KR101036106B1 - Electrode active material composition for lithium secondary battery - Google Patents
Electrode active material composition for lithium secondary battery Download PDFInfo
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Abstract
본 발명은 리튬 이차 전지용 전극 활물질 조성물에 관한 것으로서, 보다 상세하게는 자체적으로 색깔이 변하여 가해준 압력과 인장력에 대해 반응하는 발광 고분자 블렌드를 포함하는 전극 활물질 조성물에 관한 것이다. 본 발명에 따른 리튬 이차 전지용 전극 활물질 조성물은 압연에 의한 극판 변형에 의해 유발되는 형광색 변화를 통해 압연 공정에서 두께 편차가 있는 극판을 육안으로 용이하게 검출할 수 있고, 이에 따라 균일한 두께를 갖는 극판을 제조할 수 있다.
The present invention relates to an electrode active material composition for a lithium secondary battery, and more particularly, to an electrode active material composition including a light emitting polymer blend which reacts to a pressure and a tensile force applied by changing color itself. The electrode active material composition for a lithium secondary battery according to the present invention can easily detect a pole plate having a thickness variation in the rolling process with the naked eye through the fluorescent color change caused by the pole plate deformation by rolling, and thus a pole plate having a uniform thickness. Can be prepared.
리튬전지, 활물질, 발광 고분자, 광발광성 색소, 형광Lithium battery, active material, light emitting polymer, photoluminescent dye, fluorescence
Description
본 발명은 리튬 이차 전지용 전극 활물질 조성물에 관한 것으로서, 보다 상세하게는 자체적으로 색깔이 변하여 가해준 압력과 인장력에 대해 반응하는 발광 고분자 블렌드(Light-Emitting Polymer Blend)를 포함함으로써, 극판의 두께 불량 여부를 육안으로 용이하게 확인할 수 있으며, 균일한 두께를 갖는 극판을 제공할 수 있는 전극 활물질 조성물에 관한 것이다.The present invention relates to an electrode active material composition for a lithium secondary battery, and more particularly, by including a light-emitting polymer blend (Light-Emitting Polymer Blend) that reacts to pressure and tensile force applied by changing its own color, whether the thickness of the electrode plate is poor. It can be easily confirmed with the naked eye, and relates to an electrode active material composition that can provide an electrode plate having a uniform thickness.
최근, 전자기기 특히 휴대용 전자기기의 발달과 더불어, 이러한 전자기기의 구동전원으로 사용되는 이차 전지도 눈부시게 발전하고 있다. 그 중에서도 리튬 이차 전지는 높은 작동 전압, 장수명, 고에너지 밀도 등과 같은 우수한 특성으로 인하여 가장 주목받고 있는 전지 중의 하나이다.In recent years, with the development of electronic devices, in particular, portable electronic devices, secondary batteries used as driving power sources for such electronic devices have also been remarkably developed. Among them, the lithium secondary battery is one of the most attentiond batteries due to its excellent characteristics such as high operating voltage, long life, high energy density and the like.
리튬 이차 전지는 가역적으로 리튬 이온의 삽입과 탈리가 가능한 물질을 양극 및 음극으로 사용하고, 상기 양극과 음극 사이에 유기 전해액 또는 폴리머 전해액을 충전시켜 제조하며, 리튬 이온이 양극 및 음극에서 삽입/탈리될 때의 산화, 환원 반응에 의하여 전기 에너지를 생성한다. Lithium secondary batteries are prepared by reversibly inserting and desorbing lithium ions as positive and negative electrodes, and filling organic electrolyte or polymer electrolyte between the positive and negative electrodes, and lithium ions are inserted and removed from the positive and negative electrodes. When produced, electrical energy is generated by oxidation and reduction reactions.
리튬 이차 전지의 양극 활물질로는 LiCoO2, LiMn2O4, LiNiO2, LiMnO2 등과 같은 리튬 함유 금속 산화물을 사용하고 있으며, 음극 활물질로는 리튬 금속이나 그 합금, 탄소 재료 등이 사용되고 있다.Lithium-containing metal oxides such as LiCoO 2 , LiMn 2 O 4 , LiNiO 2 , LiMnO 2, and the like are used as positive electrode active materials of lithium secondary batteries, and lithium metal, alloys thereof, and carbon materials are used as negative electrode active materials.
