WO2012026067A1 - リチウムイオン二次電池負極材用粉末、これを用いたリチウムイオン二次電池負極およびキャパシタ負極、ならびにリチウムイオン二次電池およびキャパシタ - Google Patents
リチウムイオン二次電池負極材用粉末、これを用いたリチウムイオン二次電池負極およびキャパシタ負極、ならびにリチウムイオン二次電池およびキャパシタ Download PDFInfo
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- WO2012026067A1 WO2012026067A1 PCT/JP2011/004348 JP2011004348W WO2012026067A1 WO 2012026067 A1 WO2012026067 A1 WO 2012026067A1 JP 2011004348 W JP2011004348 W JP 2011004348W WO 2012026067 A1 WO2012026067 A1 WO 2012026067A1
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- WO
- WIPO (PCT)
- Prior art keywords
- negative electrode
- secondary battery
- ion secondary
- lithium ion
- powder
- Prior art date
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 131
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 131
- 239000000843 powder Substances 0.000 title claims abstract description 114
- 239000007773 negative electrode material Substances 0.000 title claims abstract description 78
- 239000003990 capacitor Substances 0.000 title claims description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 85
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 85
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 72
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 65
- 238000001237 Raman spectrum Methods 0.000 claims abstract description 21
- 238000004438 BET method Methods 0.000 claims abstract description 7
- 125000001475 halogen functional group Chemical group 0.000 claims abstract description 4
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 claims description 15
- 230000005260 alpha ray Effects 0.000 claims description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 10
- 229910052744 lithium Inorganic materials 0.000 abstract description 10
- 230000001351 cycling effect Effects 0.000 abstract 1
- 238000000034 method Methods 0.000 description 18
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- 229910052710 silicon Inorganic materials 0.000 description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 8
- 238000010586 diagram Methods 0.000 description 8
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- -1 nickel metal hydride Chemical class 0.000 description 5
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
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- GBROPGWFBFCKAG-UHFFFAOYSA-N picene Chemical compound C1=CC2=C3C=CC=CC3=CC=C2C2=C1C1=CC=CC=C1C=C2 GBROPGWFBFCKAG-UHFFFAOYSA-N 0.000 description 2
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- 229910012851 LiCoO 2 Inorganic materials 0.000 description 1
- 229910015643 LiMn 2 O 4 Inorganic materials 0.000 description 1
- 229910013870 LiPF 6 Inorganic materials 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
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- SLIUAWYAILUBJU-UHFFFAOYSA-N pentacene Chemical compound C1=CC=CC2=CC3=CC4=CC5=CC=CC=C5C=C4C=C3C=C21 SLIUAWYAILUBJU-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/134—Electrodes based on metals, Si or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/04—Hybrid capacitors
- H01G11/06—Hybrid capacitors with one of the electrodes allowing ions to be reversibly doped thereinto, e.g. lithium ion capacitors [LIC]
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/50—Electrodes characterised by their material specially adapted for lithium-ion capacitors, e.g. for lithium-doping or for intercalation
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
- H01G9/0425—Electrodes or formation of dielectric layers thereon characterised by the material specially adapted for cathode
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- H—ELECTRICITY
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/145—Liquid electrolytic capacitors
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Definitions
- the present inventors examined suppression of carbon film crystallinity. As a result, it was found that carbon having low crystallinity can be obtained by setting the carbon film forming treatment temperature to 700 ° C. or higher and 750 ° C. or lower, which is lower than the range of 800 ° C. or higher described in Patent Document 1.
- the carbon film forming treatment is performed at 700 ° C. or higher and 750 ° C. or lower, the tar component composed of polymer hydrocarbons generated during the thermal decomposition of the organic substance serving as the carbon source tends to remain in the carbon film, which will be described in the examples below.
- the powder for a negative electrode material of a lithium ion secondary battery of the present invention is a powder for a negative electrode material of a lithium ion secondary battery having a conductive carbon film on the surface of a lower silicon oxide powder.
- Te total content of tar components measured by TPD-MS is at 4000 ppm by mass or more 1 mass ppm, has a peak at 1350 cm -1 and 1580 cm -1 in the Raman spectrum, the half width of the peak of 1580 cm -1 wherein the but is 50 cm -1 or more 100 cm -1 or less.
- the peak at 1350 cm ⁇ 1 is called a D band and is a peak derived from disorder of the crystal structure of carbon, which means that carbon is close to amorphous.
- the peak height is defined as the height from the base line to the peak, with the line connecting the tails on both sides of the target peak as a straight line.
- the full width at half maximum is the length of the line formed by drawing a straight line parallel to the horizontal axis at the midpoint between the peak and the baseline at the peak wave number and the intersection of the straight line and the Raman spectrum. .
- the base line determines the upper and lower end points as follows.
- the peak of 1350 cm -1, the upper limit of the baseline 1450 cm -1, the lower limit was made 1250 cm -1, the mean value of the intensity range of the intensity is 1450 ⁇ 5 cm -1 in the upper, the intensity in the lower limit of 1550 ⁇ 5 cm -1 The average value of the intensity of the range.
