CN103441267A - Preparation method of titanium dioxide coated lithium cobalt oxide anode material - Google Patents
Preparation method of titanium dioxide coated lithium cobalt oxide anode material Download PDFInfo
- Publication number
- CN103441267A CN103441267A CN2013103796846A CN201310379684A CN103441267A CN 103441267 A CN103441267 A CN 103441267A CN 2013103796846 A CN2013103796846 A CN 2013103796846A CN 201310379684 A CN201310379684 A CN 201310379684A CN 103441267 A CN103441267 A CN 103441267A
- Authority
- CN
- China
- Prior art keywords
- titanium dioxide
- coated
- preparation
- titanium
- licoo
- 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 discloses a preparation method of a titanium dioxide coated lithium cobalt oxide anode material. The preparation method is characterized in that a titanium dioxide film is uniformly coated on the surface of the lithium cobalt oxide anode material, namely, LiCoO2. The preparation process comprises the following steps: dispersing a titanium-containing compound into a dispersing agent; sequentially adding LiCoO2 powder and deionized water; uniformly mixing; drying; and roasting to obtain the titanium dioxide coated LiCoO2 material. According to the preparation method of the titanium dioxide coated lithium cobalt oxide anode material, the components of raw materials and formulas of products are easily controlled; the large and mass production can be performed; and the electrochemical testing result shows that the lithium cobalt oxide anode material prepared by the preparation method and coated and modified by titanium dioxide is high in specific capacity and outstanding in cycle performance.
Description
Technical field
The present invention relates to a kind of preparation method of coated by titanium dioxide lithium cobaltate cathode material.Belong to the lithium ion battery electrode material technical field.
Background technology
There is α-NaFeO
2the LiCoO of type layer structure
2be at present unique industrialization be widely used in the positive electrode of commercial lithium-ion batteries on a large scale, and also will occupy dominant position for a comparatively long period of time.But LiCoO
2expensive, actual specific capacity 120-140mAh/g, be only 50% left and right of its theoretical specific capacity 274mAh/g.When the charge cutoff voltage of lithium ion battery during higher than 4.2V, LiCoO
2a large amount of Co in structure
3+will become Co
4+, Co
4+formation will cause the formation of oxygen defect, the binding force that this will weaken between transition metals cobalt and oxygen, make Co
4+be dissolved in electrolyte, thereby destroy the electrode material crystal structure, specific capacity is reduced rapidly.
For improving the problem that after charge cutoff voltage, cobalt acid lithium material cyclical stability is poor and high rate during charging-discharging is poor, more study on the modification work has been arranged at present, use metal oxide as Al
2o
3, TiO
2, MgO, CuO etc. and fast lithium ion conductor coat and process cobalt acid lithium, can improve cycle performance or minute high rate performance of material.Electrochemistry journal (Electrochimica Acta) 56 (2011) 6573-6580 have synthesized amorphous lithium phosphorus nitrogen oxide lithium ion conductor by magnetron sputtering and churned mechanically method and have coated LiCoO
2electrode material, improved the cyclical stability of material under high voltage condition.In the 3.0-4.4V voltage range, after 0.2C multiplying power circulation 40 times, lithium phosphorus nitrogen oxide lithium ion conductor coats LiCoO
2the capability retention of material reaches 90%, and now the conservation rate of pure phase only has 65%.
Electrochemistry journal (Electrochimica Acta) 56 (2011) 9027-9031 are with Cu (NO
3)
23H
2o, CH
3cOOLi, Co (CH
3cOO)
2with malic acid be raw material, synthesized nanometer CuO by sol-gel process and coated LiCoO
2electrode material, improved the high rate capability of material.This material circulates after 10 times under the 30C multiplying power, and its capability retention surpasses 90%, and under 40C and 50C multiplying power, its height ratio capacity is respectively 135mAh/g and 123mAh/g.Above method for coating preparation process commonly used and raw materials used more complicated, production cost is higher, is not easy to industrial production.