이들 활물질은 도전제 및 바인더와 혼합하여 전극 활물질 조성물을 제조한 다음, 이를 집전체 상에 코팅한 후 압연 공정을 실시한다. 압연 공정이란 리튬 이차전지의 극판 제조시 코팅 공정이 끝난 극판에 대해 활물질의 용량 밀도를 높이고 부수적으로 기재와 활물질간의 접착성을 높이는 효과를 얻기 위해 140℃ 온도의 예열과정을 거쳐 120℃ 온도로 가열된 2개의 롤 사이를 통과시켜 극판을 원하는 두께로 압축하는 공정이다.These active materials are mixed with a conductive agent and a binder to prepare an electrode active material composition, and then coated on the current collector and then subjected to a rolling process. The rolling process is heated to 120 ° C through a preheating process of 140 ° C in order to obtain an effect of increasing the capacity density of the active material and additionally improving the adhesiveness between the substrate and the active material on the coated electrode plate during the production of the electrode plate of the lithium secondary battery. It is a process of compressing an electrode plate to desired thickness by passing between two rolls.
그런데 압연 공정에서 활물질이 균일하게 압연되지 못하면 극판의 두께 편차로 인해 극판에 주름이 발생하고, 활물질의 박리 및 충전 후 극판 스웰링 등의 문제점이 발생한다.However, when the active material is not uniformly rolled in the rolling process, wrinkles occur in the electrode plate due to the thickness variation of the electrode plate, and problems such as electrode plate swelling after peeling and filling of the active material occur.
따라서 본 발명은 상술한 문제점을 해결하기 위한 것으로서, 자체적으로 색깔이 변하여 가해준 압력과 인장력에 대해 반응하는 발광 고분자 블렌드를 포함함으로써, 압연 공정에서 두께 편차가 있는 극판을 육안으로 용이하게 검출할 수 있고, 이에 따라 균일한 두께를 갖는 극판을 제공할 수 있는 리튬 이차 전지용 전극 활물질 조성물을 제공하는데 그 목적이 있다.Therefore, the present invention is to solve the above-mentioned problems, by including a light-emitting polymer blend that reacts to the pressure and the tensile force applied by changing the color itself, it is easy to visually detect the electrode plate with a thickness deviation in the rolling process In view of this, an object of the present invention is to provide an electrode active material composition for a lithium secondary battery that can provide an electrode plate having a uniform thickness.
상기 목적을 달성하기 위하여, 본 발명은,In order to achieve the above object,
활물질, 바인더; 및Active material, binder; And
고분자 매트릭스(matrix)에 광발광성 색소가 블렌드된 발광 고분자 블렌드를 포함하는 것을 특징을 하는 리튬 이차 전지용 전극 활물질 조성물을 제공한다.Provided is an electrode active material composition for a lithium secondary battery, comprising a light emitting polymer blend blended with a photoluminescent pigment in a polymer matrix.
이하 본 발명을 더욱 상세하게 설명한다.Hereinafter, the present invention will be described in more detail.
본 발명의 리튬 이차 전지용 전극 활물질은 자체적으로 색깔이 변하여 가해준 압력과 인장력에 대해 반응하는 발광 고분자 블렌드(Light-Emitting Polymer Blend)를 포함한다. 상기 발광 고분자 블렌드는 고분자 매트릭스에 광발광성(photoluminescent) 색소를 혼합하여 제조되는데, 상기 고분자 매트릭스 및 광발광성 색소의 블렌드는 다양한 표준 기술, 예를 들면 용융 블렌딩(melting-blending), 용액에서 폴리머로 색소를 확산하는 방법, 또는 색소 존재 하에 폴리머를 생성하는 방법 등을 이용하여 제조될 수 있다.The electrode active material for a lithium secondary battery of the present invention includes a light-emitting polymer blend that reacts to pressure and tensile force applied by changing its color itself. The luminescent polymer blend is prepared by mixing a photoluminescent pigment in a polymer matrix, wherein the blend of the polymer matrix and the photoluminescent pigment is pigmented into a polymer in a variety of standard techniques, for example melt-blending, solution It can be prepared using a method for diffusing, or a method for producing a polymer in the presence of a pigment.
