KR20100118808A - Method of preparing a composition for making anode of lithium secondary battery and lithium secondary battery prepared by using the same - Google Patents
Method of preparing a composition for making anode of lithium secondary battery and lithium secondary battery prepared by using the same Download PDFInfo
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- KR20100118808A KR20100118808A KR1020090037695A KR20090037695A KR20100118808A KR 20100118808 A KR20100118808 A KR 20100118808A KR 1020090037695 A KR1020090037695 A KR 1020090037695A KR 20090037695 A KR20090037695 A KR 20090037695A KR 20100118808 A KR20100118808 A KR 20100118808A
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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
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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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
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0404—Methods of deposition of the material by coating on electrode collectors
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/621—Binders
- H01M4/622—Binders being polymers
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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
- 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
Abstract
Description
본 발명은 리튬 이차전지의 음극 형성용 조성물의 제조방법과 이를 사용하여 제조된 리튬 이차전지에 관한 것으로서, 보다 상세하게는, 바인더의 균일한 분산 및 접착력 향상이 가능하여 전극의 성능을 향상시킬 수 있는 리튬 이차전지의 음극 형성용 조성물의 제조방법과 이를 사용하여 제조된 리튬 이차전지에 관한 것이다.The present invention relates to a method for preparing a composition for forming a negative electrode of a lithium secondary battery and a lithium secondary battery manufactured using the same. More particularly, uniform dispersion of a binder and adhesion can be improved, thereby improving performance of an electrode. The present invention relates to a method for preparing a composition for forming a negative electrode of a lithium secondary battery and a lithium secondary battery manufactured using the same.
최근 휴대전화, 노트북 컴퓨터, 전기 자동차 등 전지를 사용하는 전자기구의 급속한 보급에 수반하여 소형 경량이면서도 상대적으로 고 용량인 2차 전지의 수요가 급속히 증대되고 있다. 특히, 리튬 2차 전지는 경량이고 고 에너지 밀도를 가지고 있어 휴대 기기의 구동 전원으로서 각광을 받고 있다. 이에 따라, 리튬 2차 전지의 성능 향상을 위한 연구 개발 노력이 활발하게 진행되고 있다.Recently, with the rapid spread of electronic devices using batteries such as mobile phones, notebook computers, and electric vehicles, the demand for small, lightweight, and relatively high capacity secondary batteries is rapidly increasing. In particular, lithium secondary batteries have attracted attention as a driving power source for portable devices due to their light weight and high energy density. Accordingly, research and development efforts for improving the performance of lithium secondary batteries have been actively conducted.
리튬 2차 전지는 리튬 이온의 삽입(intercalations) 및 탈리(deintercalation)가 가능한 활물질로 이루어진 음극과 양극 사이에 유기 전해액 또는 폴리머 전해액을 충전시킨 상태에서 리튬 이온이 양극 및 음극에서 삽입/탈리 될 때의 산화, 환원 반응에 의해 전기 에너지를 생산한다.Lithium secondary batteries are used when lithium ions are inserted / desorbed from the positive electrode and the negative electrode in a state in which an organic or polymer electrolyte is charged between a negative electrode and a positive electrode made of an active material capable of intercalations and deintercalation of lithium ions. Produces electrical energy by oxidation and reduction reactions.
리튬 2차 전지의 양극 활물질로는 리튬 코발트 옥사이드(LiCoO2), 리튬 니켈 옥사이드(LiNiO2), 리튬 망간 옥사이드(LiMnO2) 등과 같은 전이금속 화합물이 주로 사용된다. As a cathode active material of a lithium secondary battery, transition metal compounds such as lithium cobalt oxide (LiCoO 2 ), lithium nickel oxide (LiNiO 2 ), lithium manganese oxide (LiMnO 2 ), and the like are mainly used.
그리고 음극 활물질로는 일반적으로 연화 정도가 큰 천연흑연이나 인조흑연과 같은 결정질계 탄소재료, 또는 1000 ~ 1500℃의 낮은 온도에서 탄화수소나 고분자 등을 탄화시켜 얻은 수도-그라파이트(pseudo-graphite) 구조 또는 터보스트래틱 구조를 가지는 비정질계(low crystalline) 탄소재료 등이 사용된다.In general, the negative electrode active material is a crystalline carbon material such as natural graphite or artificial graphite having a high degree of softening, or a pseudo-graphite structure obtained by carbonizing hydrocarbons or polymers at a low temperature of 1000 to 1500 ° C, or Low crystalline carbon materials and the like having a turbostatic structure are used.
