CN105680013A - Preparation method for silicon/graphite/carbon composite negative electrode material of lithium ion battery - Google Patents
Preparation method for silicon/graphite/carbon composite negative electrode material of lithium ion battery Download PDFInfo
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- CN105680013A CN105680013A CN201610050565.XA CN201610050565A CN105680013A CN 105680013 A CN105680013 A CN 105680013A CN 201610050565 A CN201610050565 A CN 201610050565A CN 105680013 A CN105680013 A CN 105680013A
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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
- 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
-
- 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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- 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
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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 invention discloses a preparation method for a silicon/graphite/carbon composite negative electrode material of a lithium ion battery. The preparation method comprises the following steps of (1) preparing an amorphous carbon source, a dispersing agent, nanometer silicon, graphite and a solvent; (2) dissolving and uniformly dispersing the amorphous carbon source and the dispersing agent in the solvent, adding the nanometer silicon and the graphite into the mixed solution, continuously and uniformly dispersing the mixed solution to obtain a mixture; (3) carrying out mechanical curing or spray drying on the mixture obtained in the step (2) to obtain a negative electrode material precursor; and (4) carrying out calcination on the negative electrode material precursor in an inertia atmosphere to obtain the silicon/graphite/carbon composite negative electrode material. By the negative electrode material obtained according to the preparation method, the volume expansion effect during the cycle process of the battery can be reduced, favorable cycle stability is acquired, and thus, the defects of low reversible capacity and poor cycle lifetime of the silicon-based negative electrode material are overcome.
Description
Technical field
The present invention relates to field of lithium ion battery material, the preparation method particularly relating to a kind of lithium ion battery silicon/graphite/carbon composite negative pole material.
Background technology
Along with the raising of lithium ion battery entirety manufacture level and relevant positive electrode performance, the theoretical limit (372mAh/g) of the lithium ion specific capacity of the carbons negative material being widely used at present has become as development and has both the bottleneck of high-energy-density, high power density, extended-life lithium ion battery. Therefore, Development of Novel in this year negative material starts to become the research emphasis in this field and focus. Wherein the theoretical specific capacity of silicon is up to 4200mAh/g, is significantly larger than existing carbons negative material, causes the special concern of people.
But when elementary silicon is as negative material, owing to the volume of reaction formation is the several times of silicon, therefore in charge and discharge process, negative pole constantly experiences expansion and shrinks, and causes that the reversible capacity of material sharply declines. In order to solve silicon cycling life-span short problem, researcher mixes the inactive elemental of relative lithium in silicon, material expansion in charge and discharge process and contraction can be effectively alleviated in the existence of inactive elemental, thus suppressing the decline of material reversible capacity, improve the cycle life of material. Also having researcher at silica-based middle addition carbons material, the existence of carbon can alleviate silicon Volumetric expansion in charge and discharge process on the one hand further, as active substance, can react with lithium on the other hand, it is provided that extra capacity. But these above-mentioned methods all can not fundamentally solve existing silicon based anode material and there is the shortcoming that reversible capacity is low, cycle life is poor. Therefore seek a kind of preparation process simple, silicon based anode material can be solved and there is the problem that reversible capacity is low, cycle life is poor and be necessary.
Summary of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art, it is provided that the preparation method of a kind of ion battery silicon/graphite/carbon composite negative pole material.
For solving above-mentioned technical problem, the technical scheme that the present invention proposes is:
The preparation method of a kind of lithium ion battery silicon/graphite/carbon composite negative pole material, comprises the following steps:
(1) amorphous carbon source, dispersant, nano-silicon, graphite and solvent are prepared;
(2) amorphous carbon source and dispersant it is dissolved in solvent and is uniformly dispersed, then being added thereto to nano-silicon and graphite, continuing to be uniformly dispersed, obtain mixture;
(3) mixture step (2) obtained solidifies or spray drying through machinery, obtains negative material presoma;
(4) described negative material presoma is calcined in an inert atmosphere, namely obtain described silicon/graphite/carbon composite negative pole material.
Above-mentioned preparation method, it is preferred that in described step (1), amorphous carbon source at least one in glucose, citric acid, phenolic resin, epoxy resin, Lauxite, furane resins, alkyd resin, acrylic resin.