- the peak of 1350 cm -1, the upper limit of the baseline 1650 cm -1, the lower limit was made 1550 cm -1, the mean value of the intensity range of the intensity is 1650 ⁇ 5 cm -1 in the upper, the intensity in the lower limit of 1550 ⁇ 5 cm -1 The average value of the intensity of the range.
- the raw material chamber 6 is formed of a cylindrical body, and a cylindrical raw material container 8 and a heating source 10 surrounding the raw material container 8 are disposed at the center thereof.
- a heating source 10 for example, an electric heater can be used.
- the tar component generated during the formation of the carbon film can be volatilized and removed from the carbon film by vacuum treatment. Moreover, when the heating holding temperature is in the above range, the generation of SiC in the vicinity of the interface between the silicon oxide and the carbon film is suppressed.
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Abstract
Description
SiOx+(44-x)/10Li++(44-x)/10e-
→ (4-x)/20Li22Si5+x/4Li4SiO4 …(1)
本発明のリチウムイオン二次電池負極材用粉末は、低級酸化珪素粉末の表面に導電性炭素皮膜を有するリチウムイオン二次電池負極材用粉末であって、TPD-MSで測定したタール成分の合計含有率が1質量ppm以上4000質量ppm以下であり、ラマンスペクトルにおいて1350cm-1および1580cm-1にピークを有し、1580cm-1のピークの半値幅が50cm-1以上100cm-1以下であることを特徴とする。
3-1.SiOxのxの算出方法
SiOxのxは、リチウムイオン二次電池負極材用粉末中のO含有率とSi含有率のモル比(O/Si)であり、例えば下記測定方法で測定したO含有率およびSi含有率を用いて算出することができる。
リチウムイオン二次電池負極材用粉末中のO含有率は、酸素濃度分析装置(Leco社製、TC436)を用いて、試料10mgを不活性ガス融解・赤外線吸収法によって分析することで定量評価した試料中のO含有量から算出する。
リチウムイオン二次電池負極材用粉末中のSi含有率は、試料に硝酸およびフッ酸を加えて試料を溶解させ、得られた溶液をICP発光分光分析装置(株式会社島津製作所製)で分析することによって定量評価下試料中のSi含有量から算出する。この方法では、Si、SiOおよびSiO2が溶解され、これらを構成するSiを検出できる。
本発明のリチウムイオン二次電池負極材用粉末において、「低級酸化珪素粉末の表面に導電性炭素皮膜を有する」とは、AlKα線(1486.6eV)を用いたX線光電子分光分析装置(XPS)で、導電性炭素皮膜の形成処理を施した低級酸化珪素粉末の表面分析を行った場合に、SiとCとのモル比の値Si/Cが0.02以下であることをいう。XPSの測定条件は表1に示す通りとする。「Si/Cが0.02以下」とは、低級酸化珪素粉末の表面のほとんどがCに覆われており、Siがほとんど露出していない状態である。
導電性炭素皮膜を形成した低級酸化珪素粉末の比表面積は、以下のBET法によって測定することができる。試料0.5gをガラスセルに入れて、200℃で約5時間、減圧乾燥する。そして、この試料について測定した液体窒素温度(-196℃)における窒素ガス吸着等温線から比表面積を算出する。測定条件は表2に示す通りとする。
リチウムイオン二次電池負極材用粉末の残留タール成分量は、以下のTPD-MS(Temperature Programmed Desorption-Mass Spectroscopy;昇温熱脱離・質量分析法)によって測定することができる。試料50mgをシリカ製セルに入れ、50mL/minのヘリウムガスフロー中で、室温から1000℃まで10K/minの速度で昇温する。そして、発生したガスを質量分析計(株式会社島津製作所製、GC/MS QP5050A)で分析する。
ラマンスペクトルは、ラマン分光装置を使用し、表3に示す条件で測定する。
炭素皮膜率は、リチウムイオン二次電池負極材用粉末の質量と、炭素濃度分析装置(Leco社製、CS400)を用いて酸素気流燃焼-赤外線吸収法によってCO2ガスを分析することで定量評価した炭素量の結果から算出する。ルツボはセラミックルツボを、助燃剤は銅を用い、分析時間は40秒とする。
リチウムイオン二次電池負極材用粉末の比抵抗ρ(Ωcm)は、下記(2)式を用いて算出する。
ρ=R×A/L …(2)
ここで、R:試料の電気抵抗(Ω)、A:試料の底面積(cm2)、L:試料の厚さ(cm)である。