상기 광발광성 색소는 내부 센서 역할을 하는데, 이들은 재료의 기계적 변형이 자체의 형광(fluorescence) 변화, 예를 들면 적색에서 녹색으로의 변화를 통하여 감지될 수 있게 한다. UV 광이 조사되는 조건 하에서 이러한 효과는 육안으로도 쉽게 볼 수 있다.The photoluminescent pigment acts as an internal sensor, which allows the mechanical deformation of the material to be detected through its fluorescence change, for example from red to green. Under the condition that UV light is irradiated, this effect can be easily seen by the naked eye.
극판의 압연공정에서 극판에 압력이 가해지면 이러한 압력에 대해 반응하는 광발성 색소의 색깔 변화로 압연에 따른 극판 변형 여부를 확인할 수 있다.When pressure is applied to the electrode plate in the rolling process of the electrode plate, it is possible to check whether the electrode plate is deformed due to the rolling due to the color change of the photoluminescent dye reacting to the pressure.
고분자 매트릭스 속에서 시아노-올리고(파라-페닐렌 비닐렌)(cyano-oligo(p-phenylene vinylene)) 색소와 같은 발광성 색소 분자들의 작은 집합체(aggregate) 들의 상분리에 의해 색상이 변화된다. 광발성 고분자 블렌드의 상(phase) 거동은 이러한 색소들의 화학적 구조, 블렌드의 조성, 및 처리 조건들을 변화시킴으로써 제어된다.The color is changed by phase separation of small aggregates of luminescent pigment molecules such as cyano-oligo (p-phenylene vinylene) pigments in the polymer matrix. The phase behavior of the photoluminescent polymer blend is controlled by changing the chemical structure of these pigments, the composition of the blend, and the processing conditions.
용해되어 있으나 고립되어 있는 색소 분자들은 단량체 발광(monomer emission)을 하며, 이러한 분자들이 고분자 매트릭스와 같은 매체 속에서 집합체로 뭉쳐졌을 때에는 전혀 다른 형광색을 내는 엑시머 발광(excimer emission)을 하게 된다. 재료의 기계적 변형, 예를 들면 압연에 따른 극판변형은 색소 집합체를 깨뜨려서 색소 분자들의 분산과 용해를 초래하여 색깔의 변화를 형성한다.The dissolved but isolated pigment molecules emit monomers, and when these molecules are aggregated together in a medium such as a polymer matrix, they emit excimer emission that produces a completely different fluorescent color. Mechanical deformation of the material, for example electrode deformation due to rolling, breaks the pigment aggregates, resulting in dispersion and dissolution of the pigment molecules to form a change in color.
상기 고분자 매트릭스는 선형 저밀도 폴리에틸렌, 폴리프로필렌, 폴리아크릴레이트, 폴리비닐리덴플로라이드, 폴리비닐플로라이드, 폴리테트라플루오로에틸렌, 폴리클로로트리플루오로에틸렌, 폴리스티렌, 아크릴로니트릴-부타디엔-스티렌 공중합체, 에틸렌-비닐아세테이트 공중합체, 및 셀룰로오스 아세테이트로 이루어진 군에서 선택되는 하나 이상의 것을 사용할 수 있다.The polymer matrix is linear low density polyethylene, polypropylene, polyacrylate, polyvinylidene fluoride, polyvinyl fluoride, polytetrafluoroethylene, polychlorotrifluoroethylene, polystyrene, acrylonitrile-butadiene-styrene copolymer One or more selected from the group consisting of ethylene-vinylacetate copolymer, and cellulose acetate can be used.
