CN104953092A - Lithium ion battery negative material and preparation method thereof - Google Patents
Lithium ion battery negative material and preparation method thereof Download PDFInfo
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- CN104953092A CN104953092A CN201510242184.7A CN201510242184A CN104953092A CN 104953092 A CN104953092 A CN 104953092A CN 201510242184 A CN201510242184 A CN 201510242184A CN 104953092 A CN104953092 A CN 104953092A
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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
- H01M4/1393—Processes of manufacture of electrodes based on 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
- H01M4/133—Electrodes based on 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
- 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
- H01M4/5835—Comprising fluorine or fluoride salts
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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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a lithium ion battery negative material and a preparation method thereof. The preparation method comprises the following steps: (1) mixing silica powder, filler carbon powder and an organic carbon source solution to obtain a precursor solution; and (2) atomizing the precursor solution, carrying into a vertical high-temperature reaction furnace by carrier gas and performing in-situ pyrolysis to obtain the lithium ion battery negative material. The lithium ion battery negative material is composed of nanoparticles of a core-shell structure, wherein the size of the nanoparticles is 10-100nm, the shell layer of the nanoparticles is a carbon coating layer, and the core of the nanoparticles is made of a composite of silica particles and filler carbon particles. According to the preparation method, an atomizing pyrolysis method is adopted for preparing the lithium ion battery negative material; liquid droplets formed by atomizing are uniform and therefore the particle size of the negative material powder prepared through pyrolysis is uniform too.
Description
Technical field
The present invention relates to technical field of lithium ion, particularly relate to a kind of lithium ion battery cathode material and its preparation method.
Background technology
In current commercial Li-ion batteries, graphite-like carbon negative pole material is widely used because it has good charge and discharge cycles stability, but graphite-like carbon negative pole material also exists shortcoming, as very limited in discharge capacity (372mAh/g); The current potential of carbon electrode current potential and lithium metal is very close to (100mV vs Li+/Li), and the dendrite that during over-charging of battery, the easy precipitating metal lithium in its surface is formed, exists potential safety hazard; In lithium ion deintercalation process repeatedly, due to the impact that solvent embeds altogether, cause the structure of material to be damaged, thus affect its cycle performance.Therefore, the research and apply of high power capacity, good cyclical stability and safe and practical lithium ion battery negative material has become the key of people's research.At present, the negative material of tool height ratio capacity, as the material such as oxide of Sn, Si, Sb and correspondence thereof, is the study hotspot of Novel anode material.But this kind of material easily causes the volumetric expansion of material in charge and discharge process, the cycle performance of battery is caused to be deteriorated.For addressing this problem people by preparing the silicon of nanoscale, increase the specific area of material, the diffusion length reducing lithium ion achieves the goal.But there is the strong tendency of again reuniting in nano level silicon grain in cyclic process.Thus there is the methods such as the special construction of buffer volumes expansion to improve the cycle performance of negative material further by forming composite material or designing preparation.
In lithium storage materials, silicon has high theoretical capacity (4200mAh/g) and moderate removal lithium embedded current potential (about 0.1-0.5V vs.Li/Li+), is very promising lithium ion battery negative material.But as previously mentioned, under height removal lithium embedded condition, there is serious bulk effect in silica-base material, causes the sharply decline of electrode cycle performance.For overcoming this change in volume problem, select effective change in volume to receive or buffer composition, effectively the homogeneous silicon-change in volume buffer composition compound of synthesis is the key effectively improving anode circulation performance.In addition, silicium cathode material owing to forming polymer inactivation film (SEI), causes its first charge-discharge coulombic efficiency very low in first charge-discharge process.For effectively silicon electrode being applied to lithium ion battery, we must improve its first charge-discharge coulombic efficiency, improve the electrochemical reaction irreversibility of silicon electrode, adopt the good material of conductivity, as the coated Si such as carbon, TiN, SiC particle effectively can improve the initial coulombic efficiency of silicon electrode, improve the stability of its circulation.
