CN104409715A - Preparation method of high-performance nitrogen-doped carbon-coated lithium titanate composite anode material of lithium ion battery - Google Patents
Preparation method of high-performance nitrogen-doped carbon-coated lithium titanate composite anode material of lithium ion battery Download PDFInfo
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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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
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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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 relates to the technical field of preparation of electrode materials of lithium ion batteries and in particular discloses a preparation method of a high-performance nitrogen-doped carbon-coated lithium titanate composite anode material of a lithium ion battery. The method comprises the following steps: firstly adding a lithium source, nano titanium dioxide and tripolycyanamide into a ball according to a certain material ratio, taking absolute ethyl alcohol as a medium, ball milling and then spray drying, subsequently calcining the materials under the inert atmosphere condition, ball milling and screening to obtain a nitrogen-doped carbon-compounded lithium titanate material which is applied to the anode material of the lithium ion battery and is high in electrochemical performance. The preparation method of the high-performance nitrogen-doped carbon-coated lithium titanate composite anode material of the lithium ion battery is simple in process; the prepared anode material is high in reversible capacity and excellent in high-magnification cycle performance.
Description
Technical field
The present invention relates to the preparing technical field of lithium ion battery electrode material, be specifically related to the preparation method of the coated lithium titanate composite lithium ion battery cathode material of a kind of high-performance nitrogen-doped carbon.
Background technology
Lithium titanate (Li
4ti
5o
12) be a kind of " zero strain " material, there is not corresponding contraction and expansion in its lattice in lithium ion deintercalation and telescopiny, so material structure is highly stable, cycle performance is also better.Lithium titanate charge and discharge platform is greatly about about 1.55V, and theoretical specific capacity is 175mAh/g, and actual specific capacity can reach 165mAh/g, and capacity contribution concentrates on land regions.In addition, lithium titanate, compared with commercial carbon negative pole material, has larger diffusion coefficient under normal temperature, usually have better chemical property and fail safe.But lithium titanate poorly conductive, under high magnification environment, special capacity fade is rapid, and adulterating coated is improve the most effective means of its performance.
Summary of the invention
For the deficiencies in the prior art, the object of the present invention is to provide a kind of preparation method of new lithium titanate composite lithium ion battery cathode material, the preparation for high-performance commercial Li-ion battery negative material provides a new approach.
Lithium salts, nano titanium oxide and melamine are first passed through wet ball grinding spraying dry by the present invention by a certain percentage, then calcine under inert atmosphere conditions, namely obtain lithium ion battery negative material with the cooled just sample of stove after ball milling screening.Abundant raw material source of the present invention, preparation technology is simple, the negative material excellent conductivity prepared, and reversible capacity is high, and cycle performance is excellent.
Object of the present invention is achieved particular by following technical scheme.
A preparation method for the lithium titanate composite lithium ion battery cathode material that high-performance nitrogen-doped carbon is coated, step is as follows:
(1) lithium source, nano titanium oxide and melamine being joined (rotating speed of ball mill is 2000 revs/min) in ball mill according to certain material ratio, take absolute ethyl alcohol as medium ball milling 1 hour;
(2) by gained slurry spraying dry after ball milling, powder mixture material is obtained;
(3) by gained powder mixture material under an inert atmosphere from room temperature to 700 DEG C, and keep 3 hours, after cooling, obtain the lithium titanate composite material head product that nitrogen-doped carbon is coated;
(4) by head product ball-milling treatment 4 hours (rotating speed of ball mill is 2000 revs/min) in ball mill, after crossing 200 mesh sieves, the lithium titanate composite material that high-performance nitrogen-doped carbon is coated is namely obtained.
Described lithium source is lithium carbonate or lithium hydroxide.
Described nano titanium oxide is anatase titanium dioxide, particle diameter 10-20nm, purity >99%, specific area 80m
2/ g.
Described inert atmosphere conditions is nitrogen or argon gas atmosphere.
The speed heated up in described step (3) is 3 DEG C/min.
