CN102024944A - Method used for preparing anode material lithium titanate of lithium ion secondary battery - Google Patents
Method used for preparing anode material lithium titanate of lithium ion secondary battery Download PDFInfo
- Publication number
- CN102024944A CN102024944A CN2010105476887A CN201010547688A CN102024944A CN 102024944 A CN102024944 A CN 102024944A CN 2010105476887 A CN2010105476887 A CN 2010105476887A CN 201010547688 A CN201010547688 A CN 201010547688A CN 102024944 A CN102024944 A CN 102024944A
- Authority
- CN
- China
- Prior art keywords
- lithium
- secondary battery
- carbon source
- ion secondary
- lithium titanate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- 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 provides a method used for preparing anode material lithium titanate of a lithium ion secondary battery. The method provided by the invention comprises the steps of mixing a Li soluble compound and anatase TiO2 at the ratio of Li to Ti of 0.8-1.1, adding organic micromolecule carbon source precursor and mixing, ball milling and drying, and insulating at the temperature of 300-550 DEG C for 2-20 hours, thus obtaining sintered precursor; then mixing the sintered precursor and organic macromolecule polymer carbon source precursor, ball milling and drying again, and insulating at the temperature of 600-900 DEG C for 2-30 hours, thus obtaining the finished product Li4Ti5O12/C composite anode material with excellent multiplying performance. The lithium titanate prepared by the method has good carbon coating effect, thus improving conductivity of a product. The lithium titanate anode material prepared by the method shows excellent multiplying performance and is applicable to power battery.
Description
Technical field
The present invention relates to a kind of preparation method of battery electrode material, particularly a kind of preparation method who is used for lithium ion secondary battery cathode material lithium titanate.
Background technology
Lithium rechargeable battery has been widely used in fields such as mobile communication, notebook computer, video camera, camera, portable instrument as the high-energy-density chemical power source, developing rapidly becomes one of present most important secondary cell.At present, the negative material of business-like lithium ion battery adopts carbon negative pole material mostly, but there are some defectives in carbon negative pole material: first in the discharge process with the electrolyte formation surface passivated membrane that reacts, cause the consumption of electrolyte and enclosed pasture efficient is lower first; The electrode potential of carbon electrode and lithium metal is close, when battery overcharge, still may cause short circuit and form dendrite at carbon electrodes precipitating metal lithium, causes safety problem etc.
Recently, spinel type lithium titanate has " zero strain " as a kind of novel negative material, and advantages such as good cycle become the focus of research gradually.Compare with traditional carbon negative pole material, " zero strain " material-lithium titanate is 1.55V with respect to the current potential of lithium metal, recovery voltage far above most electrolyte, can avoid the reduction of electrolyte and the generation of passivating film, can stop simultaneously the generation of lithium metal, have very excellent cycle performance and security performance.Therefore, lithium titanate material can be used as the negative material of lithium ion battery, is subjected to extensively being absorbed in of numerous researchers.But lithium titanate is a kind of insulating material, its poorly conductive, and capacity attenuation is fast when high current charge-discharge, high rate performance is relatively poor.Doping carbon is a kind of important channel of improving the high rate performance of lithium titanate material.At present, the lithium titanate of preparation carbon coated adopts high temperature solid-state method mostly, and the preparation technology of solid phase method is simple, and the equipment of use is realized easily, realizes the earliest in production.CN101391806A discloses a kind of manufacture method that is used for lithium ionic cell cathode material spinelle lithium titanate, and this method may further comprise the steps:
(1) compound of metatitanic acid, lithium is prepared burden according to mol ratio Li/Ti=0.8 ~ 0.88;
(2) again to the presoma that wherein adds carbon or carbon, in medium, evenly mixed 5 ~ 72 hours, dry then;
(3) under 200 ℃ ~ 500 ℃ conditions, handled 2 ~ 20 hours then;
(4) last, Synthetic 2 ~ 72 hour under 600 ℃ ~ 900 ℃ conditions obtain lithium ion battery lithium titanate with spinel structure negative material.