상기 음극 활물질로 음극을 제조하기 위해서는 음극 활물질 입자 사이 및 금속으로 이루어진 음극 집전체와의 접착력을 확보하기 위해 바인더를 사용하게 된다. 그런데 바인더를 과량으로 사용하게 되면 음극 활물질 입자를 덮어 전지의 방전 특성이 저하되고, 소량으로 사용하게 되면 집전체와의 접착력이 저하되는 문제점이 있다. 또한 음극 활물질 및 바인더의 균일한 혼합을 위해서는 통상적으로 유기 용매가 사용되는데, 이러한 유기 용매는 환경 오염의 원인이 될 수 있다.In order to prepare a negative electrode with the negative electrode active material, a binder is used to secure adhesion between the negative electrode active material particles and the negative electrode current collector made of a metal. However, when the binder is used in an excessive amount, the discharge characteristics of the battery may be reduced by covering the negative electrode active material particles, and when used in a small amount, the adhesive strength with the current collector may be reduced. In addition, in order to uniformly mix the negative electrode active material and the binder, an organic solvent is commonly used, which may cause environmental pollution.
이러한 문제를 해결하기 위하여, 한국공개 제2004-110665호는 셀룰로오스계 분산제 및 수용성 음이온계 다전해물(poly electrolyte)를 함유하는 음극 활물질용 조성물을 개시하고 있다. 그러나, 한국공개 제2004-110665호에 기재된 음극 활물질용 조성물도 여전히 바인더가 균일하게 분산되지 못해 바인더의 일부가 음극 활물질 표면을 덮게 되어, 종래의 문제점을 충분히 해결치 못하고 있다.In order to solve this problem, Korean Laid-Open Patent Publication No. 2004-110665 discloses a composition for a negative electrode active material containing a cellulose dispersant and a water-soluble anionic poly electrolyte. However, the composition for the negative electrode active material described in Korean Patent Laid-Open Publication No. 2004-110665 still fails to uniformly disperse the binder so that a part of the binder covers the surface of the negative electrode active material, which does not sufficiently solve the conventional problem.
이에 본 발명이 해결하고자 하는 과제는, 바인더의 균일한 분산이 가능하고 접착력이 우수한 리튬 이차전지의 음극 형성용 조성물의 제조방법을 제공하는 것이다.The problem to be solved by the present invention is to provide a method for producing a composition for forming a negative electrode of a lithium secondary battery capable of uniform dispersion of the binder and excellent adhesion.
또한, 본 발명은 상기 리튬 이차전지의 음극 형성용 조성물을 사용하여 전지 특성이 향상된 리튬 이차전지를 제공하는데 있다.The present invention also provides a lithium secondary battery having improved battery characteristics by using the composition for forming a negative electrode of the lithium secondary battery.
상기 과제를 해결하기 위하여, 본 발명의 리튬 이차전지의 음극 형성용 조성물의 제조방법은, (S1) 음극 활물질과 셀룰로오스계 분산제를 혼합하는 단계; (S2) 상기 혼합물에 물을 첨가하고 혼합하여 슬러리를 제조하는 단계; 및 (S3) 상기 슬러리에 바인더를 첨가하고 혼합하는 단계;를 포함한다. 본 발명의 제조방법에 따르면, 바인더가 혼합되기 전에 음극 활물질과 분산제를 먼저 균일하게 혼합한다. 분산제가 음극 활물질과 먼저 혼합됨으로써 나중에 혼합되는 바인더가 음극 활물질 형성용 조성물 내에서 균일하게 존재하는 것을 돕게 되므로, 전극 성능의 일관성을 확보할 수 있다. 또한, 분산제가 음극 활물질과 균일하게 혼합된 상태에서 바인더가 첨가되므로, 바인더의 균일한 혼합이 용이하여 음극 형성용 조성물의 제조시간도 현저하게 단축할 수 있다.In order to solve the above problems, the method for producing a composition for forming a negative electrode of a lithium secondary battery of the present invention, (S1) mixing a negative electrode active material and a cellulose-based dispersant; (S2) adding water and mixing the mixture to prepare a slurry; And (S3) adding and mixing a binder to the slurry. According to the production method of the present invention, the negative electrode active material and the dispersant are uniformly mixed first before the binder is mixed. Since the dispersant is first mixed with the negative electrode active material, the binder to be mixed later helps uniformly exist in the composition for forming the negative electrode active material, thereby ensuring consistency of electrode performance. In addition, since the binder is added in a state in which the dispersant is uniformly mixed with the negative electrode active material, uniform mixing of the binder is easy and the production time of the composition for forming a negative electrode can be significantly shortened.
