KR20050034118A - Nonaqueous electrolyte for battery - Google Patents
Nonaqueous electrolyte for battery Download PDFInfo
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- KR20050034118A KR20050034118A KR1020030069941A KR20030069941A KR20050034118A KR 20050034118 A KR20050034118 A KR 20050034118A KR 1020030069941 A KR1020030069941 A KR 1020030069941A KR 20030069941 A KR20030069941 A KR 20030069941A KR 20050034118 A KR20050034118 A KR 20050034118A
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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
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
- H01M10/0567—Liquid materials characterised by the additives
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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
- 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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- 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
본 발명은 전지용 비수전해액에 관한 것으로, 보다 상세하게는 종래의 리튬 전지용 비수 전해액에 퓨라논계 유도체를 첨가함으로써 전해액의 분해를 억제하여, 고온 방치시 전지의 두께 증가율이 현저히 감소되고, 고온에서의 용량 저장 특성이 향상된 신규 전지용 비수 전해액에 관한 것이다.The present invention relates to a nonaqueous electrolyte solution for batteries, and more particularly, to suppress decomposition of the electrolyte by adding a furanone derivative to a conventional nonaqueous electrolyte solution for lithium batteries, thereby significantly reducing the thickness increase rate of the battery when left at a high temperature, and at a high temperature. The present invention relates to a nonaqueous electrolyte solution for new batteries having improved storage characteristics.
Description
본 발명은 전지용 비수전해액에 관한 것으로, 보다 상세하게는 종래의 리튬 전지용 비수 전해액에 퓨라논계 유도체를 첨가함으로써 전해액의 분해를 억제하여, 고온 방치시 전지의 두께 증가율이 현저히 감소되고, 고온에서의 용량 저장 특성이 향상된 신규 전지용 비수 전해액에 관한 것이다.The present invention relates to a nonaqueous electrolyte solution for batteries, and more particularly, to suppress decomposition of the electrolyte by adding a furanone derivative to a conventional nonaqueous electrolyte solution for lithium batteries, thereby significantly reducing the thickness increase rate of the battery when left at a high temperature, and at a high temperature. The present invention relates to a nonaqueous electrolyte solution for new batteries having improved storage characteristics.
노트북 컴퓨터, 캠코더, 휴대폰 등에 사용되는 소형화 및 슬림화된 리튬 이차전지는 리튬이온의 탈리 및 삽입이 가능한 리튬 금속 혼합 산화물로 된 양극 물질, 탄소재료 또는 금속 리튬 등으로 된 음극, 및 혼합 유기 용매에 리튬염이 적당량 용해된 전해액으로 구성되어 있다. 이러한 리튬전지의 형태로는 코인형, 18650 원통형, 063048 각형 등이 일반적으로 사용되고 있다. 리튬 전지의 3.6 내지 3.7V 정도의 평균 방전 전압은 다른 알칼리 전지나 Ni-MH 또는 Ni-Cd전지에 비하여 높은 전력을 얻을 수 있어 유리하다.The miniaturized and slimmed lithium secondary battery used in notebook computers, camcorders, mobile phones, etc. is a cathode material made of a lithium metal mixed oxide capable of detaching and inserting lithium ions, an anode made of carbon material or metal lithium, and lithium in a mixed organic solvent. It consists of electrolyte solution in which salt was melt | dissolved in an appropriate quantity. Coins, 18650 cylinders, 063048 squares, and the like are generally used as the lithium battery. The average discharge voltage of about 3.6 to 3.7 V of the lithium battery is advantageous because high power can be obtained as compared with other alkaline batteries or Ni-MH or Ni-Cd batteries.