The chemical property of the lithium titanate of this method preparation is unsatisfactory, especially the performance under the high magnification.Because the carbon of this method preparation mainly is dispersed in the intergranular irregular fragment of lithium titanate, and the carbon granule of granule interior and surface distributed is less, thereby cause conductivity of electrolyte materials still very low, adopt the battery of this negative material preparation, chemical property is good when discharging under the low range, but when this material was applied to the electrokinetic cell of high-multiplying power discharge, the heavy-current discharge performance of battery was relatively poor.
Summary of the invention
The objective of the invention is to overcome the defective that the high magnification that exists in the prior art for preparing lithium titanate anode material is transferred poor electrical performance, a kind of preparation method who improves electronic conductivity, charge-discharge performance and the cycle performance of lithium ionic cell cathode material lithium titanate is provided.The lithium titanate anode material of this method preparation demonstrates excellent high rate performance.
For achieving the above object, the present invention adopts following technical scheme:
A kind of preparation method who is used for lithium ion secondary battery cathode material lithium titanate is characterized in that the concrete steps of this method are:
A. with Li compound and TiO
2, according to Li:Ti=(0.8～1.1): 1 mol ratio is prepared burden, and add organic molecule carbon source presoma again and mix, ball milling in medium uniformly, oven dry, sintering 2～20 hours under 300 ℃～550 ℃ conditions obtains sintered precursor then;
B. sintered precursor and the organic macromolecule polymer carbon source presoma with step a gained mixes, ball milling in uniform medium, and oven dry is incubated 2～30h then under 600 ℃～900 ℃ conditions, obtain the finished product lithium titanate powdery;
The addition of described organic molecule carbon source presoma is the phosphorus content contribution 1wt%～6wt% of the addition of the described organic molecule carbon source presoma product that can be final generation in theory; The addition of described organic macromolecule polymer carbon source presoma can be the phosphorus content contribution 6wt% ~ 12wt% of the product of final generation in theory; The mass ratio of the carbon in described organic macromolecule polymer carbon source presoma and the described organic molecule carbon source presoma is (1～5): 1
Above-mentioned TiO
2Be Detitanium-ore-type.
Above-mentioned Li compound is lithium nitrate, lithium carbonate, lithium chloride, lithium acetate, lithium citrate, lithium oxalate, lithium formate, lithium lactate or isopropyl alcohol lithium.
Above-mentioned organic molecule carbon source presoma is at least a in glucose, sucrose, urea, tartaric acid, laurate, citric acid, oxalic acid, gluconic acid, the ethylenediamine tetra-acetic acid.
The molecular weight of above-mentioned organic molecule carbon source presoma is 60-800.
Above-mentioned organic macromolecule polymer carbon source presoma is at least a among polyvinyl alcohol, polyethylene glycol, POLYPROPYLENE GLYCOL, soluble starch, phenolic resins, block compound P123, the block compound F127.
The molecular weight of above-mentioned organic macromolecule polymer carbon source presoma is 10000 ~ 300000
Above-mentioned ball-milling medium is at least a in water, ethanol, acetone, the ether; The mass ratio of ball and material is controlled to be 1～10:1 in the described mechanical milling process, and the rotating speed of ball milling is controlled at 300 ~ 550r/min; Described bake out temperature is 60 ℃～200 ℃.
Heating rate among the above-mentioned step a during sintering is controlled to be 100～200 ℃/hour;
The heating rate of sintering is controlled to be 100～300 ℃/hour among the above-mentioned steps b.
The present invention adopts the high-energy ball milling method batch mixing, can improve the uniformity that reactant mixes significantly, can improve the granule-morphology of material.In addition, the invention provides in the method for two step of lithium titanate carbon coating, the organic molecule carbon source presoma that adds during sintering in the first step decomposes the particle that obtains can be dispersed in lithium titanate particle surface and on every side, and the organic high molecular polymer carbon source of adding during sintering in second step is decomposed the carbochain that obtains, can be for the electron conduction chain be provided between the lithium titanate particle, improve the conductivity of product effectively, improve the high rate capability of electrode material.
Description of drawings
Fig. 1 is the XRD figure of the embodiment of the invention 1 product;
Fig. 2 is the charging and discharging curve of the embodiment of the invention 1 product under the 0.5C multiplying power;
Fig. 3 is the discharge cycles curve of the embodiment of the invention 1 product under different multiplying;
Fig. 4 is the charging and discharging curves of the embodiment of the invention 2 products under the 0.5C multiplying power.