본 발명의 제조방법에 따른 셀룰로오스계 분산제는 카르복시메틸셀룰로오스, 카르복시에틸셀룰로오스, 아미노에틸셀룰로오스, 옥시에틸셀룰로오스, 이들의 Na염 또는 NH4염 등을 각각 단독으로 또는 2종 이상 혼합하여 사용할 수 있으며, 그 함량은 상기 음극 활물질 100 중량부에 대하여 0.1 내지 5 중량부인 것이 바람직하다.Cellulose-based dispersant according to the production method of the present invention may be used alone or in combination of two or more of carboxymethyl cellulose, carboxyethyl cellulose, aminoethyl cellulose, oxyethyl cellulose, Na salt or NH 4 salt thereof, and the like, The content is preferably 0.1 to 5 parts by weight based on 100 parts by weight of the negative electrode active material.
본 발명의 제조방법에 있어서, 상기 (S2) 단계에서 수용성 음이온계 다전해물(poly electrolyte)을 슬러리에 더 첨가할 수 있으며, 상기 수용성 음이온계 다전해물로는 폴리아크릴계 전도성 고분자, 폴리아닐린계 전도성 고분자, 폴리아미드계 전도성 고분자, 시트르산 및 글루콘산 등을 각각 단독으로 또는 2종 이상 혼합하여 사용할 수 있으며, 그 함량은 상기 음극 활물질 100 중량부에 대하여 0.1 내지 2 중량부인 것이 바람직하다.In the production method of the present invention, in the step (S2), the water-soluble anionic polyelectrolyte may be further added to the slurry. The water-soluble anionic polyelectrolyte may be a polyacrylic conductive polymer, a polyaniline-based conductive polymer, The polyamide-based conductive polymer, citric acid and gluconic acid may be used alone or in combination of two or more thereof, and the content thereof is preferably 0.1 to 2 parts by weight based on 100 parts by weight of the negative electrode active material.
본 발명의 제조방법에 따른 바인더는 스티렌 부타디엔 러버, 니트릴 부타디엔 러버, 메틸아크릴레이트 부타디엔 러버 등을 각각 단독으로 또는 2종 이상 혼합하여 사용할 수 있으며, 그 함량은 상기 음극 활물질 100 중량부에 대하여 0.1 내지 5 중량부인 것이 바람직하다.The binder according to the manufacturing method of the present invention may be used alone or in combination of two or more of styrene butadiene rubber, nitrile butadiene rubber, methyl acrylate butadiene rubber, the content of which is 0.1 to 100 parts by weight of the negative electrode active material It is preferable that it is 5 weight part.
전술한 본 발명의 제조방법에 따라 제조된 음극 형성용 조성물이 음극 집전체 상에 코팅되어 형성된 리튬 이차전지용 음극은 리튬 이차전지에 사용될 수 있다.The negative electrode for a lithium secondary battery formed by coating the negative electrode composition prepared according to the above-described manufacturing method of the present invention on a negative electrode current collector may be used in a lithium secondary battery.
본 발명의 음극 형성용 조성물의 제조방법은 종래보다 신속하게 음극 형성용 조성물을 제조할 수 있을 뿐만 아니라 분산제의 균일한 혼합을 가능하게 하여 음극 활물질을 완전히 덮는 분산제의 양을 최소화하여, 제조되는 전극 및 전지의 성능을 향상시킬 수 있으며 활물질층의 접착력을 향상시킬 수 있다.The method for preparing a composition for forming a negative electrode of the present invention can not only prepare a composition for forming a negative electrode more quickly than before, but also enables uniform mixing of the dispersing agent to minimize the amount of the dispersant completely covering the negative electrode active material, thereby preparing the electrode. And the performance of the battery can be improved and the adhesion of the active material layer can be improved.
