CN107244693B - Li0.5TiO2Method for preparing powder material - Google Patents
Li0.5TiO2Method for preparing powder material Download PDFInfo
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- CN107244693B CN107244693B CN201710369385.2A CN201710369385A CN107244693B CN 107244693 B CN107244693 B CN 107244693B CN 201710369385 A CN201710369385 A CN 201710369385A CN 107244693 B CN107244693 B CN 107244693B
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- 239000000843 powder Substances 0.000 title claims abstract description 35
- 239000000463 material Substances 0.000 title claims abstract description 24
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052786 argon Inorganic materials 0.000 claims abstract description 10
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 5
- 230000001681 protective effect Effects 0.000 claims abstract description 4
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract 6
- 239000003638 chemical reducing agent Substances 0.000 claims abstract 2
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims 2
- 238000005406 washing Methods 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 229910018068 Li 2 O Inorganic materials 0.000 abstract 1
- 239000000376 reactant Substances 0.000 abstract 1
- 238000005245 sintering Methods 0.000 abstract 1
- 229910021152 Li0.5TiO2 Inorganic materials 0.000 description 21
- 229910007848 Li2TiO3 Inorganic materials 0.000 description 16
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 12
- 239000000047 product Substances 0.000 description 12
- 238000002156 mixing Methods 0.000 description 11
- 238000001228 spectrum Methods 0.000 description 9
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 8
- 229910052744 lithium Inorganic materials 0.000 description 8
- 229910001416 lithium ion Inorganic materials 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 229910052593 corundum Inorganic materials 0.000 description 7
- 239000010431 corundum Substances 0.000 description 7
- 238000006722 reduction reaction Methods 0.000 description 7
- 238000000227 grinding Methods 0.000 description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000001878 scanning electron micrograph Methods 0.000 description 5
- 238000007599 discharging Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 229910012616 LiTi2O4 Inorganic materials 0.000 description 3
- 229910012675 LiTiO2 Inorganic materials 0.000 description 3
- 238000001636 atomic emission spectroscopy Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000009616 inductively coupled plasma Methods 0.000 description 3
- 229910052808 lithium carbonate Inorganic materials 0.000 description 3
- 239000007773 negative electrode material Substances 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910002986 Li4Ti5O12 Inorganic materials 0.000 description 2
- 229910010252 TiO3 Inorganic materials 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 239000007770 graphite material Substances 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
- 230000002687 intercalation Effects 0.000 description 2
- 229910012465 LiTi Inorganic materials 0.000 description 1
- 229910007052 Li—Ti—O Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical class [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
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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
- C01G23/005—Alkali titanates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
本发明涉及一种功能材料Li0.5TiO2粉体的制备方法，该方法是在氩气保护条件下，以TiO2和Li2CO3作为反应物于650℃烧结8小时得到Li2TiO3粉体。以Mg粉作为还原剂，在氩气保护气氛下在高温条件下还原Li2TiO3粉体，产物中的MgO和Li2O经过稀盐酸的洗涤而去除，从而得到Li0.5TiO2粉体材料。本发明的制备温度低、能耗小，且制备工艺简单，易于工业化生产。
The invention relates to a preparation method of functional material Li 0.5 TiO 2 powder. The method is to obtain Li 2 TiO 3 powder by sintering TiO 2 and Li 2 CO 3 as reactants at 650° C. for 8 hours under the protection of argon gas. body. Using Mg powder as a reducing agent, Li 2 TiO 3 powder was reduced at high temperature under argon protective atmosphere, and MgO and Li 2 O in the product were removed by washing with dilute hydrochloric acid, thereby obtaining Li 0.5 TiO 2 powder material . The preparation temperature of the invention is low, the energy consumption is small, the preparation process is simple, and the industrial production is easy.
Description
Technical Field
The invention relates to a preparation method of an electrode material of a lithium ion battery, in particular to a negative active material Li0.5TiO2A method for preparing powder material. The invention belongs to the field of functional materials.
Background
In recent years, with the rapid development of portable consumer electronics and new energy electric vehicles, people have made higher demands on the capacity, cycle life, safety and the like of lithium ion batteries. At present, various graphite carbon materials are adopted as negative active materials of commercial lithium ion batteries, but the graphite carbon materials are close to metal lithium in lithium intercalation potential, so lithium dendrite is likely to be separated out and penetrate through battery separators, and accidents such as combustion or explosion are likely to be caused. In recent years, Li-Ti-O series compounds have attracted much attention as electrode materials for lithium ion batteries. Wherein Li4Ti5O12Has zero strain characteristic and long cycle life, and has higher lithium intercalation potential than that of metallic lithium, thereby having excellent safety. But Li4Ti5O12Has a theoretical specific capacity of only 175mAh/g and a very low conductivity of only 10 at 20 DEG C-9s/cm, which limits its application. Spinel-structured LiTi2O4Has higher conductivity as a negative electrode material, therefore, LiTi2O4Is a promising anode material. A number of preparations of LiTi have been proposed2O4Such as Kai Jiang et al, electrolyze TiO in a molten LiCl salt solution at 700 deg.C2(anatase) preparation of LiTi2O4(Journal of Power Sources 175(2008) 575-. Furthermore, Li0.5TiO2Can also be used as the cathode material of the lithium ion battery,for example, A, Kuhn, et al, use a two-step high temperature reaction to prepare Li0.5TiO2(Journal of Power Sources 92(2001)221-227)，
Li2CO3+TiO2(r)→Li2TiO3+CO2
Li2TiO3+1/2Ti+5/2TiO2→4Li0.5TiO2。
The invention utilizes Li2TiO3Li is produced by a simple magnesiothermic reduction method as a raw material0.5TiO2And (3) powder materials.
