CN105185995B - A kind of silicon/carbon/graphite in lithium ion batteries silicon-carbon composite cathode - Google Patents
A kind of silicon/carbon/graphite in lithium ion batteries silicon-carbon composite cathode Download PDFInfo
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- 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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- H01M10/05—Accumulators with non-aqueous electrolyte
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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Abstract
The invention discloses a kind of silicon/carbon/graphite in lithium ion batteries silicon-carbon composite cathode, it is characterised in that:Material layer including conducting base and coated in conducting base surface, the material layer include a graphite material and a silica-base material layer.The advantage of the invention is that:Each layer interior mechanics property of this lamination anode of the present invention is consistent with the swelling properties in charge and discharge process, is conducive to the stability of holding electrode;The thickness of each material layer of the present invention is extremely easy to control in coating procedure, easy to regulate and control the specific capacity of electrode and first coulombic efficiency;Present invention process is simple, easy to operate, it is not necessary to existing equipment is transformed, is adapted to industrialized production.
Description
Technical field
The present invention relates to a kind of battery technology field, and in particular to a kind of silicon/carbon/graphite in lithium ion batteries-silicon-carbon composite cathode.
Background technology
Compared with lead-acid battery, nickel-cadmium cell, Ni-MH battery, lithium ion battery possesses energy density height, and specific capacity is big, follows
Ring service life is grown, advantages of environment protection, in mobile phone, laptop, digital camera and digital video camera products
To being widely applied.At present, the performance of lithium ion battery can preferably meet the needs of compact electric apparatus, and in electric automobile
In the application of energy storage device, lithium ion battery still suffers from huge challenge.Therefore, high performance lithium ion battery is developed
Active material, the development and application to various lithium ion batteries are most important.Silicon based anode material is due to high power capacity, low deintercalation
Lithium voltage is low with electrolyte reactivity, advantages of environment protection, is expected to become replacement commercialized graphite cathode material at present
Material.But silicon based anode material, among practical application, low conductivity and huge bulk effect due to itself, cause material
Structural breakdown and come off during removal lithium embedded with collector so that cyclical stability declines rapidly.Although the silicon substrate in report
Negative material has higher specific capacity, but cyclical stability is all poor.
Research shows that it is one of method for effectively improving silicon based anode material cycle performance to prepare Si-C composite material.Mesh
The Si-C composite material of preceding exploitation is often respectively provided with specific capacity and preferable cyclical stability higher than 1500mAh/g.But its
Efficiency is often below 75% first, this can largely consume the lithium in electrolyte and positive electrode;The silicon-carbon of high capacity is born at the same time
Pole, its thickness of electrode is often smaller to be mismatched with positive plate thickness.Therefore in actual use, Si-C composite material often adds
It is added in existing graphite negative electrodes material, to meet present battery industry to anode coulombic efficiency first, cyclical stability and height
The requirement of capacity.Si-C composite material is mainly directly added to graphite-like and born by the preparation method of current this kind of anode in proportion
In the material paste of pole, drying is then coated, traditional mixed electrode is made.For the less low capacity silicon-carbon of bulk effect
Composite material, this method are feasible.But this traditional method is not particularly suited for the silicon carbon material of high power capacity.It is because high
The bulk effect of capacity silicon carbon material is significantly greater than graphite negative electrodes material, this will result in silicon carbide particles in mixed electrode and
Degrees of expansion of the graphite particle in process of intercalation is inconsistent, and then causes electrodes crack, crushes, and finally loses active material
It is living, cause cyclical stability poor.
CN101373826A discloses a kind of silicon of the material layer including conducting base and coated on the conducting base surface
Anode, wherein, material layer includes at least two conductive material layers and at least one silica-base material layer, and conductive material layer, which is attached to, leads
On electric matrix, and the silica-base material layer and conductive material layer are spaced, and silica-base material layer is located at two conductive material layers
It is middle.Although this method has preferable cycle performance, due to the nonactive conductive material layer of multilayer, the specific capacity of electrode
Still need to be further improved;At least two conductive layers add coating number and cost at the same time.CN101393980A discloses one
Kind carbon material is attached on conducting base, and silicon layer is attached to the silicium cathode on carbon material layer.Silicon layer in this method is to pass through magnetic
The method of control sputtering ion plating is attached to carbon material layer, and its preparation method is high to equipment requirement, of high cost, is unfavorable for industrializing
Large-scale production, while the presence of pure silicon layer is unfavorable for alleviating the volumetric expansion of silicon, and dusting rupture can occur in long-term circulation.
