CN106252646B - 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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- CN106252646B CN106252646B CN201610719053.8A CN201610719053A CN106252646B CN 106252646 B CN106252646 B CN 106252646B CN 201610719053 A CN201610719053 A CN 201610719053A CN 106252646 B CN106252646 B CN 106252646B
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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 comprising following steps: discarded cigarette butt a) is collected, is dried after cleaning；B) soluble manganese salt and soluble lithium salt are mixed according to the ratio of manganese lithium molar ratio 2:1, and obtains mixed liquor after being ultrasonically treated；C) by treated, cigarette butt is taken in the mixed liquor being immersed in, and so that mixed liquor was not had cigarette butt, is taken out and dry after immersion；It d) will treated that cigarette butt is calcined to obtain lithium manganate material through step c.Lithium manganate material produced by the present invention is hollow tubular structure, and tube wall is open structure, can alleviate the volume expansion in charge and discharge process, improve the cycle performance of lithium ion battery；Lithium manganate material produced by the present invention is the lithium manganate material for adulterating micro titanium elements, and crystal structure is more stable, can reduce the dissolution of manganese in use process, 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 preparation technical fields, more particularly, to a kind of lithium ion battery manganese
Sour lithium material synthetic method.
Background technique
Lithium ion battery has that operating voltage is high, energy density is big, have extended cycle life, self-discharge rate is small, environmentally protective etc.
Advantage is widely used in portable electronic device and electric car；LiMn2O4 is low in cost, environmental-friendly, electric due to its
Position is high, rich reserves and it is highly-safe the advantages that as the hot spot studied instantly, and the following substitution LiCoO2, LiNiO2Deng
The optimal selection of positive electrode；But during actual use, due to system expansion, the dissolution of manganese and Jiang Taile
The reasons such as effect and the cycle life for causing LiMn2O4 shorter, the especially cycle life under hot conditions, limit its reality
Border application.
Chinese patent publication No. CN103904321A, patent disclosure day are on July 2nd, 2014, disclose 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 carbon coating lithium manganate material, although can
To improve lithium manganate material to a certain extent, system expansion, manganese dissolution etc. due to caused by performance decline, but due to
Its outside uses carbon coating, so that it can not be sintered during the sintering process using air atmosphere, burns in air atmosphere in other words
The carbon coating lithium manganate material performance that knot is prepared is poor, and the carbon coating lithium manganate material of the invention must be in inert gas gas
It is sintered in atmosphere or reducing atmosphere, reduces the efficiency of lithium manganate material preparation, while also adding lithium manganate material system
Standby cost.
For another example Chinese patent publication No. CN101381108A, patent disclosure day are on March 11st, 2009, disclose a kind of conjunction
At the method for spherical lithium manganate, blended together in the invention using manganese dioxide, lithium carbonate and acetone, sodium carboxymethylcellulose, ethyl alcohol
It calcines and is made after agglutination mixture is dry, although the spherical lithium manganate material of morphological rules can be made in this kind of method,
It is added to a large amount of organic compound in colloidal mixture, in high-temperature calcination, since heating rate is higher in the present invention,
Organic compound, which decomposes generation gas, in temperature-rise period can destroy the generation of lithium manganate material pattern, cause a part of LiMn2O4
Material can not form the spherical shape of morphological rules, or even the pattern become is imperfect.
Summary of the invention
To solve the above problems, the present invention, which provides one kind, has hollow tubular pattern, large specific surface area, material crystal structure
Stablize, the good lithium ion battery lithium manganate material synthetic method of stability of material in use.
To achieve the above object, The technical solution adopted by the invention is as follows:
A kind of lithium ion battery lithium manganate material synthetic method, comprising the following steps:
A) discarded cigarette butt is collected, is dried after cleaning；
B) by the soluble manganese salt of 0.1~5mol/L and the soluble lithium salt of 0.1~5mol/L according to manganese lithium molar ratio 2:1
Ratio mixing, and be ultrasonically treated after obtain mixed liquor；
C) by treated in step a, cigarette butt takes 3~40g to be immersed in the mixed liquor that step b is obtained, and does not have mixed liquor
Cigarette butt takes out and dries after immersion；
It d) will treated that cigarette butt calcines 2~8 hours at 600~800 DEG C obtains lithium manganate material through step c.