At present, in order to reduce the volumetric expansion of silicon in removal lithium embedded process, obtain capacity higher, the silicon based anode material of stable cycle performance, kinds of experiments method is used to the silica-base material preparing various pattern, structure.As Liu N etc. discloses a kind of Si@space@C of yolk-eggshell structure.Si is intactly coated on wherein by very thin carbon-coating, and middle void layer allows Si Particle free expand and do not destroy carbon-coating.Under 0.1C, Si@space@C discharge capacity can reach 2800mAh/g; After 1000 circulations, capacity keeps 74%, coulombic efficiency 99.84% (Liu N et a1.A yolk-shell design for stabilized and scalable Li-ion battery alloy anodes [J] .Nano Lett, 2012,12 (6): 3315).Magasinski etc. adopt self assembly route to prepare the Si/C composite material with hierarchy, and reversible capacity reaches 1950mAh/g.Under 1C and 8C discharge rate, the capacity of composite electrode is respectively 1590mAh/g and 870mAh/g (Magasinski Aet a1.High-performance lithium-ion anodes using a hierarchical bottom-up approach [J] .Nature Mater, 2010,9 (4): 353.)。Fukui H etc. prepares Si/C composite material with high temperature solid state reaction, reaction temperature all controls below 1200 DEG C, to prevent generation (Fukui H et a1.Influence of polystyrene/phenyl substituents in precursors on microstructures of Si-O-C composite anodes for lithium-ion batteries [J] the .Power Sources of inertia phase SiC, 2011,196 (1): 371).
CN102790204A discloses a kind of preparation method of silicon carbon lithium ion battery cathode, a) Polymer Solution and silica flour, graphite is mixed to get mixed liquor; B) described mixed liquor is carried out freeze drying, obtain solid mixture; C) described solid mixture is sintered, obtain silicon carbon lithium ion battery cathode.The negative material particle diameter that the method obtains is excessive and uneven.
Summary of the invention
The invention provides a kind of preparation method of lithium ion battery negative material, to solve the excessive and uneven problem of existing ion cathode material lithium particle diameter.
A preparation method for lithium ion battery negative material, comprises the following steps:
(1) silica flour, filler carbon dust and organic carbon source solution are mixed, obtain precursor solution;
(2) after precursor solution being atomized, being brought in vertical high temperature reacting furnace by carrier gas and carry out original position pyrolysis, obtained described lithium ion battery negative material.
Preferably, organic carbon source is at least one in citric acid, glucose, maleic acid and sucrose.
Preferably, the solvent of described organic carbon source solution is ethanol.
Preferably, the temperature of described original position pyrolysis is 400-800 DEG C.
Preferably, the weight ratio of organic carbon source, silica flour and filler carbon dust is 2 ~ 10:1:0.5 ~ 2.
Preferably, silica flour, filler carbon dust adopt ultrasonic dissolution after adding organic carbon source solution.
Preferably, described filler carbon dust is at least one in graphite, Graphene, carbon black and carbon nano-tube.
Present invention also offers the lithium ion battery negative material utilizing described preparation method to obtain; it is mixed by the nano particle of three kinds of nucleocapsid structures and forms; nano particle is of a size of 10-100nm; the shell of three kinds of nano particles is carbon coating layer, and core is respectively silicon grain, filler carbon granule and both compound above.
The present invention utilizes spray pyrolysis to obtain lithium ion battery negative material, and the drop formed due to spraying is even, and the negative electrode material powder particle diameter that pyrolysis is formed is even too.
Accompanying drawing explanation
Fig. 1 is the structural representation of lithium ion battery negative material of the present invention.
Fig. 2 is the SEM of the lithium ion battery negative material that embodiment 1 obtains.
Fig. 3 is the cycle performance figure of the battery of the lithium ion battery negative material utilizing embodiment 1 obtained.
Embodiment
Embodiment 1
Citric acid is dissolved in 200ml ethanol, is stirred to and dissolves formation clear solution A completely.Graphite and Graphene are mixed in the ratio of 1:0.2, then the mixture of business nano silica fume, graphite and Graphene is added in solution A respectively, then ultrasonic 90 minutes, obtain precursor solution.Wherein the mixture quality ratio of citric acid, commercial silica flour, graphite and Graphene controls at 2:1:0.5.After being atomized by precursor solution, pass into vertical high temperature reacting furnace by carrier gas and carry out original position pyrolysis, obtain the nano particle of particle diameter between 10-100nm, wherein pyrolysis temperature controls at 400 DEG C.