The content of the invention
It is an object of the invention to cannot take into account height ratio capacity, high coulombic efficiency first for existing silicium cathode and well follow
A kind of the defects of ring stability, there is provided lithium ion battery stone with high specific capacity, first coulombic efficiency and cyclical stability
Ink-silicon-carbon composite cathode.
To achieve the above object, the technical scheme is that:A kind of silicon/carbon/graphite in lithium ion batteries-silicon-carbon composite cathode, its
Innovative point is:Material layer including conducting base and coated in conducting base surface, the material layer include a graphite material
The bed of material and a silica-base material layer.
Further, the graphite material is attached on conducting base, and silica-base material layer is attached on graphite material.
Further, the silica-base material layer is attached on conducting base, and graphite material is attached on silica-base material layer.
Further, the mass ratio of graphite cathode material and silicon based anode material in the material layer on the conducting base surface
For 30-1:1-10.
Further, the graphite material is the mixture of conductive agent, binding agent and graphite cathode material, wherein, lead
Electric agent accounts for gross mass percentage 0-20%, and binding agent accounts for gross mass percentage 5-50%, graphite cathode material 30-95%, the stone
Black negative material is one kind or mixture in natural or artificial graphite.
Further, the silica-base material layer is the mixture of conductive agent, binding agent and silicon based anode material, wherein, lead
Electric agent accounts for gross mass percentage 5-40%, and binding agent accounts for gross mass percentage 5-50%, silicon based anode material 10-90%, the silicon
One or more of mixing of the base negative material in silicon-carbon, silicon and silicon alloy.
Further, the binding agent is polytetrafluoroethylene (PTFE), polyvinylidene fluoride, butadiene-styrene rubber, polyacrylic acid, fiber
One or more of mixing in plain based polyalcohol, sodium alginate and guar gum.
Further, the conductive agent is one or more of mixing in carbon fiber, carbon nanotubes, acetylene black.
Beneficial effects of the present invention are as follows:
(1)Each layer interior mechanics property of this lamination anode of the present invention is consistent with the swelling properties in charge and discharge process,
Be conducive to the stability of holding electrode.
(2)The thickness of each material layer of the present invention is extremely easy to control in coating procedure, easy to regulate and control the specific capacity of electrode
Coulombic efficiency first.
(3)Present invention process is simple, easy to operate, it is not necessary to existing equipment is transformed, is adapted to industrialized production.
Embodiment
Embodiments of the present invention are illustrated by particular specific embodiment below, those skilled in the art can be by this explanation
Content disclosed by book understands other advantages and effect of the present invention easily.
Embodiment 1
It is prepared by Si-C composite material
Under Ar gas shieldeds, SiO is put into tube furnace, is warming up to 1100 DEG C with the heating rate of 10 DEG C/min, and protect
When temperature 5 is small, then Temperature fall;When temperature drops to room temperature, sample is taken out.By the mixed of the sample dispersion of taking-up to water and ethanol
Close in solution, the volume of ethanol accounts for 5%, adds the hafnium of 40wt%, then place 3 it is small when removing SiO2;Centrifugation obtains product
Porous Si, when being put into that 60 DEG C of dryings 4 are small in vacuum drying oven;Obtained porous Si is put into tube furnace, in H2/ Ar gaseous mixtures
800 DEG C are warming up under protection, at this moment closes H2/ Ar gaseous mixtures are simultaneously passed through acetylene/argon gas gaseous mixture holding 10 minutes, are then shut off
Acetylene gas, be passed through H2/ Ar gaseous mixtures, are naturally cooling to room temperature and obtain Si-C composite material.
By 80wt% graphite cathode materials, when the acetylene black stirring 2 of the adhesive polyacrylic acid and 10wt% of 10wt% is small, obtain
To uniformly mixed slurry;Then, slurry is uniformly coated on copper foil, is placed in 70oDrying is vacuumized in C vacuum drying ovens
12 it is small when, you can obtain graphite cathode, its active matter load capacity is 1.2mg/cm2;By 80wt% silicon carbon materials, the bonding of 10wt%
The acetylene black of agent polyacrylic acid and 10wt% stir 2h, obtain uniformly mixed slurry;Slurry is uniformly coated on graphite cathode
On, it is placed in 70oVacuumized in C vacuum drying ovens dry 12 it is small when;Gained graphite-silicium cathode active material load capacity is 1.6mg/
cm2;Dried pole piece passes through tabletting, then the circular pole piece with punch punching into 12 mm of diameter;Then pole piece is positioned over
80oIn the vacuum drying oven of C, when drying 6 is small.Then weighed with precision balance:Weigh after blank copper foil is beaten piece, calculating difference,
The 80% of difference is the quality of active material on electrode slice.