상기 광발광성 색소는 시아노-올리고(파라-페닐렌 비닐리덴) 색소가 사용될 수 있으며, 바람직하게는 1,4-비스(알파-시아노-4-메톡시스티릴)-2,5-디메톡시벤젠[1,4-bis(α-cyano-4-methoxystyryl)-2,5-dimethoxybenzene: 이하 'BCMDB'라 함], 1,4-비스(알파-시아노-4-메톡시스티릴)벤젠[1,4-bis(α-cyano-4-methoxystyryl)-benzene: 이하 'BCMB'라 함], 또는 1,4-비스(알파-시아노-4-(2-에틸헥실록시스티릴)-2,5-디메톡시벤젠)[1,4-bis(α-cyano-4-(2-ethylhexyloxystyrl)-2,5-dimethoxybenzene: 이하 'BCEDB'라 함] 사용된다. 상기 광발광성 색소의 함량은 고 분자 매질 중량에 대하여 0.01 내지 3중량% 포함하는 것이 바람직하다.The photoluminescent dye may be a cyano-oligo (para-phenylene vinylidene) dye, preferably 1,4-bis (alpha-cyano-4-methoxystyryl) -2,5-dimeth Methoxybenzene [1,4-bis (α-cyano-4-methoxystyryl) -2,5-dimethoxybenzene: hereinafter referred to as 'BCMDB'], 1,4-bis (alpha-cyano-4-methoxystyryl) Benzene [1,4-bis (α-cyano-4-methoxystyryl) -benzene: hereinafter referred to as 'BCMB'], or 1,4-bis (alpha-cyano-4- (2-ethylhexyloxystyryl) ), 2,5-dimethoxybenzene) [1,4-bis (α-cyano-4- (2-ethylhexyloxystyrl) -2,5-dimethoxybenzene: hereafter referred to as 'BCEDB'] of the photoluminescent pigment The content is preferably 0.01 to 3% by weight based on the weight of the high molecular medium.
상기 BCMDB, BCMB, 및 BCEDB는 크노에베노겔 반응(Knoevenagel reaction)에 의해 합성될 수 있다. 상기 화학식 1에 나타낸 바와 같이, 상기 BCMB 및 BCMDB는 (4-메톡시페닐)아세토니트릴과 각각 테레프탈디카르복시알데히드 및 2,5-디메톡시테레프탈디카르복시알데히드의 반응에 의해 합성된다. 상기 BCEDB는 (4-(2-에틸헥실록시)페닐)아세토니트릴과 2,5-디메톡시테레프탈알데히드의 반응에 의해 합성될 수 있다.The BCMDB, BCMB, and BCEDB can be synthesized by Knoevenagel reaction. As shown in Formula 1, BCMB and BCMDB are synthesized by the reaction of (4-methoxyphenyl) acetonitrile with terephthaldicarboxyaldehyde and 2,5-dimethoxyterephthaldicarboxyaldehyde, respectively. The BCEDB can be synthesized by the reaction of (4- (2-ethylhexyloxy) phenyl) acetonitrile with 2,5-dimethoxyterephthalaldehyde.
BCMDB : R = OMe, BCMB: R = HBCMDB: R = OMe, BCMB: R = H
본 발명의 리튬 이차 전지용 전극 활물질 조성물에 있어서, 상기 발광 고분 자 블렌드의 함량은 전극 활물질 총 중량에 대하여 0.1 내지 10중량%인 것이 바람직하다. 첨가량이 0.1중량% 미만이면 첨가효과가 미미하고 10중량%를 초과하는 경우에는 전지의 수명특성이 저하되는 문제점이 있어 바람직하지 않다.In the electrode active material composition for lithium secondary battery of the present invention, the content of the light emitting polymer blend is preferably 0.1 to 10% by weight based on the total weight of the electrode active material. If the added amount is less than 0.1% by weight, the effect of addition is insignificant, and if it is more than 10% by weight, there is a problem that the life characteristics of the battery is lowered, which is not preferable.
