CN105449214A - Lithium ion battery cathode material of which nano particles embedded into carbon nanosheet and preparation method of lithium ion battery cathode material - Google Patents
Lithium ion battery cathode material of which nano particles embedded into carbon nanosheet and preparation method of lithium ion battery cathode material Download PDFInfo
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- CN105449214A CN105449214A CN201610017506.2A CN201610017506A CN105449214A CN 105449214 A CN105449214 A CN 105449214A CN 201610017506 A CN201610017506 A CN 201610017506A CN 105449214 A CN105449214 A CN 105449214A
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- ion battery
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- H01M4/13—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
- 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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- 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 lithium ion battery cathode material of which nano particles are embedded into a carbon nanosheet and a preparation method of the lithium ion battery cathode material, which belong to the technical field of electrochemistry. According to the method, water-soluble organic matter (glucose, saccharose, fructose, citric acid, sodium citrate and the like) is used as a carbon source, commercial submicron particles (such as metallic tin, stibium, germanium, nonmetallic silicon and the like) are used as a particle source, sodium chloride is used as a template, the carbon source, the submicron particles and the sodium chloride are added into a ball milling tank for ball milling according to a proper proportion, and a mixture is dried and calcined. A simple ball milling method and a pyrolysis method are used for preparing the lithium ion battery cathode material of which the nano particles are uniformly embedded into the carbon nanosheet. According to the lithium ion battery cathode material of which the nano particles are uniformly embedded into the carbon nanosheet, the specific surface area is large, the surface is of a porous structure, the preparation method is simple, and the lithium ion battery cathode material has good circulation and rate performance.
Description
Technical field
The invention belongs to technical field of electrochemistry, be specifically related to a kind of lithium ion battery negative material, be specifically related to the preparation method that a kind of nano particle embeds carbon nanosheet lithium ion battery negative material, the obtained nano particle of the method evenly embeds carbon nanosheet, and as the application of lithium ion battery negative material.
Background technology
Along with the fast development of economy, energy problem becomes one of key factor of restriction social development.Lithium ion battery is as a kind of novel secondary energy sources, because having that energy density is large, self discharge is little, operating voltage is high, have extended cycle life, the good characteristic such as memory-less effect and non-environmental-pollution, be rapidly developed in recent years, be widely used in the categories of portable electronic devices such as mobile phone, digital camera, notebook computer, be considered to one of the most effective energy storage mode at present.But along with the development of society, people propose higher requirement to the performance of lithium ion battery, the energy density that especially demand is higher and power density.
But, the current mainly graphite of negative material of commercial Li-ion battery, although graphite has cheapness, environmental friendliness, high structural stability and conductivity advantages of higher, its theoretical specific capacity is low, and this makes it cannot be applied in the fields such as the electric automobile requiring high-energy-density.Therefore, find that specific capacity is large, circulation and good rate capability negative material become one of hot issue of current negative material research field.
Metal negative electrode theoretical specific capacity is high, and several times that are generally graphite theoretical specific capacity even more, is the main negative material of potential alternative graphite cathode material.The negative material that can be used as lithium ion battery at present mainly contains metallic tin, germanium, antimony and nonmetal silicon etc.Although the specific capacity of these materials is large, there is serious Volumetric expansion in these materials, and conductivity is not high yet in removal lithium embedded process, thus cause cyclical stability extreme difference, limits its application in actual production.Therefore, carry out modification to metal negative electrode material, the standard that can reach practical application seems particularly important.
The method of modifying of metal negative electrode mainly contains: nanometer, Surface coating and formation composite material etc.Nanometer mainly comprises various metal negative electrode design of material is become various nanostructure; Surface coating mainly charcoal is coated, also comprises coated to metal negative electrode of other various material; The kind forming composite material is many, can be active material also can be inert matter with the material of its compound, but its effect played is substantially identical, mainly limits its volumetric expansion or increases conductivity.Nearest research shows, is embedded into by nano particle in carbon nanosheet, then it can be used as lithium ion battery negative material can increase substantially the chemical property of metal negative electrode material.