또한, 본 발명의 음극 형성용 조성물의 제조방법은 선택적으로 수용성 음이온계 다전해물을 사용함으로써 바인더의 접착력을 높이고 전극의 전도도를 더 향상시킬 수 있다.In addition, the method for preparing a composition for forming a negative electrode of the present invention can increase the adhesive strength of the binder and further improve the conductivity of the electrode by selectively using a water-soluble anionic polyelectrolyte.
또한, 본 발명의 음극 형성용 조성물의 제조방법은 유기 용매를 사용하지 않기 때문에 친환경적이다.In addition, the method for producing a composition for forming a cathode of the present invention is environmentally friendly because it does not use an organic solvent.
이하, 본 발명의 리튬 이차전지의 음극 형성용 조성물의 제조방법을 상세히 설명하기로 한다. 본 명세서 및 청구범위에 사용된 용어나 단어는 통상적이거나 사전적인 의미로 한정해서 해석되어서는 아니 되며, 발명자는 그 자신의 발명을 가장 최선의 방법으로 설명하기 위해 용어의 개념을 적절하게 정의할 수 있다는 원칙에 입각하여 본 발명의 기술적 사상에 부합하는 의미와 개념으로 해석되어야만 한다.Hereinafter, a method of manufacturing a composition for forming a negative electrode of a lithium secondary battery of the present invention will be described in detail. The terms or words used in this specification and claims are not to be construed as limiting in their usual or dictionary meanings, and the inventors may appropriately define the concept of terms in order to best explain their invention in the best way possible. It should be interpreted as meaning and concept corresponding to the technical idea of the present invention based on the principle that the present invention.
먼저, 음극 활물질과 셀룰로오스계 분산제를 혼합한다(S1).First, the negative electrode active material and the cellulose dispersant are mixed (S1).
본 발명에서 사용할 수 있는 음극 활물질은 당분야에서 음극 활물질로 통상적으로 사용되는 재료이면 특별한 제한 없이 사용이 가능하다. 예를 들면, 구상의 고결정성 천연흑연; 타원형상, 파쇄상, 비늘상 또는 휘스커상인 천연흑연; 인조흑연; 메소카본마이크로 비즈; 메소페이즈 피치; 등방성 피치; 수지탄; 및 수도-그라파이트(pseudo-graphite) 구조 또는 터보스트래틱 구조를 갖는 비정질계 탄소 등을 각각 단독으로 또는 2종 이상 혼합하여 사용할 수 있으나,이에 한정되는 것은 아니다. 또한 상기 음극 활물질은 피복층을 구비할 수 있으며, 피복층에 주로 사용되는 재료는 저결정성의 피치, 전도성 고분자, 유기 용매 등을 혼합하여 형성될 수 있지 만 이에 한정되는 것은 아니다.The negative electrode active material that can be used in the present invention can be used without particular limitation as long as it is a material commonly used as a negative electrode active material in the art. For example, spherical highly crystalline natural graphite; Natural graphite that is oval, crushed, scaled or whiskered; Artificial graphite; Mesocarbon micro beads; Mesophase pitch; Isotropic pitch; Resin coal; And amorphous carbon having a pseudo-graphite (pseudo-graphite) structure or a turbostratic structure may be used alone or in combination of two or more, respectively, but is not limited thereto. In addition, the negative electrode active material may include a coating layer, and a material mainly used for the coating layer may be formed by mixing a low crystalline pitch, a conductive polymer, an organic solvent, and the like, but is not limited thereto.
본 발명에 따른 셀룰로오스계 분산제로는 카르복시메틸셀룰로오스, 카르복시에틸셀룰로오스, 아미노에틸셀룰로오스, 옥시에틸셀룰로오스, 이들의 Na염 또는 NH4염 등을 각각 단독으로 또는 2종 이상 혼합하여 사용할 수 있다.As the cellulose dispersant according to the present invention, carboxymethyl cellulose, carboxyethyl cellulose, aminoethyl cellulose, oxyethyl cellulose, Na salts or NH 4 salts thereof, etc. may be used alone or in combination of two or more thereof.