The lithium ion battery of 1 gained sample of example carries out charge-discharge test under 0.01-3V, the current density of 200mA/g,
Efficiency is 88.3% first for it, and effective specific capacity is 711mAh/g, and effectively specific capacity is 697mAh/g after 100 circulations.
Comparative example 1:
It is 3 in mass ratio:1 ratio silicon carbon material and graphite cathode material is uniform with mortar grinder first, is active matter
Matter.By 80wt% electrode active materials, when the acetylene black stirring 2 of the adhesive polyacrylic acid and 10wt% of 10wt% is small, mixed
Uniform slurry.Then, slurry is uniformly coated on copper foil, is placed in 70oVacuumized in C vacuum drying ovens dry 12 it is small when.
Dried pole piece passes through tabletting, then the circular pole piece with punch punching into 12 mm of diameter.Pole piece is then positioned over 80oC's
In vacuum drying oven, dry 6 h.Then weighed with precision balance:Weigh after blank copper foil is beaten piece, calculating difference, the 80% of difference
The quality of active material as on electrode slice.
The lithium ion battery of 1 gained sample of comparative example carries out charge and discharge electrical measurement under 0.01-3V, the current density of 200mA/g
Examination, efficiency is 79% first for it, and effective specific capacity is 689mAh/g, and effectively specific capacity is 569 mAh/g after 100 circulations.
Embodiment 2:
By 80wt% silicon carbon materials, the adhesive polyacrylic acid of 10wt% and the acetylene black of 10wt% stir 2 h, are mixed
Uniform slurry.Slurry is uniformly coated on copper-foil conducting electricity, is placed in 70oVacuumized in C vacuum drying ovens dry 12 it is small when,
Both silicon-based anode is obtained, its active matter load capacity is 0.8mg/cm2.By 80wt% graphite cathode materials, the adhesive poly- third of 10wt%
When the acetylene black of olefin(e) acid and 10wt% stirring 2 is small, uniformly mixed slurry is obtained.Then, slurry is uniformly coated on silicon substrate to bear
On extremely, 70 are placed inoVacuumized in C vacuum drying ovens dry 12 it is small when, you can obtain graphite cathode, gained graphite-silicium cathode activity
Material load capacity is 1.2mg/cm2.Dried pole piece passes through tabletting, then the circular pole piece with punch punching into diameter 12mm.
Pole piece is then positioned over 80oIn the vacuum drying oven of C, when drying 6 is small.
The lithium ion battery of 2 gained sample of example carries out charge-discharge test under 0.01-3V, the current density of 200mA/g,
Efficiency is 83% first for it, and effective specific capacity is 1180mAh/g, and effectively specific capacity is 1080mAh/g after 100 circulations.
Embodiment 3:
Graphite-silicon lamination anode is prepared according to embodiment 1, difference is that silicon based anode material used is less than for particle diameter
The mass ratio of the nano silica fume of 50nm, graphite and silica-base material is 30:1, binding agent used is butadiene-styrene rubber.3 gained sample of example
The lithium ion battery of product carries out charge-discharge test under 0.01-3V, the current density of 200mA/g, and efficiency is 87% first for it, is had
Effect specific capacity is 403mAh/g, and effectively specific capacity is 380mAh/g after 100 circulations.
Embodiment 4:
Graphite-silicon lamination anode is prepared according to embodiment 1, difference is that the mass ratio of graphite and silica-base material is 1:
10, binding agent used is guar gum.The lithium ion battery of 4 gained sample of example is in 0.01-3V, the current density of 200mA/g
Lower carry out charge-discharge test, efficiency is 80% first for it, and effective specific capacity be 1780mAh/g, effective specific capacity after circulating for 100 times
For 1580mAh/g.
