US20110217593A1 - Carbon-coated lithium titanium spinel - Google Patents
Carbon-coated lithium titanium spinel Download PDFInfo
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- US20110217593A1 US20110217593A1 US13/123,089 US200913123089A US2011217593A1 US 20110217593 A1 US20110217593 A1 US 20110217593A1 US 200913123089 A US200913123089 A US 200913123089A US 2011217593 A1 US2011217593 A1 US 2011217593A1
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Definitions
- the present invention relates to carbon-coated lithium titanate Li 4 Ti 5 O 12 as well as a method for its production.
- lithium titanate Li 4 Ti 5 O 12 or lithium titanium spinel for short, in particular as substitute for graphite as anode material in rechargeable lithium-ion batteries was proposed some time ago.
- Li 4 Ti 5 O 12 has a relatively constant potential difference of 1.55 V compared with lithium and achieves several 1000 charge and discharge cycles with a loss of capacity of ⁇ 20%.
- lithium titanate has a clearly more positive potential than graphite which has previously customarily been used as anode in rechargeable lithium-ion batteries.
- Li 4 Ti 5 O 12 has a long life and is non-toxic and is therefore also not to be classified as posing a threat to the environment.
- LiFePO 4 has been used as cathode material in lithium-ion batteries, with the result that a voltage difference of 2 V can be achieved in a combination of Li 4 Ti 5 O 12 and LiFePO 4 .
- Li 4 Ti 5 O 12 is obtained by means of a solid-state reaction between a titanium compound, typically TiO 2 , and a lithium compound, typically Li 2 CO 3 , at high temperatures of over 750° C., as described in U.S. Pat. No. 5,545,468 or EP 1 057 783 A1.
- Sol-gel methods for the production of Li 4 Ti 5 O 12 are also described (DE 103 19 464 A1). Furthermore, production methods by means of flame spray pyrolysis are proposed (Ernst, F. O. et al. Materials Chemistry and Physics 2007, 101 (2-3, pp. 372-378) as well as so-called “hydrothermal methods” in anhydrous media (Kalbac, M. et al., Journal of Solid State Electrochemistry 2003, 8 (1) pp. 2-6).
- EP 1 796 189 A2 proposes providing complex lithium transition metal oxides ex situ, i.e. after their complete synthesis with a carbon-containing coating.
- a disadvantage with this method is the large particle size of the contained product, in particular the secondary particle size.
- the carbon coating in this method is located on the secondary and not the primary particles, which leads to poor electrochemical properties, in particular as regards its capacity behaviour.
- this object is achieved by a carbon-containing lithium titanium oxide containing spherical (secondary) particle aggregates with a diameter of 1-80 ⁇ m consisting of lithium titanium oxide primary particles coated with carbon.
- lithium titanium oxide a lithium titanate which according to the invention includes all lithium titanium spinels of the type Li 1+x Ti 2 ⁇ x O 4 with 0 ⁇ x ⁇ 1/3 of the spatial group Fd3m and generally also all mixed lithium titanium oxides of the generic formula Li x Ti y O (0 ⁇ x, y ⁇ 1).
- the carbon-coated lithium titanium oxide according to the invention consists, as mentioned, of secondary particles which are formed of primary particles coated with carbon.
- the secondary particles are spherical in shape.
- the result of the particle size according to the invention of the secondary particles is that the current density in an electrode that contains the carbon-coated lithium titanium oxide material according to the invention is particularly high and it has a high cycle stability compared with the materials of the state of the art, in particular EP 1796 189 A2.
- the carbon-containing lithium titanium oxide according to the invention has a BET surface area (measured in accordance with DIN 66134) of 1-10 m 2 /g, preferably ⁇ 10 m 2 /g, still more preferably ⁇ 8 m 2 /g and quite particularly preferably ⁇ 5 m 2 /g.
- typical values lie in the range of from 3-5 m 2 /g.
- the primary particles coated with carbon typically have a size of ⁇ 1 ⁇ m. It is important according to the invention that the primary particles are small and at least partially coated with carbon, with the result that the current-carrying capacity and the cycle stability of an electrode containing the lithium titanium oxide according to the invention are particularly high compared with non-carbon-coated materials or materials which are not homogeneously coated or compared with materials in which only the secondary particles are coated.
- the carbon content of the lithium titanium oxide according to the invention is 0.05 to 2 wt.-%, in quite particularly preferred embodiments 0.05 to 0.5 wt.-%.
- Li 4 Ti 5 O 12 is preferred because it is particularly well-suited as electrode material.
