CN106542567A - A kind of preparation method of lithium ion battery negative material nano-ZnO - Google Patents
A kind of preparation method of lithium ion battery negative material nano-ZnO Download PDFInfo
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- CN106542567A CN106542567A CN201610902683.9A CN201610902683A CN106542567A CN 106542567 A CN106542567 A CN 106542567A CN 201610902683 A CN201610902683 A CN 201610902683A CN 106542567 A CN106542567 A CN 106542567A
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- zno
- lithium ion
- ion battery
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- negative material
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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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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- 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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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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 kind of preparation method of lithium ion battery negative material nano-ZnO, concrete preparation method is that zinc acetate is put in the Muffle furnace with heating schedule, open Muffle furnace, 500 800 DEG C of predetermined temperature is raised to from room temperature, programming rate is 35 °/min, and in predetermined temperature, 500 800 DEG C are incubated 2 10 hours, then take out, room temperature is cooled to, lithium ion battery negative material nano-ZnO is obtained.Prepare ZnO and there is excellent electrochemical cycle stability, the preparation method of the lithium ion battery negative material nano-ZnO is simple, and reaction condition is easily reached, and is adapted to be prepared on a large scale.
Description
Technical field
The present invention relates to the preparation method of lithium ion battery negative material, specifically a kind of lithium ion battery negative material use
The preparation method of nano-ZnO, belongs to field of electrochemical power source.
Background technology
With the fast development of emerging economies, global energy consumption sharp increase.Lithium ion battery is with its high voltage, height
Energy density, have extended cycle life, have a safety feature, it is with low cost the advantages of in portable electrics such as computer, camera and mobile phones
Have been obtained for being widely applied on sub- equipment.In recent years, countries in the world all actively develop lithium ion battery apply to mixing
Power electric automobile（HEV）, pure electric automobile（PEV）Deng research, but lithium ion battery is used as the main of vehicle mounted dynamic battery
Bottleneck is the performance of lithium ion battery negative material.
Graphite is current most widely used lithium ion battery negative material, however, the theoretical capacity of graphite only has 372
MAh/g, it is impossible to meet the demand of the height ratio capacity of power source.Compared to graphite, ZnO has higher theoretical capacity（978
mAh/g）, and inexpensively, easily produce, it is stable in properties, it is considered to be a promising ion cathode material lithium of tool.But, ZnO is deposited
Cyclicity it is poor, decay it is rapid the shortcomings of.Chinese patent CN105336935A discloses a kind of ZnO-Graphene lithium-ion electrics
The preparation method in pond and application, its step includes the preparation of graphite oxide, prepared by the hydro-thermal method of ZnO, the Hydrothermal Synthesiss of ZnO/RGO
Method etc., can lift ZnO cycle performances by being combined for Graphene, but the ZnO-Graphene negative pole materials made in this approach
, under the electric current density of 40mA/g, the 40th week only 307. 3mAh/g, capacity are low, and the method processing step complexity for material,
Be not suitable for large-scale production.
The content of the invention
The present invention is directed to existing technical problem, there is provided a kind of preparation side of lithium ion battery negative material nano-ZnO
Method, prepares the nano-ZnO negative material with excellent electrochemical performance by simple efficient fused salt combustion synthesis method.
For achieving the above object, the present invention provides following technical scheme：A kind of lithium ion battery negative material nano-ZnO
Preparation method, it is characterised in which comprises the following steps：
（1）Zinc acetate is put in the Muffle furnace with heating schedule, is opened Muffle furnace, predetermined temperature 500- is raised to from room temperature
800 DEG C, programming rate is 3-5 °/min, in 500-800 DEG C of insulation 2-10 hour of predetermined temperature, then takes out, is cooled to room
Temperature, obtains lithium ion battery negative material nano-ZnO.
Further, preferably, step（1）Described in zinc acetate purity ＞ 99.9%.
Compared with prior art, the invention has the beneficial effects as follows：
（1）Preparation method is simple, it is easy to operate；
（2）For low melting point (237 DEG C) zinc acetate, reaction condition is easily reached in the zinc source that the present invention is adopted；
（3）Prepared nano ZnO material electrochemical performance, has potential application in lithium ion battery.
Description of the drawings
The XRD figure of sample prepared by Fig. 1 embodiments 1.
The SEM figures of sample prepared by Fig. 2 embodiments 1.
The cycle performance figure of sample prepared by Fig. 3 embodiments 1.
Specific embodiment
Embodiment 1
A kind of preparation method of lithium ion battery negative material nano-ZnO, which comprises the following steps：
（1）The zinc acetate that purity is 99.95% is put in the Muffle furnace with heating schedule, Muffle furnace is opened, is raised to from room temperature
500-800 DEG C of predetermined temperature, programming rate are 3-5 °/min, in 500-800 DEG C of insulation 2-10 hour of predetermined temperature, Ran Houqu
Go out, be cooled to room temperature, obtain lithium ion battery negative material nano-ZnO.
X-ray diffraction is determined and shows that obtained nano-ZnO is wurtzite structure（Accompanying drawing 1）, determined by stereoscan photograph
Show that nano ZnO particles size is ~ 40 nm（Accompanying drawing 2）.
