CN106159227A - silicon-carbon composite lithium ion battery cathode material and preparation method thereof - Google Patents
silicon-carbon composite lithium ion battery cathode material and preparation method thereof Download PDFInfo
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- CN106159227A CN106159227A CN201610600122.3A CN201610600122A CN106159227A CN 106159227 A CN106159227 A CN 106159227A CN 201610600122 A CN201610600122 A CN 201610600122A CN 106159227 A CN106159227 A CN 106159227A
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention provides a kind of silicon-carbon composite lithium ion battery cathode material and preparation method thereof, material includes the cobalt/cobalt oxide outside substrate, substrate, the carbon-coating outside cobalt/cobalt oxide, substrate is micron silicon, nano-silicon or porous silicon, and cobalt/cobalt oxide is selected from cobalt oxide, cobalt sesquioxide or Cobalto-cobaltic oxide；Preparation method includes step: prepare silica flour, is joined by silica flour in alkali salt solution and mixes, and adds cobalt salt solution, and washing is dried, calcining, obtains Si/CoxOyPowder；By Si/CoxOyPowder and carbon source stir, dry, smash to pieces, calcine, and i.e. obtain composite lithium ion battery cathode material Si/CoxOy/C；The present invention is at the surface bag last layer Co of silicon basexOyAfter solve silicon volumetric expansion problem in charge and discharge process, trilaminate material Si/Co wellxOy/ C makes the cycle performance of lithium battery, reversible capacity, high rate performance etc. to get the maximum optimization.
Description
Technical field
The present invention relates to lithium ion battery negative material field, specifically a kind of Si/CoxOy/ C composite lithium ion cell is born
Pole material and preparation method thereof.
Background technology
In recent years, government of various countries has had been lifted to new strategic lattice to attention and the concern of new energy field
Office.China is also emphasizing the development of new energy technology, especially in terms of new-energy automobile, using the development of new-energy automobile as me
One important symbol of state's industrial development.Along with the rapid emergence of China's new-energy automobile, provide dynamic as new-energy automobile
The demand of the lithium battery of power the most greatly adds.Under the overall background complying with whole world situation, the key technology of lithium ion battery
Research also achieves breakthrough progress.Meanwhile, the scientific seminar about lithium ion battery carries out the most in succession, among these
Just there is " 2016 China's lithium electricity industrial technology and the Application meeting " held for representative with China, became in Guangzhou March 31
Merit is held.
The feature that preferably lithium ion battery negative material possesses should have high specific capacity, good chemical stability with
The diffusion coefficient of the compatibility and electric conductivity, lithium ion is bigger, charging-discharging structure change is little, material is easy to get, and preparation technology is simple.
Along with the development of new energy technology, common lithium ion battery cannot meet the demand that people are daily.In order to find out one
Good cycle, reversible capacity height, good rate capability etc. can meet business-like demand, also can meet people's daily life
Need.The author demonstrates this Si/Co through repeatedly trialxOy/ C composite has as lithium ion battery negative material
Advantage.First be that silicon reserves on earth are very abundant, price is relatively low, environmental protection and be prone to excellent with other Material cladding etc.
Point.Si/CoxOyThis composite of/C has many good qualities as lithium cell cathode material, first just solves silicon at charge and discharge process
In volumetric expansion problem, owing to the volumetric expansion of silicon causes the pulverizing of active substance, cause reversible capacity to be substantially reduced, destroy
The cycle performance of lithium battery.Bag last layer CoxOyAfter can solve this problem well, secondly be coated with last layer at outermost layer
Amorphous carbon, can optimize its electric conductivity.Find through experiment, the cycle performance of lithium battery after trilaminate material is compound, can
Inverse capacity, high rate performance etc. can get the maximum optimization.
Summary of the invention
The shortcoming of prior art in view of the above, it is an object of the invention to provide a kind of silicon-carbon composite lithium ion cell
Negative material, described material includes the cobalt/cobalt oxide outside substrate, substrate, the carbon-coating outside cobalt/cobalt oxide, and described substrate is 1-
The micron silicon of 10um or 20-100nm nano-silicon or porous silicon, described cobalt/cobalt oxide selected from cobalt oxide, cobalt sesquioxide or
Cobalto-cobaltic oxide.