The ratio of described lithium source (in elemental lithium), nano titanium oxide amount of substance is 1:1, the quality adding melamine is lithium source, both titanium dioxide quality sum 2.5% ~ 10%.
Compared with prior art, the advantage of the inventive method and beneficial effect are:
Add the high melamine of nitrogen content by original position, make lithium titanate add the carbon source of rich nitrogen type in the preparation, after heat treatment, define the lithium titanate composite material that nitrogen-doped carbon is coated.Nitrogen-atoms is in the ortho position of carbon atom in the periodic table of elements, radius is close, but its electronegativity is higher than carbon, therefore nitrogen atom doping can keep lattice structure and the duct of carbon, the extra lone pair electrons of nitrogen-atoms can give the negative electrical charge of carbon skeleton extended system, thus effectively improve the surface polarity of carbon, strengthen transmission performance and the chemical reactivity of electronics.Effectively enhance lithium titanate conductivity and electrochemical reaction performance.Preparation technology of the present invention is simple, cheap in a word, utilizes the property that N doping shows, and the material prepared has the plurality of advantages such as efficiency for charge-discharge is high, discharge and recharge reaction good reversibility, Stability Analysis of Structures, cycle performance are excellent.
Accompanying drawing explanation
The scanning electron microscope (SEM) photograph of the coated lithium titanate composite lithium ion battery cathode material of high-performance nitrogen-doped carbon prepared by Fig. 1 embodiment 3.
The CV curve chart of the coated lithium titanate composite lithium ion battery cathode material of high-performance nitrogen-doped carbon prepared by Fig. 2 embodiment 3.
X-the ray powder diffraction pattern of material prepared by Fig. 3 embodiment 1 ~ 4 and comparative example.
The discharge curve of material under 1C condition prepared by Fig. 4 embodiment 1 ~ 4 and comparative example.
Fig. 1 result shows, the coated lithium titanate composite material of the high-performance nitrogen-doped carbon prepared of embodiment 3 is graininess, and the product pattern obtained by other embodiments is consistent with embodiment 3, does not repeat.Fig. 2 show by embodiment 3 resulting materials assemble half-cell before 3 weeks CV curve (Shanghai Chen Hua Instrument Ltd. produce CHI660E electrochemical workstation on test, test condition is 1.0 ~ 2.5V, sweeps fast 0.1mVs
-1),
Obvious redox peak is there is in figure.Fig. 3 is the x-ray diffraction pattern of each embodiment and comparative example, corresponding with numbering 49-0207 lithium titanate crystal diffraction peak in standard card JCPDS, demonstrates pure phase face-centered cubic spinel type lithium titanate structure.Fig. 4 result shows, combination electrode material prepared by embodiment 1 ~ 4 has good chemical property, good cycling stability, mainly because the introducing of N element makes material surface polarity improve, the transmission performance of electronics and chemical reactivity strengthen, and make materials exhibit go out excellent chemical property.The material that embodiment 1 ~ 4 and comparative example are prepared is under 1C condition, and initial discharge capacity is 224.8mAh/g, 205.2mAh/g, 176.7mAh/g, 214.0mAh/g, 141.7mAh/g respectively; After circulating 100 weeks, discharge capacity is respectively: 109.4mAh/g, 116.8mAh/g, 159.9mAh/g, 139.3mAh/g, 89.7mAh/g.
Embodiment
Applicant will be described in further detail the inventive method in conjunction with specific embodiments below, and object is to enable those skilled in the art be expressly understood the present invention.Following examples should not be understood to the restriction to claims of the present invention request protection range in any degree.
Raw material lithium source used in following examples and comparative example, nano titanium oxide (anatase titanium dioxide, particle diameter 10-20nm, purity >99%, specific area 80m
2/ g), melamine, absolute ethyl alcohol be conventional analysis pure reagent, all purchased from Shanghai Chemical Reagent Co., Ltd., Sinopharm Group.