- the object of the present invention is further achieved by a method for the production of carbon-containing lithium titanium oxide comprising the steps of
- the lithium titanium spinels Li 1 ⁇ x Ti 2 ⁇ x O 4 as already described above of the spatial group Fd3m or the mixed lithium titanium oxides of the generic formula Li x Ti y O can be obtained.
- the final carbon content of the lithium titanium oxide according to the invention can also be set during the mixing.
- solvent is here defined such that at least one constituent of the starting substances is at least partially soluble in the solvent, i.e. has a solubility product L of at least 0.5.
- the solvent is preferably water.
- one constituent of the starting substances is readily soluble in water, i.e. it has a solubility product L of at least 10.
- the atomic ratio of Li to Ti is 4:5, with the result that in particular phase-pure Li 4 Ti 5 O 12 with a carbon coating can be obtained.
- phase-pure is meant here that, within the limits of the usual measurement accuracy, no TiO 2 can be detected in the rutile phase by means of XRD measurements.
- the lithium salt for carrying out the method according to the invention is selected from the group consisting of LiOH, LiNO 3 , Li 2 CO 3 , Li 2 O, LiHCO 3 , and lithium acetate, since an aqueous solution to which the other starting compounds can be added can be produced particularly easily from these starting compounds.
- TiO 2 in anatase form or in amorphous form is used, which advantageously does not change into rutile as a result of the method according to the invention.
- the carbon-containing compounds which are suitable for carrying out the method according to the invention are selected for example from hydrocarbons, such as for example polycyclic aromatics and their compounds, perylene and its compounds, polymers and copolymers, such as for example polyolefins, polypropylene copolymers in powder form, styrene-polybutadiene block copolymers, sugars and their derivatives.
- hydrocarbons such as for example polycyclic aromatics and their compounds, perylene and its compounds, polymers and copolymers, such as for example polyolefins, polypropylene copolymers in powder form, styrene-polybutadiene block copolymers, sugars and their derivatives.
- Particularly preferred polymers are polyolefins, polybutadienes, polyvinyl alcohol, condensation products from phenol, polymers derived from furfuryl, styrene derivatives, divinylbenzene derivatives, naphthol perylene, acrylonitrile and vinyl acetate, gelatin, cellulose, starch and their esters and ethers and mixtures thereof.
- sugars has proved to be quite particularly preferred for carrying out the method according to the invention, since these dissolve particularly well in water.
- lactose, sucrose and saccharose are quite particularly preferred, lactose being the most preferred.
- the drying step b) typically takes place in the form of so-called spray drying, in which the obtained mixture is finely sprayed through a nozzle and precipitates in the form of a pre-product.
- spray drying any other method in which the starting compounds are homogeneously mixed and then introduced into a gas stream for drying can also be used.
- these methods are for example fluid-bed drying, rolling granulation and drying or freeze-drying alone or in combination.
- Spray drying is quite particularly preferred and typically takes place in a temperature gradient of from 90-300° C.
- the obtained spray-dried pre-product is calcined at a temperature of from 700 to 1000° C., preferably under a protective atmosphere, in order to avoid possible secondary reactions during the calcining which could lead to undesired results, such as e.g. the oxidation of the carbon coating.
- Suitable protective gases are e.g. nitrogen, argon, etc. or mixtures thereof.
- the present invention also relates to a lithium titanium oxide obtainable by the method according to the invention which is characterized by a particularly small BET surface area and a small particle size of the primary particles as well as of the secondary particles formed from the primary particles, as has already been described above.
- an electrode which contains the carbon-coated lithium titanium oxide according to the invention is an anode.
- the electrode has a capacity ratio between 1C and 4C of >85% and a discharge capacity of at least 165 mAh/g at C/10 in a lithium-ion secondary battery.
- FIG. 1 an SEM micrograph of carbon-coated Li 4 Ti 5 O 12 according to the invention
- FIG. 2 the diagram showing the charge and discharge capacity of an electrode containing an (in-situ) carbon-coated lithium titanate according to the invention
- FIG. 3 the charge and discharge capacity of ex-situ coated lithium titanate as comparison
- FIG. 4 an SEM micrograph of a subsequently (ex-situ) carbon-coated Li 4 Ti 5 O 12 ;
- FIG. 5 an SEM micrograph of uncoated Li 4 Ti 5 O 12 ;
- FIG. 6 the charge and discharge capacity of the uncoated Li 4 Ti 5 O 12 ; the current was the same during charging and during discharging.
- LiOH.H 2 O as well as TiO 2 in anatase form are used below as starting products.
- the water content in the case of commercially available LiOH.H 2 O (from Merck) varies from batch to batch and was determined prior to synthesis.