Summary of the invention
The present invention proposes a kind of preparation method of coated by titanium dioxide lithium cobaltate cathode material, adopt the wet-mixed synthesis technique, directly utilize grinding that titanium-containing compound and cobalt acid lithium particle is dispersed in dispersant, thereby obtain the mixture of titanium-containing compound and cobalt acid lithium, then add deionized water dry after hydrolysis, then prepare the lithium cobaltate cathode material of the coated by titanium dioxide of chemical property excellence through high-temperature heat treatment.Concrete preparation method is as follows:
After evenly spreading to after ethanol or acetone soln by titanium-containing compound (as butyl titanate, tetraethyl titanate, isopropyl titanate), add cobalt acid lithium (LiCoO
2) powder ground, thereby obtain the mixture of titanium-containing compound and cobalt acid lithium, then add deionized water dry after hydrolysis, with 2-10 ℃/min speed, be warming up to 300-600 ℃ and calcining at constant temperature 2-10 hour, make coated by titanium dioxide LiCoO after naturally cooling
2positive electrode.Wherein, count in mass ratio titanium-containing compound: dispersant: LiCoO
2: deionized water is 1:500-5000:50-1000:50-1000.
By LiCoO
2and the synthetic coated by titanium dioxide LiCoO of employing the inventive method
2positive electrode respectively with conductive carbon black and binding agent polyvinylidene fluoride (PVDF) in mass ratio 90:10:10 mix, be coated on aluminium foil, be cut into anode pole piece after drying, in 100 ℃ of vacuumizes 24 hours.Take lithium metal as to electrode, by electrolyte LiPF
6salt is dissolved in the mixed solution of the ethylene carbonate (EC) that mass ratio is 1:1:1/dimethyl carbonate (DMC)/methyl ethyl carbonate (EMC) and forms electrolyte, and the concentration of electrolyte is 1mol/L, in the argon gas glove box, is assembled into button cell.Adopt the blue electric CT2001A type cell tester in Wuhan to carry out electrochemical property test, the charging/discharging voltage scope is 3.0V-4.5V (vs.Li
+/ Li), test result as shown in Figure 2.With the LiCoO do not coated
2compare coated by titanium dioxide LiCoO
2specific capacity performance and cyclical stability be improved significantly.
The method that the present invention prepares the coated by titanium dioxide lithium cobaltate cathode material has following remarkable advantage: the titanium-containing compound that 1) the present invention adopts is as reactant, in the grinding distribution process, Direct Uniform is dispersed in cobalt acid lithium particle surface, in hydrolysis reaction, at surface in situ, forms TiO
2coating layer, coat evenly; 2) grinding distribution of the present invention prepares the method for coated by titanium dioxide lithium cobaltate cathode material; material composition and product formula are easily controlled; be suitable for large-scale production in enormous quantities; electro-chemical test shows to adopt the lithium cobaltate cathode material of the synthetic alumina-coated modification of the present invention; specific capacity is high, and cycle performance is good.
The accompanying drawing explanation
Fig. 1 is the pure phase LiCoO in embodiment 1
2the SEM figure of material;
The coated by titanium dioxide LiCoO that Fig. 2 is embodiment 1 gained
2positive electrode, i.e. LiCoO
2/ TiO
2sEM figure; Contrast Fig. 1 and 2, the cobalt acid lithium granule-morphology of process this method modification remains unchanged substantially, can not destroy pure cobalt acid lithium granule-morphology, keeps the good processing characteristics of pure phase material.