이러한 높은 구동 전압을 나타내기 위해서는 충방전 영역인 0 내지 4.2V에서 전기화학적으로 안정한 전해액 조성이 필요하며, 따라서 탄산에틸렌(ethylene carbonate, EC), 탄산디메틸(dimethyl carbonate, DMC), 탄산디에틸(diethyl carbonate, DEC) 등의 탄산염계 유기용매와 분리막과의 흡윤성 증가를 위하여 플루오로벤젠(Fluorobenzene, FB)을 적절히 혼합하여 전해액 용매로 사용한다. 전해액의 용질로 통상 LiPF6, LiBF4, LiClO4, LiN(C2F5SO 3)2 등의 리튬염을 사용하며, 이들은 전지 내에서 리튬이온의 공급원으로 작용하여 리튬 전지의 기본적인 작동을 가능하게 한다. 그러나 이와 같이 제조된 비수 전해액은 Ni-MH 또는 Ni-Cd전지에 사용되는 수계 전해액에 비하여 이온 전도도가 현저하게 낮기 때문에 고율 충방전 등에서 불리한 점으로 작용하기도 한다.In order to exhibit such a high driving voltage, an electrochemically stable electrolyte composition is required in the charge / discharge region of 0 to 4.2 V. Therefore, ethylene carbonate (EC), dimethyl carbonate (DMC), and diethyl carbonate ( Fluorobenzene (FB) is suitably mixed and used as an electrolyte solvent in order to increase the absorbency between the carbonate organic solvent such as diethyl carbonate (DEC) and the separator. As the solute of the electrolyte, lithium salts such as LiPF 6 , LiBF 4 , LiClO 4, and LiN (C 2 F 5 SO 3 ) 2 are commonly used. They function as a source of lithium ions in the battery, thereby enabling basic operation of the lithium battery. Let's do it. However, the nonaqueous electrolyte prepared as described above may have disadvantages in high rate charging and discharging because the ion conductivity is significantly lower than that of the aqueous electrolyte used in Ni-MH or Ni-Cd batteries.
리튬 전지의 초기 충전시 양극으로 사용되는 리튬 금속 복합 산화물로부터 나온 리튬 이온은 음극으로 사용되는 흑연(결정질 또는 비결정질) 전극으로 이동하여, 흑연 전극의 층간에 삽입(intercalation)된다. 이 때 리튬은 반응성이 강하므로 흑연 음극 표면에서 전해액과 음극을 구성하는 탄소가 반응하여 Li2CO3, Li2 O, LiOH 등의 화합물을 형성한다. 이들 화합물은 흑연 음극의 표면에 일종의 부동태 피막(passivation layer)을 형성하게 되는데, 이러한 피막을 SEI(Solid electrolyte interface) 필름이라고 한다. 상기 SEI 필름은 일단 형성되면 이온 터널의 역할을 수행하여 리튬 이온만을 통과시키게 된다. SEI 필름은 이러한 이온 터널의 효과로 리튬 이온을 용매화시켜, 전해액 중에서 리튬이온과 함께 이동하는 분자량이 큰 유기용매 분자, 예를 들면 EC, DMC, DEC 등이 흑연 음극에 함께 삽입되어 흑연 음극의 구조가 붕괴되는 것을 막아 준다. 일단 SEI 필름이 형성되고 나면, 리튬 이온은 다시는 흑연 음극 또는 다른 물질과 부반응을 하지 않게 되고, 상기 SEI 필름 형성에 소모된 전하량은 비가역 용량으로 방전시 가역적으로 반응하지 않는 특성을 갖는다. 따라서 더 이상의 전해액 분해가 발생하지 않고 전해액 중의 리튬 이온의 양이 가역적으로 유지되어 안정적인 충방전이 유지된다 참조: J. Power Sources (1994) 51: 79~104).In the initial charging of a lithium battery, lithium ions derived from a lithium metal composite oxide used as a positive electrode move to a graphite (crystalline or amorphous) electrode used as a negative electrode, and are intercalated between layers of the graphite electrode. At this time, since lithium is highly reactive, the electrolyte and the carbon constituting the cathode react on the graphite cathode surface to form compounds such as Li 2 CO 3 , Li 2 O, and LiOH. These compounds form a kind of passivation layer on the surface of the graphite cathode, which is called a solid electrolyte interface (SEI) film. Once formed, the SEI film functions as an ion tunnel to pass only lithium ions. The SEI film solvates lithium ions by the effect of this ion tunnel, and organic solvent molecules having a large molecular weight, such as EC, DMC, DEC, etc., that move with lithium ions in the electrolyte are inserted together in the graphite cathode to form a graphite anode. It prevents the structure from collapsing. Once the SEI film is formed, lithium ions again do not react sideways with the graphite cathode or other material, and the amount of charge consumed to form the SEI film has a property of not reversibly reacting upon discharge with an irreversible capacity. Thus, no further electrolyte decomposition occurs and the amount of lithium ions in the electrolyte is reversibly maintained to maintain stable charging and discharging. J. Power Sources (1994) 51: 79-104).
