CN106252646A - A kind of lithium ion battery lithium manganate material synthetic method - Google Patents
A kind of lithium ion battery lithium manganate material synthetic method Download PDFInfo
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- CN106252646A CN106252646A CN201610719053.8A CN201610719053A CN106252646A CN 106252646 A CN106252646 A CN 106252646A CN 201610719053 A CN201610719053 A CN 201610719053A CN 106252646 A CN106252646 A CN 106252646A
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- lithium
- manganate material
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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
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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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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- 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
A kind of lithium ion battery lithium manganate material synthetic method, it comprises the following steps: a) collects discarded cigarette end, cleans post-drying；B) soluble manganese salt and soluble lithium salt are mixed according to the ratio of manganese lithium mol ratio 2:1, and after supersound process, obtain mixed liquor；C) cigarette end after processing takes and is immersed in the mixed liquor obtained, and makes mixed liquor not have cigarette end, takes out and dry after immersion；D) the cigarette end calcining after step c processes is obtained lithium manganate material.The lithium manganate material that the present invention prepares is hollow tubular structure, and its tube wall is open structure, it is possible to alleviates the volumetric expansion in charge and discharge process, improves the cycle performance of lithium ion battery；The lithium manganate material that the present invention prepares is the lithium manganate material of doping trace amount of titanium element, and crystal structure is more stable, it is possible to reduces the dissolving of manganese during using, can improve lithium ion battery capacity fade problem during charge and discharge cycles.
Description
Technical field
The present invention relates to lithium ion battery electrode material preparing technical field, especially relate to a kind of lithium ion battery manganese
Acid lithium material synthetic method.
Background technology
Lithium ion battery has that running voltage is high, energy density big, has extended cycle life, self-discharge rate is little, environmental protection etc.
Advantage, is widely used in portable electric appts and electric automobile；LiMn2O4 is owing to it is with low cost, environmental friendliness, electricity
High, the rich reserves in position and safety advantages of higher become the focus instantly studied, and are also following replacement LiCoO2, LiNiO2Deng
The optimum selection of positive electrode；But, during actually used, due to system expansion, the dissolving of manganese and Jiang Taile
The former cycle life thus resulted under the cycle life that LiMn2O4 is shorter, especially hot conditions such as effect, limits its reality
Border is applied.
Chinese patent publication No. CN103904321A, patent disclosure day is on July 2nd, 2014, discloses a kind of lithium ion
The high-temperature solid phase preparation method of cell negative electrode material LiMn2O4, this kind of lithium manganate material is that carbon is coated with lithium manganate material, although can
To improve lithium manganate material to a certain extent, the hydraulic performance decline caused due to reasons such as system expansion, manganese dissolvings, but due to
Carbon cladding is used so that it cannot use air atmosphere to sinter in sintering process, burns the most in air atmosphere outside it
The carbon cladding lithium manganate material poor-performing that knot is prepared, the carbon cladding lithium manganate material of this invention must be at indifferent gas bromhidrosis
Atmosphere or reducing atmosphere are sintered, reduce efficiency prepared by lithium manganate material, also add lithium manganate material system simultaneously
Standby cost.
And for example Chinese patent publication No. CN101381108A, patent disclosure day is on March 11st, 2009, discloses a kind of conjunction
The method of globulate LiMn2O4, uses manganese dioxide, lithium carbonate and acetone, sodium carboxymethyl cellulose, ethanol to blend together in this invention
Agglutination mixture is calcined prepared after drying, although this kind of method can prepare the spherical lithium manganate material of pattern rule, but
It with the addition of substantial amounts of organic compound in colloidal mixture, when high-temperature calcination, owing in the present invention, heating rate is higher,
In temperature-rise period, organic compound decomposition produces gas and can destroy the generation of lithium manganate material pattern, causes a part of LiMn2O4
Material cannot form the spherical of pattern rule, and the pattern even become is imperfect.
Summary of the invention
For solving the problems referred to above, the present invention provides one to have hollow tubular pattern, and specific surface area is big, material crystal structure
Stable, use the lithium ion battery lithium manganate material synthetic method that middle stability of material is good.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of lithium ion battery lithium manganate material synthetic method, comprises the following steps:
A) collect discarded cigarette end, clean post-drying；
B) by the soluble manganese salt of 0.1～5mol/L and the soluble lithium salt of 0.1～5mol/L according to the ratio of manganese lithium mol ratio 2:1
Example mixes, and obtains mixed liquor after supersound process；
C) cigarette end after processing in step a takes 3～40g and is immersed in the mixed liquor that step b obtains, and makes mixed liquor not have cigarette
Head, takes out after immersion and dries；
D) cigarette end after step c processes is calcined 2～8 hours at 600～800 DEG C and obtained lithium manganate material.