Pure phase LiCoO in Fig. 3, embodiment 1
2the coated by titanium dioxide LiCoO of material and embodiment 1 gained
2positive electrode, i.e. LiCoO
2/ TiO
2cycle performance curve under different multiplying; As can be seen from Figure 3, in the charging/discharging voltage scope of 3-4.5V, after 0.2C, 0.5C, 1C, lower 80 charge and discharge cycles of 2C different multiplying, the capacity of pure phase cobalt acid lithium material is down to 70.2mAh/g, and the cobalt of modification acid lithium capacity still has 155.9 mAh/g.Explanation has had significantly raising by the relatively unmodified cobalt acid of the cyclical stability lithium of the cobalt acid lithium material of modification of the present invention, and especially, under the high power charging-discharging condition that stability is had to considerable influence, the improvement of stability is more obvious.
embodiment
embodiment 1
Calculate in mass ratio titanium-containing compound: dispersant: LiCoO
2: the ratio that deionized water is 1:5000:1000:1000, the 0.0071g tetraethyl titanate is distributed in 6ml ethanol, then add successively and then add successively 1g cobalt acid lithium powder and 1ml deionized water, mix, dry, obtain presoma; The presoma that obtains is warming up to 300 ℃ and constant temperature 2 hours with 2 ℃/min speed, then naturally cools to room temperature, obtain coated by titanium dioxide LiCoO of the present invention
2product, wherein in the coated by titanium dioxide layer, the quality of titanium is LiCoO
20.1% of quality.
embodiment 2
Calculate in mass ratio, i.e. titanium in titanium-containing compound: dispersant: LiCoO
2: the ratio that deionized water is 1:500:50:50, the 0.142g tetraethyl titanate is distributed in 12ml acetone, then add successively 1g cobalt acid lithium powder and 1ml deionized water, mix, dry, obtain presoma; The presoma that obtains is warming up to 400 ℃ and constant temperature 2 hours with 5 ℃/min speed, then naturally cools to room temperature, obtain coated by titanium dioxide LiCoO of the present invention
2product, wherein in the coated by titanium dioxide layer, the quality of titanium is LiCoO
22% of quality.
embodiment 3
Calculate in mass ratio, i.e. titanium in titanium-containing compound: dispersant: LiCoO
2: the ratio that deionized water is 1:4000:500:400, the 0.0118g isopropyl titanate is distributed in 10ml ethanol, then add successively 1g cobalt acid lithium powder and 0.8ml deionized water, mix, dry, obtain presoma; The presoma that obtains is warming up to 600 ℃ and constant temperature 10 hours with 10 ℃/min speed, then naturally cools to room temperature, obtain coated by titanium dioxide LiCoO of the present invention
2product, wherein in the coated by titanium dioxide layer, the quality of titanium is LiCoO
20.2% of quality.
embodiment 4
Calculate in mass ratio, i.e. titanium in titanium-containing compound: dispersant: LiCoO
2: the ratio that deionized water is 1:1000:200:100, the 0.295g isopropyl titanate is distributed in 6ml acetone, then add successively 1g cobalt acid lithium powder and 0.5ml deionized water, mix, dry, obtain presoma; The presoma that obtains is warming up to 500 ℃ and constant temperature 10 hours with 5 ℃/min speed, then naturally cools to room temperature, obtain coated by titanium dioxide LiCoO of the present invention
2product, wherein in the coated by titanium dioxide layer, the quality of titanium is LiCoO
20.5% of quality.
embodiment 5
Calculate in mass ratio, i.e. titanium in titanium-containing compound: dispersant: LiCoO
2: the ratio that deionized water is 1:2000:100:100, the 0.0475g tetraethyl titanate is distributed in 25ml acetone, then add successively 1g cobalt acid lithium powder and 1ml deionized water, mix, dry, obtain presoma; The presoma that obtains is warming up to 400 ℃ and constant temperature 6 hours with 3 ℃/min speed, then naturally cools to room temperature, obtain coated by titanium dioxide LiCoO of the present invention
2product, wherein in the coated by titanium dioxide layer, the quality of titanium is LiCoO
21% of quality.
embodiment 6
Calculate in mass ratio, i.e. titanium in titanium-containing compound: dispersant: LiCoO
2: the ratio that deionized water is 1:3000:70:60, the 0.0713g tetraethyl titanate is distributed in 56ml ethanol, then add successively 1g cobalt acid lithium powder and 0.9ml deionized water, mix, dry, obtain presoma; The presoma that obtains is warming up to 300 ℃ and constant temperature 8 hours with 6 ℃/min speed, then naturally cools to room temperature, obtain coated by titanium dioxide LiCoO of the present invention
2product, wherein in the coated by titanium dioxide layer, the quality of titanium is LiCoO
21.5% of quality.