It is a further object to provide the preparation side of a kind of described silicon-carbon composite lithium ion battery cathode material
Method, comprises the steps:
(1) micron silicon of 1-10um or 20-100nm nano-silicon or porous silicon are prepared as silica flour；
(2) above-mentioned silica flour is joined mix homogeneously in alkali salt solution, be subsequently adding cobalt salt solution, wherein Elements C o:OH-
Mol ratio be 1:2, under vacuum state stirring reaction, be washed out being dried, the powder obtained after drying calcined,
Si/CoxOyPowder；
(3) by Si/CoxOyPowder and carbon source mix and blend, then dry, smash to pieces, calcine, and i.e. obtains compound lithium ion electricity
Pond negative material Si/CoxOy/C。
It is preferred that, described alkali salt solution is selected from ammonia, sodium hydroxide, potassium hydroxide.
It is preferred that, described cobalt salt solution is selected from cobalt nitrate, cobaltous sulfate, cobaltous chloride.
It is preferred that, described carbon source is selected from glucose, graphite, PVDF, Graphene.It is former that the effect of carbon source is to provide C
Son.
It is preferred that, the mass ratio of described carbon source and silica flour is 2:10.It is demonstrated experimentally that the property that such ratio is made
Can be optimum.
It is preferred that, the powder obtained after drying is calcined under nitrogen, oxygen or air atmosphere by step (2).
Cobalt powder is calcined in a nitrogen atmosphere and is obtained cobalt oxide, and under oxygen atmosphere, calcining obtains cobalt sesquioxide, forges in air atmosphere
Burning obtains Cobalto-cobaltic oxide.In step (2), heating rate is 5 DEG C/min, and the condition of high temperature lower persistent period is 1h.So it is easier to
Form the oxide of the cobalt of single-phase
It is preferred that, OH in alkali salt solution-Molar concentration is 0.0125mol/L～0.05mol/L.It is demonstrated experimentally that
Such concentration best performance.
It is preferred that, in cobalt salt solution, the molar concentration of Elements C o is 0.0313mol/L～0.125mol/L.Experiment
Prove, such concentration best performance.
It is preferred that, the porous silicon in described step (1) is: hole size be 10nm～30nm micron silicon or
Person's hole size is the nano-silicon of 0.5nm～2nm.
If silicon power raw material is more than the size required, can be by vibration at high speed ball mill by the size reduction of silicon raw material, will
Micron silicon wears into nano level silicon, then silicon raw material carries out nanorize, or is made by silicon raw material by the method for chemical etching
The silicon of loose structure.Wherein the nanorize of silicon is divided into zero dimension (nano silicon particles), one-dimensional (silicon nanowires or nanotube), two wieners
Rice silicon (silicon nano thin-film).
Step (1) uses silica-based be the negative material that known capacity is the highest as negative material, theoretical capacity is
High up to 4200mA h g-1, and the electromotive force of lithium ionic insertion/deinsertion is the lowest, is especially suitable for doing lithium ion battery negative material.
When the ball mill used carries out ball milling to silicon raw material, the volume adding silicon raw material does not exceeds the 1/3 of ball grinder, enters
The granularity of the silicon raw material entering ball grinder can not be more than 1mm.
Nano-silicon zero dimension (silicon nanoparticle) has huge specific surface area, can suppress the volume that Lithium-ion embeding causes
Expand.Plus the carbon of outermost layer cladding, the electric conductivity of active material can be strengthened, improve cyclical stability.
Nano-silicon one-dimensional (silicon nanowires or nano-tube) with direct growth on a current collector, can reduce its volumetric expansion
Rate.Owing to every nano wire all grows on a current collector, therefore it has good electric conductivity.
Nano-silicon two dimension (silicon nano thin-film) contains less interface relative to silicon nanoparticle, and electric charge is more prone to pass
Lead, there is higher coulombic efficiency.