Cigarette end i.e. cigarette filter, is mainly made up of the acetate fiber of the cork paper wrapping inner layer of outer layer, for increasing cigarette end
Breathability, cork paper adds a small amount of fine particle calcium carbonate and titanium white as filler, simultaneously for increasing in acetate fiber manufacture process
The intensity of acetate fiber also adds a small amount of fine particle calcium carbonate titanium white as filler；Acetate fiber in cigarette end is the fiber of micro-nano, vinegar
Ester fiber intensity and elasticity are the most excellent, and the hydrophilic of acetate fiber is excellent, and aqueous solution is liable to stick to acetate fiber
Surface, the specific surface area of acetate fiber is big simultaneously, can adsorb substantial amounts of ion.Soluble lithium salt is rubbed with lithium with soluble manganese salt
After your ratio than 2:1 is mixed and sonicated for, obtains manganese lithium mixed liquor, discarded cigarette end after treatment is put in mixed liquor
Soak, owing to the acetate fiber in discarded cigarette end has bigger specific surface area and good hydrophilic, cigarette end absorbs
Substantial amounts of mixed liquor, the simultaneously substantial amounts of lithium ion of acetate fiber surface adsorption and manganese ion.The useless of a large amount of mixed liquor will be adsorbed with
Abandon after cigarette end dries, leave substantial amounts of manganese salt and lithium salts on acetate fiber surface, now will be adsorbed with the discarded of manganese salt and lithium salts
Cigarette end is calcined, and will generate lithium manganate material.Owing to the present invention using discarded cigarette end synthesize as lithium manganate material
Template, particularly using the acetate fiber in discarded cigarette end as templated synthesis acetate fiber, the lithium manganate material of synthesis is hollow
Tubulose, and its tube wall is loose and porous structure, and this is owing to, in calcination process, acetate fiber decomposes produces gas
Body, the lithium manganate material of impact surrounding is caused, and the structure of this kind of hollow can prevent LiMn2O4 material in charge and discharge process
Material expands, and can improve the cycle performance of lithium ion battery.Simultaneously because in discarded cigarette end, whether cork paper is still
Acetate fiber all uses a small amount of titanium white as filler, and therefore these a small amount of titanium whites, titanium elements is also into LiMn2O4 in other words
In the lattice of material, the lithium manganate material of formation can be regarded as a kind of titanium doped lithium manganate material, due to the doping of titanium, changes
Become the crystal structure of lithium manganate material, be that the crystal structure of lithium manganate material is the most stable, decrease at charge and discharge process
The dissolving of middle manganese, can be effectively improved lithium ion battery capacity fade problem during charge and discharge cycles.
As preferably, when drying in step a and c, drying temperature is 50～70 DEG C.
As preferably, when drying in step c, drying temperature is 60 DEG C.
Controlling relatively low drying temperature, one can reduce the consumption of the energy, and two are possible to prevent the heat in overtemperature
Under effect, in discarded cigarette end, manganese, lithium migrate, and cause manganese, lithium skewness.
As preferably, in step c, discarded cigarette end soak time in mixed liquor is 0.5～3 hour.
As preferably, soluble manganese salt is the one in manganese acetate, manganese nitrate, manganese sulfate or manganese chloride.
As preferably, soluble lithium salt is lithium nitrate or lithium sulfate.
As preferably, in step d, heating rate during calcining is 1～10 DEG C per minute.
As preferably, in step d, heating rate during calcining is 1 DEG C per minute.
Calcination process arranges the heating rate of reduction, the catabolic process of acetate fiber can be made the most a bit, it is also possible to
Make the speed producing gas in catabolic process relatively slow, so can ensure to produce the manganese of appropriate gas impact hollow structure
While acid lithium material tube wall, it is ensured that will not be too big because producing gas velocity, thoroughly destroy the hollow tubular knot of lithium manganate material
Structure.
Therefore, the method have the advantages that
(1) lithium manganate material that the present invention prepares is hollow tubular structure, and its tube wall is open structure, it is possible to alleviate discharge and recharge
Volumetric expansion in journey, improves the cycle performance of lithium ion battery；
(2) lithium manganate material that the present invention prepares is the lithium manganate material of doping trace amount of titanium element, and crystal structure is more stable, energy
During enough minimizing uses, the dissolving of manganese, can improve lithium ion battery capacity fade problem during charge and discharge cycles.
