CN107658469A - A kind of quick method for preparing the graphene-based positive electrode of fast charging type - Google Patents
A kind of quick method for preparing the graphene-based positive electrode of fast charging type Download PDFInfo
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- CN107658469A CN107658469A CN201710990560.XA CN201710990560A CN107658469A CN 107658469 A CN107658469 A CN 107658469A CN 201710990560 A CN201710990560 A CN 201710990560A CN 107658469 A CN107658469 A CN 107658469A
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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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- 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
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Abstract
The invention discloses a kind of quick method for preparing the graphene-based positive electrode of fast charging type, its step is：Using Fe(NO3)39H2O as source of iron, lithium dihydrogen phosphate is phosphorus source and lithium source, using monohydrate potassium as carbon source, is configured to certain density LiFePO4 precursor aqueous solution, add appropriate graphene oxide solution, fully ultrasound, stirring, with ensure graphene uniform it is scattered in the solution, the solution prepared is added in fluid reservoir, under reducing atmosphere, spray pyrolysis is carried out, obtains black powder product.Advantages of the present invention：1. under solution state, graphene mixes with raw material, compared with traditional solid phase mixing, achievable dispersed and uniform cladding of the graphene on active material of the present invention, it is ensured that the stability and uniformity of product.2. the present invention uses spray pyrolysis one-step method for synthesizing, simple production process is reliable, product stable and consistent, and power consumption is low, environment-friendly, is a kind of method of suitable industrialization large-scale production.
Description
Technical field
The present invention relates to a kind of simple and easy method for preparing the graphene-based positive electrode of fast charging type.
Background technology
As the ring of key one in lithium ion battery --- positive electrode technology is that serious restriction lithium ion battery is wide at present
The key factor of general application and development, develops high-power, high power capacity, cheap, the positive electrode of safety and stability increasingly into
For the extensive approval and an urgent demand in market.Olivine-type LiFePO4 is because its cycle performance is excellent, and security performance protrudes, to ring
Border is friendly, it is cheap the advantages that, turn into one of positive electrode of most application potential and Development volue.Yet with ferric phosphate
The architectural characteristic of lithium in itself so that its electron conduction and ion mobility are relatively low, greatly limit it and are filled in high current
Application in terms of electric discharge.To improve the electric conductivity and ionic mobility of LiFePO4, using carbon material or other conductive materials pair
It is a kind of currently used LiFePO4 method of modifying that LiFePO4, which carries out Surface coating,.
Graphene has special two-dimensional nano layer structure, has a good chemical stability, high mechanical strength and excellent
Different electric conductivity, for the Surface coating to LiFePO4, the side reaction between electrode material and electrolyte can be reduced, increased
The electric conductivity of electrode material, improve chemical property, especially big circulation performance.But traditional solid phase synthesis process is still
Problems be present, such as：Graphene can not be dispersed on active material；The purity of LiFePO4 should not control；Crystal grain
Easy reunion of growing up；Complex process；Cycle is grown；High energy consumption；Graphene accounting height etc..
In order to preferably realize application of the graphene in lithium ion battery, spray pyrolysis are in lithium ion battery material system
It is standby above to have obtained many research and application.Because raw material mixes under solution state, the uniform of component is ensure that, can accurately be controlled
Stoichiometric proportion processed, it is especially suitable for multicomponent composite powder；Micro mist is formed by micron-sized droplet, typically in rule it is spherical,
It is few to reunite, without follow-up grinding, it ensure that the high-purity of product, high activity.It is simple based on its process, without subsequent treatment,
Production process is continuous, efficiency high, is a kind of effective ways for the superfine powder for being especially suitable for industrialization large-scale production.Therefore,
The present invention uses spray pyrolysis method, and graphene oxide mixes in the case where solution is mounted in solution state with raw material, with traditional solid phase
Mixed phase ratio, achievable dispersed and uniform cladding of the graphene on active material of the present invention, it is ensured that the stabilization of product
Property and uniformity.The high rate performance of prepared graphene-based positive electrode, cyclical stability is greatly enhanced, especially big
Excellent stability is shown during rate charge-discharge.Using one-step method for synthesizing, simple production process is reliable, and product is stable
Unanimously, consume energy low, it is environment-friendly, it is a kind of method of suitable industrialization large-scale production.