Above-mentioned preparation method, it is preferred that in described step (1), dispersant one in Polyethylene Glycol and polyvinyl alcohol.
Above-mentioned preparation method, it is preferred that in described step (1), nano-silicon, graphite quality ratio is 1: 3～8; The quality of amorphous carbon source accounts for the 7%～12% of nano-silicon and graphite gross mass; The quality of dispersant accounts for the 3%～8% of nano-silicon and graphite gross mass.
Above-mentioned preparation method, it is preferred that the temperature of calcining is 500～2000 DEG C; The time of calcining is 1～24h.
Above-mentioned preparation method, it is preferred that in described step (1), one or more in water, ethanol, propanol, butanol of solvent.
Above-mentioned preparation method, it is preferred that in described step (1), graphite is one or more in spherical graphite, crystalline flake graphite, Delanium.
Compared with prior art, it is an advantage of the current invention that:
(1) preparation method of the present invention, utilizes the layer structure of graphite in raw material can play alleviation silicon-base alloy Volumetric expansion in discharge and recharge engineering; Amorphous carbon can suppress the reunion of granule, nano silica fume is effectively made to be uniformly dispersed in the specific area porous presoma of synthesis, the presoma of final synthesizing high specific surface area porous polymer resin-coating silicon so that bulk effect weakens significantly, and cycle performance is excellent; Then gained presoma is dried; and under protective atmosphere and carry out roasting at specific temperature; alleviate the Volumetric expansion in cyclic process, it is thus achieved that good stable circulation performance, thus solving silicon based anode material there is the defect that reversible capacity is low, cycle life is poor.
(2) agraphitic carbon generated in preparation method process of the present invention can suppress internal silica-based reunion in electrochemistry cyclic process, particle growth effectively; And agraphitic carbon itself has electro-chemical activity, it is provided that extra lithium storage content.
Accompanying drawing explanation
Fig. 1 is the electron-microscope scanning figure of the silicon/graphite/carbon composite negative pole material of the embodiment of the present invention 1 preparation.
Fig. 2 is the XRD figure spectrum of the silicon/graphite/carbon composite negative pole material of the embodiment of the present invention 1 preparation.
Fig. 3 is the charge-discharge performance curve chart that silicon/graphite/carbon composite negative pole material prepared by the embodiment of the present invention 1 makes battery.
Fig. 4 is the electron-microscope scanning figure of the silicon/graphite/carbon composite negative pole material of the embodiment of the present invention 3 preparation.
Fig. 5 is the XRD figure spectrum of the silicon/graphite/carbon composite negative pole material of the embodiment of the present invention 3 preparation.
Fig. 6 is voltage-specific volume spirogram that silicon/graphite/carbon composite negative pole material prepared by the embodiment of the present invention 3 makes battery.
Fig. 7 is the charge-discharge performance curve chart that silicon/graphite/carbon composite negative pole material prepared by the embodiment of the present invention 3 makes battery.
Detailed description of the invention
For the ease of understanding the present invention, below in conjunction with Figure of description and preferred embodiment, the present invention is made more comprehensively, describes meticulously, but protection scope of the present invention is not limited to embodiment in detail below.
Unless otherwise defined, the implication that all technical term used hereinafter is generally understood that with those skilled in the art is identical. Technical term used herein is intended merely to the purpose describing specific embodiment, is not intended to limit the scope of the invention.
Except there being special instruction, the various reagent used in the present invention, raw material are can commodity commercially or can pass through the product that known method prepares.
Embodiment 1:
The preparation method of the lithium ion battery silicon of a kind of present invention/graphite/carbon composite negative pole material, comprises the following steps:
(1) 1:4 weighs nano-silicon and graphite (mixture of spherical graphite and crystalline flake graphite) in mass ratio; Weigh the polyethylene glycol 200 (following shorthand PEG-200) of nano-silicon and the glucose of graphite gross mass 10%, nano-silicon and graphite gross mass 5% again.
(2) glucose and PEG-200 are dissolved in ultra-pure water, add nano-silicon and graphite (mixture of spherical graphite and crystalline flake graphite), stirring at normal temperature 30 minutes, then ultrasonic disperse 2h, be stirred for 2h after ultrasonic, obtain finely dispersed mixture.