In sum, the preparation method of the lithium cobaltate cathode material of a kind of coated by titanium dioxide modification of the present invention, the coated by titanium dioxide lithium cobaltate cathode material made by the method is compared with pure phase cobalt acid lithium material, its specific capacity performance and cyclical stability have obtained obvious improvement, and its preparation technology is simple, be suitable for the characteristics of industrial-scale production.
Above said content is the basic explanation under conceiving for the present invention only, and, according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.
Claims (5)
1. the preparation method of a coated by titanium dioxide lithium cobaltate cathode material, is characterized in that the preparation method is as follows: after titanium-containing compound is evenly spread to dispersant, add cobalt acid lithium (LiCoO
2) powder ground, thereby obtain the mixture of titanium-containing compound and cobalt acid lithium, then add deionized water dry after hydrolysis, calcining, make coated by titanium dioxide LiCoO after naturally cooling
2positive electrode.
2. the preparation method of coated by titanium dioxide lithium cobaltate cathode material according to claim 1, is characterized in that: count in mass ratio titanium-containing compound: dispersant: LiCoO
2: deionized water is 1:500-5000:50-1000:50-1000.
3. the preparation method of coated by titanium dioxide lithium cobaltate cathode material according to claim 1, is characterized in that: dry presoma is warming up to 300-600 ℃ and calcining at constant temperature 2-10 hour with 2-10 ℃/min speed.
4. the preparation method of coated by titanium dioxide lithium cobaltate cathode material according to claim 1 is characterized in that: titanium-containing compound is a kind of in butyl titanate, tetraethyl titanate, isopropyl titanate.
5. the preparation method of coated by titanium dioxide lithium cobaltate cathode material according to claim 1, it is characterized in that: dispersant is ethanol or acetone.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013103796846A CN103441267A (en) | 2013-08-28 | 2013-08-28 | Preparation method of titanium dioxide coated lithium cobalt oxide anode material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013103796846A CN103441267A (en) | 2013-08-28 | 2013-08-28 | Preparation method of titanium dioxide coated lithium cobalt oxide anode material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103441267A true CN103441267A (en) | 2013-12-11 |
Family
ID=49694951
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2013103796846A Pending CN103441267A (en) | 2013-08-28 | 2013-08-28 | Preparation method of titanium dioxide coated lithium cobalt oxide anode material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103441267A (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103618080A (en) * | 2013-12-19 | 2014-03-05 | 长沙矿冶研究院有限责任公司 | Pretreatment method of cobaltosic oxide for preparing high-voltage lithium cobalt oxide, high-voltage lithium cobalt oxides anode material and preparation method of high-voltage lithium cobalt oxide |
| CN103956472A (en) * | 2014-05-04 | 2014-07-30 | 张萍 | Preparation method of multi-element cathode material covered with titanium oxide |
| CN104617267A (en) * | 2015-01-21 | 2015-05-13 | 长沙矿冶研究院有限责任公司 | Ultrathin TiO2 coating layer of lithium battery cathode material, lithium battery cathode material and preparation method of lithium battery cathode material |
| CN106571452A (en) * | 2016-10-26 | 2017-04-19 | 浙江天能能源科技股份有限公司 | Lithium ion battery positive electrode material and preparation method thereof |