Summary of the invention
For the deficiencies in the prior art, technical problem to be solved by this invention is that commercialization graphite cathode capacity is too low, the object of this invention is to provide a kind of nano particle and embed carbon nanosheet lithium ion battery cathode material and its preparation method, this material lithium storage content is high, good cycle, preparation method is simple, and cost is low, is easy to extensive preparation.The nano particle that the present invention proposes embeds carbon nanosheet lithium ion battery negative material, it not the simple composite of nano particle and carbon nanosheet, but nano particle is embedded in carbon nanosheet uniformly, nano particle is combined with carbon nanosheet closely, incrust, and there are good electron conduction and the ion guide general character, by overcoming the technical problem of nano particle cycle performance difference, improve graphite cathode capacity.
The present invention adopts following technical scheme, and its feature is:
A kind of nano particle embeds the preparation method of carbon nanosheet lithium ion battery negative material, it is characterized in that, with organic substance soluble in water for carbon source, commercialization micro-sized metal particle or micron order nonmetal particle are particle source, sodium chloride is template, by carbon source, particle source and sodium chloride mixing, high-energy ball milling, after oven dry, the solid mixture of formation under mixed atmosphere, in tube furnace in the temperature range of 600 ~ 750 DEG C pyrolysis processing, after cooling, washing and drying, obtain described lithium ion battery negative material.
The preferred mass of described particle, carbon source and sodium chloride is than being (0.6 ~ 1.0): (3 ~ 5): (30 ~ 50).
Described method specifically comprises the following steps:
1) precursor power: take (0.6 ~ 1.0) g commercialization micro-sized metal particle or micron order nonmetal particle, (3 ~ 5) g carbon source and (30 ~ 50) g sodium chloride, put into ball grinder, add (5 ~ 20) mL distilled water, with 500rpm speed ball milling (10 ~ 20) h, the mixture obtained is put into baking oven, after 60 ~ 80 DEG C of oven dry, puts into tube furnace;
2) presoma pyrolysis processing: under hydrogen and inert gas mixed atmosphere, carries out pyrolysis processing with (2 ~ 5) DEG C/min temperature programming to 600 ~ 750 DEG C, keeps more than 2h changing at temperature, is then cooled to room temperature;
3) reprocessing: by the distilled water washing removing sodium chloride template of the black dilatant after calcining, then be washed with distilled water to neutral rear dry.
Described organic substance is preferably from the organic substance that glucose, sucrose, fructose, citric acid and natrium citricum etc. are soluble in water.
Described mixed atmosphere refers to a kind of mist in hydrogen and nitrogen, argon gas two kinds of gases.
More specifically, for metallic tin, nano particle of the present invention embeds the preparation of carbon nanosheet lithium ion battery negative material, comprises the following steps:
1) precursor power: with citric acid (or glucose, sucrose, fructose and natrium citricum) for carbon source, commercialization micro-sized metal tin is particle source, take sodium chloride as template, take (0.6 ~ 1.0) g commercialization micro-sized metal tin, (3 ~ 5) g citric acid (or glucose, sucrose, fructose and natrium citricum) and (30 ~ 50) g sodium chloride, put into ball grinder, add (5 ~ 20) mL distilled water, with 500rpm speed ball milling (10 ~ 20) h, the mixture obtained is put into baking oven, after 60 ~ 80 DEG C of oven dry, puts into tube furnace;
2) presoma pyrolysis processing: the even shakedown of obtained precursor samples is sprinkled upon and burns bottom boat, burning boat is placed in tube furnace flat-temperature zone, first logical nitrogen 30min, to get rid of the air in tube furnace, then the mist of logical argon gas and hydrogen, carry out temperature programming to 750 DEG C with 2 DEG C/min and carry out carbonization, at 750 DEG C, be incubated 2h, be then cooled to room temperature.Take out product, obtain black expanded solids.
3) reprocessing: joined in 500mL beaker by the black dilatant after calcining, add 400mL distilled water, filters, washing removing sodium chloride template, drier after being washed with distilled water to neutrality.
