CN108155372A - A kind of lithium titanate material and its preparation and application - Google Patents
A kind of lithium titanate material and its preparation and application Download PDFInfo
- Publication number
- CN108155372A CN108155372A CN201611098897.1A CN201611098897A CN108155372A CN 108155372 A CN108155372 A CN 108155372A CN 201611098897 A CN201611098897 A CN 201611098897A CN 108155372 A CN108155372 A CN 108155372A
- Authority
- CN
- China
- Prior art keywords
- lithium titanate
- titanate material
- material described
- powder
- fluorographite
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- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 70
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 68
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 239000000463 material Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 18
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000003990 capacitor Substances 0.000 claims abstract description 5
- 239000007772 electrode material Substances 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract description 4
- -1 modified lithium titanate Chemical class 0.000 claims abstract 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical group CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 3
- 239000011737 fluorine Substances 0.000 claims description 3
- 229910052731 fluorine Inorganic materials 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 229910052796 boron Inorganic materials 0.000 claims description 2
- 239000003610 charcoal Substances 0.000 claims description 2
- 239000002019 doping agent Substances 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 206010016766 flatulence Diseases 0.000 abstract description 6
- 239000006228 supernatant Substances 0.000 description 6
- 125000005909 ethyl alcohol group Chemical group 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 238000002604 ultrasonography Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
Classifications
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
-
- 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
-
- 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
-
- 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
- Y02E60/13—Energy storage using capacitors
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Power Engineering (AREA)
- Inorganic Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The present invention relates to a kind of modified lithium titanate materials, are 100 in mass ratio by lithium titanate powder and fluorinated graphene and/or fluorographite:1~1:4 mix.It is used in lithium titanate battery or lithium titanate capacitor use as electrode material.Effectively inhibit lithium titanate battery flatulence problem.
Description
Technical field
The present invention relates to electrochemical energy storage field, specifically, referring to lithium titanate battery and lithium titanate capacitor.
Background technology
Spinel type lithium titanate (LTO) due to not deformed upon substantially in charge and discharge process, is referred to as zero strain
Electrode material.With good application prospect.The advantage major embodiment of LTO is in the following areas：1st, LTO has larger lithium ion
Solid diffusion coefficient, has the performance of excellent quick charge repid discharge (5 minutes>80%DOD)；The cathode phase such as 2 and graphite
There is fine cryogenic property than LTO；3rd, safety is good.Be not in the security risks such as the analysis Li dendrite of the cathode such as graphite.4th, it is excellent
Different cycle performance.To sum up, it is considered as one since lithium titanate material has excellent structural stability and security performance
The excellent negative material of kind dynamic lithium battery and mixed capacitor has wide in terms of electric vehicle and extensive energy storage
Application prospect.
But it is not carried out ripe industrialized development so far, main cause is lithium titanate battery in charge and discharge cycles and storage
There are problems that " inflatable " during depositing, i.e., inside battery constantly generates gas, and battery performance is caused drastically to decline, this is to restrict in fact
The biggest obstacle of border application, and become industry common recognition.Only solve the problems, such as flatulence, lithium titanate battery could be really practical
Change.
Invention content
To solve technical problem underlying mentioned above, provide it is a kind of have the function of the lithium titanate of inhibition flatulence very well and
Preparation method.
In order to achieve the above objectives, the specific technical solution that uses of the present invention is prepared containing fluorinated graphene (or fluorination
Graphite) lithium titanate material, realize fluorinated graphene (or fluorographite) to lithium titanate protect, inhibit flatulence.
It is 100 in mass ratio by lithium titanate powder and fluorinated graphene and/or fluorographite:1~1:4 mix.
The mass ratio of the lithium titanate powder and fluorinated graphene and/or fluorographite is 20:1~1:2.
The lithium titanate powder is lithium titanate, one or two kinds of mixing in doped lithium titanate；The grain of lithium titanate powder
Spend is 0.02 micron -100 microns；
In doped lithium titanate dopant elements be aluminium, boron, potassium, manganese, nickel, iron oxide red it is one or more kinds of, doping
0.01wt%-10wt%.
The fluorinated graphene or the fluorine charcoal ratio of fluorographite are 0.3-1.3, wherein being preferably 0.6-1.2, most
That excellent is 0.8-1.1.
The preparation method of the lithium titanate material is by lithium titanate powder and fluorinated graphene and/or fluorographite, is put
Enter in solvent, ultrasonic disperse 0.1-12 hours, centrifuge, remove supernatant, will be deposited in 70 degree -120 degree vacuum drying to get to
Lithium titanate material.
The supersonic frequency is set as 20-50KHZ.
The solvent is acetone, one or more kinds of mixing in ethyl alcohol, isopropanol, formic acid, acetic acid, butanol
Object；It is preferably one or two kinds of in acetone, ethyl alcohol.
Mass ratio 1%-50% of the lithium titanate powder in solvent.
The lithium titanate material is used in lithium titanate battery or lithium titanate capacitor use as electrode material.The present invention's
Advantageous effect
In ultrasonic procedure, realize fluorinated graphene (or fluorographite) and lithium titanate is effectively compound, fluorographite
The fluorine on surface and the hydroxyl of lithium titanate form hydrogen bond, make lithium titanate surface passivation, and then inhibit lithium titanate flatulence.
