CN109841795A - A kind of preparation method of negative electrode of lithium ion battery - Google Patents
A kind of preparation method of negative electrode of lithium ion battery Download PDFInfo
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- CN109841795A CN109841795A CN201910195146.9A CN201910195146A CN109841795A CN 109841795 A CN109841795 A CN 109841795A CN 201910195146 A CN201910195146 A CN 201910195146A CN 109841795 A CN109841795 A CN 109841795A
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- lithium ion
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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
A kind of preparation method of negative electrode of lithium ion battery, belongs to lithium battery technology and novel energy resource material technology field.Firstly, ferrous salt, ammonium chloride and glucose are uniformly mixed in mortar, it is placed in sintering in tube furnace and obtains carbon/ferriferrous oxide composite material；Then polyimide binder is added in N-Methyl pyrrolidone, is uniformly mixed, sequentially adds conductive black and above-mentioned carbon/ferriferrous oxide composite material, stirred, obtain cathode coating slurry；Finally, cathode coating slurry is evenly applied on collector, dries, lithium ion battery negative electrode can be obtained.A kind of preparation method of negative electrode of lithium ion battery provided by the invention, easy to operate, at low cost, environmental pollution is small, improves the cyclical stability and cyclic specific capacity of lithium ion battery, has good application prospect in new energy field.
Description
Technical field
The invention belongs to lithium battery technologies and novel energy resource material technology field, and in particular to a kind of novel lithium ion battery
The preparation method of cathode.
Background technique
It is close to the energy density of lithium ion battery, power with the development of electric car industry and the rise of energy storage industry
Degree, cycle performance and the requirement of safety are also promoted rapidly, and key components of the negative electrode material as lithium ion battery
Naturally it has received widespread attention.Wherein, ferroso-ferric oxide has many advantages, such as that volume production is sufficient, at low cost, pollution-free, highly-safe,
It is a kind of very good negative electrode material of prospect.But ferroso-ferric oxide also has the problem similar with other metal oxides,
It can there is a phenomenon where volume expansions, structure collapses during its charge and discharge cycles；Meanwhile Kynoar is used at present
(PVDF) it as cathode pole piece made from binder, with the volume expansion of ferroso-ferric oxide, the corrosion of electrolyte and can follow
The increase of ring number and avalanche is broken, capacity decline poor so as to cause lithium ion battery cyclical stability is fastly, conductivity is low etc. asks
Topic.
Summary of the invention
It is an object of the present invention to which it is negative to propose a kind of novel lithium ion battery for defect existing for background technique
The preparation method of pole.The present invention has been obtained by the improvement to negative electrode material system and binder with excellent stable circulation
The negative electrode of lithium ion battery of property and specific capacity.
To achieve the above object, The technical solution adopted by the invention is as follows:
A kind of preparation method of negative electrode of lithium ion battery, specifically includes the following steps:
Ferrous salt, ammonium chloride and glucose are uniformly mixed by step 1 in mortar, are then placed into tube furnace, in nitrogen
Under gas atmosphere, 8h~12h is sintered at a temperature of 800 DEG C~900 DEG C, cooled to room temperature is taken out, and carbon/tetra- oxidations can be obtained
Three iron composite materials；Wherein, the content of the ferrous salt is 20~25wt%, and the content of ammonium chloride is 20~25wt%, grape
The content of sugar is 50~60wt%；
Polyimides (model PY2006T) binder is added in N-Methyl pyrrolidone step 2, is uniformly mixed,
Then conductive black is sequentially added and carbon/ferriferrous oxide composite material that step 1 obtains, stirring obtains cathode coating slurry；
Wherein, the content of the carbon/ferriferrous oxide composite material is 75~90wt%, the content of the conductive black is 5~
15wt%, the content of the polyimides are 5~20wt%；The viscosity of the cathode coating slurry is greater than 800ppm；
The cathode coating slurry that step 2 obtains is evenly applied on collector by step 3, and lithium ion can be obtained in drying
Negative pole piece of battery.
Process based on the lithium ion battery negative electrode assembled battery that the present invention obtains specifically: be used for electro-chemical test
Half-cell be assemblied in the glove box full of ar gas environment and carry out, fabricated material include above-mentioned cathode pole piece, to electrode, every
Film, electrolyte, anode cover, negative electrode casing, spring leaf and gasket.Wherein, metal lithium sheet is used to electrode；Diaphragm guarantees inside battery
Lithium ion is transmitted while positive and negative anodes are not short-circuit and permeates electrolyte, and 2400 glass fibre of Gelgard can be used；Electrolyte uses
Lithium hexafluorophosphate solution.The lithium ion battery of assembling has outstanding cyclical stability and specific capacity.
Preferably, the mass ratio of ferrous salt, ammonium chloride described in step 1 and glucose is 1:1:2.