Embodiment
The present invention is described in detail below by instantiation, but protection scope of the present invention is not subject to these examples of implementation.
Embodiment 1: according to mol ratio Li:Ti=1, take by weighing the Detitanium-ore-type TiO of 6.96g
2(analyzing pure), the lithium acetate of 8.88g (analyzing pure) and 0.79g sucrose join in the ball grinder, add the agate ball of 50g and the absolute ethyl alcohol of 100ml subsequently, the sealing ball grinder, on ball mill with the rotating speed ball milling of 400r/min 10 hours, the mixed slurry that obtains mixing.Slurry is transferred in the drying basin, put into 80 ℃ of oven dry of baking oven and obtain presoma.Precursor powder is placed in the tube furnace, under argon shield, is warming up to 500 ℃ of insulations with 150 ℃/hour heating rates and raw material was tentatively decomposed in 6 hours, wait to reduce to 20 ~ 50 ℃ after, obtain the pre-burning powder.The pre-burning powder is put into ball grinder, adds the polyethylene glycol of 3.5g, add the agate ball of 30g and the absolute ethyl alcohol of 50ml subsequently, on ball mill with the rotating speed ball milling of 400r/min 5 hours, the mixed slurry that obtains mixing.Slurry is transferred in the drying basin, put into 80 ℃ of oven dry of baking oven and obtain the black powder, powder is placed in the tube furnace; under argon shield; be warming up to 800 ℃ of insulations 15 hours with 120 ℃/hour heating rates, naturally cool to 20 ~ 50 ℃ after, obtain the Li of carbon coated
4Ti
5O
12Composite material.Fig. 1 is the XRD figure of gained sample.As seen, the equal and Li of the position of each diffraction maximum of XRD figure of synthetic product and relative intensity
4Ti
5O
12Standard card match, do not have any dephasign.Fig. 2 is for to do positive pole with this material, metal lithium sheet is done the simulated battery that negative pole is assembled into, under the 0.5C multiplying power, the first charge-discharge curve, as seen from the figure, the material that is synthesized has excellent charging and discharging platform and higher reversible capacity, and discharge capacity can reach 149mAh/g, charge and discharge platform is smooth, demonstrates embedding lithium performance preferably.Fig. 3 is under 0.5C, 1C and the 2C multiplying power, the discharge cycles curve of this sample, and material list reveals excellent cycle performance as can be seen, is a kind of electrode material of excellence.
Embodiment 2: according to mol ratio Li:Ti=0.85, take by weighing the Detitanium-ore-type TiO of 6.96g
2(analyzing pure), the lithium acetate of 7.55g (analyzing pure) and 1.4g glucose join in the ball grinder, add the agate ball of 35g and the absolute ethyl alcohol of 90ml subsequently, the sealing ball grinder, on ball mill with the rotating speed ball milling of 380r/min 8 hours, the mixed slurry that obtains mixing.Slurry is transferred in the drying basin, put into 80 ℃ of oven dry of baking oven and obtain presoma.Precursor powder is placed in the tube furnace, under argon shield, is warming up to 500 ℃ of insulations with 180 ℃/hour heating rates and raw material was tentatively decomposed in 4 hours, wait to reduce to 20 ~ 50 ℃ after, obtain the pre-burning powder.The pre-burning powder is put into ball grinder, adds the polyvinyl alcohol of 3.8g, add the agate ball of 35g and the absolute ethyl alcohol of 60ml subsequently, on ball mill with the rotating speed ball milling of 350r/min 15 hours, the mixed slurry that obtains mixing.Slurry is transferred in the drying basin, put into 80 ℃ of oven dry of baking oven and obtain the black powder, powder is placed in the tube furnace; under argon shield; be warming up to 750 ℃ of insulations 12 hours with 150 ℃/hour heating rates, naturally cool to 20 ~ 50 ℃ after, obtain the Li of carbon coated
4Ti
5O
12Composite material.Fig. 4 is for to do positive pole with this material, metal lithium sheet is done the simulated battery that negative pole is assembled into, charging and discharging curve under the 0.5C multiplying power, as seen from the figure, the material that is synthesized has excellent charging and discharging platform and higher reversible capacity, discharge capacity can reach 144mAh/g, and charge and discharge platform is smooth, demonstrates embedding lithium performance preferably.