(3) finely dispersed mixture step (2) obtained stirs solidification at 80 DEG C and is evaporated and is placed in drying baker dry, obtains negative material presoma.
(4) negative material presoma is placed in argon gas atmosphere (Ar flow is 400mL/min) and rises to 700 DEG C with the heating rate of 5 DEG C/min, then insulation roasting 2h, namely obtain silicon/graphite/carbon composite negative pole material, its electron-microscope scanning figure and XRD diffraction pattern to see respectively shown in Fig. 1 and Fig. 2.
The silicon prepared by the present embodiment/graphite/carbon composite negative pole material prepares into battery, and the charge-discharge performance of test battery, as it is shown on figure 3, the first discharge specific capacity of battery reaches 670.2mAh/g.
Embodiment 2:
The preparation method of the lithium ion battery silicon of a kind of present invention/graphite/carbon composite negative pole material, comprises the following steps:
(1) 1:4 weighs nano-silicon and graphite (mixture of spherical graphite and crystalline flake graphite) in mass ratio; Weigh again nano-silicon and graphite gross mass 10% phenolic resin, nano-silicon and graphite gross mass 5% PEG-200.
(2) phenolic resin and PEG-200 are dissolved in ethanol, add nano-silicon and graphite (mixture of spherical graphite and crystalline flake graphite), stirring at normal temperature 30 minutes, then ultrasonic disperse 2h, be stirred for 2h after ultrasonic, obtain finely dispersed mixture.
(3) finely dispersed mixture step (2) obtained stirs solidification at 80 DEG C and is evaporated and is placed in drying baker dry, obtains negative material presoma.
(4) being placed in by negative material presoma in argon gas atmosphere (Ar flow 400mL/min) and rise to 700 DEG C with the heating rate of 5 DEG C/min, then insulation roasting 2h, namely obtains silicon/graphite/carbon composite negative pole material.
The silicon prepared by the present embodiment/graphite/carbon composite negative pole material prepares into battery, the charge-discharge performance of test battery, the initial charge capacity 624.8mAh/g of battery, and after 50 times circulate, charging capacity still has 503mAh/g.
Embodiment 3:
The preparation method of the lithium ion battery silicon of a kind of present invention/graphite/carbon composite negative pole material, comprises the following steps:
(1) 1:4 weighs nano-silicon and graphite (mixture of spherical graphite and crystalline flake graphite) in mass ratio; Weigh nano-silicon and the PEG-200 of the glucose of graphite gross mass 10%, nano-silicon and graphite gross mass 5% again.
(2) glucose, PEG-200 are dissolved in ultra-pure water, add nano-silicon and graphite (mixture of spherical graphite and crystalline flake graphite), stirring at normal temperature 30 minutes, then ultrasonic disperse 2h, be stirred for 2h after ultrasonic, obtain finely dispersed mixture.
(3) the finely dispersed mixture that step (2) obtains is carried out spray drying, obtain negative material presoma.
(4) negative material presoma is placed in argon gas atmosphere (Ar flow 400mL/min) and rises to 700 DEG C with the heating rate of 5 DEG C/min, then insulation roasting 2h, namely obtains silicon/graphite/carbon composite negative pole material (electron-microscope scanning figure and XRD figure are shown in Fig. 4 and Fig. 5 respectively).
The silicon prepared by the present embodiment/graphite/carbon composite negative pole material prepares into battery, the chemical property of test battery is as shown in Figure 6, Figure 7, the first discharge specific capacity of battery reaches 897.7mAh/g, and after circulation electric discharge in 50 weeks, the specific discharge capacity of battery is 615.6mAh/g.
Embodiment 4:
The preparation method of the lithium ion battery silicon of a kind of present invention/graphite/carbon composite negative pole material, comprises the following steps:
(1) 1:4 weighs nano-silicon and graphite (mixture of spherical graphite and crystalline flake graphite) in mass ratio; Weigh again nano-silicon and the phenolic resin of graphite gross mass 10%, nano-silicon and graphite gross mass 10% PEG-200.