Preferably, it is 80~85wt%, the conductive black that carbon/ferriferrous oxide composite material content is stated in step 2
Content be 10~15wt%, the content of the polyimides is 10~15wt%.
Further, the temperature of drying described in step 3 is 105 DEG C, and environment is vacuum, and the time is 8~12h.
Further, in the cathode pole piece that step 3 obtains, negative electrode material with a thickness of 60~200 μm, preferably 90 μm.
Further, the method for coating described in step 3 is the modes such as casting film-forming, blade coating, extrusion coated.
Compared with prior art, the invention has the benefit that
A kind of preparation method of negative electrode of lithium ion battery provided by the invention, easy to operate, at low cost, environmental pollution is small,
Under the premise of the volume expansion for solving ferroso-ferric oxide and the bracket avalanche for doing with PVDF cathode pole piece, improve lithium from
The cyclical stability and cyclic specific capacity of sub- battery have good application prospect in new energy field.
Detailed description of the invention
Fig. 1 is carbon/ferriferrous oxide composite material XRD spectrum that the embodiment of the present invention 1 obtains；
Fig. 2 is carbon/ferriferrous oxide composite material SEM image that the embodiment of the present invention 1 obtains；
Fig. 3 is the cycle performance curve of the battery for the cathode pole piece assembling that the embodiment of the present invention 1 and comparative example 1 obtain.
Specific embodiment
Further more comprehensively detailed description is carried out to the present invention below in conjunction with specific embodiments and the drawings, it is described herein
Specific embodiment be only applicable to explain the present invention, be not restricted to the present invention.
Embodiment 1
The ferrous salt of the present embodiment is the powdered green vitriol commercially available from Aladdin, and ammonium chloride is commercially available from Aladdin
Pulverulent solids, glucose be Aladdin commercially available from pulverulent solids, polyimides be Suzhou product praise the limited public affairs of Optoelectronics Technology
Take charge of produced negative electrode binder thermoplastic polyimide (model PY2006T).
A kind of preparation method of negative electrode of lithium ion battery, specifically includes the following steps:
Step 1 uniformly mixes the green vitriol of 0.5g, the ammonium chloride of 0.5g and 1g glucose in mortar,
It is then placed into tube furnace, tube furnace is risen to 800 DEG C with the heating rate of 3 DEG C/min, in a nitrogen atmosphere, 800 DEG C of temperature
Degree is lower to be sintered 8h, and cooled to room temperature is taken out, carbon/ferriferrous oxide composite material can be obtained；
Polyimides (model PY2006T) binder of 0.1g is added in the N-Methyl pyrrolidone of 3ml step 2, stirs
It mixing 1h to be uniformly mixed, obtains clear red tan solution, the conductive black of 0.1g is then added, stirring 1h is uniformly mixed, then plus
Enter the carbon/ferriferrous oxide composite material for the 0.8g that step 1 obtains, stirs 4h, obtain cathode coating slurry；
The cathode coating slurry that step 2 obtains is evenly applied to apply on carbon copper foil by step 3, under vacuum conditions, 105
At a temperature of DEG C, lithium ion battery negative electrode is can be obtained in dry 8h.
The cathode that the cathode pole piece that step 3 is obtained uses sheet-punching machine punching to obtain diameter as 12mm, and according to negative electrode casing,
Gasket, spring leaf, diaphragm, electrolyte, cathode, gasket, anode cover assembled in sequence at button cell.Using charge and discharge instrument into
The test of row constant current charge-discharge mode, charge voltage cutoff 3.0V, discharge voltage cut-off are 0.01V, current density 0.5C, are surveyed
Trying temperature is 25 DEG C, and circulation result is as shown in Figure 3.
Comparative example 1
Compared with Example 1, difference is comparative example 1: the polyimide binder in step 2 such as is replaced at the quality
Kynoar；Remaining step is same as Example 1.
Comparative example 2
Compared with Example 1, difference is comparative example 2: the polyimide binder in step 2 such as is replaced at the quality
Polyimides commercially available from Aladdin；Remaining step is same as Example 1.The battery of obtained cathode pole piece assembling, circulation are steady
Qualitative and specific capacity is very poor, and the capacity of first lap is 104mAh/g, and rapidly, capacity attenuation arrives after being recycled to 20 circles for decaying later
1mAh/g, battery is almost without capacity.
Fig. 1 is the XRD spectrum of carbon/ferriferrous oxide composite material and ferroso-ferric oxide that the embodiment of the present invention 1 obtains；By
Fig. 1 is it is found that the composite material of carbon and ferroso-ferric oxide has successfully been prepared in the embodiment of the present invention 1.
Fig. 2 is carbon/ferriferrous oxide composite material SEM image that the embodiment of the present invention 1 obtains；As shown in Figure 2, implement
In the composite material that example 1 obtains, ferriferrous oxide particles are evenly distributed on carbon shell..