Embodiment 3: according to mol ratio Li:Ti=0.8, take by weighing the Detitanium-ore-type TiO of 6.96g
2(analyzing pure), 7.1g lithium acetate (analyzing pure), 1.2g glucose and the citric acid of 1.5g, join in the ball grinder, add the agate ball of 35g and the absolute ethyl alcohol of 120ml subsequently, the sealing ball grinder, on ball mill with the rotating speed ball milling of 380r/min 6 hours, the mixed slurry that obtains mixing.Slurry is transferred in the drying basin, put into 80 ℃ of oven dry of baking oven and obtain presoma.Precursor powder is placed in the tube furnace, under argon shield, is warming up to 500 ℃ of insulations with 120 ℃/hour heating rates and raw material was tentatively decomposed in 2 hours, wait to reduce to 20 ~ 50 ℃ after, obtain the pre-burning powder.The pre-burning powder is put into ball grinder, adds the soluble starch of 1.8g and the block compound P123 of 2g, add the agate ball of 25g and the absolute ethyl alcohol of 50ml subsequently, on ball mill with the rotating speed ball milling of 400r/min 12 hours, the mixed slurry that obtains mixing.Slurry is transferred in the drying basin, put into 80 ℃ of oven dry of baking oven and obtain the black powder, powder is placed in the tube furnace; under argon shield; be warming up to 800 ℃ of insulations 10 hours with 150 ℃/hour heating rates, naturally cool to 20 ~ 50 ℃ after, obtain the Li of carbon coated
4Ti
5O
12Composite material.
Embodiment 4: according to mol ratio Li:Ti=0.85, take by weighing the Detitanium-ore-type TiO of 6.96g
2(analyzing pure), the lithium acetate of 7.55g (analyzing pure) sucrose of 1.5g and the oxalic acid of 2.4g join in the ball grinder, add the agate ball of 35g and the absolute ethyl alcohol of 120ml subsequently, the sealing ball grinder, on ball mill with the rotating speed ball milling of 300r/min 8 hours, the mixed slurry that obtains mixing.Slurry is transferred in the drying basin, put into 80 ℃ of oven dry of baking oven and obtain presoma.Precursor powder is placed in the tube furnace, under argon shield, is warming up to 500 ℃ of insulations with 180 ℃/hour heating rates and raw material was tentatively decomposed in 6 hours, wait to reduce to 20 ~ 50 ℃ after, obtain the pre-burning powder.The pre-burning powder is put into ball grinder, adds the phenolic resins of 1g, add the agate ball of 30g and the absolute ethyl alcohol of 60ml subsequently, on ball mill with the rotating speed ball milling of 350r/min 4 hours, the mixed slurry that obtains mixing.Slurry is transferred in the drying basin, put into 80 ℃ of oven dry of baking oven and obtain the black powder, powder is placed in the tube furnace; under argon shield; be warming up to 750 ℃ of insulations 12 hours with 160 ℃/hour heating rates, naturally cool to 20 ~ 50 ℃ after, obtain the Li of carbon coated
4Ti
5O
12Composite material.
Embodiment 5: according to mol ratio Li:Ti=0.85, take by weighing the Detitanium-ore-type TiO of 6.96g
2(analyzing pure), the citric acid of the lithium acetate of 7.55g (analyzing pure) 1.2g joins in the ball grinder, add the agate ball of 50g and the absolute ethyl alcohol of 100ml subsequently, the sealing ball grinder, on ball mill with the rotating speed ball milling of 350r/min 12 hours, the mixed slurry that obtains mixing.Slurry is transferred in the drying basin, put into 80 ℃ of oven dry of baking oven and obtain presoma.Precursor powder is placed in the tube furnace, under argon shield, is warming up to 500 ℃ of insulations with 160 ℃/hour heating rates and raw material was tentatively decomposed in 5 hours, wait to reduce to 20 ~ 50 ℃ after, obtain the pre-burning powder.The pre-burning powder is put into ball grinder, adds the POLYPROPYLENE GLYCOL of 1.5g, add the agate ball of 35g and the absolute ethyl alcohol of 55ml subsequently and mix, on ball mill with the rotating speed ball milling of 450r/min 5 hours, the mixed slurry that obtains mixing.Slurry is transferred in the drying basin, put into 80 ℃ of oven dry of baking oven and obtain the black powder, powder is placed in the tube furnace; under argon shield; be warming up to 800 ℃ of insulations 20 hours with 120 ℃/hour heating rates, naturally cool to 20 ~ 50 ℃ after, obtain the Li of carbon coated
4Ti
5O
12Composite material.
