CN105591108B - A kind of preparation method of SiOx-C composite materials for negative electrode of lithium ion battery - Google Patents
A kind of preparation method of SiOx-C composite materials for negative electrode of lithium ion battery Download PDFInfo
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- CN105591108B CN105591108B CN201610128926.8A CN201610128926A CN105591108B CN 105591108 B CN105591108 B CN 105591108B CN 201610128926 A CN201610128926 A CN 201610128926A CN 105591108 B CN105591108 B CN 105591108B
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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
- H01M4/58—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
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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
- 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
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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
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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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 is a kind of SiO being used to prepare negative electrode of lithium ion batteryxThe method of C composite.This method, as carbon source, is mixed to get colloidal sol with silicon source, and colloidal sol is poured into culture dish film forming, prepares SiO using citric acidx- C presomas, SiO is made in high-temperature calcination under inert gas atmosphere protection laterxC composite.Repeatability of the invention is strong, and production cost is low, and operating procedure is simple, is suitble to mass production.
Description
Technical field
The present invention relates to the technical fields of lithium ion battery negative material, more particularly to a kind of to be used for negative electrode of lithium ion battery
SiOxThe preparation method of C composite.
Background technology
With the worsening of global environment and the continuous consumption of non-renewable energy resources, we must pay attention to new energy
It develops and utilizes.In the past 20 years, research service life is long, energy density is high, the mechanism of new electrochemical power sources of safety nuisance free is always
The focus of scientific research personnel.The development of battery technology and play important function using to the change of energy resource structure.Lithium ion
Battery has been applied to various mobile devices, such as smart mobile phone, laptop field since its performance is very superior.With
The development for lithium ion battery, can be applied to the high-energy-density in electric vehicle field and energy-accumulating power station field, the long-life, it is low at
This lithium ion battery will be as the emphasis of research.The negative material of lithium ion battery be the key that determine its chemical property because
Element, however the graphite cathode material theoretical capacity of business is only 372mAh/g, it is difficult to meet people to height ratio capacity battery
Demand.Therefore, finding can replace the novel anode material system of graphite imperative.
In various non-carbons negative materials, silicon materials (theoretical capacity is up to 4200mAh/g) with its unique advantage and
Potentiality are expected to become the lithium ion battery negative material with development prospect.However, silicon materials are larger during Li insertion extraction
Volume change can cause the destruction of material structure and mechanical dusting, cause electrode capacity decaying rapid, greatly reduce battery
Cycle performance, to hinder its commercial application.
The problem of for silicium cathode material encountered in commercial application, at present researcher mainly by two methods come
Improve the property of silicium cathode, the i.e. Composite of the nanosizing of scantling and material.Nanosizing is made by reducing particle size
The tension that volume expansion generates is easy release, to prevent Particle Breakage, while shortening lithium ion (Li+) transmission range, accelerate
Transmission speed；But simple nano silicon particles have higher surface energy and defect, macroscopic property is unstable, is easy
Reunite in charge and discharge process, to cause battery capacity rapid decay.And Composite is by nano silicon material and with buffering
The material of function mixes, and forms it into the structures such as physics cladding, on the one hand this structure can buffer silicon volume expansion/contraction and cause
Huge stress effect and nano particle reunion, improve cycle life, on the other hand can improve the conductivity of silicon materials, improve
Its high rate performance.104362315 A of CN report a kind of silicon-carbon composite cathode material low cost preparation method, anti-by magnesium heat
The silica in raw graphite after purification should be restored, the compound of porous silicon and graphite is obtained, then carries out surface cladding, is obtained
Silicon-carbon composite cathode material for lithium ion battery.CN 102694155A report a kind of Si-C composite material and its preparation
Method and the lithium ion battery for using the material preparation.The preparation method of the Si-C composite material includes the following steps：(1) by one
The composite material of silicon dioxide coated nano silicon made from silica, porous carbon basis material, excessive hydrofluoric acid solution are mixed
It closes, obtains the composite material for being compounded with nano-silicon particle between porous carbon basis material hole；(2) it is coated with high molecular polymer
The composite material of nano-silicon particle is compounded between porous carbon basis material hole, under an inert atmosphere, heating obtains porous carbon
The Si-C composite material of ball cladding.CN103441250A reports a kind of lithium rechargeable battery composite negative pole material, it is
Using oxide containing silicon as raw material, with graphite and pitch ball milling mixing, conductive metal salt is added, at high-energy ball milling method and high warm
Reason is prepared.Although the above-mentioned prior art makes the electric conductivity of silica-base material be improved by doped carbon, generally deposit
The shortcomings that be：The Si-C composite material size prepared is larger, is unevenly distributed, and makes to still have volume in charge and discharge process
Swelling, to limit removal lithium embedded performance, the cycle performance of material, and preparation process is complicated, and repeatability is poor, affects silicon
Extensive use of the carbon negative pole material in lithium ion battery.Therefore, exploitation performance is more excellent, stable and preparation process is simple,
To be preferably applied for the preparation of lithium ion battery, this becomes is closed reproducible Si-C composite material by those skilled in the art
The focus of note.