(2) phenolic resin and PEG-200 are dissolved in ethanol, add nano-silicon and graphite (mixture of spherical graphite and crystalline flake graphite), stirring at normal temperature 30 minutes, then ultrasonic disperse 2h, be stirred for 2h after ultrasonic, obtain finely dispersed mixture.
(3) finely dispersed mixture step (2) obtained stirs solidification at 80 DEG C and is evaporated and is placed in drying baker dry, obtains negative material presoma.
(4) being placed in by negative material presoma in argon gas atmosphere (Ar flow 400mL/min) and rise to 700 DEG C with the heating rate of 5 DEG C/min, then insulation roasting 2h, namely obtains silicon/graphite/carbon composite negative pole material.
The silicon prepared by the present embodiment/graphite/carbon composite negative pole material prepares into battery, the charge-discharge performance of test battery, initial charge capacity 624.8mAh/g, after 50 times circulate, and charging capacity 503mAh/g.
Claims (7)
1. the preparation method of lithium ion battery silicon/graphite/carbon composite negative pole material, it is characterised in that comprise the following steps:
(1) amorphous carbon source, dispersant, nano-silicon, graphite and solvent are prepared;
(2) amorphous carbon source and dispersant it is dissolved in solvent and is uniformly dispersed, then being added thereto to nano-silicon and graphite, continuing to be uniformly dispersed, obtain mixture;
(3) mixture step (2) obtained solidifies or spray drying through machinery, obtains negative material presoma;
(4) described negative material presoma is calcined in an inert atmosphere, namely obtain described silicon/graphite/carbon composite negative pole material.
2. preparation method as claimed in claim 1, it is characterised in that in described step (1), amorphous carbon source at least one in glucose, citric acid, phenolic resin, epoxy resin, Lauxite, furane resins, alkyd resin, acrylic resin.
3. preparation method as claimed in claim 1, it is characterised in that in described step (1), dispersant one in Polyethylene Glycol and polyvinyl alcohol.
4. preparation method as claimed in claim 1, it is characterised in that in described step (1), nano-silicon, graphite quality ratio is 1: 3～8;The quality of amorphous carbon source accounts for the 7%～12% of nano-silicon and graphite gross mass; The quality of dispersant accounts for the 3%～8% of nano-silicon and graphite gross mass.
5. preparation method as claimed in claim 1, it is characterised in that in described step (4), the temperature of calcining is 500～2000 DEG C; The time of calcining is 1～24h.
6. the preparation method as described in any one of Claims 1 to 5, it is characterised in that in described step (1), one or more in water, ethanol, propanol, butanol of solvent.
7. the preparation method as described in any one of Claims 1 to 5, it is characterised in that in described step (1), graphite is one or more in spherical graphite, crystalline flake graphite, Delanium.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107275571A (en) * | 2017-08-18 | 2017-10-20 | 华南师范大学 | A kind of full battery of lithium sulfide/nano-silicone wire/carbon and preparation method and application |
| CN108039477A (en) * | 2017-12-20 | 2018-05-15 | 徐会丽 | A kind of composite negative pole material of stabilization and its preparation method and application |
| CN108336342A (en) * | 2018-02-28 | 2018-07-27 | 宁波富理电池材料科技有限公司 | Si/SiOx/C composite negative pole materials, preparation method and lithium ion battery |
| CN109461890A (en) * | 2017-09-06 | 2019-03-12 | 丰域科技（北京）有限公司 | Silicon-carbon cathode material, preparation method and lithium ion battery |
| CN109585794A (en) * | 2017-09-28 | 2019-04-05 | 江苏津谊新能源科技有限公司 | A kind of preparation method of lithium ion battery silicon/graphite/carbon composite negative pole material |
| CN109755509A (en) * | 2018-12-21 | 2019-05-14 | 江苏大学 | A kind of lithium ion battery Si@Nb2O5The preparation method of composite negative pole material |