Said method is prepared nano metal tin particle by simple ball-milling method in conjunction with pyrolysismethod and is embedded carbon nanosheet lithium ion battery negative material, is that a kind of nano metal tin uniform particle is embedded in carbon nanosheet.The composite material of gained is used for lithium ion battery negative, tests its chemical property in lithium ion battery.
The invention has the advantages that: the nano particle that nano particle of the present invention embeds in carbon nanosheet lithium ion battery negative material is evenly embedded in carbon nanosheet.In the structure of this composite material, in charge and discharge process, nano particle is being electrochemical reaction center, the significant contributor of specific capacity, although carbon nanosheet also has, deintercalation enters, the ability of lithium, mainly plays the transmitting effect of ion and electronics and in charge and discharge process, suppresses the Volumetric expansion of nano particle.Therefore in cyclic process, the structure of electrode is unlikely to avalanche, thus ensure that the good circulation ability of electrode.Adopt this composite material can obtain capacity as lithium ion battery negative material high, the lithium ion battery negative material of good cycle, under the current density of 100mA/g, its first capacity up to 2000mAh/g, under the current density of 500mA/g, the capacity after 100 times that circulates also is far longer than business-like graphite cathode material up to its performance of 800mAh/g.
Accompanying drawing explanation
Fig. 1 nano particle embeds the illustraton of model of carbon nanosheet lithium ion battery negative material.
Fig. 2 silicon nano embeds the TEM figure of carbon nanosheet lithium ion battery negative material.
Embodiment
Describe the present invention below in conjunction with instantiation.Protection scope of the present invention is not limited with embodiment, but is limited by claim.
Embodiment 1
Nano metal tin particle embeds the preparation method of carbon nanosheet lithium ion battery negative material, comprises the following steps:
(1) precursor power: take citric acid as carbon source, commercialization micro-sized metal tin is particle source, take sodium chloride as template, take 0.6g commercialization micro-sized metal tin, 3g citric acid and 30g sodium chloride, put into ball grinder, add 10mL distilled water, with 500rpm speed ball milling 20h, the mixture obtained is put into baking oven, after 80 DEG C of oven dry, puts into tube furnace.
(2) presoma pyrolysis processing: the even shakedown of obtained precursor samples is sprinkled upon and burns bottom boat, burning boat is placed in tube furnace flat-temperature zone, first logical nitrogen 30min, to get rid of the air in tube furnace, then the mist of logical argon gas and hydrogen, carry out temperature programming to 750 DEG C with 2 DEG C/min and carry out carbonization, at 750 DEG C, be incubated 2h, be then cooled to room temperature.Take out product, obtain black expanded solids.
(3) reprocessing: joined in 500mL beaker by the black dilatant after calcining, add 400mL distilled water, filters, washing removing sodium chloride template, drier after being washed with distilled water to neutrality.
Embodiment 2
Similar to embodiment 1, difference is, the present embodiment step (1) precursor power method is: take natrium citricum as carbon source, and commercialization micro-sized metal tin is particle source, take sodium chloride as template, take 0.6g commercialization micro-sized metal tin, 3g natrium citricum and 30g sodium chloride, put into ball grinder, add 10mL distilled water, with 500rpm speed ball milling 20h, the mixture obtained is put into baking oven, after 80 DEG C of oven dry, puts into tube furnace.
Embodiment 3
Similar to embodiment 1, difference is, the present embodiment step (1) precursor power method is: take natrium citricum as carbon source, and commercialization micron order silica flour is particle source, take sodium chloride as template, take 0.6g commercialization micron order silica flour, 3g natrium citricum and 30g sodium chloride, put into ball grinder, add 10mL distilled water, with 500rpm speed ball milling 20h, the mixture obtained is put into baking oven, after 80 DEG C of oven dry, puts into tube furnace.
Claims (10)
1. a nano particle embeds carbon nanosheet lithium ion battery negative material, nano particle is embedded in carbon nanosheet, nano particle and carbon nanosheet are combined closely, it is characterized in that: described lithium ion battery negative material is the carbon nanosheet evenly embedding nano particle.