Cigarette butt, that is, cigarette filter is mainly made of the acetate fiber of the cork paper wrapping inner layer of outer layer, to increase cigarette butt
Gas permeability, add a small amount of light calcium and titanium white as filler in cork paper, while to increase in acetate fiber manufacturing process
The intensity of acetate fiber also adds a small amount of light calcium titanium white as filler；Acetate fiber in cigarette butt is the fiber of micro-nano, vinegar
Ester fiber intensity and elasticity are all more excellent, and the hydrophily of acetate fiber is excellent, and aqueous solution is liable to stick to acetate fiber
Surface, while the large specific surface area of acetate fiber, can adsorb a large amount of ion.Soluble lithium salt is rubbed with soluble manganese salt with lithium
After your ratio than 2:1 is mixed and sonicated, manganese lithium mixed liquor is obtained, discarded cigarette butt after processing is put into mixed liquor
It is impregnated, since the acetate fiber discarded in cigarette butt has biggish specific surface area and good hydrophily, is absorbed in cigarette butt
A large amount of mixed liquor, while a large amount of lithium ion of acetate fiber adsorption and manganese ion.The useless of a large amount of mixed liquors will be adsorbed with
After abandoning cigarette butt drying, on acetate fiber surface, there are a large amount of manganese salts and lithium salts, will be adsorbed with the discarded of manganese salt and lithium salts at this time
Cigarette butt is calcined, and lithium manganate material will be generated.Due to what is synthesized using discarded cigarette butt as lithium manganate material in the present invention
Template, especially using the acetate fiber in discarded cigarette butt as templated synthesis acetate fiber, the lithium manganate material of synthesis is hollow
Tubulose, and its tube wall is loose and porous structure, this is because in calcination process, acetate fiber is generated gas by thermal decomposition
Body impacts caused by the lithium manganate material of surrounding, this kind of hollow structure 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 butt, whether cork paper or
Acetate fiber is all using a small amount of titanium white as filler, therefore these a small amount of titanium whites, and titanium elements also enter LiMn2O4 in other words
In the lattice of material, the lithium manganate material of formation can be regarded as the titanium doped lithium manganate material of one kind and change due to the doping of titanium
The crystal structure for having become lithium manganate material is that the crystal structure of lithium manganate material is more stable, reduces in charge and discharge process
The dissolution of middle manganese can effectively improve lithium ion battery capacity fade problem during charge and discharge cycles.
Preferably, drying temperature is 50~70 DEG C when drying in step a and c.
Preferably, drying temperature is 60 DEG C when drying in step c.
Lower drying temperature is controlled, one can reduce the consumption of the energy, and two can prevent the heat in overtemperature
Manganese, lithium migrate in discarded cigarette butt under effect, and manganese, lithium is caused to be unevenly distributed.
Preferably, discarding cigarette butt soaking time in mixed liquor in step c is 0.5~3 hour.
Preferably, soluble manganese salt is one of manganese acetate, manganese nitrate, manganese sulfate or manganese chloride.
Preferably, soluble lithium salt is lithium nitrate or lithium sulfate.
Preferably, in step d, heating rate when calcining is 1~10 DEG C per minute.
Preferably, in step d, heating rate when calcining is 1 DEG C per minute.
The heating rate of reduction is set in calcination process, the decomposable process of acetate fiber can be made more slowly, it can also be with
So that the rate that gas is generated in decomposable process is slower, it in this way can be in the manganese for guaranteeing the suitable gas impact hollow structure of generation
While sour lithium material tube wall, guarantee will not be too big because generating gas velocity, thoroughly destroys the hollow tubular knot of lithium manganate material
Structure.
Therefore, the invention has the following advantages:
(1) lithium manganate material produced by the present invention is hollow tubular structure, and tube wall is open structure, can alleviate charge and discharge
Volume expansion in electric process improves the cycle performance of lithium ion battery；
(2) lithium manganate material produced by the present invention is the lithium manganate material for adulterating micro titanium elements, and crystal structure is more steady
It is fixed, the dissolution of manganese in use process can be reduced, lithium ion battery capacity attenuation during charge and discharge cycles can be improved and asked
Topic.