| CN109935808A (en) * | 2019-02-27 | 2019-06-25 | 福建翔丰华新能源材料有限公司 | A method of silicon-carbon cathode material is prepared based on micron silicon wafer |
| CN110571420A (en) * | 2019-09-09 | 2019-12-13 | 浙江师范大学 | method for synthesizing silicon/graphite/amorphous carbon/conductive carbon black quaternary composite material by using industrial metallurgical silicon |
| CN110931749A (en) * | 2019-12-06 | 2020-03-27 | 天津工业大学 | Aluminum oxide doped silicon/dual-carbon composite negative electrode material and preparation method thereof |
| CN112234179A (en) * | 2020-10-26 | 2021-01-15 | 郑州中科新兴产业技术研究院 | Preparation method of high-capacity silicon-based negative electrode material |
| CN112366294A (en) * | 2020-07-31 | 2021-02-12 | 万向一二三股份公司 | Graphite/silicon/carbon composite negative electrode material and preparation method thereof |
| CN113479890A (en) * | 2021-06-30 | 2021-10-08 | 松山湖材料实验室 | Silicon-based negative electrode material and preparation method and application thereof |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107275571A (en) * | 2017-08-18 | 2017-10-20 | 华南师范大学 | A kind of full battery of lithium sulfide/nano-silicone wire/carbon and preparation method and application |
| CN109461890A (en) * | 2017-09-06 | 2019-03-12 | 丰域科技（北京）有限公司 | Silicon-carbon cathode material, preparation method and lithium ion battery |
| CN109461890B (en) * | 2017-09-06 | 2020-04-28 | 丰域科技（北京）有限公司 | Silicon-carbon negative electrode material, preparation method thereof and lithium ion battery |
| CN109585794A (en) * | 2017-09-28 | 2019-04-05 | 江苏津谊新能源科技有限公司 | A kind of preparation method of lithium ion battery silicon/graphite/carbon composite negative pole material |
| CN108039477A (en) * | 2017-12-20 | 2018-05-15 | 徐会丽 | A kind of composite negative pole material of stabilization and its preparation method and application |
| CN108336342A (en) * | 2018-02-28 | 2018-07-27 | 宁波富理电池材料科技有限公司 | Si/SiOx/C composite negative pole materials, preparation method and lithium ion battery |
| CN108336342B (en) * | 2018-02-28 | 2020-10-13 | 宁波富理电池材料科技有限公司 | Si/SiOx/C composite negative electrode material, preparation method thereof and lithium ion battery |
| CN109755509A (en) * | 2018-12-21 | 2019-05-14 | 江苏大学 | A kind of lithium ion battery Si@Nb2O5The preparation method of composite negative pole material |
| CN109935808A (en) * | 2019-02-27 | 2019-06-25 | 福建翔丰华新能源材料有限公司 | A method of silicon-carbon cathode material is prepared based on micron silicon wafer |
| CN110571420B (en) * | 2019-09-09 | 2021-05-18 | 浙江师范大学 | Method for synthesizing silicon/graphite/amorphous carbon/conductive carbon black quaternary composite material by using industrial metallurgical silicon |
| CN110571420A (en) * | 2019-09-09 | 2019-12-13 | 浙江师范大学 | method for synthesizing silicon/graphite/amorphous carbon/conductive carbon black quaternary composite material by using industrial metallurgical silicon |
| CN110931749A (en) * | 2019-12-06 | 2020-03-27 | 天津工业大学 | Aluminum oxide doped silicon/dual-carbon composite negative electrode material and preparation method thereof |
| CN112366294A (en) * | 2020-07-31 | 2021-02-12 | 万向一二三股份公司 | Graphite/silicon/carbon composite negative electrode material and preparation method thereof |
| CN112234179A (en) * | 2020-10-26 | 2021-01-15 | 郑州中科新兴产业技术研究院 | Preparation method of high-capacity silicon-based negative electrode material |
| CN113479890A (en) * | 2021-06-30 | 2021-10-08 | 松山湖材料实验室 | Silicon-based negative electrode material and preparation method and application thereof |
| CN113479890B (en) * | 2021-06-30 | 2022-12-27 | 松山湖材料实验室 | Silicon-based negative electrode material and preparation method and application thereof |
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Inventor after: Chen Haiqing Inventor after: Niu Shasha Inventor after: Liu Jun Inventor after: Jiang Guanghui Inventor before: Chen Haiqing Inventor before: Niu Shasha Inventor before: Liu Jun Inventor before: Jiang Guanghui |
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Application publication date: 20160615 |