Embodiment 1
A preparation method for the lithium titanate composite lithium ion battery cathode material that high-performance nitrogen-doped carbon is coated, step is as follows:
Lithium hydroxide, nano titanium oxide and melamine are joined (rotating speed of ball mill is 2000 revs/min) in ball mill, take absolute ethyl alcohol as medium ball milling 1 hour (rotating speed of ball mill is 2000 revs/min), wherein the ratio of the amount of substance of lithium hydroxide and nano titanium oxide is 1:1, the quality of melamine be lithium hydroxide, nano titanium oxide quality sum 2.5%.By gained slurry spraying dry after ball milling, obtain powder mixture material.Gained powder mixture material is pressed in a nitrogen atmosphere ramp to the 700 DEG C calcining of 3 DEG C/min from room temperature, and be incubated 3 hours, after cooling, obtain the lithium titanate composite material head product that nitrogen-doped carbon is coated.By head product ball-milling treatment 4 hours (rotating speed of ball mill is 2000 revs/min) in ball mill, after crossing 200 mesh sieves, namely obtain the lithium titanate composite material that high-performance nitrogen-doped carbon is coated.
Embodiment 2
A preparation method for the lithium titanate composite lithium ion battery cathode material that high-performance nitrogen-doped carbon is coated, step is as follows:
Lithium carbonate, nano titanium oxide and melamine are joined (rotating speed of ball mill is 2000 revs/min) in ball mill, take absolute ethyl alcohol as medium ball milling 1 hour (rotating speed of ball mill is 2000 revs/min), wherein the ratio of the amount of substance of lithium carbonate and nano titanium oxide is 0.5:1, the quality of melamine be lithium carbonate, nano titanium oxide quality sum 7.5%.By gained slurry spraying dry after ball milling, obtain powder mixture material.Gained powder mixture material is pressed under an argon atmosphere ramp to the 700 DEG C calcining of 3 DEG C/min from room temperature, and be incubated 3 hours, after cooling, obtain the lithium titanate composite material head product that nitrogen-doped carbon is coated.By head product ball-milling treatment 4 hours (rotating speed of ball mill is 2000 revs/min) in ball mill, after crossing 200 mesh sieves, namely obtain the lithium titanate composite material that high-performance nitrogen-doped carbon is coated.
Embodiment 3
A preparation method for the lithium titanate composite lithium ion battery cathode material that high-performance nitrogen-doped carbon is coated, step is as follows:
Lithium hydroxide, nano titanium oxide and melamine are joined (rotating speed of ball mill is 2000 revs/min) in ball mill, take absolute ethyl alcohol as medium ball milling 1 hour (rotating speed of ball mill is 2000 revs/min), wherein the ratio of the amount of substance of lithium hydroxide and nano titanium oxide is 1:1, the quality of melamine be lithium hydroxide, nano titanium oxide quality sum 5%.By gained slurry spraying dry after ball milling, obtain powder mixture material.Gained powder mixture material is pressed in a nitrogen atmosphere ramp to the 700 DEG C calcining of 3 DEG C/min from room temperature, and be incubated 3 hours, after cooling, obtain the lithium titanate composite material head product that nitrogen-doped carbon is coated.By head product ball-milling treatment 4 hours (rotating speed of ball mill is 2000 revs/min) in ball mill, after crossing 200 mesh sieves, namely obtain the lithium titanate composite material that high-performance nitrogen-doped carbon is coated.
Embodiment 4
A preparation method for the lithium titanate composite lithium ion battery cathode material that high-performance nitrogen-doped carbon is coated, step is as follows:
Lithium hydroxide, nano titanium oxide and melamine are joined (rotating speed of ball mill is 2000 revs/min) in ball mill, take absolute ethyl alcohol as medium ball milling 1 hour (rotating speed of ball mill is 2000 revs/min), wherein the ratio of the amount of substance of lithium hydroxide and nano titanium oxide is 1:1, the quality of melamine be lithium hydroxide, nano titanium oxide quality sum 10%.By gained slurry spraying dry after ball milling, obtain powder mixture material.Gained powder mixture material is pressed under an argon atmosphere ramp to the 700 DEG C calcining of 3 DEG C/min from room temperature, and be incubated 3 hours, after cooling, obtain the lithium titanate composite material head product that nitrogen-doped carbon is coated.By head product ball-milling treatment 4 hours (rotating speed of ball mill is 2000 revs/min) in ball mill, after crossing 200 mesh sieves, namely obtain the lithium titanate composite material that high-performance nitrogen-doped carbon is coated.
