CN103456948A - Preparation method of lithium ion secondary battery manganese titanate (III) lithium anode material - Google Patents
Preparation method of lithium ion secondary battery manganese titanate (III) lithium anode material Download PDFInfo
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- CN103456948A CN103456948A CN2013104410551A CN201310441055A CN103456948A CN 103456948 A CN103456948 A CN 103456948A CN 2013104410551 A CN2013104410551 A CN 2013104410551A CN 201310441055 A CN201310441055 A CN 201310441055A CN 103456948 A CN103456948 A CN 103456948A
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- 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 preparation method of a lithium ion secondary battery manganese titanate (III) lithium anode material, and belongs to the technical field of chemical material preparation. According to the preparation method, lithium carbonate, manganic oxide and titanium dioxide are used as raw materials, glucose is used as a carbon source, and through adjustment of power, temperature rise time, constant temperature time and other parameters of a microwave solid phase instrument, the manganese titanate lithium (LiMnTiO4) anode material wrapped by carbon is directly obtained. The microwave solid phase method is used for synthesis of the manganese titanate lithium wrapped by carbon, the purity of the manganese titanate lithium wrapped by carbon is high, 0.5C specific discharge capacity is up to about 148.2mAh/g, and the discharge capacity can still be kept higher than 135 mAh/g after 100 weeks. The raw materials of the preparation method are simple and easy to obtain, cost is low, and the preparation process is simple and suitable for large-scale production.
Description
Technical field
The invention belongs to the electrochemical power source technical field of material, adopt Microwave Solid method synthesizing lithium ion battery carbon to coat the manganese titanate lithium anode material.
Background technology
Lithium ion battery is the new generation of green environmental protection of performance brilliance, reproducible chemical energy source, at present just incomparable with other battery
Advantage has been captured rapidly the applications such as mobile phone, notebook computer, miniature camera, digital camera, electric tool, electric automobile, and likely replaces cadmium nickel and Ni-H cell for space industry.Positive electrode is one of critical material of manufacturing lithium ion battery.At present, the commercial Li-ion battery positive electrode mainly contains cobalt acid lithium, LiMn2O4, but cobalt resource is limited, expensive, poor safety performance, and big for environment pollution, can't in electrokinetic cell, apply.The advantages such as lithium manganate having spinel structure has aboundresources, energy density is high, cost is low, pollution-free, fail safe is good are desirable anode material for lithium-ion batteries.One of focus.But in charge and discharge process, the capacity attenuation problem is its commercial key factor of restriction all the time, finishing and doping be its chemical property of modification effectively, finishing can coat the material that the anti-electrolyte of one deck corrodes at electrode surface, effectively suppresses dissolving and the electrolyte decomposition of manganese.Doping can improve the stability of lithium manganate having spinel structure frame structure, effectively suppresses the Jahn-Teller effect in charge and discharge process.Finishing and doping combination can be improved to the chemical property of material undoubtedly.And that the synthetic method of lithium manganate having spinel structure has is a variety of, mainly contain high temperature solid-state method, melt impregnation, microwave process for synthesizing, sol-gal process, emulsification seasoning, coprecipitation, Pechini method and hydrothermal synthesis method.Manganese titanate (III) lithium anode material that the present invention adopts the synthetic a kind of lithium ion battery with practical prospect of Microwave Solid method to use.The Microwave Solid method, be to utilize the high-frequency microwave energy, produces very large energy and discharge huge heat in the very short time, thereby promote the generation of chemical reaction, and be a kind of mode of heating of environment-friendly and green.Synthetic motion and the impact velocity that can significantly accelerate reaction molecular of microwave heating, be conducive to the formation of nucleus, can limit the increase of crystal grain, can within the shorter time, synthesize less, the more uniform nano material of particle diameter.The microwave current synthetic technology has been widely used in the preparation of nano material.
Manganese titanate lithium anode material theoretical capacity is 154mAh/g, and long service life, recycle number of times high, environmental protection, but pure manganese titanate lithium cyclical stability is bad, by research, finds that carbon coats the cyclical stability that can improve the manganese titanate lithium.
Summary of the invention
In order to address the above problem, the present invention proposes the Microwave Solid synthetic method that a kind of carbon coats the manganese titanate lithium anode material.
Described method comprises the steps:
Step 1: routine 1.1:1:1 takes lithium carbonate, manganese sesquioxide managnic oxide, titanium dioxide in molar ratio, takes the glucose that accounts for product 10%;
Step 2: taken medicine is fully ground in agate mortar to 1h;
Step 3: ground medicine is placed in mould and is pressed into sheet;
Step 4: the sheet pressed is placed on to the Microwave Solid method and answers in instrument the power heating at 1000w, at 800 ℃ of constant temperature 30min, reaction automatically is cooled to 80 ℃ and can takes out and obtain LiMnTiO after finishing
4positive electrode.
Beneficial effect of the present invention is: synthetic fast, environmental protection, easily industrialization, the material electrochemical performance excellence.