본 발명의 전극 활물질 조성물에 있어서, 상기 활물질은 양극 활물질로서 LiCoO2, LiNiO2, LiMnO2, LiMn2O4, 및 LiNi1-x-y CoxMyO2로 이루어진 군에서 선택된 하나 이상의 리튬 금속 산화물 또는 리튬 금속 복합 산화물을 포함하는 것이 바람직하다. 여기서 M은 Mn, Co, Al, 또는 Mn 중 어느 하나이며, 0≤x≤1, 0≤y≤1, 0≤x+y≤1를 나타낸다.In the electrode active material composition of the present invention, the active material is at least one lithium metal oxide selected from the group consisting of LiCoO 2 , LiNiO 2 , LiMnO 2 , LiMn 2 O 4 , and LiNi 1-xy Co x M y O 2 Or a lithium metal composite oxide. M is either Mn, Co, Al, or Mn, and represents 0 ≦ x ≦ 1, 0 ≦ y ≦ 1, and 0 ≦ x + y ≦ 1.
또한 상기 활물질은 음극 활물질로서 결정질 탄소, 비정질 탄소, 탄소 복합체 및 리튬 금속으로 이루어진 군에서 선택되는 것을 사용할 수 있다.In addition, the active material may be used as the negative electrode active material selected from the group consisting of crystalline carbon, amorphous carbon, carbon composite and lithium metal.
본 발명의 전극 활물질 조성물에 있어서, 상기 바인더는 폴리비닐리덴플로라이드, 폴리테트라플로오로에틸렌, 스티렌-부타디엔 고무, 및 비닐리덴 플로라이드와 헥사플루오로프로필렌의 공중합체로 이루어진 군에서 선택되는 하나 이상의 것이 사용될 수 있다. 상기 바인더의 함량은 상기 활물질 총 중량에 대하여 1 내지 9중량%인 것이 바람직하다.In the electrode active material composition of the present invention, the binder is at least one selected from the group consisting of polyvinylidene fluoride, polytetrafluoroethylene, styrene-butadiene rubber, and copolymers of vinylidene fluoride and hexafluoropropylene. May be used. The content of the binder is preferably 1 to 9% by weight based on the total weight of the active material.
이하 본 발명의 바람직할 실시예 및 비교예를 기재한다. 그러나 하기 실시예는 본 발명의 바람직한 일 실시예일 뿐 본 발명이 하기 실시예에 한정되는 것은 아니다.Hereinafter, preferred examples and comparative examples of the present invention are described. However, the following examples are only preferred examples of the present invention, and the present invention is not limited to the following examples.
실시예 1Example 1
선형 저밀도 폴리에틸렌과 0.18중량%의 BCMDB를 180℃에서 약 10분간 혼합한 후 급랭하여 발광 고분자 블렌드를 제조하였다.Linear low density polyethylene and 0.18% by weight of BCMDB were mixed at 180 ° C. for about 10 minutes and then quenched to prepare a light emitting polymer blend.
양극 활물질인 LiCoO2, 바인더인 폴리비닐리덴 플로라이드(PVDF), 및 발광 고분자 블렌드인 선형 저밀도 폴리에틸렌/BCMDB의 블렌드를 96 : 2 : 2의 중량비로 N-메틸피롤리돈(NMP)에 첨가하여 양극 활물질 슬러리를 제조하였다. 상기 양극 활물질 슬러리를 알루미늄 호일 위에 도포하고 건조한 후 롤프레스로 압연하고 소정 치수로 절단하여 양극 극판을 제조하였다.
A blend of positive electrode active material LiCoO 2 , binder polyvinylidene fluoride (PVDF), and light emitting polymer blend, linear low density polyethylene / BCMDB, was added to N-methylpyrrolidone (NMP) at a weight ratio of 96: 2: 2. A positive electrode active material slurry was prepared. The positive electrode active material slurry was applied on an aluminum foil, dried, rolled with a roll press, and cut into predetermined dimensions to prepare a positive electrode plate.