상기 셀룰로오스계 분산제의 함량은 상기 음극 활물질 100 중량부에 대하여 0.1 내지 5 중량부인 것이 바람직하다. 상기 함량이 0.1 중량부 미만이면 코팅 효과가 미미하여 성능 발현이 충분치 않고, 5 중량부 초과이면 활물질 표면을 과다하게 덮게 되어 전지의 성능이 저하될 수 있다.The content of the cellulose-based dispersant is preferably 0.1 to 5 parts by weight based on 100 parts by weight of the negative electrode active material. If the content is less than 0.1 parts by weight, the coating effect is insignificant, and the performance is not sufficient. If the content is more than 5 parts by weight, the surface of the active material may be excessively covered, thereby degrading the performance of the battery.
다음으로, 음극 활물질과 셀룰로오스계 분산제의 혼합물에 물을 첨가하고 혼합하여 슬러리를 제조한다(S2).Next, water is added to the mixture of the negative electrode active material and the cellulose dispersant and mixed to prepare a slurry (S2).
본 발명의 리튬 이차전지의 음극 형성용 조성물의 제조방법은 유기 용매를 사용하지 않으므로 친환경적이다. 사용될 수 있는 물은 증류수, 초순수(D.I water) 등이 바람직하다.Since the method for preparing a composition for forming a negative electrode of the lithium secondary battery of the present invention does not use an organic solvent, it is environmentally friendly. The water that can be used is preferably distilled water, ultrapure water (D.I water) and the like.
선택적으로, 본 공정에서 수용성 음이온계 다전해물(poly eletrolyte)을 슬러리에 더 첨가할 수 있다. 수용성 음이온계 다전해물은 바인더의 접착력 및 전극의 전기전도도를 더욱 향상 시킬 수 있다.Optionally, water soluble anionic polyelectrolytes may be further added to the slurry in this process. The water-soluble anionic polyelectrolyte can further improve the adhesion of the binder and the electrical conductivity of the electrode.
본 발명에 따른 수용성 음이온계 다전해물(poly eletrolyte)로는 폴리아크릴계 전도성 고분자, 폴리아닐린계 전도성 고분자, 폴리아미드계 전도성 고분자 등의 전도성 고분자; 시트르산, 글루콘산 등의 약산(mild acid) 등을 각각 단독으로 또는 2종 이상 혼합하여 사용할 수 있다.The water-soluble anionic polyelectrolyte according to the present invention includes a conductive polymer such as a polyacrylic conductive polymer, a polyaniline conductive polymer, and a polyamide conductive polymer; Mild acid, such as citric acid and gluconic acid, etc. can be used individually or in mixture of 2 or more types, respectively.
상기 수용성 음이온계 다전해물의 함량은 상기 탄소계 음극 활물질 100 중량부에 대하여 0.1 내지 2 중량부인 것이 바람직한데, 그 함량이 0.1 중량부 미만이면 다전해물 첨가로 기대되는 개선효과의 발현이 미미하고, 2 중량부 초과이면 전지 성능이 저하될 수 있다.The content of the water-soluble anionic polyelectrolyte is preferably 0.1 to 2 parts by weight with respect to 100 parts by weight of the carbon-based negative electrode active material. If the content is less than 0.1 part by weight, the improvement effect expected by addition of the polyelectrolyte is insignificant. If it is more than 2 parts by weight, battery performance may decrease.
다음으로, 상기 슬러리에 바인더를 첨가하고 혼합한다(S3).Next, a binder is added to the slurry and mixed (S3).
본 발명에 따른 바인더는 합성고무계 바인더가 바람직하며, 구체적인 예를 들면 스티렌 부타디엔 러버, 니트릴 부타디엔 러버, 메틸아크릴레이트 부타디엔 러버 등을 각각 단독으로 또는 2종 이상 혼합하여 사용할 수 있으며, 바람직하게는 의 스티렌 부타디엔계 합성 고무를 사용할 수 있다.The binder according to the present invention is preferably a synthetic rubber binder, and specific examples thereof may include styrene butadiene rubber, nitrile butadiene rubber, methyl acrylate butadiene rubber, or the like, respectively, or a mixture of two or more kinds thereof. Butadiene-based synthetic rubber can be used.
