
The mass fraction of activating agent is 8%, and the mass fraction of urea is 32%.By obtained pre-composition and spherical corundum abrasive sand by 3:1
Ratio mixing after, be added in the grinding tank body of high speed star lapping machine, grinding tank body carry out vacuum sealing processing after carry out
Grinding.The revolving speed of master is adjusted to rotate with the revolving speed of 200rpm, high speed grinding reacts 5.5h, after the reaction was completed, will obtain particle,
Frosted mixture removes the coarse granule of frosted and partial size > 0.1 μm, obtains amidated nano particle by sub-sieve.
Claims (8)
1. a kind of preparation method of lithium battery anode film for additive, it is characterised in that the specific method is as follows:
(1) HIGH-PURITY SILICON, polyacrylamide, urea, surfactant are filled in a high speed mixer with the revolving speed of 600-1200rpm
Divide and mix, disperse 10-30min, obtains pre-composition；The quality sum of pre-composition is in terms of 100% mass fraction, wherein HIGH-PURITY SILICON
Mass fraction is 10 ~ 60%, and the mass fraction of polyacrylamide is 2-25%, and the mass fraction of surfactant is 5-10%, urea
Mass fraction be 10-70%；
(2) pre-composition that step (1) obtains and abrasive sand are added to the grinding of high speed star lapping machine in the ratio of 0.5 ~ 4:1
In tank body, grinding tank body is ground after carrying out vacuum sealing processing, is adjusted the revolving speed of master and is revolved with the revolving speed of 200-750rpm
Turn, 0.5~6h of high speed grinding；
(3) so that step (2) is obtained particle, frosted mixture by sieve, remove frosted, air current classifying removes the thick of partial size > 0.1 μm
Particle obtains amidated nano particle, i.e. lithium battery anode film for additive.
2. a kind of preparation method of lithium battery anode film for additive according to claim 1, it is characterised in that: described high-purity
Silicon is powdered silicon, and particle size distribution is less than 10 μm.
3. a kind of preparation method of lithium battery anode film for additive according to claim 1, it is characterised in that: the height
The granularity of pure powdered silicon is less than 1 μm.
4. a kind of preparation method of lithium battery anode film for additive according to claim 1, it is characterised in that: the table
Face activating agent is isopropanol, pyridine, n-hexane, glycerine, furans, 1,3- epoxypentane, at least two in chloroform.
5. a kind of preparation method of lithium battery anode film for additive according to claim 1, it is characterised in that: the surface
Activating agent is made of isopropanol, glycerine and chloroform.
6. a kind of preparation method of lithium battery anode film for additive according to claim 1, it is characterised in that: described is poly-
Acrylamide, urea powder, surfactant are in advance in the condition heating melting of isolation air.
7. a kind of preparation method of lithium battery anode film for additive according to claim 1, it is characterised in that: described high-purity
In the pre-composition that silicon, polyacrylamide, urea, surfactant form, the mass fraction of HIGH-PURITY SILICON is 50%, polyacrylamide
Mass fraction be 15%, the mass fraction of surfactant is 5%, and the mass fraction of urea is 30%.
8. a kind of lithium battery anode film for additive, it is characterized in that being prepared by any one of the claim 1-7 preparation method
The lithium battery anode film for additive arrived is wrapped by and amidated nano high purity silicon for one kind.
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