Embodiment 2
Citric acid is dissolved in 200ml ethanol, is stirred to and dissolves formation clear solution A completely.Graphite and Graphene are mixed in the ratio of 1:0.6, then the mixture of business nano silica fume, graphite and Graphene is added in solution A respectively, then ultrasonic 110 minutes, obtain precursor solution.Wherein the mixture quality ratio of citric acid, commercial silica flour, graphite and Graphene controls at 5:1:1.After precursor solution is atomized, passes into vertical high temperature reacting furnace by carrier gas and carry out original position pyrolysis, obtain the nano particle of particle diameter between 10-100nm.Wherein original position pyrolysis temperature controls at 500 DEG C, and jet velocity controls at 25mL.min
-1.
Embodiment 3
Citric acid is dissolved in 200ml ethanol, is stirred to and dissolves formation clear solution A completely.Graphite and Graphene are mixed in the ratio of 1:1, then the mixture of business nano silica fume, graphite and Graphene is added in solution A respectively, then ultrasonic 140 minutes, obtain precursor solution.Wherein the mass ratio of the mixture of citric acid, commercial silica flour, graphite and Graphene controls at 10:1:2.After precursor solution is atomized, passes into vertical high temperature reacting furnace by carrier gas and carry out original position pyrolysis, obtain the nano particle of particle diameter between 10-100nm.Wherein pyrolysis temperature controls at 600 DEG C.
Embodiment 4
Glucose is dissolved in 200ml ethanol, is stirred to and dissolves formation clear solution A completely.Carbon black and Graphene are mixed in the ratio of 1:0.2, then the mixture of business nano silica fume, carbon black and Graphene is added in solution A respectively, then ultrasonic 90 minutes, obtain precursor solution.Wherein the mixture quality ratio of glucose, commercial silica flour, carbon black and Graphene controls at 2:1:0.5.After being atomized by precursor solution, pass into vertical high temperature reacting furnace by carrier gas and carry out original position pyrolysis, obtain the nano particle of particle diameter between 10-100nm, wherein pyrolysis temperature controls at 400 DEG C.
Embodiment 5
Glucose is dissolved in 200ml ethanol, is stirred to and dissolves formation clear solution A completely.Carbon black and Graphene are mixed in the ratio of 1:0.6, then the mixture of business nano silica fume, carbon black and Graphene is added in solution A respectively, then ultrasonic 110 minutes, obtain precursor solution.Wherein the mixture quality ratio of glucose, commercial silica flour, carbon black and Graphene controls at 5:1:1.After being atomized by precursor solution, pass into vertical high temperature reacting furnace by carrier gas and carry out original position pyrolysis, obtain the nano particle of particle diameter between 10-100nm, wherein pyrolysis temperature controls at 500 DEG C.
Embodiment 6
Glucose is dissolved in 200ml ethanol, is stirred to and dissolves formation clear solution A completely.Carbon black and Graphene are mixed in the ratio of 1:1, then the mixture of business nano silica fume, carbon black and Graphene is added in solution A respectively, then ultrasonic 140 minutes, obtain precursor solution.Wherein the mass ratio of the mixture of glucose, commercial silica flour, carbon black and Graphene controls at 10:1:2.After being atomized by precursor solution, pass into vertical high temperature reacting furnace by carrier gas and carry out original position pyrolysis, obtain the nano particle of particle diameter between 10-100nm, wherein pyrolysis temperature controls at 600 DEG C.
Embodiment 7
By sucrose dissolved in 200ml ethanol, be stirred to and dissolve formation clear solution A completely.Carbon nano-tube and Graphene are mixed in the ratio of 1:0.2, then the mixture of business nano silica fume, carbon nano-tube and Graphene is added in solution A respectively, then ultrasonic 90 minutes, obtain precursor solution.Wherein the mixture quality ratio of sucrose, commercial silica flour, carbon nano-tube and Graphene controls at 2:1:0.5.After being atomized by precursor solution, pass into vertical high temperature reacting furnace by carrier gas and carry out original position pyrolysis, obtain the nano particle of particle diameter between 10-100nm, wherein pyrolysis temperature controls at 400 DEG C.