Detailed description of the invention
Fig. 1 is the X ray diffracting spectrum of lithium manganate material produced by the present invention；
Fig. 2 is the surface sweeping electron microscope of lithium manganate material produced by the present invention；
Fig. 3 is the high rate performance figure of lithium manganate material produced by the present invention；
Fig. 4 is 1C charge and discharge electric energy figure under the room temperature of lithium manganate material produced by the present invention；
Fig. 5 is 1C charge and discharge electric energy figure at 60 DEG C of lithium manganate material produced by the present invention.
Specific embodiment
Further description of the technical solution of the present invention With reference to embodiment.
Embodiment 1
A kind of lithium ion battery lithium manganate material synthetic method, comprising the following steps:
A) discarded cigarette butt is collected, is dried after cleaning, drying temperature is 60 DEG C；
B) by the lithium nitrate solution of the manganese nitrate solution of 0.2mol/L and 0.1mol/L according to the ratio of manganese lithium molar ratio 2:1
Mixing, and mixed liquor is obtained after being ultrasonically treated；
C) by treated in step a, cigarette butt takes 10g to be immersed in the mixed liquor that step b is obtained, and mixed liquor is made not have cigarette
Head takes out and dries after immersion；Discarded cigarette butt soaking time in mixed liquor is 1 hour, and drying temperature is 60 DEG C；
It d) will treated that cigarette butt calcines 3 hours in 700 DEG C of air atmospheres obtains lithium manganate material through step c；Calcining
When heating rate be 1 DEG C per minute.
Embodiment 2
A kind of lithium ion battery lithium manganate material synthetic method, comprising the following steps:
A) discarded cigarette butt is collected, is dried after cleaning, drying temperature is 50 DEG C；
B) by the lithium nitrate solution of the acetic acid manganese solution of 0.1mol/L and 0.1mol/L according to the ratio of manganese lithium molar ratio 2:1
Mixing, and mixed liquor is obtained after being ultrasonically treated；
C) by treated in step a, cigarette butt takes 3g to be immersed in the mixed liquor that step b is obtained, and mixed liquor is made not have cigarette
Head takes out and dries after immersion；Discarded cigarette butt soaking time in mixed liquor is 0.5 hour, and drying temperature is 50 DEG C；
It d) will treated that cigarette butt calcines 2 hours in 600 DEG C of air atmospheres obtains lithium manganate material through step c；Calcining
When heating rate be 1 DEG C per minute.
Embodiment 3
A kind of lithium ion battery lithium manganate material synthetic method, comprising the following steps:
A) discarded cigarette butt is collected, is dried after cleaning, drying temperature is 60 DEG C；
B) lithium sulfate solution of the manganese sulfate solution of 4mol/L and 2mol/L are mixed according to the ratio of manganese lithium molar ratio 2:1
It closes, and obtains mixed liquor after being ultrasonically treated；
C) by treated in step a, cigarette butt takes 15g to be immersed in the mixed liquor that step b is obtained, and mixed liquor is made not have cigarette
Head takes out and dries after immersion；Discarded cigarette butt soaking time in mixed liquor is 1.5 hours, and drying temperature is 60 DEG C；
It d) will treated that cigarette butt calcines 5 hours in 650 DEG C of air atmospheres obtains lithium manganate material through step c；Calcining
When heating rate be 3 DEG C per minute.
Embodiment 4
A kind of lithium ion battery lithium manganate material synthetic method, comprising the following steps:
A) discarded cigarette butt is collected, is dried after cleaning, drying temperature is 70 DEG C；
B) lithium sulfate solution of the manganese chloride solution of 5mol/L and 5mol/L are mixed according to the ratio of manganese lithium molar ratio 2:1
It closes, and obtains mixed liquor after being ultrasonically treated；
C) by treated in step a, cigarette butt takes 40g to be immersed in the mixed liquor that step b is obtained, and mixed liquor is made not have cigarette
Head takes out and dries after immersion；Discarded cigarette butt soaking time in mixed liquor is 3 hours, and drying temperature is 70 DEG C；
It d) will treated that cigarette butt calcines 8 hours in 800 DEG C of air atmospheres obtains lithium manganate material through step c；Calcining
When heating rate be 10 DEG C per minute.