한편 박형의 각형 전지에서는 상술한 SEI 형성 반응 중에 탄산염계 유기용매의 분해로부터 발생하는 CO, CO2, CH4, C2H6 등의 기체 발생으로 인하여 충전시 전지의 두께가 팽창하는 문제가 발생한다(참조: J. Power Sources (1998) 72: 66~70). 또한 만충전 상태에서 고온 저장시(예: 4.2V까지 만충전 후 85℃에서 4시간 방치) 시간이 경과함에 따라 상기의 SEI 필름이 증가된 전기화학적 에너지와 열 에너지에 의하여 서서히 붕괴되어, 노출된 음극 표면과 주위의 전해액이 반응하는 부반응이 지속적으로 발생하게 된다. 이때의 계속적인 기체발생으로 인하여 전지 내부의 내압이 상승하게 되며, 그 결과 각형 전지와 PLI(Polymer lithium ion) 전지의 경우 전지의 두께가 증가하여 세트 장착 자체를 어렵게 만드는 문제를 유발한다.On the other hand, in the thin square battery, the thickness of the battery is expanded during charging due to the generation of gases such as CO, CO 2 , CH 4 , and C 2 H 6 generated from decomposition of the carbonate-based organic solvent during the above-mentioned SEI formation reaction. (See J. Power Sources (1998) 72: 66-70). In addition, when stored at high temperature in a fully charged state (for example, left at 85 ° C. for 4 hours after being fully charged to 4.2V), the SEI film is gradually decayed due to increased electrochemical energy and thermal energy. Side reactions continue to occur between the cathode surface and the surrounding electrolyte. In this case, the internal pressure of the battery increases due to the continuous gas generation, and as a result, in the case of the square battery and the polymer lithium ion (PLI) battery, the thickness of the battery increases, which causes the problem of making the set itself difficult.
본 발명은 상기와 같은 종래 기술의 문제점을 해결하기 위한 것으로, 종래의 리튬 전지용 비수 전해액에 퓨라논계 유도체를 첨가함으로써 전해액의 분해를 억제하여, 고온 방치시 전지의 두께 증가율이 현저히 감소되고 고온에서의 용량 저장 특성이 향상된 신규 리튬 전지용 비수 전해액을 제공하는 것을 목적으로 한다.The present invention is to solve the problems of the prior art as described above, by suppressing the decomposition of the electrolyte by adding a furanone-based derivative to the conventional non-aqueous electrolyte for lithium batteries, the rate of increase in thickness of the battery is significantly reduced at high temperatures and at high temperatures An object of the present invention is to provide a nonaqueous electrolyte solution for a lithium battery having improved capacity storage characteristics.
즉, 본 발명은 0.8 내지 2 M의 리튬염이 용해된 전지용 비수 전해액에 있어서, 하기 화학식 1로 표시되는 테트로닉 산 0.01 내지 20중량%가 첨가된 것을 특징으로 하는 전지용 비수 전해액에 관한 것이다.That is, the present invention relates to a nonaqueous electrolyte solution for batteries, wherein 0.01 to 20% by weight of a tetronic acid represented by the following formula (1) is added to the nonaqueous electrolyte solution for batteries in which 0.8 to 2 M of lithium salt is dissolved.