Comparative example 1
Being that 1:1 joins (rotating speed of ball mill is 2000 revs/min) in ball mill by lithium hydroxide, nano titanium oxide by the ratio of amount of substance, take absolute ethyl alcohol as medium ball milling 1 hour (rotating speed of ball mill is 2000 revs/min).By gained slurry spraying dry after ball milling, obtain powder mixture material.Gained powder mixture material is pressed under an argon atmosphere ramp to the 700 DEG C calcining of 3 DEG C/min from room temperature, and be incubated 3 hours, after cooling, obtain lithium titanate head product.By head product ball-milling treatment 4 hours (rotating speed of ball mill is 2000 revs/min) in ball mill, after crossing 200 mesh sieves, namely obtain lithium titanate material.
Respectively the lithium ion battery negative material that embodiment 1 ~ 4 and comparative example 1 obtain is made half-cell and carry out chemical property mensuration, half-cell assembly method is as follows:
Be 80wt%:15wt%:5wt% mixing in mass ratio by testing sample, Super P Li conductive black and polyvinylidene fluoride (A Kema Kynoar binding agent HSV900 type), mix well with 1-METHYLPYRROLIDONE, stir into thick, be coated on Copper Foil, at 80 DEG C, vacuum (-0.1MPa), drying 20 hours, is cut into the circular film that diameter is about 1cm after cooling.Half-cell adopts CR2016 type button cell to assemble in glove box, and barrier film is Celgard 2400 polypropylene diaphragm, and electrolyte is 1M LiPF
6ethylene carbonate (EC) (in mixed electrolytic solution, the volume ratio of EC, DEC is 1:1, LiPF in mixed electrolytic solution with diethyl carbonate (DEC) mixed electrolytic solution
6concentration is 1M), be circular lithium sheet (diameter 1.5cm) of commercialization to electrode, electrochemical property test carries out on indigo plant electric CT2001A type battery test system (Wuhan Land Electronic Co., Ltd.'s production).
Claims (4)
1. a preparation method for the lithium titanate composite lithium ion battery cathode material that high-performance nitrogen-doped carbon is coated, step is as follows:
(1) joining in ball mill by lithium source, nano titanium oxide and melamine according to certain material ratio, take absolute ethyl alcohol as medium ball milling 1 hour;
(2) by gained slurry spraying dry after ball milling, powder mixture material is obtained;
(3) by gained powder mixture material under an inert atmosphere from room temperature to 700 DEG C, and keep 3 hours, after cooling, obtain the lithium titanate composite material head product that nitrogen-doped carbon is coated;
(4) by head product ball-milling treatment 4 hours in ball mill, after crossing 200 mesh sieves, the lithium titanate composite material that high-performance nitrogen-doped carbon is coated is namely obtained;
Described lithium source is lithium carbonate or lithium hydroxide;
Described lithium source in the ratio of elemental lithium, nano titanium oxide amount of substance for 1:1, the quality adding melamine is lithium source, both titanium dioxide quality sum 2.5% ~ 10%.
2. preparation method according to claim 1, is characterized in that: described nano titanium oxide is anatase titanium dioxide, particle diameter 10-20 nm, purity >99%, specific area 80 m
2/ g.
3. preparation method according to claim 1, is characterized in that: described inert atmosphere conditions is nitrogen or argon gas atmosphere.