Disclosure of Invention
The invention aims to provide Li0.5TiO2A method for preparing powder material. The material has the advantages of excellent electrochemical performance, simple preparation process, low energy consumption and low cost.
The invention is realized by the following scheme:
1. adding TiO into the mixture2Powder with Li2CO3Fully grinding and mixing according to a certain molar ratio, and then preserving heat for 8 hours at 650 ℃ in a heating furnace under the atmosphere of high-purity argon to obtain Li2TiO3。
2. Mixing Li2TiO3Fully grinding and mixing the powder and Mg powder according to a certain molar ratio, putting the mixed powder into a heating furnace for heating, and introducing high-purity argon as protective gas. The reaction temperature is kept at 600-640 ℃ for 3-6 h. Washing the reaction product in an acid solution, filtering and drying to obtain Li0.5TiO2And (3) powder materials.
Compared with the prior art, the invention has the following advantages:
1. li prepared by the invention0.5TiO2The powder material has high specific capacity and excellent charge-discharge cycling stability.
2. The preparation method has the advantages of low preparation temperature, high efficiency, energy conservation, simple and convenient process flow, low cost and easy industrial production.
Drawings
FIG. 1 Li2TiO3X of (a)A diffraction spectrum of radiation and (b) a scanning electron micrograph.
FIG. 2 Li2TiO3Li obtained by keeping the temperature of the Li and Mg powder at 600 ℃ for 6h0.5TiO2The (a) X-ray diffraction spectrum and (b) scanning electron micrograph of (a); (c) li0.5TiO2Constant current charge-discharge cycle performance.
FIG. 3 Li2TiO3Li obtained by keeping the temperature of the Li and Mg powder at 620 ℃ for 4h0.5TiO2The (a) X-ray diffraction spectrum and (b) scanning electron micrograph of (a); (c) li0.5TiO2Constant current charge-discharge cycle performance.
FIG. 4 Li2TiO3Li obtained by keeping the temperature of the Li and Mg powder at 640 ℃ for 3h0.5TiO2The (a) X-ray diffraction spectrum and (b) scanning electron micrograph of (a); (c) li0.5TiO2Constant current charge-discharge cycle performance.
Detailed Description
Example 1
Adding TiO into the mixture2Powder with Li2CO3Respectively weighing corresponding masses according to a molar ratio of 1:1.05, and fully grinding and uniformly mixing the two materials. The mixed sample is contained in a corundum crucible and is kept at 650 ℃ for 8 hours in a tubular furnace filled with high-purity argon to obtain Li2TiO3And (3) powder materials.
Mixing Li2TiO3Weighing two samples with corresponding mass according to the molar ratio of 2:1.05 with Mg, fully grinding and mixing, placing the fully mixed samples in a corundum crucible, and then placing the corundum crucible into a tubular furnace filled with high-purity argon for heat preservation at 600 ℃ for 6 hours to perform magnesiothermic reduction reaction. Putting the product obtained after the reaction into a dilute hydrochloric acid solution, stirring for 1h, then repeatedly washing the remainder with alcohol and deionized water, centrifuging and drying to obtain Li0.5TiO2And (3) powder materials.
FIG. 1(a) is Li2TiO3X-ray diffraction spectrum of (1), with Li2TiO3The standard spectrum (PDF #33-0831) of (A) is completely consistent, indicating that under the condition, pure-phase Li can be obtained2TiO3. FIG. 2(b) is Li2TiO3Scanning electrodeMirror photograph, from which Li can be seen2TiO3The particle size of (A) is about 100 to 300 nm.
FIG. 2(a) is an X-ray diffraction spectrum of a magnesiothermic reduction product, together with a hexagonal structure of LiTiO2The standard map (PDF #40-1053) of (A) was completely matched. Atomic emission spectrometry of inductively coupled plasma showed that the atomic ratio of Li to Ti in the product was 0.5:1, and thus the product was Li0.5TiO2. FIG. 2(b) is Li0.5TiO2The scanning electron microscope photo of the powder material has a particle size of 100-200 nm. Mixing Li0.5TiO2The powder material is prepared into a lithium ion experimental battery, and FIG. 2(c) shows Li0.5TiO2At a current density of 0.11mA cm-2Cycling performance under current density conditions. The first charging/discharging specific capacity is 137.9/309.9mAh/g, and after 100 cycles, the first charging/discharging specific capacity is 44.9/45.4mAh/g respectively.