With the nano-ZnO of the present invention:SP:PVDF=8:1:1 (weight ratio), plus NMP mixing is tuned into pulpous state in right amount, coats
The drying on Copper Foil and in the vacuum drying oven makes negative plate in 12 hours, with metal lithium sheet be to electrode, Celgard films be every
Film, electrolyte are 1M liPF6/ EC+DEC+DMC=1:1:1, CR2032 type batteries are assembled in the glove box of argon protection.
Set of cells stands 8h after installing, then constant current charge-discharge test is carried out with CT2001A battery test systems, and test voltage is 0.02
~3V.Fig. 3 is cycle performance figure of the prepared nano-ZnO as lithium ion battery negative, first under 0.5 A/g electric current densities
Secondary specific discharge capacity is up to 1099 mAh/g, and after 40 circulations, specific discharge capacity is respectively 328.3 mAh/g, it is shown that very well
Stable circulation performance.
Claims (2)
1. a kind of preparation method of lithium ion battery negative material nano-ZnO, it is characterised in which comprises the following steps：
（1）Zinc acetate is put in the Muffle furnace with heating schedule, is opened Muffle furnace, predetermined temperature 500- is raised to from room temperature
800 DEG C, programming rate is 3-5 °/min, in 500-800 DEG C of insulation 2-10 hour of predetermined temperature, then takes out, is cooled to room
Temperature, obtains lithium ion battery negative material nano-ZnO.
2. preparation method according to claim 1, it is characterised in that step（1）In, described zinc acetate purity ＞
99.9%。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610902683.9A CN106542567A (en) | 2016-10-18 | 2016-10-18 | A kind of preparation method of lithium ion battery negative material nano-ZnO |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610902683.9A CN106542567A (en) | 2016-10-18 | 2016-10-18 | A kind of preparation method of lithium ion battery negative material nano-ZnO |
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| CN106542567A true CN106542567A (en) | 2017-03-29 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107170961A (en) * | 2017-04-06 | 2017-09-15 | 华南师范大学 | The preparation method and application of carbon-nitrogen doped ternary metal oxide |
| CN107792890A (en) * | 2017-09-15 | 2018-03-13 | 福建翔丰华新能源材料有限公司 | The method for preparing nano NiO lithium ion battery negative material |
| CN109647584A (en) * | 2018-12-10 | 2019-04-19 | 桂林理工大学 | A kind of sand milling method of modifying of lithium ion battery mineral negative electrode material |
Citations (3)
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| CN103241764A (en) * | 2013-05-30 | 2013-08-14 | 中国科学院上海光学精密机械研究所 | Preparation method of three-dimensional zinc oxide flower-like structure |
| CN103833067A (en) * | 2014-02-17 | 2014-06-04 | 西安工程大学 | Preparation method of nanometer zinc oxide powder |
| CN104998633A (en) * | 2015-07-23 | 2015-10-28 | 陕西科技大学 | Firework-shaped nano-ZnO photocatalyst prepared based on one-step calcination method and method thereof |
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2016
- 2016-10-18 CN CN201610902683.9A patent/CN106542567A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103241764A (en) * | 2013-05-30 | 2013-08-14 | 中国科学院上海光学精密机械研究所 | Preparation method of three-dimensional zinc oxide flower-like structure |
| CN103833067A (en) * | 2014-02-17 | 2014-06-04 | 西安工程大学 | Preparation method of nanometer zinc oxide powder |
| CN104998633A (en) * | 2015-07-23 | 2015-10-28 | 陕西科技大学 | Firework-shaped nano-ZnO photocatalyst prepared based on one-step calcination method and method thereof |
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| ANIL VITHAL GHULE ET AL.: "In situ thermo-TOF-SIMS stdecomposition of zinc acetate dihydrateudy of thermal", 《JOURNAL OF MASS SPECTROMETRY》 * |
| ANIL VITHAL GHULE ET AL.: "Simultaneous thermogravimetric analysis and in situ thermo-Raman spectroscopic investigation of thermal decomposition of zinc acetate dehydrate forming zinc oxide nanoparticles", 《CHEMICAL PHYSICS LETTERS》 * |
| SHEO K. MISHRA ET AL.: "(ZnO nanoparticles: Structural, optical and photoconductivity characteristics", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
| 赵新宇等: "二水合醋酸锌热分解机理与动力学", 《华东理工大学学报》 * |
| 赵新宇等: "喷雾热解合成ZnO超细粒子工艺及机理研究", 《无机材料学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107170961A (en) * | 2017-04-06 | 2017-09-15 | 华南师范大学 | The preparation method and application of carbon-nitrogen doped ternary metal oxide |
| CN107792890A (en) * | 2017-09-15 | 2018-03-13 | 福建翔丰华新能源材料有限公司 | The method for preparing nano NiO lithium ion battery negative material |
| CN109647584A (en) * | 2018-12-10 | 2019-04-19 | 桂林理工大学 | A kind of sand milling method of modifying of lithium ion battery mineral negative electrode material |
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Application publication date: 20170329 |