4. preparation method according to claim 1, is characterized in that: the speed heated up in described step (3) is 3 DEG C/min.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104979556A (en) * | 2015-05-15 | 2015-10-14 | 三峡大学 | Nitrogen-doped Cu3P/C-Cu lithium-ion battery negative electrode material and preparation method thereof |
| CN105206820A (en) * | 2015-09-16 | 2015-12-30 | 湖北工程学院 | High-performance lithium titanate composite electrode material and preparation method thereof |
| CN105470477A (en) * | 2015-11-12 | 2016-04-06 | 南阳师范学院 | Preparation method of high-performance nitrogen-doped and carbon-coated Ti<2>Nb<10>O<29> composite electrode material |
| CN105529465A (en) * | 2016-02-26 | 2016-04-27 | 南阳师范学院 | Nitrogen-doped carbon-coated titanium niobate composite electrode material and preparation method thereof |
| CN106450265A (en) * | 2016-12-06 | 2017-02-22 | 长沙理工大学 | In-situ nitrogen-doped carbon coated lithium titanate composite electrode material and preparation method thereof |
| CN107492647A (en) * | 2017-08-16 | 2017-12-19 | 深圳市比克动力电池有限公司 | Lithium ion battery negative material, cathode material preparation method and lithium ion battery |
| CN107732175A (en) * | 2017-09-26 | 2018-02-23 | 山东大学 | A kind of graphene and the common coated porous lithium titanate of nitrogen-doped carbon and preparation method thereof |
| CN107814534A (en) * | 2017-11-13 | 2018-03-20 | 河海大学 | It is a kind of can be with the eco-concrete and preparation method thereof of algal control, antimicrobial corrosion |
| CN109319830A (en) * | 2018-11-13 | 2019-02-12 | 北方奥钛纳米技术有限公司 | Lithium titanate material and preparation method thereof, negative electrode tab, battery |
| CN114551858A (en) * | 2022-03-01 | 2022-05-27 | 深圳博磊达新能源科技有限公司 | Lithium titanate composite material and preparation method thereof |
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| CN102013476A (en) * | 2010-11-04 | 2011-04-13 | 苏州大学 | Method for preparing lithium titanate/titanium nitride composite material |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104979556A (en) * | 2015-05-15 | 2015-10-14 | 三峡大学 | Nitrogen-doped Cu3P/C-Cu lithium-ion battery negative electrode material and preparation method thereof |
| CN105206820A (en) * | 2015-09-16 | 2015-12-30 | 湖北工程学院 | High-performance lithium titanate composite electrode material and preparation method thereof |
| CN105470477A (en) * | 2015-11-12 | 2016-04-06 | 南阳师范学院 | Preparation method of high-performance nitrogen-doped and carbon-coated Ti<2>Nb<10>O<29> composite electrode material |
| CN105529465A (en) * | 2016-02-26 | 2016-04-27 | 南阳师范学院 | Nitrogen-doped carbon-coated titanium niobate composite electrode material and preparation method thereof |
| CN106450265A (en) * | 2016-12-06 | 2017-02-22 | 长沙理工大学 | In-situ nitrogen-doped carbon coated lithium titanate composite electrode material and preparation method thereof |
| CN106450265B (en) * | 2016-12-06 | 2018-11-16 | 长沙理工大学 | A kind of situ Nitrogen Doping carbon coating lithium titanate combination electrode material and preparation method thereof |
| CN107492647A (en) * | 2017-08-16 | 2017-12-19 | 深圳市比克动力电池有限公司 | Lithium ion battery negative material, cathode material preparation method and lithium ion battery |
| CN107732175A (en) * | 2017-09-26 | 2018-02-23 | 山东大学 | A kind of graphene and the common coated porous lithium titanate of nitrogen-doped carbon and preparation method thereof |
| CN107814534A (en) * | 2017-11-13 | 2018-03-20 | 河海大学 | It is a kind of can be with the eco-concrete and preparation method thereof of algal control, antimicrobial corrosion |
| CN109319830A (en) * | 2018-11-13 | 2019-02-12 | 北方奥钛纳米技术有限公司 | Lithium titanate material and preparation method thereof, negative electrode tab, battery |
| CN114551858A (en) * | 2022-03-01 | 2022-05-27 | 深圳博磊达新能源科技有限公司 | Lithium titanate composite material and preparation method thereof |
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| C06 | Publication | ||
| PB01 | Publication | ||
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Application publication date: 20150311 |