Accompanying drawing explanation
Fig. 1 is the X ray diffracting spectrum of the lithium manganate material that the present invention prepares；
Fig. 2 is the surface sweeping Electronic Speculum figure of the lithium manganate material that the present invention prepares；
Fig. 3 is the high rate performance figure of the lithium manganate material that the present invention prepares；
Fig. 4 be the lithium manganate material that the present invention prepares room temperature under 1C charge and discharge electric energy figure；
Fig. 5 be 60 DEG C of the lithium manganate material that the present invention prepares at 1C charge and discharge electric energy figure.
Detailed description of the invention
Below in conjunction with detailed description of the invention, technical scheme is further described.
Embodiment 1
A kind of lithium ion battery lithium manganate material synthetic method, comprises the following steps:
A) collecting discarded cigarette end, clean post-drying, drying temperature is 60 DEG C；
B) manganese nitrate solution of 0.2mol/L and the lithium nitrate solution of 0.1mol/L are mixed according to the ratio of manganese lithium mol ratio 2:1
Close, and after supersound process, obtain mixed liquor；
C) cigarette end after processing in step a takes 10g and is immersed in the mixed liquor that step b obtains, and makes mixed liquor not have cigarette end, leaching
Take out after bubble and dry；Discarded cigarette end soak time in mixed liquor is 1 hour, and drying temperature is 60 DEG C；
D) cigarette end after step c processes is calcined 3 hours in 700 DEG C of air atmospheres and obtained lithium manganate material；During calcining
Heating rate is 1 DEG C per minute.
Embodiment 2
A kind of lithium ion battery lithium manganate material synthetic method, comprises the following steps:
A) collecting discarded cigarette end, clean post-drying, drying temperature is 50 DEG C；
B) the manganese acetate solution of 0.1mol/L and the lithium nitrate solution of 0.1mol/L are mixed according to the ratio of manganese lithium mol ratio 2:1
Close, and after supersound process, obtain mixed liquor；
C) cigarette end after processing in step a takes 3g and is immersed in the mixed liquor that step b obtains, and makes mixed liquor not have cigarette end, leaching
Take out after bubble and dry；Discarded cigarette end soak time in mixed liquor is 0.5 hour, and drying temperature is 50 DEG C；
D) cigarette end after step c processes is calcined 2 hours in 600 DEG C of air atmospheres and obtained lithium manganate material；During calcining
Heating rate is 1 DEG C per minute.
Embodiment 3
A kind of lithium ion battery lithium manganate material synthetic method, comprises the following steps:
A) collecting discarded cigarette end, clean post-drying, drying temperature is 60 DEG C；
B) manganese sulfate solution of 4mol/L and the lithium sulfate solution of 2mol/L are mixed according to the ratio of manganese lithium mol ratio 2:1, and
Mixed liquor is obtained after supersound process；
C) cigarette end after processing in step a takes 15g and is immersed in the mixed liquor that step b obtains, and makes mixed liquor not have cigarette end, leaching
Take out after bubble and dry；Discarded cigarette end soak time in mixed liquor is 1.5 hours, and drying temperature is 60 DEG C；
D) cigarette end after step c processes is calcined 5 hours in 650 DEG C of air atmospheres and obtained lithium manganate material；During calcining
Heating rate is 3 DEG C per minute.
Embodiment 4
A kind of lithium ion battery lithium manganate material synthetic method, comprises the following steps:
A) collecting discarded cigarette end, clean post-drying, drying temperature is 70 DEG C；
B) manganese chloride solution of 5mol/L and the lithium sulfate solution of 5mol/L are mixed according to the ratio of manganese lithium mol ratio 2:1, and
Mixed liquor is obtained after supersound process；
C) cigarette end after processing in step a takes 40g and is immersed in the mixed liquor that step b obtains, and makes mixed liquor not have cigarette end, leaching
Take out after bubble and dry；Discarded cigarette end soak time in mixed liquor is 3 hours, and drying temperature is 70 DEG C；
D) cigarette end after step c processes is calcined 8 hours in 800 DEG C of air atmospheres and obtained lithium manganate material；During calcining
Heating rate is 10 DEG C per minute.
Properties Testing:
1.XRD structured testing:
As it is shown in figure 1, above-described embodiment is prepared lithium manganate material collection of illustrative plates after XRD tests and lithium manganate having spinel structure
The standard card JCPDS NO.35-0782 of material compares, it is possible to clearly tell (111) in lithium manganate having spinel structure,
(311), (222), (331), (511), each corresponding diffraction maximum such as (440) and (531), wherein there is Mn in figure2O3Diffraction maximum
Illustrate the lithium manganate material of synthesis exists the Mn of trace2O3, the Mn of these trace2O3It is owing to high temperature is led in calcination process
Cause what Li volatilization caused.