Invention content
It is lacked the purpose of the present invention is, electric conductivity big for silicon based anode material bulk effect of the existing technology are poor
Point, and it is rapid with the lithium ion battery negative material capacity attenuation of its preparation, and cycle life is low and high rate performance is poor lacks
It falls into, it is proposed that a kind of easy-operating SiO that can be used for preparing negative electrode of lithium ion batteryxThe method of C composite.This method is adopted
It uses citric acid as carbon source, is mixed to get colloidal sol with silicon source, and colloidal sol is poured into culture dish film forming, prepares SiOx- C forerunners
Body, SiO is made in high-temperature calcination under inert gas atmosphere protection laterxC composite.Repeatability of the invention is strong, is produced into
This is low, and operating procedure is simple, is suitble to mass production.
Technical scheme is as follows：
A kind of SiO for negative electrode of lithium ion batteryxThe preparation method of C composite, includes the following steps：
Step 1：It by the hydrochloric acid of ethyl orthosilicate (TEOS) and 0.1~2mol/L, is successively dissolved in absolute ethyl alcohol, stirs
Obtain clarification mixed solution；
Wherein, quality compares ethyl orthosilicate：0.1~2mol/L hydrochloric acid：Absolute ethyl alcohol=1：(0.5~4.5)：(1~6)；
Step 2：Citric acid and ethylene glycol are dissolved in deionized water, clarification mixed solution is stirred to get.
Wherein, quality compares citric acid：Ethylene glycol：Deionized water=1:(0.4~4):(2~6)；
Step 3：The solution that step 2 is obtained is poured into the obtained solution of step 1, colloidal sol is obtained after magnetic agitation；
Wherein, molar ratio citric acid：Ethyl orthosilicate=1：(1~6)；
Step 4：Colloidal sol obtained by step 3 is poured into glass culture dish, liquid is made just to be paved with glass culture dish bottom,
Then glass culture dish is placed in drying box or dried at room temperature, form film；Wherein, the thickness of film is 0.1~1mm.
Step 5：Film is taken out from glass culture dish, is placed in mortar and is ground into fine powder, the fine powder after grinding is placed in
High temperature process furnances under argon gas atmosphere are warming up to 800~1400 DEG C with 5~15 DEG C/min, keep the temperature 0.5~3h, carry out high temperature and forge
It burns.Wait for that temperature drops to room temperature to get to SiOxC composite.
Stirring in step one, two and three is specially to be stirred with the rotating speed of 50~400r/min using magnetic stirrer
Mix 30~60min.
The above-mentioned SiO for negative electrode of lithium ion batteryxThe preparation method of C composite, wherein involved raw material
It is commercially available, equipment used and technique are known to those skilled in the art.
Compared with prior art, the method for the present invention has substantive distinguishing features outstanding as follows：
1, SiO of the inventionxC composite, as preparing negative electrode of lithium ion battery, can by the high capacity characteristics of silicon and
The electric conductivity of carbon combines, while the flexibility of carbon can limit Volumetric expansion of the silicon after embedded lithium ion, improve
The cycle performance of material；Its reversible capacity is much larger than the capacity (372mAh/g) of existing common graphite cathode material, and recycles
Performance is stablized.
2, experimental implementation of the invention is simple and practicable, and compared with magnesium reduction process, the present invention prepares composite material institute's used time
Between it is shorter, resulting materials reversible capacities is high, and cost of material is low, safety non-pollution, is suitble to industrialized production.
3, SiO of the inventionxC composite preparation method mainly prepares two colloidal sol, high-temperature calcination steps.Colloidal sol
Silica element loses seldom in high-temperature burning process afterwards so that SiOxPreparing for C composite is reproducible, and performance is stablized.
Compared with prior art, marked improvement possessed by the method for the present invention is as follows：
1, compared with 104362315 A of prior art CN, CN 102694155A, CN103441250A, material in this method
The preparation process of material is simple and practicable, and required cost of material is low, safety non-pollution, and the preparation time of the composite material is short, can weigh
Multiple operability is high, is suitble to industrialized production.
2, the SiO prepared by the present inventionxWhen C composite is as lithium ion battery negative material, in the multiplying power of 0.1C
Under, discharge capacity is 1221mAh/g for the first time, and for cycle after 20 weeks, the specific discharge capacity of battery, can with high up to 830mAh/g
Inverse capacity.
Description of the drawings
The invention will be further described with reference to the accompanying drawings and examples.