2. nano particle embeds carbon nanosheet lithium ion battery negative material as claimed in claim 1, it is characterized in that: described carbon nanosheet is prepared by particle source, carbon source and sodium chloride.
3. nano particle embeds carbon nanosheet lithium ion battery negative material as claimed in claim 2, it is characterized in that: the mass ratio of described particle source, carbon source and sodium chloride is 0.6 ~ 1.0:3 ~ 5:30 ~ 50.
4. nano particle embeds carbon nanosheet lithium ion battery negative material as claimed in claim 2, it is characterized in that: described particle source is micro-size particles.
5. nano particle embeds carbon nanosheet lithium ion battery negative material as claimed in claim 4, it is characterized in that: described micro-size particles is micro-sized metal tin or micron order silica flour.
6. nano particle embeds carbon nanosheet lithium ion battery negative material as claimed in claim 2, it is characterized in that: described carbon source is organic substance.
7. nano particle embeds carbon nanosheet lithium ion battery negative material as claimed in claim 6, it is characterized in that: described organic substance is one or more in glucose, sucrose, fructose, citric acid or natrium citricum organic substance soluble in water.
8. a preparation method for lithium ion battery negative material, comprises the steps:
(1) precursor power: take particle source, carbon source and sodium chloride and distilled water puts into ball grinder, carries out ball milling, the mixture obtained is put into baking oven and dries;
(2) presoma pyrolysis processing: the mixture of having dried is put into tube furnace, under the mixed atmosphere of hydrogen and inert gas, pyrolysis processing is carried out in heating, after carrying out isothermal holding, is cooled to room temperature, takes out the black dilatant after pyrolysis processing;
(3) reprocessing: by the distilled water washing removing sodium chloride template of the black dilatant after pyrolysis processing, then be washed with distilled water to neutral rear dry.
9. preparation method as claimed in claim 8, it is characterized in that: the rotating speed of described ball milling is 500rpm, and Ball-milling Time is 10 ~ 20h, the temperature of described oven dry is 60 ~ 80 DEG C; Described hydrogen and inert gas refer to the gas of hydrogen and nitrogen or argon gas wherein a kind of gas and vapor permeation.
10. preparation method as claimed in claim 8, is characterized in that: the condition of described pyrolysis processing is for 2 ~ 5 DEG C/min temperature programming to 600 ~ 750 DEG C, and the time of described isothermal holding is more than 2h.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105826535A (en) * | 2016-05-16 | 2016-08-03 | 上海交通大学 | Three-dimensional porous carbon-loaded Na2Ge4O9 compound and preparation method thereof |
| CN106315553A (en) * | 2016-08-11 | 2017-01-11 | 东莞市基泰新材料技术有限公司 | Lithium-ion-battery cathode material and preparing method thereof |
| CN107331836A (en) * | 2017-06-09 | 2017-11-07 | 天津大学 | The carbon nanosheet network structure load germanic acid ferrum nano material of three-dimensional communication and preparation and application |
| CN108110235A (en) * | 2017-12-13 | 2018-06-01 | 吉林大学 | A kind of hollow nickel-NiO nanoparticle/porous carbon nanoscale twins composite material and preparation method and application |
| CN108807892A (en) * | 2018-06-06 | 2018-11-13 | 郑州中科新兴产业技术研究院 | A kind of preparation method of asphaltic base silicon-carbon nanometer sheet lithium cell negative pole material |
| CN108807919A (en) * | 2016-09-23 | 2018-11-13 | 河北工业大学 | A kind of preparation method of three-dimensional carbon skeleton |
| CN110386626A (en) * | 2018-04-16 | 2019-10-29 | 中国科学技术大学 | A kind of cobalt protoxide thin slice, preparation method and its decompose the application in water entirely in visible light catalytic |