Claims (10)
1. preparation method who is used for lithium ion secondary battery cathode material lithium titanate is characterized in that the concrete steps of this method are:
A. with Li compound and TiO
2, according to Li:Ti=(0.8～1.1): 1 mol ratio is prepared burden, and add organic molecule carbon source presoma again and mix, ball milling in medium uniformly, oven dry, sintering 2～20 hours under 300 ℃～550 ℃ conditions obtains sintered precursor then;
B. sintered precursor and the organic macromolecule polymer carbon source presoma with step a gained mixes, ball milling in uniform medium, and oven dry is incubated 2～30h then under 600 ℃～900 ℃ conditions, obtain finished product lithium carbonate powder;
The addition of c. described organic molecule carbon source presoma is the phosphorus content contribution 1wt%～6wt% of the final product that generates in theory; The addition of described organic macromolecule polymer carbon source presoma is the phosphorus content contribution 6wt% ~ 12wt% of the final product that generates in theory; The mass ratio of the carbon in described organic macromolecule polymer carbon source presoma and the described organic molecule carbon source presoma is (1～5): 1.
2. the preparation method who is used for lithium ion secondary battery cathode material lithium titanate according to claim 1 is characterized in that described TiO
2Be Detitanium-ore-type.
3. the preparation method who is used for lithium ion secondary battery cathode material lithium titanate according to claim 1 is characterized in that described Li compound is lithium nitrate, lithium carbonate, lithium chloride, lithium acetate, lithium citrate, lithium oxalate, lithium formate, lithium lactate or isopropyl alcohol lithium.
4. the preparation method who is used for lithium ion secondary battery cathode material lithium titanate according to claim 1 is characterized in that described organic molecule carbon source presoma is at least a in glucose, sucrose, urea, tartaric acid, laurate, citric acid, oxalic acid, gluconic acid, the ethylenediamine tetra-acetic acid.
5. according to claim 1 or the 4 described preparation methods that are used for lithium ion secondary battery cathode material lithium titanate, the molecular weight that it is characterized in that described organic molecule carbon source presoma is 60-800.
6. the preparation method who is used for lithium ion secondary battery cathode material lithium titanate according to claim 1 is characterized in that described organic macromolecule polymer carbon source presoma is at least a among polyvinyl alcohol, polyethylene glycol, POLYPROPYLENE GLYCOL, soluble starch, phenolic resins, block compound P123, the block compound F127.
7. the preparation method who is used for lithium ion secondary battery cathode material lithium titanate according to claim 1 is characterized in that the molecular weight of described organic macromolecule polymer carbon source presoma is 10000 ~ 300000.
8. the preparation method who is used for lithium ion secondary battery cathode material lithium titanate according to claim 1 is characterized in that described ball-milling medium is at least a in water, ethanol, acetone, the ether; The mass ratio of ball and material is controlled to be 1～10:1 in the described mechanical milling process, and the rotating speed of ball milling is controlled at 300 ~ 550r/min; Described bake out temperature is 60 ℃～200 ℃.
9. the preparation method who is used for lithium ion secondary battery cathode material lithium titanate according to claim 1, the heating rate when it is characterized in that sintering among the described step a is controlled to be 100～200 ℃/hour.