상기 바인더의 함량은 상기 탄소계 음극 활물질 100 중량부에 대하여 0.1 내지 5 중량부인 것이 바람직하다. 그 함량이 0.1 중량부 미만이면 접착력이 저하되어 집전체와 활물질 간의 접착 신뢰성이 저하되고, 5 중량부 초과이면 입자간의 전기 전도도를 저하시켜 전지 성능이 저하될 수 있다.The content of the binder is preferably 0.1 to 5 parts by weight based on 100 parts by weight of the carbon-based negative electrode active material. If the content is less than 0.1 parts by weight, the adhesive force is lowered, thereby reducing the adhesion reliability between the current collector and the active material. If the content is more than 5 parts by weight, the electrical conductivity between the particles may be lowered, thereby degrading battery performance.
전술한 제조방법으로 제조된 리튬 이차전지의 음극 형성용 조성물은 음극 집전체에 소정의 두께로 코팅되어 리튬 이차전지의 음극을 형성할 수 있다. 또한, 본 발명에 따른 음극은, 소정 두께로 양극 집전체에 코팅되어 제조된 양극을 세퍼레이터를 사이에 두고 대향시킨 후 세퍼레이터에 리튬 이차전지용 전해액을 함침시키면 반복적인 충방전이 가능한 리튬 이차전지의 제조에 적용 가능하다. 이러한 리튬 이차전지 제조 방법은 본 발명이 속한 기술분야에서 통상의 지식을 가진 자에게 널리 알려져 있으므로 상세한 설명은 생략하기로 한다. The composition for forming a negative electrode of the lithium secondary battery manufactured by the above-described manufacturing method may be coated on a negative electrode current collector to a predetermined thickness to form a negative electrode of the lithium secondary battery. In addition, the negative electrode according to the present invention, the positive electrode is coated on the positive electrode current collector to a predetermined thickness to face the separator with a separator therebetween to impregnate the lithium secondary battery electrolyte in the separator to produce a rechargeable secondary battery that can be repeatedly charged and discharged Applicable to Since such a lithium secondary battery manufacturing method is well known to those skilled in the art to which the present invention pertains, a detailed description thereof will be omitted.
이하, 본 발명을 구체적으로 설명하기 위해 실시예를 들어 상세하게 설명하기로 한다. 그러나, 본 발명에 따른 실시예는 여러 가지 다른 형태로 변형될 수 있으며, 본 발명의 범위가 아래에서 상술하는 실시예에 한정되는 것으로 해석되어서는 안 된다. 본 발명의 실시예는 당업계에서 평균적인 지식을 가진 자에게 본 발명을 보다 완전하게 설명하기 위해서 제공되는 것이다.Hereinafter, the present invention will be described in detail with reference to Examples. However, the embodiments according to the present invention can be modified into various other forms, and the scope of the present invention should not be construed as being limited to the embodiments described below. The embodiments of the present invention are provided to more completely explain the present invention to those skilled in the art.
실시예 1Example 1
비정질 탄소로 피복된 구상의 천연흑연 분말 100중량부에 카르복시메틸셀룰로오스 파우더(CMC 2200: Carboxyl-Methyl Cellulose, 日,Daicel社) 1 중량부를 첨가한 후에 Nauta Mixer를 55Hz의 속도로 60분 동안 교반하였다. 사용된 CMC2200입자는 평균입경이 약 5 ㎛ 이하이다. 상기 혼합물 30g을 증류수 30ml에 넣고 교반기를 사용하여 750 rpm의 속도로 1 시간동안 교반하였다. 교반이 완료된 후, 상기 흑연분말 100 중량부 대비 스티렌 부타디엔 러버(SBR: Styrene Butadiene Rubber, 日, Zeon社) 1 중량부를 첨가하고 750rpm의 속도로 15분간 교반 후, 구리 호일 위에 균일한 두께로 도포하여 전극을 제조하였다.To 100 parts by weight of spherical natural graphite powder coated with amorphous carbon, 1 part by weight of carboxymethyl cellulose powder (CMC 2200: Carboxyl-Methyl Cellulose, Japan, Daicel) was added and the Nauta Mixer was stirred at a speed of 55 Hz for 60 minutes. . The CMC2200 particles used had an average particle diameter of about 5 μm or less. 30 g of the mixture was added to 30 ml of distilled water, and stirred at a speed of 750 rpm for 1 hour using a stirrer. After stirring was completed, 1 part by weight of styrene butadiene rubber (SBR: Styrene Butadiene Rubber, Japan, Zeon, Inc.) was added to 100 parts by weight of the graphite powder, stirred at a speed of 750 rpm for 15 minutes, and then coated on a copper foil with a uniform thickness. An electrode was prepared.