Embodiment 5:
Graphite-silicon lamination anode is prepared according to embodiment 1, difference is binding agent polyacrylic acid, and conductive agent is used
Carbon nanotubes.The lithium ion battery of 5 gained sample of example carries out charge and discharge electrical measurement under 0.01-3V, the current density of 200mA/g
Examination, efficiency is 83% first for it, and effective specific capacity is 678mAh/g, and effectively specific capacity is 534mAh/g after 100 circulations.
Embodiment 6:
Graphite-silicon lamination anode is prepared according to embodiment 1, difference is binding agent sodium alginate, and conductive agent is used
Carbon fiber.The lithium ion battery of 6 gained sample of example carries out charge-discharge test under 0.01-3V, the current density of 200mA/g,
Efficiency is 79% first for it, and effective specific capacity is 656mAh/g, and effectively specific capacity is 561mAh/g after 100 circulations.
Embodiment 7:
Graphite-silicon lamination anode is prepared according to embodiment 1, difference is binding agent polyvinylidene fluoride, conductive
Agent acetylene black.The lithium ion battery of 6 gained sample of example carries out charge and discharge electrical measurement under 0.01-3V, the current density of 200mA/g
Examination, efficiency is 79% first for it, and effective specific capacity is 677mAh/g, and effectively specific capacity is 556mAh/g after 100 circulations.
Embodiment 8:
Graphite-silicon lamination anode is prepared according to embodiment 1, difference is that the mass ratio of graphite and silica-base material is
25:2, binding agent used is guar gum.The lithium ion battery of 8 gained sample of example is close in 0.01-3V, the electric current of 200mA/g
Degree is lower to carry out charge-discharge test, and efficiency is 81% first for it, and effective specific capacity is 522mAh/g, effective specific volume after 100 circulations
Measure as 479mAh/g.
Embodiment 9:
Graphite-silicon lamination anode is prepared according to embodiment 1, difference is that the mass ratio of graphite and silica-base material is
18:1, binding agent used is guar gum.The lithium ion battery of 9 gained sample of example is close in 0.01-3V, the electric current of 200mA/g
Degree is lower to carry out charge-discharge test, and efficiency is 81% first for it, and effective specific capacity is 456mAh/g, effective specific volume after 100 circulations
Measure as 419mAh/g.
Embodiment 10:
Graphite-silicon lamination anode is prepared according to embodiment 1, difference is that the mass ratio of graphite and silica-base material is
15:1, binding agent used is polyacrylic acid.The lithium ion battery of 10 gained sample of example is close in 0.01-3V, the electric current of 200mA/g
Degree is lower to carry out charge-discharge test, and efficiency is 77% first for it, and effective specific capacity is 467mAh/g, effective specific volume after 100 circulations
Measure as 409mAh/g.
Embodiment 11:
Graphite-silicon lamination anode is prepared according to embodiment 1, difference is that the mass ratio of graphite and silica-base material is 7:
1, binding agent used is polyacrylic acid.The lithium ion battery of 11 gained sample of example is in 0.01-3V, the current density of 200mA/g
Lower carry out charge-discharge test, efficiency is 80% first for it, and effective specific capacity be 678mAh/g, effective specific capacity after circulating for 100 times
For 603mAh/g.
Embodiment 12:
Graphite-silicon lamination anode is prepared according to embodiment 1, difference is that the mass ratio of graphite and silica-base material is 1:
3, binding agent used is polyacrylic acid.The lithium ion battery of 12 gained sample of example is in 0.01-3V, the current density of 200mA/g
Lower carry out charge-discharge test, efficiency is 81% first for it, and effective specific capacity be 2564mAh/g, effective specific capacity after circulating for 100 times
For 2251mAh/g.
Embodiment 13:
Graphite-silicon lamination anode is prepared according to embodiment 1, difference is that the mass ratio of graphite and silica-base material is 1:
6, silicon raw material is nano silica fume, and binding agent used is polyacrylic acid.The lithium ion battery of 13 gained sample of example in 0.01-3V,
Charge-discharge test is carried out under the current density of 200mA/g, efficiency is 78% first for it, and effective specific capacity is 2998mAh/g, 100
Effective specific capacity is 2766mAh/g after secondary circulation.