Specific embodiment
Embodiment 1,
Lithium titanate powder 10g, the fluorinated graphene 5g that granularity is 10 microns are put into 100ml absolute ethyl alcohols, ultrasound point
It dissipates 10 hours, centrifugation removes supernatant, will be deposited in 100 degree of vacuum drying to get to the lithium titanate material containing fluorinated graphene
Material.
Embodiment 2,
By lithium titanate powder 10g, the fluorographite 4g that granularity is 20 microns, it is put into 100ml acetone, ultrasonic disperse 12 is small
When, centrifugation removes supernatant, will be deposited in 80 degree of vacuum drying to get to the lithium titanate material containing fluorinated graphene.
Embodiment 3,
Lithium titanate powder 10g, the fluorinated graphene 5g that granularity is 50 microns are put into 100ml absolute ethyl alcohols, ultrasound point
It dissipates 10 hours, centrifugation removes supernatant, will be deposited in 100 degree of vacuum drying to get to the lithium titanate material containing fluorinated graphene
Material.
Embodiment 4,
Lithium titanate powder 10g, the fluorinated graphene 5g that granularity is 1 micron are put into 100ml absolute ethyl alcohols, ultrasound point
It dissipates 10 hours, centrifugation removes supernatant, will be deposited in 100 degree of vacuum drying to get to the lithium titanate material containing fluorinated graphene
Material.
Comparative example 1,
By the lithium titanate powder 10g that granularity is 10 microns, it is put into 100ml absolute ethyl alcohols, ultrasonic disperse 10 hours, from
The heart removes supernatant, will be deposited in 100 degree of vacuum drying to get to the lithium titanate material of comparison.
Table 1 is assembled into 053048 type rectangular cell for lithium titanate battery and recycles thickness variation data and battery energy density
(being based on active material), test condition are 60 degrees Celsius, 2C charge and discharge cycles, blanking voltage 1.6-2.8V.
Table 1
As can be seen that the lithium titanate group in lithium titanate material and comparative example containing fluorinated graphene (or fluorographite)
The battery of dress is compared, and the thickness change of battery is significantly much smaller；Illustrate that fluorinated graphene (or fluorographite) can be good at
Inhibit lithium titanate flatulence, but also do not interfere with the energy density of battery.
Claims (9)
1. a kind of modified lithium titanate material, it is characterised in that：
It is 100 in mass ratio by lithium titanate powder and fluorinated graphene and/or fluorographite:1~1:4 mix.
2. according to lithium titanate material described in claim 1, it is characterised in that：
The mass ratio of the lithium titanate powder and fluorinated graphene and/or fluorographite is 20:1~1:2.
3. according to lithium titanate material described in claim 1, it is characterised in that：
The lithium titanate powder is lithium titanate, one or two kinds of mixing in doped lithium titanate；The granularity of lithium titanate powder is
0.02 micron -100 microns；
In doped lithium titanate dopant elements be aluminium, boron, potassium, manganese, nickel, iron oxide red it is one or more kinds of, doping 0.01wt%-
10wt%.
4. according to lithium titanate material described in claim 1, it is characterised in that：
The fluorinated graphene or the fluorine charcoal ratio of fluorographite are 0.3-1.3, wherein be preferably 0.6-1.2, it is optimal
It is 0.8-1.1.
5. according to lithium titanate material described in claim 1, it is characterised in that：The preparation method of the lithium titanate material is by metatitanic acid
Lithium powder and fluorinated graphene and/or fluorographite, are put into solvent, ultrasonic disperse 0.1-12 hours, centrifugation, in removing
Clear liquid will be deposited in 70 degree of -120 degree vacuum drying to get to lithium titanate material.
6. according to lithium titanate material described in claim 5, it is characterised in that：
The supersonic frequency is set as 20-50KHZ.
7. according to lithium titanate material described in claim 6, it is characterised in that：
The solvent is acetone, one or more kinds of mixtures in ethyl alcohol, isopropanol, formic acid, acetic acid, butanol.
8. according to lithium titanate material described in claim 5, it is characterised in that：Mass ratio 1%- of the lithium titanate powder in solvent
50%.
9. according to lithium titanate material described in claim 1-8, it is characterised in that：The lithium titanate material is used for as electrode material
It is used in lithium titanate battery or lithium titanate capacitor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611098897.1A CN108155372B (en) | 2016-12-04 | 2016-12-04 | Lithium titanate material and preparation and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611098897.1A CN108155372B (en) | 2016-12-04 | 2016-12-04 | Lithium titanate material and preparation and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108155372A true CN108155372A (en) | 2018-06-12 |
| CN108155372B CN108155372B (en) | 2020-05-26 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611098897.1A Active CN108155372B (en) | 2016-12-04 | 2016-12-04 | Lithium titanate material and preparation and application thereof |
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| Country | Link |
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| CN (1) | CN108155372B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111244402A (en) * | 2018-11-29 | 2020-06-05 | 中国科学院大连化学物理研究所 | Fluorinated graphene modified lithium titanate material, preparation and application |
| CN114551844A (en) * | 2022-03-01 | 2022-05-27 | 深圳博磊达新能源科技有限公司 | Lithium titanate composite negative electrode material and preparation method thereof |
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2016
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Patent Citations (5)
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| CN114551844B (en) * | 2022-03-01 | 2024-07-05 | 深圳博磊达新能源科技有限公司 | Lithium titanate composite negative electrode material and preparation method thereof |
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| CN108155372B (en) | 2020-05-26 |
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