- a suspension of LiOH/TiO 2 /lactose was produced at 30-35° C., by first dissolving LiOH.H 2 O in water and then adding TiO 2 in anatase form as well as lactose while stirring:
- the lactose had the effect of reducing the viscosity of the original suspension, with the result that 25% less water had to be used for the production of a corresponding suspension than in the case without the addition of the lactose.
- the mixture was then spray dried in a Nubilosa spray dryer at a starting temperature of approx. 300° C. and an end temperature of 100° C.
- porous spherical aggregates of the order of several micrometres formed.
- FIG. 1 shows the carbon-coated lithium titanate according to the invention with 0.2 wt.-% total carbon content (60 g lactose/kg LiOH+TiO 2 ), while FIG. 5 shows an uncoated lithium titanate also obtained by means of spray drying.
- the carbon-containing compound in the starting products of the method according to the invention acts as sintering incubator and leads to clearly smaller particles.
- Uncoated lithium titanate was produced according to the method from Example 1, i.e. without addition of lactose.
- Charge/discharge cycles were then carried out with the material according to the invention as well as with the material of the comparison examples, i.e. with the subsequently coated lithium titanate (according to EP 1 796 198 A2) as well as with the uncoated lithium titanate which were both obtained by means of the same method.
- the anode consisted in each case of 85% active material, 10% Super P carbon black and 5% PVDF 21256 binder. The measurements took place with the material according to the invention or comparison materials as anode in a half cell compared with metal lithium.
- the active mass content of the electrode was 2.2 mg/cm 2 .
- the range covered in the cycles was 1.0-2.0 volts.
- FIG. 2 shows charge/discharge curves of carbon-coated lithium titanate according to the invention, wherein the capacity ratio between 1C and 4C was 87.5%; the current was the same during charging and during discharging.
- the material according to the invention in which only 75% of the capacity was measured at 4C, is better.
- the current was the same during charging and during discharging.
- the coated in-situ carbon-coated lithium titanate according to the invention has major advantages as regards its capacity ratio compared with a subsequently applied carbon coating or uncoated lithium titanate.
Applications Claiming Priority (3)
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DE102008050692.3 | 2008-10-07 | ||
DE102008050692.3A DE102008050692B4 (de) | 2008-10-07 | 2008-10-07 | Kohlenstoffbeschichteter Lithiumtitan-Spinell |
PCT/EP2009/007196 WO2010040516A1 (de) | 2008-10-07 | 2009-10-07 | Kohlenstoffbeschichteter lithiumtitan-spinell |
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PCT/EP2009/007196 A-371-Of-International WO2010040516A1 (de) | 2008-10-07 | 2009-10-07 | Kohlenstoffbeschichteter lithiumtitan-spinell |
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US14/193,923 Division US9085491B2 (en) | 2008-10-07 | 2014-02-28 | Carbon-coated lithium titanium spinel |
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US13/123,089 Abandoned US20110217593A1 (en) | 2008-10-07 | 2009-10-07 | Carbon-coated lithium titanium spinel |
US14/193,923 Active US9085491B2 (en) | 2008-10-07 | 2014-02-28 | Carbon-coated lithium titanium spinel |
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US (2) | US20110217593A1 (de) |
EP (1) | EP2349931B1 (de) |
JP (2) | JP5671467B2 (de) |
KR (1) | KR101358000B1 (de) |
CN (1) | CN102186775B (de) |
CA (1) | CA2738853A1 (de) |
DE (1) | DE102008050692B4 (de) |
TW (1) | TWI461366B (de) |
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US20130236784A1 (en) * | 2012-03-07 | 2013-09-12 | Leyden Energy | Surface treatment of electrochemically active materials for rechargeable cells |
US20130302690A1 (en) * | 2012-05-08 | 2013-11-14 | Korea Institute Of Science And Technology | Method for coating carbon on lithium titanium oxide-based anode active material nanoparticles and carbon-coated lithium titanium oxide-based anode active material nanoparticles produced by the method |
US20140328005A1 (en) * | 2013-05-03 | 2014-11-06 | Samhwa Capacitor Co., Ltd. | Lithium titanium oxide (lto)/carbon composite, preparation method for lto/carbon composite, negative electrode material using lto/carbon composite, and hybrid super capacitor using negative electrode material |