The invention have the benefit that silicon reserves on earth are very abundant, price is relatively low, environmental protection, it is easy to
Other Material cladding, but the volumetric expansion of silicon can cause the pulverizing of active substance, causes reversible capacity to be substantially reduced and then broken
The cycle performance of bad lithium battery, the present invention is at the surface bag last layer Co of silicon basexOyAfter solve silicon well in discharge and recharge
Volumetric expansion problem in journey, improves the cycle performance of battery, and reversible capacity is high, good rate capability, at the outermost layer of material
It is coated with its electric conductivity of the laggard one-step optimization of last layer amorphous carbon.Finding through experiment, trilaminate material Si/CoxOy/C makes lithium
The cycle performance of battery, reversible capacity, high rate performance etc. can get the maximum optimization.
Accompanying drawing explanation
Fig. 1 is the silica flour raw-material SEM figure of micron-scale.
Fig. 2 is the silica flour raw-material SEM figure of loose structure.
Fig. 3 is the Si/Co that step of the present invention (2) is prepared afterwardsxOySEM figure.
Fig. 4 is the Si/Co that step of the present invention (2) is prepared afterwardsxOyEDS figure.
Fig. 5 is the Si/Co that the present invention finally preparesxOyThe SEM figure of/C composite.
Fig. 6 is the Si/Co that the present invention finally preparesxOyThe EDS figure of/C composite.
Fig. 7 is the micron porous silicon charging and discharging curve schematic diagram that the present invention records.
Fig. 8 is the nano-structure porous silicon charging and discharging curve schematic diagram that the present invention records.
Fig. 9 is the Co that content is 12% that the present invention recordsxOyThe micron porous silicon charging and discharging curve schematic diagram of coating.
Detailed description of the invention
Below by way of specific instantiation, embodiments of the present invention being described, those skilled in the art can be by this specification
Disclosed content understands other advantages and effect of the present invention easily.The present invention can also be by the most different concrete realities
The mode of executing is carried out or applies, the every details in this specification can also based on different viewpoints and application, without departing from
Various modification or change is carried out under the spirit of the present invention.
Embodiment 1
The preparation method of a kind of silicon-carbon composite lithium ion battery cathode material, comprises the steps:
(1) by vibration at high speed ball mill by the size reduction of silicon raw material, when using ball mill that silicon raw material is carried out ball milling,
The volume adding silicon raw material does not exceeds the 1/3 of ball grinder, and the granularity of the silicon raw material entering ball grinder can not be more than 1mm.By silicon
Raw material is put into the time in high speed ball mill and not can exceed that 1h, 15min to be interrupted.The rotating speed of ball mill cannot be below
900r/min, carries out ball milling by dry method or wet method.The micron silicon of 1-10um is obtained as silica flour after ball milling；
(2) above-mentioned silica flour is joined mix homogeneously in ammonia, OH in ammonia spirit-Molar concentration is 0.0125mol/L.
Being subsequently adding cobalt nitrate solution, in cobalt nitrate solution, the molar concentration of Co is 0.0313mol/L, makes Elements C o:OH-Mol ratio
For 1:2, under vacuum state, stirring reaction, is washed out being dried, is calcined by the powder obtained after drying, obtain Si/CoO powder
End；
(3) by Si/CoO powder and glucose mix and blend, then dry, smash to pieces, calcine in a nitrogen atmosphere, i.e. obtain
Composite lithium ion battery cathode material Si/CoO/C.The mass ratio of described carbon source and silica flour is 2:10.It is demonstrated experimentally that such ratio
The best performance that example is made.
The silicon-carbon composite lithium ion battery cathode material that said method obtains, described material includes outside substrate, substrate
CoO、CoCarbon-coating outside O, described substrate is the micron silicon of 1-10um.
Embodiment 2
The preparation method of a kind of silicon-carbon composite lithium ion battery cathode material, comprises the steps:
(1) silicon raw material is carried out nanorize, the nanorize of silicon be divided into zero dimension (nano silicon particles), one-dimensional (silicon nanowires or
Nanotube), two-dimensional nano silicon (silicon nano thin-film).Nano-silicon zero dimension (silicon nanoparticle) has huge specific surface area, permissible
The volumetric expansion that suppression Lithium-ion embeding causes.Plus the carbon of outermost layer cladding, the electric conductivity of active material can be strengthened, improve
Cyclical stability.Nano-silicon one-dimensional (silicon nanowires or nano-tube) with direct growth on a current collector, can reduce its volume
Expansion rate.Owing to every nano wire all grows on a current collector, therefore it has good electric conductivity.Nano-silicon two dimension (receive by silicon
Rice thin film) contain less interface relative to silicon nanoparticle, electric charge is more prone to conduction, has higher coulombic efficiency.?