Embodiment 14:
Graphite-silicon lamination anode is prepared according to embodiment 1, difference is that the mass ratio of graphite and silica-base material is 1:
8, silicon raw material is nano silica fume, and binding agent used is fiber based polyalcohol.The lithium ion battery of 14 gained sample of example is in 0.01-
Charge-discharge test is carried out under the current density of 3V, 200mA/g, efficiency is 76% first for it, and effective specific capacity is 3012mAh/g, one
Effectively specific capacity is 2813mAh/g after hundred circulations.
Embodiment 15:
Graphite-silicon lamination anode is prepared according to embodiment 1, difference is that the mass ratio of graphite and silica-base material is 1:
9, silicon raw material is nano silica fume, and binding agent used is fiber based polyalcohol.The lithium ion battery of 13 gained sample of example is in 0.01-
Charge-discharge test is carried out under the current density of 3V, 200mA/g, efficiency is 73% first for it, and effective specific capacity is 2967mAh/g, one
Effectively specific capacity is 2678mAh/g after hundred circulations.
Above-described embodiment is presently preferred embodiments of the present invention, is not the limitation to technical solution of the present invention, as long as
The technical solution that can be realized without creative work on the basis of above-described embodiment, is regarded as falling into patent of the present invention
Rights protection scope in.
Claims (3)
- A kind of 1. silicon/carbon/graphite in lithium ion batteries-silicon-carbon composite cathode, it is characterised in that:Including conducting base and coated in conductive base The material layer in body surface face, the material layer include a graphite material and a silica-base material layer;It is prepared by Si-C composite material Method is as follows:Under Ar gas shieldeds, SiO is put into tube furnace, 1100 DEG C are warming up to the heating rate of 10 DEG C/min, And keep the temperature5 it is small when, then Temperature fall;When temperature drops to room temperature, sample is taken out;By in the mixed solution of the sample dispersion of taking-up to water and ethanol, the volume of ethanol accounts for 5%, adds the hafnium of 40wt%, then Place 3 it is small when removing SiO2;Centrifugation obtains the porous Si of product, when being put into that 60 DEG C of dryings 4 are small in vacuum drying oven;It will obtain Porous Si be put into tube furnace, in H2/ Ar is mixedClose and be warming up to 800 DEG C under the protection of gas, at this moment close H2/ Ar gaseous mixtures are simultaneously passed through acetylene/argon gas gaseous mixture holding 10 Minute, it is then shut off acetylene gas, is passed through H2/ Ar gaseous mixtures, are naturally cooling to room temperature and obtain Si-C composite material;By 80wt% Graphite cathode material, when the acetylene black stirring 2 of the adhesive polyacrylic acid and 10wt% of 10wt% is small, obtains uniformly mixed Slurry;Then, slurry is uniformly coated on copper foil, be placed in 70 DEG C of vacuum drying ovens vacuumize dry 12 it is small when, you can obtain Graphite cathode is obtained, its active matter load capacity is 1.2mg/cm2;By 80wt% silicon carbon materials, the adhesive polyacrylic acid of 10wt% 2h is stirred with the acetylene black of 10wt%, obtains uniformly mixed slurry;Slurry is uniformly coated on graphite cathode, is placed in 70 Vacuumized in DEG C vacuum drying oven dry 12 it is small when;Gained graphite-silicium cathode active material load capacity is 1.6mg/cm2 。
- A kind of 2. silicon/carbon/graphite in lithium ion batteries-silicon-carbon composite cathode according to claim 1, it is characterised in that:It is described to lead The mass ratio of graphite cathode material and silicon based anode material is 30-1 in the material layer of electric matrix surface:1-10.
- A kind of 3. silicon/carbon/graphite in lithium ion batteries-silicon-carbon composite cathode according to claim 1, it is characterised in that:The graphite Material layer is the mixture of conductive agent, binding agent and graphite cathode material, wherein, conductive agent accounts for gross mass percentage 10%, bonds Agent accounts for gross mass percentage 10%, graphite cathode material 80%, and the graphite cathode material is in natural or artificial graphite One kind or mixture.
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CN105633346A (en) * | 2016-04-01 | 2016-06-01 | 中国科学技术大学 | Silicon anode of lithium-ion battery and preparation method of silicon anode and lithium-ion battery |
CN107565117B (en) * | 2017-09-08 | 2023-01-31 | 广东猛狮新能源科技股份有限公司 | Silicon/graphite composite negative electrode material and preparation method thereof |
CN114784225A (en) * | 2022-05-27 | 2022-07-22 | 华中科技大学 | Composite cathode structure and application thereof in lithium ion battery |
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