The content of the invention
The present invention uses spray pyrolysis method, and graphene oxide mixes in the case where solution is mounted in solution state with raw material, with biography
The solid phase mixing of system is compared, achievable dispersed and uniform cladding of the graphene on active material of the present invention, it is ensured that production
The stability and uniformity of thing.The high rate performance of prepared graphene-based positive electrode, cyclical stability are greatly enhanced,
Excellent stability is especially shown during high rate charge-discharge.Using the method for one-step synthesis, simple production process can
Lean on, product stable and consistent, power consumption is low, environment-friendly, is a kind of method of suitable industrialization large-scale production.
The main technological steps of the present invention are as follows：
(1) using Fe(NO3)39H2O as source of iron, lithium dihydrogen phosphate is phosphorus source and lithium source, using monohydrate potassium as carbon source, configuration
Into certain density LiFePO4 precursor aqueous solution, appropriate graphene oxide solution is then added, fully ultrasound, stirring, to protect
Card graphene oxide is uniformly dispersed in solution.Afterwards, the solution prepared is added in fluid reservoir.
(2) diamond heating is opened to assigned temperature, and spray pyrolysis system is passed through using H2/Ar gas as also Primordial Qi and carrier gas
In system, micron order drop caused by ultrasonic atomizer, it is brought into by carrier gas in pyrolysis reactor furnace, completes drying at high temperature, heat
The physical-chemical reaction process such as decomposition, the spheric granules of formation rule.
(3) it is final product that black powder is collected at collector.Collector must maintain sufficiently high temperature, prevent
Only moisture condensation, result in blockage.
It is an advantage of the invention that：1. under solution state, graphene mixes with raw material, compared with traditional solid phase mixing,
Achievable dispersed and uniform cladding of the graphene on active material of the present invention, it is ensured that the stability of product with it is consistent
Property.2. the present invention uses spray pyrolysis one-step method for synthesizing, simple production process is reliable, product stable and consistent, and consume energy low, environment
Close friend, it is a kind of method of suitable industrialization large-scale production.It is 3. excellent due to the good chemical stability of graphene itself
Electric conductivity and mechanical flexibility, the high rate performance of the graphene-based positive electrode prepared by the present invention, cyclical stability obtain significantly
Improve, excellent stability is especially shown during high rate charge-discharge.
Brief description of the drawings
Fig. 1 is that present invention specific implementation preparation technology obtains the ESEM of product.
Fig. 2 is that present invention specific implementation preparation technology obtains the X-ray diffractogram of product.
Cycle performances of the Fig. 3 under 5C multiplying powers.
Embodiment
Below in conjunction with the accompanying drawings and the invention will be further described by embodiment, but it should be noted that embodiment not
Form the restriction to the claimed scope of the invention.
Embodiment
1. blending process；With the Fe(NO3)39H2O of electronic balance precise 30.3,10.0 g monohydrate potassium,
7.8g lithium dihydrogen phosphates are configured to orange solution, then graphene oxide solution are added dropwise in solution above, ultrasound
0.5h, stir 1h spraying precursor liquids derived above.
2. spray pyrolysis process；Diamond heating is opened to assigned temperature, with H2/ Ar gaseous mixtures are as also Primordial Qi and load
Gas is passed through in spray pyrolysis system, micron order drop caused by ultrasonic atomizer, is brought into by carrier gas in pyrolysis reactor furnace, in height
Temperature is lower to complete the physical-chemical reaction process such as drying, thermal decomposition, the spheric granules of formation rule.
3. collect；It is final product that black powder is collected at collector.Collector must maintain sufficiently high temperature
Degree, prevents moisture condensation, results in blockage.
Claims (1)
- A kind of 1. quick method for preparing the graphene-based positive electrode of fast charging type, it is characterised in that method and step is：(1) using Fe(NO3)39H2O as source of iron, lithium dihydrogen phosphate is phosphorus source and lithium source, using monohydrate potassium as carbon source, configuration Into certain density LiFePO4 precursor aqueous solution, appropriate graphene oxide solution is then added, fully ultrasound, stirring, to protect Demonstrate,prove graphene uniform it is scattered in the solution；The solution prepared is added in fluid reservoir；(2) open diamond heating and arrive assigned temperature, using H2/Ar gas as and Primordial Qi and carrier gas are passed through in spray pyrolysis system, Micron order drop caused by ultrasonic atomizer, is brought into pyrolysis reactor furnace by carrier gas, completes drying, thermal decomposition etc. at high temperature Physical-chemical reaction process, the spheric granules of formation rule；(3) it is final product that black powder is collected at collector；Collector must maintain sufficiently high temperature, prevent water Vapour condenses, and results in blockage.