Fig. 1 is the SiO obtained by the embodiment of the present invention 1xThe X-ray diffractogram of C composite.
Fig. 2 is the SiO obtained by the embodiment of the present invention 1xFilling when C composite is as lithium ion battery negative material
Discharge curve.
Fig. 3 is the SiO obtained by the embodiment of the present invention 1xFollowing when C composite is as lithium ion battery negative material
Ring performance curve.
Specific implementation mode
Embodiment 1
The first step prepares SiOxC composite：
8.33g ethyl orthosilicates and the 0.1mol/L hydrochloric acid of 16.66g are weighed, is dissolved in 24.99g absolute ethyl alcohols, makes quality
Compare ethyl orthosilicate：0.1mol/L hydrochloric acid：Absolute ethyl alcohol=1：2：3.1h is stirred with 200r/min, in this, as silicon source solution.
The ethylene glycol for weighing 3.8428g citric acids and 5.7642g is dissolved in 15.37g deionized waters, and quality compares citric acid：Ethylene glycol：It goes
Ionized water=1：1.5：4.1h is stirred with 200r/min, in this, as carbon source solution.Molar ratio citric acid：Ethyl orthosilicate=1：
2.Carbon source solution is poured into silicon source solution, 30min is stirred with 200r/min, obtains colloidal sol.Colloidal sol is poured into glass culture dish
In, glass culture dish is placed in and dries 30h at room temperature, forms the film of 0.5mm.Film is taken out from glass culture dish, is set
It is ground into fine powder in mortar, the fine powder after grinding is placed in the high temperature process furnances under argon gas atmosphere, 900 are warming up to 5 DEG C/min
DEG C, 1h is kept the temperature, waits for that temperature drops to room temperature to get to SiOxC composite sample.(wherein, X represents SiOx and is amorphous,
This field is typically considered between x ranging from 0~2)
Fig. 1 is the SiO obtained by the present embodimentxThe X-ray diffractogram of C composite.Prepared product is carried out
XRD (XRD, smart Lab, the production of Rigaku company) is analyzed, as can be seen from the figure SiOxOne is presented at 20 ° or so by-C
The diffraction maximum of steamed bun shape, shows SiOxThe amorphous feature of C composite.
Second step, the preparation of battery cathode sheet and the assembling of half-cell：
By SiO obtainedxC composite is 8: 1 according to mass ratio with conductive agent acetylene black and binder Kynoar
: 1 ratio is placed in mortar, and grinding is uniform, then instills N-methyl pyrrolidinone solvent, ground and mixed is at slurry, by slurry
Uniformly blade coating is dried for 24 hours on copper foil, at 55 DEG C, is pushed flakiness in 5MPa pressure using tablet press machine, is obtained negative plate.By institute
Obtain SiOx- C negative plates, metal lithium sheet, battery case, diaphragm, gasket and spring leaf are placed in the glove box full of argon gas and carry out
Battery assembles, and obtains button CR2025 half-cells.
Chemical property analysis (BTS-5V5mA, new prestige) is carried out to prepared sample.Fig. 2 is obtained by the present embodiment
SiOxCharging and discharging curve when-C is as lithium ion battery negative material.It can be seen from the figure that under the multiplying power of 0.1C, warp
After crossing preceding 10 charge and discharge cycles, specific discharge capacity can still keep 877mAh/g.
Fig. 3 is the SiO obtained by the present embodimentxCycle performance curve when-C is as lithium ion battery negative material.From
It can be seen from the figure that, under the multiplying power of 0.1C, discharge capacity is 1221mAh/g for the first time, and cycle is after 20 weeks, SiOxThe reversible appearance of-C
Amount is up to 830mAh/g.The reversible capacity of electrode material significantly improves and stable cycle performance.
Embodiment 2
The first step prepares SiOxC composite：
Silicon source solution, carbon source solution preparation and on glass culture dish form a film the step of with embodiment 1, difference
For resulting materials are warming up to 800 DEG C with 5 DEG C/min, 1h is kept the temperature, waits for that temperature drops to room temperature to get to SiOxC composite sample
Product.
Second step, the preparation of battery cathode sheet and the assembling of half-cell：With embodiment 1.
Products obtained therefrom is all amorphous Si OxC composite；Compared with Example 1, the present embodiment resulting materials are in 0.1C
Multiplying power under, for the first time discharge capacity be 1209mAh/g, by 20 times cycle after, reversible capacity 814mAh/g.
Embodiment 3
The first step prepares SiOxC composite：
Silicon source solution, carbon source solution preparation and on glass culture dish form a film the step of with embodiment 1, difference
For resulting materials are warming up to 1000 DEG C with 5 DEG C/min, 1h is kept the temperature, waits for that temperature drops to room temperature to get to SiOxC composite
Sample.
Second step, the preparation of battery cathode sheet and the assembling of half-cell：With embodiment 1.