실시예 2Example 2
실시예1에서 증류수에 PANI(폴리아닐린, Aldrich社) 0.3 g을 첨가한 것을 제외하고는, 실시예1과 동일한 방법으로 전극을 제조하였다.An electrode was manufactured in the same manner as in Example 1, except that 0.3 g of PANI (polyaniline, Aldrich) was added to distilled water in Example 1.
비교예 1Comparative Example 1
비정질 탄소로 피복된 구상의 천연흑연 분말 30g을 증류수 30ml에 넣고, 상기 탄소재 음극 활물질 100 중량부 대비 CMC2200 1 중량부 및 SBR 1 중량부를 첨가한 후, 교반기를 사용하여 750 rpm의 속도로 1 시간 동안 교반하고, 구리 호일 위에 균일한 두께로 도포하여 전극을 제조하였다.30 g of spherical natural graphite powder coated with amorphous carbon was added to 30 ml of distilled water, 1 part by weight of CMC2200 and 1 part by weight of SBR were added to 100 parts by weight of the carbonaceous anode active material, and then agitated at a speed of 750 rpm using a stirrer for 1 hour. Was stirred and applied to a uniform thickness on a copper foil to prepare an electrode.
실험예Experimental Example
상기 실시예 및 비교예에 대해 다음과 같은 시험을 실시하여 특성을 평가하였다. 그 평가결과는 하기 표 1과 같다.The following test was performed about the said Example and the comparative example, and the characteristic was evaluated. The evaluation results are shown in Table 1 below.
(1) 접착력 평가(1) Adhesion Evaluation
180°Peel test로 수행하였다. 실시예 및 비교예에 따라 제조된 음극 극판을 100 mm X 15 mm의 길이로 자른 후, 300mm/min의 속도로 50mm 구간 사이의 슬러리를 벗겨내는 동안의 힘을 측정하여 평균값을 구하였다.180 ° Peel test was performed. The negative electrode plates prepared according to Examples and Comparative Examples were cut to a length of 100 mm X 15 mm, and the average value was determined by measuring the force during stripping of the slurry between 50 mm sections at a speed of 300 mm / min.
(2) 전지 특성(2) battery characteristics
상기 실시예 및 비교예에 따라 제조된 음극과, 양극 활물질로 LiCoO2을 사용하여 제조된 양극, 세퍼레이터로 Celgard 2400, 및 비수 전해액으로 EC:DEC=3:7로 혼합한 1M LiPF6를 사용하여 코인형 전지(coin cell)를 제조하였다.Using a negative electrode prepared according to the above Examples and Comparative Examples, a positive electrode prepared using LiCoO 2 as a positive electrode active material, Celgard 2400 as a separator, and EC: DEC = 3: 7 as a nonaqueous electrolyte using 1M LiPF 6 Coin-type cells were prepared.
충방전 시험은 전위를 0.01~1.5V의 범위로 규제하여, 충전 전류 0.5mA/㎠로 0.01V 될 때까지 충전하고, 또한 0.01V의 전압을 유지하며, 충전전류가 0.02mA/㎠ 될 때까지 충전을 계속하였다. 그리고 방전전류는 0.5mA/㎠로 1.5V까지의 방전을 행하였다. 표 1에서 사이클 효율은 충전한 전기용량에 대한 방전한 전기용량의 비율을 나타낸다.The charge / discharge test regulates the potential in the range of 0.01 to 1.5V, charges until it becomes 0.01V at a charging current of 0.5mA / cm 2, maintains a voltage of 0.01V, and charges until 0.02mA / cm 2. Charging continued. The discharge current was discharged up to 1.5 V at 0.5 mA / cm 2. In Table 1, the cycle efficiency represents the ratio of discharged capacitance to charged capacitance.
상기 표 1에 나타난 바와 같이, 본원발명에 따른 실시예1 내지 실시예2에 따른 음극의 접착력은 비교예보다 상당히 우수함을 알 수 있다. 또한 전반적인 전지특성도 비교예의 전지보다 우수함을 알 수 있다.As shown in Table 1, it can be seen that the adhesion of the negative electrode according to Examples 1 to 2 according to the present invention is significantly superior to the comparative example. In addition, it can be seen that the overall battery characteristics are also superior to the battery of the comparative example.
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