10. the preparation method who is used for lithium ion secondary battery cathode material lithium titanate according to claim 1 is characterized in that the heating rate of sintering among the described step b is controlled to be 100～300 ℃/hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105476887A CN102024944A (en) | 2010-11-17 | 2010-11-17 | Method used for preparing anode material lithium titanate of lithium ion secondary battery |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105476887A CN102024944A (en) | 2010-11-17 | 2010-11-17 | Method used for preparing anode material lithium titanate of lithium ion secondary battery |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102024944A true CN102024944A (en) | 2011-04-20 |
Family
ID=43865990
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010105476887A Pending CN102024944A (en) | 2010-11-17 | 2010-11-17 | Method used for preparing anode material lithium titanate of lithium ion secondary battery |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102024944A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102633300A (en) * | 2011-12-07 | 2012-08-15 | 天津市贝特瑞新能源材料有限责任公司 | Carbon-coated lithium titanate cathode material as well as preparation method and applications thereof |
| CN102738463A (en) * | 2012-06-28 | 2012-10-17 | 北京理工大学 | Surface coating modification method of lithium vanadium phosphate cathode material by use of EDTA as carbon source |
| CN103515589A (en) * | 2013-09-09 | 2014-01-15 | 江苏华东锂电技术研究院有限公司 | Preparation method of lithium ion battery electrode active material |
| CN103682298A (en) * | 2013-11-27 | 2014-03-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Lanthanum-doped lithium titanate composite material and preparation method and application thereof |
| CN104600280A (en) * | 2015-01-27 | 2015-05-06 | 中国东方电气集团有限公司 | Method for preparing carbon-coated lithium titanate |
| WO2018154595A1 (en) * | 2017-02-21 | 2018-08-30 | International Advanced Research Centre For Powder Metallurgy And New Materials (Arci) | A method of producing high performance lithium titanate anode material for lithium ion battery applications |
| 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 |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1837057A (en) * | 2006-04-13 | 2006-09-27 | 复旦大学 | Li4Ti5O12 materials with spinel structure and preparation process and use thereof |
| CN101000960A (en) * | 2006-12-29 | 2007-07-18 | 深圳市贝特瑞电子材料有限公司 | Composite lithium titanate electrode material and preparation method thereof |
| CN101378119A (en) * | 2008-10-06 | 2009-03-04 | 天津巴莫科技股份有限公司 | Method for preparing carbon-coating type lithium titanate for lithium ion battery |
| CN101494288A (en) * | 2008-01-27 | 2009-07-29 | 比亚迪股份有限公司 | Preparation method for lithium ion secondary battery anode material ferric lithium phosphate |
| CN101759227A (en) * | 2008-12-24 | 2010-06-30 | 比亚迪股份有限公司 | Lithium titanate composite material and preparation method thereof |
-
2010
- 2010-11-17 CN CN2010105476887A patent/CN102024944A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1837057A (en) * | 2006-04-13 | 2006-09-27 | 复旦大学 | Li4Ti5O12 materials with spinel structure and preparation process and use thereof |
| CN101000960A (en) * | 2006-12-29 | 2007-07-18 | 深圳市贝特瑞电子材料有限公司 | Composite lithium titanate electrode material and preparation method thereof |
| CN101494288A (en) * | 2008-01-27 | 2009-07-29 | 比亚迪股份有限公司 | Preparation method for lithium ion secondary battery anode material ferric lithium phosphate |
| CN101378119A (en) * | 2008-10-06 | 2009-03-04 | 天津巴莫科技股份有限公司 | Method for preparing carbon-coating type lithium titanate for lithium ion battery |
| CN101759227A (en) * | 2008-12-24 | 2010-06-30 | 比亚迪股份有限公司 | Lithium titanate composite material and preparation method thereof |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102633300A (en) * | 2011-12-07 | 2012-08-15 | 天津市贝特瑞新能源材料有限责任公司 | Carbon-coated lithium titanate cathode material as well as preparation method and applications thereof |
| CN102738463A (en) * | 2012-06-28 | 2012-10-17 | 北京理工大学 | Surface coating modification method of lithium vanadium phosphate cathode material by use of EDTA as carbon source |
| CN103515589B (en) * | 2013-09-09 | 2016-02-10 | 江苏华东锂电技术研究院有限公司 | A kind of preparation method of lithium ion battery electrode active material |
| CN103515589A (en) * | 2013-09-09 | 2014-01-15 | 江苏华东锂电技术研究院有限公司 | Preparation method of lithium ion battery electrode active material |
| CN103682298A (en) * | 2013-11-27 | 2014-03-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Lanthanum-doped lithium titanate composite material and preparation method and application thereof |