試料の電気抵抗は、例えば、デジタルマルチメーター(岩通計測株式会社製、VOAC7513)を用いた二端子法によって測定することができる。この場合、試料は、粉末抵抗測定用治具(治具部:内径20mmのステンレス製、枠部:ポリテトラフルオロエチレン製)に試料0.20gを充填し、20kgf/cm2で60秒間加圧して成形し、成形した試料の厚さはマイクロメーターで測定する。
図3は、酸化珪素の製造装置の構成例を示す図である。この装置は、真空室5と、真空室5内に配置された原料室6と、原料室6の上部に配置された析出室7とを備える。
低級酸化珪素粉末の表面への導電性炭素皮膜の形成は、CVD等により行う。具体的には、装置としてロータリーキルンを用い、ガスとして炭素源である炭化水素ガスまたは有機物含有ガスと、不活性ガスとの混合ガスを用いて行う。
導電性炭素皮膜を形成した低級酸化珪素粉末には、真空下で、600℃以上750℃以下の温度に10分以上保持する真空処理を施す。真空処理は、低級酸化珪素粉末を真空槽に収容した状態で行い、真空槽の内圧は、油拡散ポンプを用いて1Pa以下に保つ。この内圧は、ピラニー真空計を用いて測定する。
本発明のリチウムイオン二次電池負極材用粉末およびリチウムイオン二次電池負極を用いた、コイン形状のリチウムイオン二次電池の構成例を、前記図1を参照して説明する。同図に示すリチウムイオン二次電池の基本的構成は、上述の通りである。
1-1.リチウムイオン二次電池の構成
リチウムイオン二次電池の構成は、前記図1に示すコイン形状とした。
充放電試験には、二次電池充放電試験装置(株式会社ナガノ製)を用いた。充電は、リチウムイオン二次電池の両極間の電圧が0Vに達するまでは1mAの定電流で行い、電圧が0Vに達した後は、0Vを維持したまま充電を行った。その後、電流値が20μAを下回った時点で充電を終了した。放電は、リチウムイオン二次電池の両極間の電圧が1.5Vに達するまでは1mAの定電流で行った。以上の充放電試験は10サイクル行った。
上記条件で作製したリチウムイオン二次電池について充放電試験を行い、サイクル容量維持率を指標として評価を行った。また、リチウムイオン二次電池負極材用粉末の比抵抗も測定した。これらの値を試験条件と併せて表4に示す。サイクル容量維持率とは、10サイクル目の放電容量を初回放電容量で除した値であり、この値が大きいほどサイクル特性が良好であることを示す。
2:負極、 2a:作用極ケース、 2b:作用極集電体、
2c:作用極、 3:セパレーター、 4:ガスケット、 5:真空室、
6:原料室、 7:析出室、 8:原料容器、 9:混合造粒原料、
10:加熱源、 11:析出基体、 12:低級酸化珪素
Claims (10)
- 低級酸化珪素粉末の表面に導電性炭素皮膜を有するリチウムイオン二次電池負極材用粉末であって、
TPD-MSで測定したタール成分の合計含有率が1質量ppm以上4000質量ppm以下であり、
ラマンスペクトルにおいて1350cm-1および1580cm-1にピークを有し、1580cm-1のピークの半値幅が50cm-1以上100cm-1以下であることを特徴とするリチウムイオン二次電池負極材用粉末。 - BET法で測定した比表面積が0.3m2/g以上40m2/g以下であることを特徴とする請求項1に記載のリチウムイオン二次電池負極材用粉末。
- ラマンスペクトルにおいて、1350cm-1のピークの高さI1350と1580cm-1のピークの高さI1580の比の値I1350/I1580が、0.1<I1350/I1580<1.4を満足することを特徴とする請求項1または2に記載のリチウムイオン二次電池負極材用粉末。
- 前記導電性炭素皮膜の占める割合が0.2質量%以上10質量%以下であることを特徴とする請求項1~3のいずれかに記載のリチウムイオン二次電池負極材用粉末。
- 比抵抗が40000Ωcm以下であることを特徴とする請求項1~4のいずれかに記載のリチウムイオン二次電池負極材用粉末。
- CuKα線を用いたX線回折装置で測定した場合に、2θ=10°~30°に現れるSiOxに由来するハローの最大値P1と、2θ=28.4±0.3°に現れるSi(111)の最強線ピークの値P2が、P2/P1<0.01を満たすことを特徴とする請求項1~5のいずれかに記載のリチウムイオン二次電池負極材用粉末。
- 請求項1~6のいずれかに記載のリチウムイオン二次電池負極材用粉末を用いたリチウムイオン二次電池負極。
- 請求項1~6のいずれかに記載のリチウムイオン二次電池負極材用粉末を用いたキャパシタ負極。
- 請求項7に記載のリチウムイオン二次電池負極を用いたリチウムイオン二次電池。
- 請求項8に記載のキャパシタ負極を用いたキャパシタ。
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Also Published As
Publication number | Publication date |
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US20130149606A1 (en) | 2013-06-13 |
JPWO2012026067A1 (ja) | 2013-10-28 |
KR20130061733A (ko) | 2013-06-11 |
EP2610949A4 (en) | 2014-02-26 |
CN103081188B (zh) | 2015-09-23 |
JP5584299B2 (ja) | 2014-09-03 |
CN103081188A (zh) | 2013-05-01 |
EP2610949A1 (en) | 2013-07-03 |
KR101513819B1 (ko) | 2015-04-20 |
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