After obtain 20-100nm nano-silicon as silica flour；
(2) above-mentioned silica flour is joined mix homogeneously in sodium hydroxide solution, OH in sodium hydroxide solution-Molar concentration is
0.05mol/L, is subsequently adding cobalt sulfate solution, and in cobalt sulfate solution, the molar concentration of Elements C o is 0.125mol/L, makes element
Co:OH-Mol ratio be 1:2, under vacuum state, stirring reaction, is washed out being dried, by the powder that obtains after drying at oxygen
Calcine under atmosphere, obtain Si/Co2O3Powder；
(3) by Si/Co2O3Powder and graphite mix and blend, then dry, smash to pieces, calcine, and i.e. obtains compound lithium ion electricity
Pond negative material Si/Co2O3/C.The mass ratio of described carbon source and graphite is 2:10.It is demonstrated experimentally that the property that such ratio is made
Can be optimum.
The silicon-carbon composite lithium ion battery cathode material that said method obtains, described material includes outside substrate, substrate
Co2O3、Co2O3Outside carbon-coating, described substrate is 20-100nm nano-silicon, and described cobalt/cobalt oxide is cobalt sesquioxide.
Embodiment 3
The preparation method of a kind of silicon-carbon composite lithium ion battery cathode material, comprises the steps:
(1) silicon raw material is made the silica flour of loose structure by the method for chemical etching, and described silica flour is: hole size is
The micron silicon of 10nm～30nm or the nano-silicon that hole size is 0.5nm～2nm.
(2) above-mentioned silica flour being joined mix homogeneously in potassium hydroxide solution, in potassium hydroxide solution, OH-molar concentration is
0.035mol/L, is subsequently adding cobalt chloride solution, and in cobalt chloride solution solution, the molar concentration of Elements C o is 0.065mol/L, makes
The mol ratio of Elements C o:OH-is 1:2, stirring reaction under vacuum state, and washing is dried the most afterwards, the powder that will obtain after drying
Calcine in air atmosphere, obtain Si/Co3O4Powder；
(3) by Si/Co3O4Powder and PVDF mix and blend, the time of stirring is 1h.Then dry, smash to pieces, calcine, calcining
Temperature cannot be below 500 DEG C, the persistent period is 6h.I.e. obtain composite lithium ion battery cathode material Si/Co3O4/C.Described carbon
The mass ratio of source and PVDF is 2:10.It is demonstrated experimentally that the best performance that such ratio is made.
The silicon-carbon composite lithium ion battery cathode material that said method obtains, described material includes outside substrate, substrate
Co3O4、Co3O4Outside carbon-coating, described substrate is porous silicon.
Fig. 7 is the etched micron porous silicon half-cell charging and discharging curve as anelectrode.Can be seen that and put for the first time
Electricity capacitance is 3020mAh g-1, compared with the half-cell made as anelectrode with the micron silicon not etched, electric discharge electricity for the first time
Capacity adds 700mAh g-1.Capacitance has significantly to be increased this is because etching is allowed to the edge that micron silicon surface area increases
Therefore.
Fig. 8 is the half-cell charging and discharging curve that the silicon of nano-scale is made as anelectrode.Discharge capacity is for the first time
3030mAh·g-1, about add 33% compared with the half-cell charging and discharging curve made as anelectrode with micron silicon.The most such as
This, the half-cell that nano-silicon is made as anelectrode, can also maintain in capacitance after 15 charge and discharge cycles
1200mAh·g-1, this illustrates that the silicon grain of nano-scale is alleviated in charge and discharge process effectively compared to micron-sized silicon
The expansion issues of silicon materials.
Fig. 9 is the Co of content 12%xOyThe micron porous silicon charging and discharging curve of coating.Discharge capacity is for the first time
3600mAh·g-1, compared with the half-cell charging and discharging curve made as anelectrode with micron porous silicon, discharge capacity has substantially
Increase and inducing capacity fading rate significantly decrease.This illustrates the Co of 12%xOyThe micron porous silicon modified can effectively reduce
The feature that silicon materials inducing capacity fading in charge and discharge process is serious.