| US20160218355A1 (en) * | 2015-01-27 | 2016-07-28 | Dongfang Electric Corporation | Method for Preparing Carbon-Coated Lithium Titanate |
| CN104600280A (en) * | 2015-01-27 | 2015-05-06 | 中国东方电气集团有限公司 | Method for preparing carbon-coated lithium titanate |
| US9923199B2 (en) * | 2015-01-27 | 2018-03-20 | Dongfang Electric Corporation | Method for preparing carbon-coated lithium titanate |
| WO2018154595A1 (en) * | 2017-02-21 | 2018-08-30 | International Advanced Research Centre For Powder Metallurgy And New Materials (Arci) | A method of producing high performance lithium titanate anode material for lithium ion battery applications |
| KR20190121291A (en) * | 2017-02-21 | 2019-10-25 | 인터내셔날 애드밴스드 리서치 센터 폴 파우더 메탈러지 앤드 뉴 머테리얼스 (에이알씨아이) | Manufacturing method of high performance lithium titanate anode material for application to lithium ion battery |
| US11001506B2 (en) | 2017-02-21 | 2021-05-11 | International Advanced Research Centre For Powder Metallurgy And New Materials (Arci) | Method of producing high performance lithium titanate anode material for lithium ion battery applications |
| KR102512034B1 (en) | 2017-02-21 | 2023-03-21 | 인터내셔날 애드밴스드 리서치 센터 폴 파우더 메탈러지 앤드 뉴 머테리얼스 (에이알씨아이) | Manufacturing method of high performance lithium titanate anode material for application in lithium ion battery |
| 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 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102064324A (en) | Lithium titanate anode material for modified lithium ion power batteries and preparation method thereof | |
| JP6095218B2 (en) | Method for producing active material coated with solid electrolyte, solution for forming layer containing solid electrolyte of all-solid lithium secondary battery, all-solid lithium secondary battery and method for producing the same | |
| CN102024944A (en) | Method used for preparing anode material lithium titanate of lithium ion secondary battery | |
| CN102820458A (en) | Synthetic method of nitrogen-enriched carbon coated lithium titanate composite material prepared by introduction of ionic liquid as carbon source | |
| CN101609883B (en) | Preparation method of nano-silver particle dispersed Li4Ti5O12 thin film lithium ion battery negative electrode | |
| CN101702431A (en) | Preparation method of lithium titanium negative electrode composite material for lithium ion battery | |
| CN102891303A (en) | Lithium ion secondary battery cathode material yttrium-doped lithium titanate and its preparation method and use | |
| CN101777644A (en) | Method for preparing carbon-encapsulated magnesium-doped lithium ion battery cathode material lithium titanate | |
| CN107093739B (en) | Potassium manganese oxide for potassium ion battery anode material and preparation method thereof | |
| CN103066265A (en) | Sodium ion battery negative pole active substance and preparation method and application thereof | |
| CN102044665A (en) | Preparation method of yttrium-containing lithium titanate serving as cathode material of lithium ion secondary battery | |
| CN103346308A (en) | Preparation method and use of fluorine-doped lithium titanate lithium ion battery cathode material | |
| CN102633300A (en) | Carbon-coated lithium titanate cathode material as well as preparation method and applications thereof | |
| CN101800307A (en) | Method for preparing carbon-coated manganese-doped lithium titanate negative electrode material of lithium ion battery | |
| CN103390748B (en) | A kind of preparation method of alumina-coated lithium cobaltate cathode material | |
| CN102249297A (en) | Method for preparing lithium titanate powder | |
| CN102593444A (en) | Preparation method of carbon-coated lithium titanate and product of carbon-coated lithium titanate | |
| CN109888256A (en) | A kind of Si@SiOx@N doping TiO2-δMaterial and its preparation method and application | |
| CN103280575B (en) | The preparation method of lithium ion secondary battery anode material nickle cobalt lithium manganate | |
| CN111029552A (en) | High-voltage high-rate lithium cobalt oxide cathode material and preparation method thereof | |
| CN102945952A (en) | Method for preparing anode material carbon coated lithium titanate for lithium ion power batteries | |
| CN101764227A (en) | Lithium ferrosilicon silicate/carbon composite cathode material and preparation method thereof | |
| CN103579599A (en) | Preparation method of yttrium-containing lithium ion battery cathode material lithium titanate carbon-coated composite material | |
| CN104577090A (en) | Method for preparing carbon and oxide composite modified lithium titanate material | |
| CN103779549B (en) | The preparation method of even particulate dispersion lithium ion battery electrode material nano lithium titanate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20110420 |