| CN106876793A (en) * | 2017-03-15 | 2017-06-20 | 山东威林特新能源科技有限公司 | A kind of lithium titanate battery preparation method of high circulation performance |
| CN109119621A (en) * | 2018-09-11 | 2019-01-01 | 乳源东阳光磁性材料有限公司 | Lithium lanthanum titanate-lithium titanate coated nickel cobalt lithium aluminate anode material and preparation method thereof |
| CN109761287A (en) * | 2018-12-29 | 2019-05-17 | 合肥融捷能源材料有限公司 | A kind of high-rate type lithium cobaltate and its preparation method and application |
| CN111029552A (en) * | 2019-12-24 | 2020-04-17 | 天津巴莫科技有限责任公司 | High-voltage high-rate lithium cobalt oxide cathode material and preparation method thereof |
| CN111533134A (en) * | 2020-05-08 | 2020-08-14 | 蒋达金 | Preparation method of lithium iron borate |
| CN112174220A (en) * | 2020-09-22 | 2021-01-05 | 中国计量大学 | Titanium dioxide coated cobaltosic oxide honeycomb pore nanowire material and preparation and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080032185A1 (en) * | 2002-12-23 | 2008-02-07 | 3M Innovative Properties Company | Cathode composition for rechargeable lithium battery |
-
2013
- 2013-08-28 CN CN2013103796846A patent/CN103441267A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080032185A1 (en) * | 2002-12-23 | 2008-02-07 | 3M Innovative Properties Company | Cathode composition for rechargeable lithium battery |
Non-Patent Citations (2)
| Title |
|---|
| 吴锋: "TiO2包覆对LiCo1/3Ni1/3Mn1/3O2材料的表面改性", 《物理化学学报》 * |
| 孙文彬: "LiCoO2的TiO2包覆原理探索研究", 《电源技术》 * |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103618080A (en) * | 2013-12-19 | 2014-03-05 | 长沙矿冶研究院有限责任公司 | Pretreatment method of cobaltosic oxide for preparing high-voltage lithium cobalt oxide, high-voltage lithium cobalt oxides anode material and preparation method of high-voltage lithium cobalt oxide |
| CN103618080B (en) * | 2013-12-19 | 2015-10-28 | 长沙矿冶研究院有限责任公司 | Prepare the preprocess method, high voltage lithium cobalt oxide anode and preparation method thereof of high voltage cobalt acid lithium cobaltosic oxide |
| CN103956472A (en) * | 2014-05-04 | 2014-07-30 | 张萍 | Preparation method of multi-element cathode material covered with titanium oxide |
| CN103956472B (en) * | 2014-05-04 | 2016-02-24 | 陈梦佳 | A kind of preparation method of polynary positive pole material of titanium-oxide-coated |
| CN104617267A (en) * | 2015-01-21 | 2015-05-13 | 长沙矿冶研究院有限责任公司 | Ultrathin TiO2 coating layer of lithium battery cathode material, lithium battery cathode material and preparation method of lithium battery cathode material |
| CN104617267B (en) * | 2015-01-21 | 2017-02-22 | 长沙矿冶研究院有限责任公司 | Ultrathin TiO2 coating layer of lithium battery cathode material, lithium battery cathode material and preparation method of lithium battery cathode material |
| CN106571452A (en) * | 2016-10-26 | 2017-04-19 | 浙江天能能源科技股份有限公司 | Lithium ion battery positive electrode material and preparation method thereof |
| CN106876793A (en) * | 2017-03-15 | 2017-06-20 | 山东威林特新能源科技有限公司 | A kind of lithium titanate battery preparation method of high circulation performance |
| CN109119621A (en) * | 2018-09-11 | 2019-01-01 | 乳源东阳光磁性材料有限公司 | Lithium lanthanum titanate-lithium titanate coated nickel cobalt lithium aluminate anode material and preparation method thereof |
| CN109761287A (en) * | 2018-12-29 | 2019-05-17 | 合肥融捷能源材料有限公司 | A kind of high-rate type lithium cobaltate and its preparation method and application |
| CN109761287B (en) * | 2018-12-29 | 2021-08-27 | 合肥融捷能源材料有限公司 | High-rate lithium cobalt oxide and preparation method and application thereof |