[화학식 1][Formula 1]
이하에서 본 발명을 보다 상세하게 설명한다.Hereinafter, the present invention will be described in more detail.
본 발명의 리튬 전지용 비수 전해액의 제조에 사용되는 유기 용매로는 에틸렌카보네이트(EC), 프로필렌카보네이트(PC)와 같은 환형 탄산염계 유기용매, 디메틸카보네이트(DMC), 디에틸카보네이트(DEC), 에틸메틸카보네이트(EMC), 메틸프로필카보네이트(MPC), 에틸프로필카보네이트(EPC)와 같은 선형 탄산염계 유기용매 등을 예로 들 수 있다. 바람직하게는 일종 이상의 환형 탄산염계 유기용매 및 일종 이상의 선형 탄산염계 유기용매를 혼합하여 사용하며, 보다 바람직하게는 에틸렌 카보네이트, 에틸메틸 카보네이트, 디에틸 카보네이트를 1:1:1의 비율로 혼합하여 사용한다. 이외에도, 필요에 따라 아세트산프로필, 아세트산메틸, 아세트산에틸, 아세트산부틸, 프로피온산메틸, 프로피온산에틸, 플루오르벤젠 등의 용매를 추가로 혼합하여 사용할 수 있다. 각 유기용매의 혼합비는 본 발명의 목적을 저해하지 않는 한 특별히 제한 받는 것은 아니며, 통상의 리튬 전지용 비수 전해액 제조 시의 혼합비를 따른다.Organic solvents used in the preparation of the nonaqueous electrolyte solution for lithium batteries of the present invention include cyclic carbonate organic solvents such as ethylene carbonate (EC) and propylene carbonate (PC), dimethyl carbonate (DMC), diethyl carbonate (DEC), and ethyl methyl. Linear carbonate organic solvents such as carbonate (EMC), methylpropyl carbonate (MPC), ethyl propyl carbonate (EPC), and the like. Preferably, one or more cyclic carbonate organic solvents and one or more linear carbonate organic solvents are mixed and used. More preferably, ethylene carbonate, ethyl methyl carbonate, and diethyl carbonate are mixed in a ratio of 1: 1: 1. do. In addition, solvents, such as propyl acetate, methyl acetate, ethyl acetate, butyl acetate, methyl propionate, ethyl propionate, and fluorobenzene, can be further mixed and used as needed. The mixing ratio of each organic solvent is not particularly limited as long as the object of the present invention is not impaired, and the mixing ratio in the production of a nonaqueous electrolyte solution for a lithium battery is usually used.
한편, 본 발명의 비수 전해액에 포함되는 리튬염으로는 LiPF6, LiClO4, LiAsF6, LiBF4, LiN(C2F5SO3)2 등을 예로 들 수 있으며, 이들을 단독으로 또는 이종 이상 혼합하여 사용할 수 있다. 보다 바람직하게는 LiPF6를 사용한다. 그 첨가 농도는 0.8 내지 2.0M의 범위이다. 상기 리튬염의 첨가농도가 0.8M 미만인 경우에는 이온 전도도가 저하되는 문제점이 있고, 2.0M을 초과하는 경우에는 전해액의 점도가 증가되어 이온 전도도가 저하되는 문제점이 있다.Meanwhile, examples of the lithium salt contained in the nonaqueous electrolyte solution of the present invention include LiPF 6 , LiClO 4 , LiAsF 6 , LiBF 4, LiN (C 2 F 5 SO 3 ) 2 , and the like, and these may be used alone or in combination of two or more thereof. Can be used. More preferably LiPF 6 is used. The addition concentration is the range of 0.8-2.0M. If the concentration of the lithium salt is less than 0.8M, there is a problem that the ionic conductivity is lowered. If the lithium salt is more than 2.0M, the viscosity of the electrolyte is increased and the ion conductivity is lowered.