Example 2
Prepared Li2TiO3Weighing two samples with corresponding mass according to the molar ratio of 2:1.2 with Mg, fully grinding and mixing, placing the fully mixed samples in a corundum crucible, and then placing the corundum crucible into a tubular furnace filled with high-purity argon for heat preservation at 620 ℃ for 4 hours to carry out magnesiothermic reduction reaction. Putting the product obtained after the reaction into a dilute hydrochloric acid solution, stirring for 1h, then repeatedly washing the remainder with alcohol and deionized water, centrifuging and drying to obtain Li0.5TiO2And (3) powder materials.
FIG. 3(a) is an X-ray diffraction spectrum of a magnesiothermic reduction product, together with LiTiO2The standard map (PDF #40-1053) is consistent. Atomic emission spectrometry of inductively coupled plasma showed that the atomic ratio of Li to Ti in the product was 0.5:1, and thus the product was Li0.5TiO2. FIG. 3(b) is a scanning electron micrograph thereof, Li0.5TiO2The particle size of the powder is about 100 nm. Mixing Li0.5TiO2The powder material was prepared into lithium ion experimental batteries, and FIG. 3(c) shows Li0.5TiO2At a current density of 0.11mA cm-2Cycling performance under the conditions. The first charging/discharging specific capacity is 136.49/289.5mAh/g, and the specific capacity is divided after 100 times of circulationRespectively 55.1/55.6 mAh/g.
Example 3
Prepared Li2TiO3Weighing two samples with corresponding mass according to the molar ratio of 2:1.4 with Mg, fully grinding and mixing, placing the fully mixed samples in a corundum crucible, and then placing the corundum crucible into a tubular furnace filled with high-purity argon for heat preservation at 640 ℃ for 3 hours to carry out magnesiothermic reduction reaction. Putting the product obtained after the reaction into a dilute hydrochloric acid solution, stirring for 1h, then repeatedly washing the remainder with alcohol and deionized water, centrifuging and drying to obtain Li0.5TiO2And (3) powder materials.
FIG. 4(a) is an X-ray diffraction spectrum of a magnesiothermic reduction product, together with LiTiO2The standard map (PDF #40-1053) is consistent. Atomic emission spectrometry of inductively coupled plasma showed that the atomic ratio of Li to Ti in the product was 0.5:1, and thus the product was Li0.5TiO2. FIG. 4(b) is Li0.5TiO2Scanning Electron microscope Picture of powder Material, Li0.5TiO2The particle size is between 100 and 200 nm. Mixing Li0.5TiO2The powder material was prepared into lithium ion experimental batteries, and FIG. 4(c) shows Li0.5TiO2At a current density of 0.11mA cm-2Cycling performance under the conditions. The first charging/discharging specific capacity is 109.9/272.6mAh/g, and the specific capacity after 100 cycles is 58.7/59.2mAh/g respectively.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101402469A (en) * | 2008-10-31 | 2009-04-08 | 桂林工学院 | Method of producing spinel structured lithium titanate |
| CN101580273A (en) * | 2009-06-12 | 2009-11-18 | 清华大学 | High energy density spinel structural lithium titanate material and preparation method thereof |
| CN104045108A (en) * | 2014-06-19 | 2014-09-17 | 湖南大学 | Method for preparing TiO powder material |
| CN104477979A (en) * | 2014-12-17 | 2015-04-01 | 湖南大学 | A kind of method for preparing LiTi204 powder material |
| CN104752708A (en) * | 2013-12-25 | 2015-07-01 | 北京有色金属研究总院 | Li2TiO3 powder material, preparation method of Li2TiO3 powder material, and method for preparing spinel lithium titanate with Li2TiO3 powder material |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI254031B (en) * | 2005-05-10 | 2006-05-01 | Aquire Energy Co Ltd | Manufacturing method of LixMyPO4 compound with olivine structure |
| EP2586086B1 (en) * | 2010-06-25 | 2017-03-08 | Max-Planck-Gesellschaft zur Förderung der Wissenschaften e.V. | An electrode material for a lithium-ion battery and a method of manufacturing the same |
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- 2017-05-23 CN CN201710369385.2A patent/CN107244693B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101402469A (en) * | 2008-10-31 | 2009-04-08 | 桂林工学院 | Method of producing spinel structured lithium titanate |
| CN101580273A (en) * | 2009-06-12 | 2009-11-18 | 清华大学 | High energy density spinel structural lithium titanate material and preparation method thereof |
| CN104752708A (en) * | 2013-12-25 | 2015-07-01 | 北京有色金属研究总院 | Li2TiO3 powder material, preparation method of Li2TiO3 powder material, and method for preparing spinel lithium titanate with Li2TiO3 powder material |
| CN104045108A (en) * | 2014-06-19 | 2014-09-17 | 湖南大学 | Method for preparing TiO powder material |
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Non-Patent Citations (2)
| Title |
|---|
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| On the synthesis conditions for tailoring lithium composition in ramsdellite phases: Application for Li-ion batteries;A. Soares et al.;《Journal of Power Sources》;20111116;第208卷;440-446 * |
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