| CN111029552A (en) * | 2019-12-24 | 2020-04-17 | 天津巴莫科技有限责任公司 | High-voltage high-rate lithium cobalt oxide cathode material and preparation method thereof |
| CN111533134A (en) * | 2020-05-08 | 2020-08-14 | 蒋达金 | Preparation method of lithium iron borate |
| CN112174220A (en) * | 2020-09-22 | 2021-01-05 | 中国计量大学 | Titanium dioxide coated cobaltosic oxide honeycomb pore nanowire material and preparation and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103441267A (en) | Preparation method of titanium dioxide coated lithium cobalt oxide anode material | |
| CN103474625B (en) | A kind of Olivine-type Cathode Material in Li-ion Batteries method for coating of nucleocapsid structure | |
| Ding et al. | Improvement of electrochemical properties of layered LiNi1/3Co1/3Mn1/3O2 positive electrode material by zirconium doping | |
| Liu et al. | Fluorine doping and Al2O3 coating Co-modified Li [Li0. 20Ni0. 133Co0. 133Mn0. 534] O2 as high performance cathode material for lithium-ion batteries | |
| CN104201323A (en) | Preparation method of alumina coated lithium cobaltate positive electrode material | |
| CN101807696A (en) | Titanium phosphate lithium material used for cathode of lithium ion battery and preparation method thereof | |
| CN105140492A (en) | Cobalt-nickel lithium manganate composite positive electrode material with surface wrapped by lithium zirconate and preparation method | |
| Nie et al. | Effects of precursor particle size on the performance of LiNi0. 5Co0. 2Mn0. 3O2 cathode material | |
| CN101752562B (en) | Compound doped modified lithium ion battery anode material and preparation method thereof | |
| CN102738458A (en) | Surface modification method of lithium-rich cathode material | |
| Hou et al. | Drastic enhancement in the rate and cyclic behavior of LiMn2O4 electrodes at elevated temperatures by phosphorus doping | |
| CN104779385B (en) | A kind of height ratio capacity anode material for lithium-ion batteries and preparation method thereof | |
| Sun et al. | Cu doped LiNi0. 5Mn1. 5− xCuxO4 (x= 0, 0.03, 0.05, 0.10, 0.15) with significant improved electrochemical performance prepared by a modified low temperature solution combustion synthesis method | |
| CN103390748B (en) | A kind of preparation method of alumina-coated lithium cobaltate cathode material | |
| CN103956475A (en) | Method for preparing lithium titanate of lithium ion battery cathode material | |
| CN105185954A (en) | LiAlO2 coated LiNi1-xCoxO2 lithium-ion battery positive electrode material and preparation method thereof | |
| CN104638242A (en) | Method for synthesizing lithium ion battery cathode material lithium iron phosphate through in situ polymerizing and cladding | |
| CN103594708B (en) | One is appraised at the current rate iron-based composite positive pole and preparation method thereof | |
| CN104253265A (en) | Cation-doped and modified lithium ion battery (4:4:2)type ternary cathode material and preparation method thereof | |
| Guo et al. | Effects of sodium substitution on properties of LiMn2O4 cathode for lithium ion batteries | |
| CN103762354A (en) | LiNi0.5Mn1.5O4 material, preparation method thereof as well as lithium ion battery | |
| CN108091854A (en) | A kind of high-voltage spinel type anode material for lithium-ion batteries of Anion-cation multiple dope and preparation method thereof | |
| CN102299316A (en) | Layered oxide lithium ion battery anode and preparation method thereof | |
| CN102386412A (en) | Lithium ion battery anode Li3V2(PO4)3/C composite material and preparation method thereof | |
| CN109103452A (en) | The preparation method of nano lithium iron manganese anode composite material |
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: 20131211 |