실시예 2Example 2
음극 활물질인 결정성 흑연, 바인더인 PVDF, 및 발광 고분자 블렌드인 선형 저밀도 폴리에틸렌/BCMDB의 블렌드를 96 : 2 : 2의 중량비로 NMP에 첨가하여 음극 활물질 슬러리를 제조하였다. 상기 음극 활물질 슬러리를 구리 호일 상에 도포하고 건조한 후 압연하고 소정 치수로 절단하여 음극 극판을 제조하였다.
A negative active material slurry was prepared by adding a blend of crystalline graphite as a negative electrode active material, PVDF as a binder and linear low density polyethylene / BCMDB as a light emitting polymer blend to NMP in a weight ratio of 96: 2: 2. The negative electrode active material slurry was applied on a copper foil, dried, rolled, and cut into predetermined dimensions to prepare a negative electrode plate.
비교예 1Comparative Example 1
상기 실시예 1과 동일한 양극 활물질 슬러리를 알루미늄 호일 위에 도포하고 건조한 후 압연 공정을 진행하지 않고 양극 극판을 제조하였다.
The same positive electrode active material slurry as in Example 1 was applied on an aluminum foil, dried, and a positive electrode plate was manufactured without a rolling process.
비교예 2Comparative Example 2
상기 실시예 2와 동일한 음극 활물질 슬러리를 구리 호일 위에 도포하고 건조한 후 압연 공정을 진행하지 않고 음극 극판을 제조하였다.The same negative electrode active material slurry as in Example 2 was coated on a copper foil, dried, and a negative electrode plate was manufactured without a rolling process.
상기 실시예 1-2 및 비교예 1-2에 따라 제조된 양극 극판 및 음극 극판을 UV 램프 하에서 방출하는 색깔을 확인하여, 그 결과를 표 1에 나타내었다.
The color of the positive electrode plate and the negative electrode plate prepared according to Example 1-2 and Comparative Example 1-2 was confirmed under the UV lamp, and the results are shown in Table 1.
표 1을 참조하면, 실시예 1 및 실시예 2에 따라 제조된 양극 극판 및 음극 극판은 압연에 의해 발광 고분자 블렌드에 포함된 광발광성 색소 분자들이 분해되어 녹색에서 적색으로의 색상 변화를 일으켰다.Referring to Table 1, the positive electrode plate and the negative electrode plate prepared according to Examples 1 and 2 decomposed photoluminescent pigment molecules contained in the light emitting polymer blend by rolling, thereby causing a color change from green to red.
상술한 바와 같이, 본 발명의 발광 고분자 블렌드를 포함하는 리튬 이차 전지용 전극 활물질 조성물은 압연에 의한 극판 변형에 의해 유발되는 형광색 변화를 통해 압연 공정에서 두께 편차가 있는 극판을 육안으로 용이하게 검출할 수 있고, 이에 따라 균일한 두께를 갖는 극판을 제조할 수 있다. 또한 전지의 용량 특성이 균일한 리튬 이차 전지를 제공할 수 있다.As described above, the electrode active material composition for a lithium secondary battery including the light-emitting polymer blend of the present invention can easily detect the electrode plate having a thickness deviation in the rolling process through the fluorescent color change caused by the electrode plate deformation by rolling. Thus, an electrode plate having a uniform thickness can be produced. It is also possible to provide a lithium secondary battery having a uniform capacity characteristic of the battery.
본 발명에 대해 상기 실시예를 참고하여 설명하였으나, 이는 예시적인 것에 불과하며, 본 발명에 속하는 기술 분야의 통상의 지식을 가진 자라면 이로부터 다 양한 변형 및 균등한 타 실시예가 가능하다는 점을 이해할 것이다. 따라서 본 발명의 진정한 기술적 보호범위는 첨부된 특허청구범위의 기술적 사상에 의해 정해져야 할 것이다.Although the present invention has been described with reference to the above embodiments, it is merely exemplary, and it will be understood by those skilled in the art that various modifications and equivalent other embodiments are possible. will be. Therefore, the true technical protection scope of the present invention will be defined by the technical spirit of the appended claims.
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