The principle of above-described embodiment only illustrative present invention and effect thereof, not for limiting the present invention.Any ripe
Above-described embodiment all can be modified under the spirit and the scope of the present invention or change by the personage knowing this technology.Cause
This, have usually intellectual and completed under technological thought without departing from disclosed spirit in all art
All equivalence modify or change, must be contained by the claim of the present invention.
Claims (10)
1. a silicon-carbon composite lithium ion battery cathode material, it is characterised in that: described material includes the cobalt outside substrate, substrate
Carbon-coating outside oxide, cobalt/cobalt oxide, described substrate is the micron silicon of 1-10um or 20-100nm nano-silicon or porous
Silicon, described cobalt/cobalt oxide is selected from cobalt oxide, cobalt sesquioxide or Cobalto-cobaltic oxide.
2. the preparation method of the silicon-carbon composite lithium ion battery cathode material described in claim 1, it is characterised in that include as follows
Step:
(1) micron silicon of 1-10um or 20-100nm nano-silicon or porous silicon are prepared as silica flour；
(2) above-mentioned silica flour is joined mix homogeneously in alkali salt solution, be subsequently adding cobalt salt solution, wherein Elements C o:OH-Rub
Your ratio is 1:2, and under vacuum state, stirring reaction, is washed out being dried, is calcined by the powder obtained after drying, obtain Si/
CoxOyPowder；
(3) by Si/CoxOyPowder and carbon source mix and blend, then dry, smash to pieces, calcine, and i.e. obtains composite lithium ion cell and bears
Pole material Si/CoxOy/C。
The preparation method of silicon-carbon composite lithium ion battery cathode material the most according to claim 2, it is characterised in that: described
Alkali salt solution is selected from ammonia, sodium hydroxide, potassium hydroxide.
The preparation method of silicon-carbon composite lithium ion battery cathode material the most according to claim 2, it is characterised in that: described
Cobalt salt solution is selected from cobalt nitrate, cobaltous sulfate, cobaltous chloride.
The preparation method of silicon-carbon composite lithium ion battery cathode material the most according to claim 2, it is characterised in that: described
Carbon source is selected from glucose, graphite, PVDF, Graphene.
The preparation method of silicon-carbon composite lithium ion battery cathode material the most according to claim 2, it is characterised in that: described
The mass ratio of carbon source and silica flour is 2:10.
The preparation method of silicon-carbon composite lithium ion battery cathode material the most according to claim 2, it is characterised in that: step
(2) in, the powder obtained after drying is calcined under nitrogen, oxygen or air atmosphere.
The preparation method of silicon-carbon composite lithium ion battery cathode material the most according to claim 2, it is characterised in that: alkali salt
OH in solution-Molar concentration is 0.0125mol/L～0.05mol/L.
The preparation method of silicon-carbon composite lithium ion battery cathode material the most according to claim 2, it is characterised in that: cobalt salt
In solution, the molar concentration of Elements C o is 0.0313mol/L～0.125mol/L.
The preparation method of silicon-carbon composite lithium ion battery cathode material the most according to claim 2, it is characterised in that: institute
The porous silicon stated in step (1) is: hole size is the micron silicon of 10nm～30nm or hole size is 0.5nm's～2nm
Nano-silicon.
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| CN108735982A (en) * | 2018-03-31 | 2018-11-02 | 华南师范大学 | Sheet Si oxide and carbon and cobalt black composite material and preparation method |
| CN110943208A (en) * | 2019-12-13 | 2020-03-31 | 成都爱敏特新能源技术有限公司 | Graphite negative electrode material of high-temperature lithium ion battery and preparation method of graphite negative electrode material |
| WO2020187040A1 (en) * | 2019-03-19 | 2020-09-24 | Ningde Amperex Technology Limited | Anode material, and electrochemical device and electronic device using the same |
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| WO2020187040A1 (en) * | 2019-03-19 | 2020-09-24 | Ningde Amperex Technology Limited | Anode material, and electrochemical device and electronic device using the same |
| CN110943208A (en) * | 2019-12-13 | 2020-03-31 | 成都爱敏特新能源技术有限公司 | Graphite negative electrode material of high-temperature lithium ion battery and preparation method of graphite negative electrode material |
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