Embodiment 8
By sucrose dissolved in 200ml ethanol, be stirred to and dissolve formation clear solution A completely.Carbon nano-tube and Graphene are mixed in the ratio of 1:0.6, then the mixture of business nano silica fume, carbon nano-tube and Graphene is added in solution A respectively, then ultrasonic 110 minutes, obtain precursor solution.Wherein the mixture quality ratio of sucrose, commercial silica flour, carbon nano-tube and Graphene controls at 5:1:1.After being atomized by precursor solution, pass into vertical high temperature reacting furnace by carrier gas and carry out original position pyrolysis, obtain the nano particle of particle diameter between 10-100nm, wherein pyrolysis temperature controls at 500 DEG C.
Embodiment 9
By sucrose dissolved in 200ml ethanol, be stirred to and dissolve formation clear solution A completely.Carbon nano-tube and Graphene are mixed in the ratio of 1:1, then the mixture of business nano silica fume, carbon nano-tube and Graphene is added in solution A respectively, then ultrasonic 140 minutes, obtain precursor solution.Wherein the mass ratio of the mixture of sucrose, commercial silica flour, carbon nano-tube and Graphene controls at 10:1:2.After being atomized by precursor solution, pass into vertical high temperature reacting furnace by carrier gas and carry out original position pyrolysis, obtain the nano particle of particle diameter between 10-100nm, wherein pyrolysis temperature controls at 600 DEG C.
Claims (8)
1. a preparation method for lithium ion battery negative material, comprises the following steps:
(1) silica flour, filler carbon dust and organic carbon source solution are mixed, obtain precursor solution;
(2) after precursor solution being atomized, being brought in vertical high temperature reacting furnace by carrier gas and carry out original position pyrolysis, obtained described lithium ion battery negative material.
2. the preparation method of lithium ion battery negative material as claimed in claim 1, is characterized in that: organic carbon source is at least one in citric acid, glucose, maleic acid and sucrose.
3. the preparation method of lithium ion battery negative material as claimed in claim 1, is characterized in that: the solvent of described organic carbon source solution is ethanol.
4. the preparation method of lithium ion battery negative material as claimed in claim 1, is characterized in that: the temperature of described original position pyrolysis is 400 ~ 800 DEG C.
5. the preparation method of lithium ion battery negative material as claimed in claim 1, is characterized in that: the weight ratio of organic carbon source, silica flour and filler carbon dust is 2 ~ 10:1:0.5 ~ 2.
6. the preparation method of lithium ion battery negative material as claimed in claim 1, is characterized in that: silica flour, filler carbon dust adopt ultrasonic dissolution after adding organic carbon source solution.
7. the preparation method of lithium ion battery negative material as claimed in claim 1, is characterized in that: described filler carbon dust is at least one in graphite, Graphene, carbon black and carbon nano-tube.
8. utilize the lithium ion battery negative material that preparation method obtains as described in claim 1 ~ 7, it is characterized in that, be the nano particle of nucleocapsid structure, nano particle is of a size of 10-100nm, the shell of nano particle is carbon coating layer, and core is the compound of silicon grain and filler carbon granule.
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Cited By (6)
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| CN106558686A (en) * | 2015-09-30 | 2017-04-05 | 萧镇能 | Preparation method of carbon-coated silicon/silicon carbide composite active material |
| CN107863498A (en) * | 2017-09-20 | 2018-03-30 | 广东省稀有金属研究所 | A kind of preparation method of cathode material of lithium-ion power battery |
| CN109638229A (en) * | 2017-10-09 | 2019-04-16 | 珠海市三顺纳米新材料有限公司 | Silicon-carbon composite cathode material and preparation method thereof and lithium ion battery |
| CN110416515A (en) * | 2019-07-24 | 2019-11-05 | 东莞东阳光科研发有限公司 | Lithium ion battery, lithium ion battery negative material and preparation method |
| CN110690432A (en) * | 2019-10-16 | 2020-01-14 | 北京车和家信息技术有限公司 | Lithium silicon carbon composite material for lithium ion battery and preparation method and application thereof |
| CN112520792A (en) * | 2021-01-30 | 2021-03-19 | 浙江博瓦德新材料科技有限公司 | Method for preparing nickel protoxide by recycling nickel precipitate |
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