The present invention sends out and has synthesized the manganese titanate lithium that carbon coats by Microwave Solid, and the manganese titanate lithium purity that the carbon of gained coats is high, and the 0.5C specific discharge capacity can reach the 148.2mAh/g left and right.The raw material that the present invention uses is simple and easy to get, and cost is low, and preparation technology simply is suitable for large-scale production.
The accompanying drawing explanation
Fig. 1 is X-ray diffraction (XRD) spectrogram that the carbon that obtains in embodiment coats manganese titanate (III) lithium anode material;
Fig. 2 is positive electrode infrared (IR) spectrogram of manganese titanate (III) lithium that obtains in embodiment;
Fig. 3 is projection Electronic Speculum (TEM) figure of manganese titanate (III) lithium anode material that obtains in embodiment;
Fig. 4 is the charging and discharging curve of manganese titanate (III) lithium anode material that obtains in embodiment;
Fig. 5 is the cycle life figure of manganese titanate (III) lithium anode material that obtains in embodiment.
Embodiment
Below in conjunction with accompanying drawing and specific embodiment, the present invention will be further described in detail:
Specific embodiment:
Take respectively in proportion 0.84g Li
2cO
3, 0.74g Mn
2o
3, 0.8g TiO
2, 0.4gC
6h
12o
6,load weighted medicine is placed in to agate mortar and fully grinds 1h, by the ground sample mould compressing tablet of packing into, the sheet pressed is put into to Microwave Solid instrument 15min under 1000w power and be warming up to 800 ℃ of constant temperature 30min, reacted rear and naturally be cooled to below 80 ℃, made carbon and coat the manganese titanate lithium anode material.As shown in Figure 1, as shown in Figure 2, projection Electronic Speculum (TEM) figure is as Fig. 3 for infrared spectrum for the XRD spectra of the carbon coating manganese titanate lithium anode material prepared, and as shown in Figure 4, the cycle life curve as shown in Figure 5 for charging and discharging curve.
The above embodiment is only the preferred embodiments of the invention, should point out, for this area, is not breaking away under the prerequisite of creating conception of the present invention, and some distortion of making and improvement all belong to protection scope of the present invention.
Claims (5)
1. the preparation method of manganese titanate (III) lithium anode material that a lithium rechargeable battery is used, characteristics are, and take lithium salts, manganese sesquioxide managnic oxide, titanium dioxide is raw material, and glucose is carbon source, with the standby lithium ion battery LiMnTiO of Microwave Solid legal system
4the method of positive electrode, its concrete synthesis step is as follows:
By lithium, iron and titanium material in molar ratio Li:Mn:Ti=1.1:1:1 take, and take 10% glucose of product, be placed in agate mortar and fully grind 1h, after compressing tablet in the Microwave Solid instrument under 1000w power 15min be warming up to 800 ℃ and constant temperature 30min, temperature can obtain with after near 80 ℃ of stove, taking out reactant manganese titanate (III) lithium (LiMnTiO that carbon coats
4) positive electrode.
2. preparation method's raw material of manganese titanate (III) lithium anode material that a kind of lithium rechargeable battery according to claim 1 is used comprise: the lithium source comprises lithium carbonate, lithium nitrate, lithium oxalate, lithium hydroxide, lithium acetate etc., the manganese source comprises manganese carbonate, manganese nitrate, manganese oxalate, manganese sesquioxide managnic oxide, manganese dioxide etc., and the titanium source comprises titanyl sulfate, titanium dioxide, butyl titanate, titanium tetrachloride etc.
3. the preparation method of manganese titanate (III) lithium anode material that a kind of lithium rechargeable battery is used according to claim 1, its characteristics are that programming rate is fast, and the mode of heating environmental protection does not need inert gas shielding, and the time, short speed was fast.
4. the preparation method of manganese titanate (III) lithium anode material that a kind of lithium rechargeable battery is used according to claim 1 is characterized in that microwave power is 500-4000w, and be 5-30min heating time.
5. the preparation method of manganese titanate (III) lithium anode material that a kind of lithium rechargeable battery is used according to claim 1 is characterized in that the microwave synthesis device can be domestic microwave instrument, industrial microwave instrument or other light wave microwave instrument.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105576199A (en) * | 2015-12-09 | 2016-05-11 | 山东精工电子科技有限公司 | Preparation method of novel nano manganese lithium titanate LiMnxTiO4 cathode material |
| CN109904395A (en) * | 2017-12-08 | 2019-06-18 | 中国石油化工股份有限公司 | A kind of molybdenum disulfide-graphene composite material |
-
2013
- 2013-09-25 CN CN2013104410551A patent/CN103456948A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105576199A (en) * | 2015-12-09 | 2016-05-11 | 山东精工电子科技有限公司 | Preparation method of novel nano manganese lithium titanate LiMnxTiO4 cathode material |
| CN109904395A (en) * | 2017-12-08 | 2019-06-18 | 中国石油化工股份有限公司 | A kind of molybdenum disulfide-graphene composite material |
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Application publication date: 20131218 |