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| CN201710990560.XA CN107658469A (en) | 2017-10-23 | 2017-10-23 | A kind of quick method for preparing the graphene-based positive electrode of fast charging type |
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| CN201710990560.XA CN107658469A (en) | 2017-10-23 | 2017-10-23 | A kind of quick method for preparing the graphene-based positive electrode of fast charging type |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109167027A (en) * | 2018-08-20 | 2019-01-08 | 合肥国轩电池材料有限公司 | A kind of redox graphene/carbon coating/composite ferric lithium phosphate material preparation method |
| CN110581323A (en) * | 2019-09-25 | 2019-12-17 | 深圳清华大学研究院 | In-situ regeneration method of waste lithium iron phosphate battery positive electrode material |
| CN112531098A (en) * | 2020-12-24 | 2021-03-19 | 广东省科学院化工研究所 | Flexible thermoelectric material and preparation method thereof |
| US11101457B2 (en) * | 2017-11-08 | 2021-08-24 | Korea Basic Science Institute | Manufacturing method for cathode active material complex, and lithium secondary battery including the cathode active material complex |
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| CN1805182A (en) * | 2005-01-14 | 2006-07-19 | 湖南瑞翔新材料有限公司 | New preparation method of positive and negative electrode materials of lithium ion secondary cell by spraying thermal decomposition |
| CN103794760A (en) * | 2013-12-20 | 2014-05-14 | 中国科学院理化技术研究所 | Lithium iron phosphate composite material coated with ternary carbon source and preparation method of material |
| CN104752693A (en) * | 2013-12-30 | 2015-07-01 | 北京有色金属研究总院 | Preparation method for lithium ion battery anode material lithium iron phosphate/graphene compound |
| CN106299303A (en) * | 2016-09-27 | 2017-01-04 | 深圳复兴新能源科技有限公司 | A kind of preparation method of lithium iron phosphate positive material |
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2017
- 2017-10-23 CN CN201710990560.XA patent/CN107658469A/en active Pending
Patent Citations (4)
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| CN1805182A (en) * | 2005-01-14 | 2006-07-19 | 湖南瑞翔新材料有限公司 | New preparation method of positive and negative electrode materials of lithium ion secondary cell by spraying thermal decomposition |
| CN103794760A (en) * | 2013-12-20 | 2014-05-14 | 中国科学院理化技术研究所 | Lithium iron phosphate composite material coated with ternary carbon source and preparation method of material |
| CN104752693A (en) * | 2013-12-30 | 2015-07-01 | 北京有色金属研究总院 | Preparation method for lithium ion battery anode material lithium iron phosphate/graphene compound |
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| MU-RONG YANG等: ""LiFePO4/carbon cathode materials prepared by ultrasonic spray pyrolysis"", 《JOURNAL OF POWER SOURCES》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11101457B2 (en) * | 2017-11-08 | 2021-08-24 | Korea Basic Science Institute | Manufacturing method for cathode active material complex, and lithium secondary battery including the cathode active material complex |
| CN109167027A (en) * | 2018-08-20 | 2019-01-08 | 合肥国轩电池材料有限公司 | A kind of redox graphene/carbon coating/composite ferric lithium phosphate material preparation method |
| CN110581323A (en) * | 2019-09-25 | 2019-12-17 | 深圳清华大学研究院 | In-situ regeneration method of waste lithium iron phosphate battery positive electrode material |
| CN110581323B (en) * | 2019-09-25 | 2021-10-22 | 深圳清华大学研究院 | In-situ regeneration method of waste lithium iron phosphate battery positive electrode material |
| CN112531098A (en) * | 2020-12-24 | 2021-03-19 | 广东省科学院化工研究所 | Flexible thermoelectric material and preparation method thereof |
| CN112531098B (en) * | 2020-12-24 | 2023-08-22 | 广东省科学院化工研究所 | Flexible thermoelectric material and preparation method thereof |
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