Properties Testing:
1.XRD structured testing:
As shown in Figure 1, being prepared map of the lithium manganate material after XRD is tested and spinel-type manganese in above-described embodiment
The standard card JCPDS NO.35-0782 of sour lithium material compares, and can clearly tell in lithium manganate having spinel structure
(111), each corresponding diffraction maximum such as (311), (222), (331), (511), (440) and (531), wherein there are Mn in figure2O3
Diffraction maximum illustrates that there are micro Mn in the lithium manganate material of synthesis2O3, these micro Mn2O3Be in calcination process due to
Caused by high temperature causes Li to volatilize.
2. Scanning Electron microscopy surface pattern test:
As shown in Fig. 2, lithium manganate material made from above-described embodiment carries out the test of Scanning Electron microscopy surface micromorphology,
By Fig. 2 it can be found that the lithium manganate material synthesized is hollow tubular, tube wall is coarse, protects with the appearance of acetate fiber in discarded cigarette butt
It holds similar.
3. lithium ion battery high rate performance is tested:
As shown in figure 3, lithium manganate material made from above-described embodiment assembles lithium ion battery according to the prior art, and to phase
The lithium ion battery answered carries out high rate performance test, by Fig. 3 it can be found that the ratio that discharges under the small multiplying power of lithium ion battery obtained
Capacity maintains 100mAh/g or more, even if specific discharge capacity also in 50mAh/g or more, has good under 50C multiplying power
High rate performance.
4. lithium ion battery charge-discharge performance is tested:
As shown in Figure 4,5, lithium manganate material made from above-described embodiment assembles lithium ion battery according to the prior art, and right
Corresponding lithium ion battery carries out the test of room temperature charge-discharge performance and the test of high temperature (60 DEG C) charge-discharge performance respectively；
Available from figure 4, its specific discharge capacity still maintains 120mAh/g or more after 1000 cycle charge-discharges；It can be obtained by Fig. 5,
At high temperature (60 DEG C), its specific discharge capacity still maintains 110mAh/g after 1000 cycle charge-discharges.Therefore,
Lithium manganate material made from above-described embodiment, which whether all has under room temperature or high temperature, measures high cycle performance.
Claims (6)
1. a kind of lithium ion battery lithium manganate material synthetic method, it is characterised in that the following steps are included:
A) discarded cigarette butt is collected, is dried after cleaning；
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 molar ratio 2:1
Example mixing, and mixed liquor is obtained after being ultrasonically treated；The soluble manganese salt is manganese acetate, manganese nitrate, manganese sulfate or manganese chloride
One of, the soluble lithium salt is lithium nitrate or lithium sulfate；
C) by treated in step a, cigarette butt takes 3~40g to be immersed in the mixed liquor that step b is obtained, and mixed liquor is made not have cigarette
Head takes out and dries after immersion；
It d) will treated that cigarette butt calcines 2~8 hours at 600~800 DEG C obtains lithium manganate material through step c.
2. a kind of lithium ion battery lithium manganate material synthetic method according to claim 1, it is characterised in that: the step
When drying in rapid a and c, drying temperature is 50~70 DEG C.
3. a kind of lithium ion battery lithium manganate material synthetic method according to claim 1 or 2, it is characterised in that: institute
It states when being dried in step c, drying temperature is 60 DEG C.
4. a kind of lithium ion battery lithium manganate material synthetic method according to claim 1, it is characterised in that: the step
It is 0.5~3 hour that cigarette butt soaking time in mixed liquor is discarded in rapid c.
5. a kind of lithium ion battery lithium manganate material synthetic method according to claim 1, it is characterised in that: the step
In rapid d, heating rate when calcining is 1~10 DEG C per minute.
6. a kind of lithium ion battery lithium manganate material synthetic method according to claim 1 or 5, it is characterised in that: institute
It states in step d, heating rate when 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 |
|---|
| 尖晶石锰酸锂的制备与改性研究;刘立振;《中国优秀硕士学位论文全文数据库工程科技Ⅱ辑》;20150215;第C042-1335页 |
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