Fig. 3 is the cycle performance curve of the battery for the cathode pole piece assembling that the embodiment of the present invention 1 and comparative example 1 obtain；By
Fig. 3 is it is found that the battery that the embodiment of the present invention 1 assembles has good cyclical stability, and specific discharge capacity maintains 500mAh/
G or so, and the decline of the capacity of comparative example is obvious.
In a kind of preparation method of negative electrode of lithium ion battery provided by the invention, by cathode material in cathode coating material
The improvement of material and binder, volume expansion, the structure for efficiently solving ferroso-ferric oxide negative electrode material are broken and traditional poly- inclined
The lithium ion battery of the brokenness of vinyl fluoride bracket, obtained cathode pole piece assembling has good cyclical stability and specific volume
Amount.
Above to the explanation of all embodiment and comparative examples, carry out professional and technical personnel in the field to the present invention real
Now and utilize.All any modifications within principle of the invention, made, replacement and improvement etc., should be included in the present invention
Protection scope within.
Claims (2)
1. a kind of preparation method of negative electrode of lithium ion battery, specifically includes the following steps:
Ferrous salt, ammonium chloride and glucose are uniformly mixed by step 1 in mortar, are then placed into tube furnace, in nitrogen gas
Under atmosphere, 8h~12h is sintered at a temperature of 800 DEG C~900 DEG C, cooled to room temperature is taken out, carbon/ferroso-ferric oxide can be obtained
Composite material；Wherein, the content of the ferrous salt is 20~25wt%, and the content of ammonium chloride is 20~25wt%, glucose
Content is 50~60wt%；
Polyimide binder is added in N-Methyl pyrrolidone step 2, is uniformly mixed, then sequentially adds conduction
Carbon/ferriferrous oxide composite material that carbon black and step 1 obtain, stirring, obtains cathode coating slurry；Wherein, the carbon/tetra- oxygen
The content for changing three iron composite materials is 75~90wt%, and the content of the conductive carbon black is 5~15wt%, the polyimides
Content is 5~20wt%；
The cathode coating slurry that step 2 obtains is evenly applied on collector by step 3, and lithium ion battery can be obtained in drying
Cathode pole piece.
2. the preparation method of negative electrode of lithium ion battery according to claim 1, which is characterized in that state carbon/tetra- oxygen in step 2
The content for changing three iron composite materials is 80~85wt%, and the content of the conductive carbon black is 10~15wt%, the polyimides
Content be 10~15wt%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112614981A (en) * | 2020-12-20 | 2021-04-06 | 桂林理工大学 | Two-dimensional sheet Fe for lithium ion battery3O4Preparation method of/C composite electrode material |
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| CN102612774A (en) * | 2009-11-18 | 2012-07-25 | 丰田自动车株式会社 | Lithium secondary battery and process for producing same |
| CN102623692A (en) * | 2012-03-21 | 2012-08-01 | 新疆大学 | Method for preparing anode material of ferroferric oxide and carbon composite lithium battery |
| CN102790217A (en) * | 2012-07-26 | 2012-11-21 | 天津大学 | Carbon cladded ferriferrous oxide negative electrode material of lithium ion battery and preparation method thereof |
| CN103956482A (en) * | 2014-03-28 | 2014-07-30 | 北京理工大学 | Preparation method of foamed ferroferric oxide/carbon composite negative electrode material of lithium ion battery |
| CN107946548A (en) * | 2016-10-13 | 2018-04-20 | 内蒙古欣源石墨烯科技有限公司 | Store up the preparation method of oxide/lithium ferrite and the compound lithium ion battery negative material of carbon |
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2019
- 2019-03-14 CN CN201910195146.9A patent/CN109841795A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102612774A (en) * | 2009-11-18 | 2012-07-25 | 丰田自动车株式会社 | Lithium secondary battery and process for producing same |
| CN102623692A (en) * | 2012-03-21 | 2012-08-01 | 新疆大学 | Method for preparing anode material of ferroferric oxide and carbon composite lithium battery |
| CN102790217A (en) * | 2012-07-26 | 2012-11-21 | 天津大学 | Carbon cladded ferriferrous oxide negative electrode material of lithium ion battery and preparation method thereof |
| CN103956482A (en) * | 2014-03-28 | 2014-07-30 | 北京理工大学 | Preparation method of foamed ferroferric oxide/carbon composite negative electrode material of lithium ion battery |
| CN107946548A (en) * | 2016-10-13 | 2018-04-20 | 内蒙古欣源石墨烯科技有限公司 | Store up the preparation method of oxide/lithium ferrite and the compound lithium ion battery negative material of carbon |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112614981A (en) * | 2020-12-20 | 2021-04-06 | 桂林理工大学 | Two-dimensional sheet Fe for lithium ion battery3O4Preparation method of/C composite electrode material |
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