| CN110416532A (en) * | 2019-08-20 | 2019-11-05 | 广东工业大学 | A kind of battery composite material and preparation method thereof, electrode slice and battery |
| CN111600005A (en) * | 2020-06-16 | 2020-08-28 | 广西师范大学 | Preparation method of lithium ion battery negative electrode material porous Si/C composite material |
| CN111646472A (en) * | 2020-05-22 | 2020-09-11 | 兰州理工大学 | Method for in-situ preparation of porous silicon-carbon composite negative electrode material |
| CN111785947A (en) * | 2020-07-23 | 2020-10-16 | 合肥国轩高科动力能源有限公司 | Composite negative electrode material and preparation method and application thereof |
| CN112919491A (en) * | 2019-12-05 | 2021-06-08 | 中国科学院深圳先进技术研究院 | Preparation method and application of zeolite molecular sieve dominant silicon source material |
| CN113903912A (en) * | 2021-09-30 | 2022-01-07 | 常熟理工学院 | Preparation method of carbon-loaded titanium carbide material, product obtained by preparation method and application of product |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105826535B (en) * | 2016-05-16 | 2018-09-11 | 上海交通大学 | Three-dimensional porous carbon loads Na2Ge4O9Compound and preparation method thereof |
| CN105826535A (en) * | 2016-05-16 | 2016-08-03 | 上海交通大学 | Three-dimensional porous carbon-loaded Na2Ge4O9 compound and preparation method thereof |
| CN106315553A (en) * | 2016-08-11 | 2017-01-11 | 东莞市基泰新材料技术有限公司 | Lithium-ion-battery cathode material and preparing method thereof |
| CN108807919A (en) * | 2016-09-23 | 2018-11-13 | 河北工业大学 | A kind of preparation method of three-dimensional carbon skeleton |
| CN108807919B (en) * | 2016-09-23 | 2021-01-19 | 河北工业大学 | Preparation method of three-dimensional carbon skeleton |
| CN107331836A (en) * | 2017-06-09 | 2017-11-07 | 天津大学 | The carbon nanosheet network structure load germanic acid ferrum nano material of three-dimensional communication and preparation and application |
| CN108110235B (en) * | 2017-12-13 | 2020-10-09 | 吉林大学 | Hollow nickel-nickel oxide nanoparticle/porous carbon nanosheet layer composite material and preparation method and application thereof |
| CN108110235A (en) * | 2017-12-13 | 2018-06-01 | 吉林大学 | A kind of hollow nickel-NiO nanoparticle/porous carbon nanoscale twins composite material and preparation method and application |
| CN110386626A (en) * | 2018-04-16 | 2019-10-29 | 中国科学技术大学 | A kind of cobalt protoxide thin slice, preparation method and its decompose the application in water entirely in visible light catalytic |
| CN108807892A (en) * | 2018-06-06 | 2018-11-13 | 郑州中科新兴产业技术研究院 | A kind of preparation method of asphaltic base silicon-carbon nanometer sheet lithium cell negative pole material |
| CN110416532A (en) * | 2019-08-20 | 2019-11-05 | 广东工业大学 | A kind of battery composite material and preparation method thereof, electrode slice and battery |
| CN112919491A (en) * | 2019-12-05 | 2021-06-08 | 中国科学院深圳先进技术研究院 | Preparation method and application of zeolite molecular sieve dominant silicon source material |
| CN112919491B (en) * | 2019-12-05 | 2022-08-05 | 中国科学院深圳先进技术研究院 | Preparation method and application of zeolite molecular sieve dominant silicon source material |
| CN111646472A (en) * | 2020-05-22 | 2020-09-11 | 兰州理工大学 | Method for in-situ preparation of porous silicon-carbon composite negative electrode material |
| CN111600005A (en) * | 2020-06-16 | 2020-08-28 | 广西师范大学 | Preparation method of lithium ion battery negative electrode material porous Si/C composite material |
| CN111600005B (en) * | 2020-06-16 | 2022-04-22 | 广西师范大学 | Preparation method of lithium ion battery negative electrode material porous Si/C composite material |
| CN111785947A (en) * | 2020-07-23 | 2020-10-16 | 合肥国轩高科动力能源有限公司 | Composite negative electrode material and preparation method and application thereof |
| CN113903912A (en) * | 2021-09-30 | 2022-01-07 | 常熟理工学院 | Preparation method of carbon-loaded titanium carbide material, product obtained by preparation method and application of product |
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Application publication date: 20160330 |