2. Scanning Electron microscopy surface pattern test:
As in figure 2 it is shown, the lithium manganate material that above-described embodiment prepares carries out the test of Scanning Electron microscopy surface micromorphology, by scheming
2 it appeared that the lithium manganate material of synthesis is hollow tubular, and tube wall is coarse, keeps phase with the appearance of acetate fiber in discarded cigarette end
Similar.
3. lithium ion battery high rate performance test:
As it is shown on figure 3, the lithium manganate material that above-described embodiment prepares assembles lithium ion battery according to prior art, and to accordingly
Lithium ion battery carries out high rate performance test, by Fig. 3 it is found that specific discharge capacity under the little multiplying power of prepared lithium ion battery
Maintaining more than 100mAh/g, even if under 50C multiplying power, its specific discharge capacity also at more than 50mAh/g, has good multiplying power
Performance.
4. lithium ion battery charge-discharge performance test:
As shown in Figure 4,5, the lithium manganate material that above-described embodiment prepares assembles lithium ion battery according to prior art, and to accordingly
Lithium ion battery carry out respectively room temperature charge-discharge performance test and high temperature (60 DEG C) charge-discharge performance test；By scheming
4 can obtain, and after 1000 cycle charge-discharges, its specific discharge capacity still maintains more than 120mAh/g；Can be obtained by Fig. 5, at height
In the case of temperature (60 DEG C), after 1000 cycle charge-discharges, its specific discharge capacity still maintains 110mAh/g.Therefore, above-mentioned
The lithium manganate material cycle performance that whether all the amount of having is high under room temperature or high temperature that embodiment prepares.
Claims (8)
1. a lithium ion battery lithium manganate material synthetic method, it is characterised in that comprise the following steps:
A) collect discarded cigarette end, clean post-drying；
B) by the soluble manganese salt of 0.1～5mol/L and the soluble lithium salt of 0.1～5mol/L according to the ratio of manganese lithium mol ratio 2:1
Example mixes, and obtains mixed liquor after supersound process；
C) cigarette end after processing in step a takes 3～40g and is immersed in the mixed liquor that step b obtains, and makes mixed liquor not have cigarette
Head, takes out after immersion and dries；
D) cigarette end after step c processes is calcined 2～8 hours at 600～800 DEG C and obtained lithium manganate material.
A kind of lithium ion battery lithium manganate material synthetic method the most according to claim 1, it is characterised in that: described step
When drying in rapid a and c, drying temperature is 50～70 DEG C.
A kind of lithium ion battery lithium manganate material synthetic method the most according to claim 1 and 2, it is characterised in that: institute
When stating drying in step c, drying temperature is 60 DEG C.
A kind of lithium ion battery lithium manganate material synthetic method the most according to claim 1, it is characterised in that: described step
In rapid c, discarded cigarette end soak time in mixed liquor is 0.5～3 hour.
A kind of lithium ion battery lithium manganate material synthetic method the most according to claim 1, it is characterised in that: described
Soluble manganese salt is the one in manganese acetate, manganese nitrate, manganese sulfate or manganese chloride.
A kind of lithium ion battery lithium manganate material synthetic method the most according to claim 1, it is characterised in that: described
Soluble lithium salt is lithium nitrate or lithium sulfate.
A kind of lithium ion battery lithium manganate material synthetic method the most according to claim 1, it is characterised in that: described step
In rapid d, heating rate during calcining is 1～10 DEG C per minute.
8. according to a kind of lithium ion battery lithium manganate material synthetic method described in claim 1 or 7, it is characterised in that: institute
Stating in step d, heating rate during calcining is 1 DEG C per minute.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104347853A (en) * | 2014-09-24 | 2015-02-11 | 秦皇岛中科远达电池材料有限公司 | Lithium manganate composite positive electrode material, a preparing method thereof and a lithium-ion battery |
| CN105762344A (en) * | 2016-04-26 | 2016-07-13 | 熊菊莲 | Electrode and preparation method of electrode material |
| CN105789550A (en) * | 2016-04-26 | 2016-07-20 | 熊菊莲 | Electrode and preparation method of electrode material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104347853A (en) * | 2014-09-24 | 2015-02-11 | 秦皇岛中科远达电池材料有限公司 | Lithium manganate composite positive electrode material, a preparing method thereof and a lithium-ion battery |
| CN105762344A (en) * | 2016-04-26 | 2016-07-13 | 熊菊莲 | Electrode and preparation method of electrode material |
| CN105789550A (en) * | 2016-04-26 | 2016-07-20 | 熊菊莲 | Electrode and preparation method of electrode material |
Non-Patent Citations (1)
| Title |
|---|
| 刘立振: "尖晶石锰酸锂的制备与改性研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅱ辑》 * |
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