Products obtained therefrom is all amorphous Si OxC composite；Compared with Example 1, the present embodiment resulting materials are in 0.1C
Multiplying power under, for the first time discharge capacity be 1216mAh/g, by 20 times cycle after, reversible capacity 821mAh/g.
Embodiment 4
The first step prepares SiOxC composite：
The hydrochloric acid for weighing 8.33g ethyl orthosilicates and the 0.1mol/L of 8.33g is dissolved in 24.99g absolute ethyl alcohols, quality
Compare ethyl orthosilicate：0.1mol/L hydrochloric acid：Absolute ethyl alcohol=1：1：3.1h is stirred with 200r/min, in this, as silicon source solution.
It weighs 2.562g citric acids to be dissolved in 10.248g deionized waters with 5.124g ethylene glycol, quality compares citric acid：Ethylene glycol：Go from
Sub- water=1：2：4.1h is stirred with 200r/min, in this, as carbon source solution.Molar ratio citric acid：Ethyl orthosilicate=1：3.Its
He is the same as embodiment 1.
Second step, the preparation of battery cathode sheet and the assembling of half-cell：With embodiment 1.
Products obtained therefrom is all amorphous Si OxC composite；Compared with Example 1, the present embodiment resulting materials are in 0.1C
Multiplying power under, for the first time discharge capacity be 1210mAh/g, by 20 times cycle after, reversible capacity 819mAh/g.
Unaccomplished matter of the present invention is known technology.
Claims (1)
1. a kind of SiO for negative electrode of lithium ion batteryxThe preparation method of C composite, it is characterized in that including the following steps：
Step 1：It by the hydrochloric acid of ethyl orthosilicate (TEOS) and 0.1~2mol/L, is successively dissolved in absolute ethyl alcohol, stirs to get
Clarify mixed solution；
Wherein, quality compares ethyl orthosilicate：0.1~2mol/L hydrochloric acid：Absolute ethyl alcohol=1：(0.5~4.5)：(1~6)；
Step 2：Citric acid and ethylene glycol are dissolved in deionized water, clarification mixed solution is stirred to get；
Wherein, quality compares citric acid：Ethylene glycol：Deionized water=1:(0.4~4):(2~6)；
Step 3：The solution that step 2 is obtained is poured into the obtained solution of step 1, colloidal sol is obtained after magnetic agitation；
Wherein, molar ratio citric acid：Ethyl orthosilicate=1：(1~6)；
Step 4：Colloidal sol obtained by step 3 is poured into glass culture dish, so that liquid is just paved with glass culture dish bottom, then
Glass culture dish is placed in drying box or is dried at room temperature, film is formed；Wherein, the thickness of film is 0.1~1mm；
Step 5：Film is taken out from glass culture dish, is placed in mortar and is ground into fine powder, the fine powder after grinding is placed in argon gas
High temperature process furnances under atmosphere are warming up to 800~1400 DEG C with 5~15 DEG C/min, keep the temperature 0.5~3h, carry out high-temperature calcination, wait for
Temperature drops to room temperature to get to SiOxC composite；
Stirring in step one, two and three is specially to stir 30 using magnetic stirrer with the rotating speed of 50~400r/min
~60min.
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| CN107342407B (en) * | 2017-06-26 | 2019-12-10 | 合肥国轩高科动力能源有限公司 | Porous carbon loaded mesoporous SiO x/C composite anode material and preparation method thereof |
| CN109449423A (en) * | 2018-11-13 | 2019-03-08 | 东莞市凯金新能源科技股份有限公司 | Hollow/porous structure the silicon based composite material of one kind and its preparation method |
| CN114566639A (en) * | 2022-01-17 | 2022-05-31 | 苏州科技大学 | SiO (silicon dioxide)x/C composite material and preparation method and application thereof |
| CN117650245A (en) * | 2024-01-29 | 2024-03-05 | 陕西晶泰新能源科技有限公司 | Lithium battery anode material and preparation method and application thereof |
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| CN103236534B (en) * | 2013-04-24 | 2015-11-11 | 北京科技大学 | A kind of preparation method of lithium ion battery silicon oxide/carbon composite negative pole material |
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| "SiOx-C dual-phase glass for lithium ion battery anode with high capacity and stable cycling performance";pengpeng lv，等;《Journal of power sources》;20150115;第274卷;第543页右栏第2.1节、第544页左栏第3节 * |
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Application publication date: 20160518 Assignee: Heyuan Qiangxin Energy Technology Co.,Ltd. Assignor: SYNERGY INNOVATION INSTITUTE OF GDUT, HEYUAN Contract record no.: X2023980036111 Denomination of invention: A preparation method of SiOx-C composite material for negative electrode of lithium-ion batteries Granted publication date: 20181106 License type: Common License Record date: 20230531 |