US20150318536A1 (en) * | 2011-11-28 | 2015-11-05 | Renault S.A.S. | Production of a material based on li4ti5o12 with milling in the presence of carbon |
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- 2009-10-07 US US13/123,089 patent/US20110217593A1/en not_active Abandoned
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- 2009-10-07 KR KR1020117009922A patent/KR101358000B1/ko active IP Right Grant
- 2009-10-07 EP EP09737344.3A patent/EP2349931B1/de not_active Not-in-force
- 2009-10-07 JP JP2011530412A patent/JP5671467B2/ja active Active
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Cited By (16)
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US20150318536A1 (en) * | 2011-11-28 | 2015-11-05 | Renault S.A.S. | Production of a material based on li4ti5o12 with milling in the presence of carbon |
US20130236784A1 (en) * | 2012-03-07 | 2013-09-12 | Leyden Energy | Surface treatment of electrochemically active materials for rechargeable cells |
US9048496B2 (en) * | 2012-03-07 | 2015-06-02 | A123 Systems Llc | Surface treatment of electrochemically active materials for rechargeable cells |
US20130302690A1 (en) * | 2012-05-08 | 2013-11-14 | Korea Institute Of Science And Technology | Method for coating carbon on lithium titanium oxide-based anode active material nanoparticles and carbon-coated lithium titanium oxide-based anode active material nanoparticles produced by the method |
US9865866B2 (en) * | 2012-05-08 | 2018-01-09 | Korea Institute Of Science And Technology | Method for coating carbon on lithium titanium oxide-based anode active material nanoparticles and carbon-coated lithium titanium oxide-based anode active material nanoparticles produced by the method |
US20150372348A1 (en) * | 2013-02-04 | 2015-12-24 | Leclanché Sa | Electrolyte composition for electrochemical cell |
US20140328005A1 (en) * | 2013-05-03 | 2014-11-06 | Samhwa Capacitor Co., Ltd. | Lithium titanium oxide (lto)/carbon composite, preparation method for lto/carbon composite, negative electrode material using lto/carbon composite, and hybrid super capacitor using negative electrode material |
US9520240B2 (en) * | 2013-05-03 | 2016-12-13 | Samhwa Capacitor Co., Ltd. | Lithium titanium oxide (LTO)/carbon composite, preparation method for LTO/carbon composite, negative electrode material using LTO/carbon composite, and hybrid super capacitor using negative electrode material |
US10276863B2 (en) | 2013-06-14 | 2019-04-30 | Kuraray Co., Ltd. | Non-stoichiometric titanium compound-carbon composite, method for producing same, negative electrode active material and lithium ion secondary battery |
US10553868B2 (en) | 2014-12-02 | 2020-02-04 | Kabushiki Kaisha Toshiba | Negative electrode active material, nonaqueous electrolyte battery, battery pack and vehicle |
US10665360B2 (en) | 2014-12-16 | 2020-05-26 | Otsuka Chemical Co., Ltd. | Method for producing composite body of lithium titanate particles and carbonaceous material, and composite body of lithium titanate particles and carbonaceous material |
US10505186B2 (en) | 2015-01-30 | 2019-12-10 | Kabushiki Kaisha Toshiba | Active material, nonaqueous electrolyte battery, battery pack and battery module |
US10511014B2 (en) | 2015-01-30 | 2019-12-17 | Kabushiki Kaisha Toshiba | Battery module and battery pack |
US10516163B2 (en) | 2015-03-13 | 2019-12-24 | Kabushiki Kaisha Toshiba | Active material, nonaqueous electrolyte battery, battery pack and battery module |
US10439218B2 (en) | 2017-03-24 | 2019-10-08 | Kabushiki Kaisha Toshiba | Active material, electrode, secondary battery, battery pack, and vehicle |
CN112736233A (zh) * | 2021-01-14 | 2021-04-30 | 武汉船用电力推进装置研究所(中国船舶重工集团公司第七一二研究所) | 一种锂离子电池电极活性物质、制备方法及其电极和电池 |
Also Published As
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JP5671467B2 (ja) | 2015-02-18 |
KR101358000B1 (ko) | 2014-02-04 |
DE102008050692B4 (de) | 2014-04-03 |
JP5657582B2 (ja) | 2015-01-21 |
TWI461366B (zh) | 2014-11-21 |
JP2012121803A (ja) | 2012-06-28 |
TW201024222A (en) | 2010-07-01 |
WO2010040516A1 (de) | 2010-04-15 |
US9085491B2 (en) | 2015-07-21 |
US20140175687A1 (en) | 2014-06-26 |
CA2738853A1 (en) | 2010-04-15 |
CN102186775A (zh) | 2011-09-14 |
JP2012505137A (ja) | 2012-03-01 |
CN102186775B (zh) | 2015-11-25 |
EP2349931B1 (de) | 2018-12-05 |
KR20110069128A (ko) | 2011-06-22 |
DE102008050692A1 (de) | 2010-04-08 |
EP2349931A1 (de) | 2011-08-03 |
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