본 발명의 비수전해액에는 하기 화학식 1로 표시되는 퓨라논계 유도체인 테트로닉산(Tetronic Acid)을 0.01 내지 20.0 중량%, 바람직하게는 0.1 내지 10중량% 첨가됨을 특징으로 한다. 상기 함량이 0.01중량% 미만인 경우에는 전해액의 분해 를 억제하여, 고온 방치시 전지의 두께 증가율을 감소시키는 것이 어렵고, 20중량%를 초과하는 경우에는 수명과 같은 전지성능이 저하되는 문제점이 있다.The nonaqueous electrolyte of the present invention is characterized in that 0.01 to 20.0% by weight of Tetronic Acid (Tetronic Acid), which is a furanone derivative represented by the following Chemical Formula 1, preferably 0.1 to 10% by weight is added. If the content is less than 0.01% by weight to suppress the decomposition of the electrolyte, it is difficult to reduce the thickness increase rate of the battery when left at a high temperature, when it exceeds 20% by weight there is a problem that the battery performance such as life is lowered.
본 발명의 리튬 전지용 비수 전해액을 사용하여 통상의 방법에 따라 리튬 전지를 제조할 수 있으며, 이와 같이 제조된 리튬 전지는 고온(80℃, 10일)에서 방치하여도 전해액의 분해에 따른 전지 내부의 기체 발생이 억제되기 때문에, 전지의 두께가 팽창하는 부풀림 현상이 방지되고, 고온에서의 용량 저장특성 또한 우수해지는 효과가 있다.The lithium battery may be manufactured according to a conventional method using the nonaqueous electrolyte solution for lithium batteries of the present invention, and the lithium battery thus prepared may be stored inside the battery due to decomposition of the electrolyte even when left at a high temperature (80 ° C. for 10 days). Since gas generation is suppressed, the swelling phenomenon in which the thickness of the battery is expanded is prevented, and the capacity storage characteristic at high temperature is also excellent.
이하, 실시예를 통하여 본 발명을 보다 구체적으로 설명하고자 하나, 이러한 실시예들은 단지 설명의 목적을 위한 것으로 본 발명을 제한하는 것으로 해석해서는 안 된다. Hereinafter, the present invention will be described in more detail with reference to examples, but these examples are for illustrative purposes only and should not be construed as limiting the present invention.
실시예 및 비교예Examples and Comparative Examples
에틸렌카보네이트(EC), 에틸메틸카보네이트(EMC), 디에틸카보네이트(DEC)를 1:1:1의 비율(v/v)로 혼합한 후, 용질로서 LiPF6을 1M 용해시켜 기본 전해액으로 하고, 이 기본 전해액에 대하여 테트로닉산을 표 1에 표시된 함량으로 첨가하여 전해액을 제조하였다.Ethylene carbonate (EC), ethyl methyl carbonate (EMC) and diethyl carbonate (DEC) were mixed at a ratio of 1: 1: 1 (v / v), and then 1M of LiPF 6 was dissolved as a solute to obtain a basic electrolyte solution. For this basic electrolyte solution, tetronic acid was added in the amounts shown in Table 1 to prepare an electrolyte solution.
리튬전지는 각형 423048 전지의 형태로 제조되었다. 음극의 활물질로는 흑연을 사용하였고, 결착제로 PVDF를 사용하다. 양극의 활물질로는 LiCoO2를 사용하였고 결착제로 PVDF를 사용하였다. 도전제로 아세틸렌블랙을 사용하였다.The lithium battery was manufactured in the form of a square 423048 battery. Graphite was used as the active material of the negative electrode, and PVDF was used as the binder. LiCoO 2 was used as an active material of the positive electrode and PVDF was used as a binder. Acetylene black was used as the conductive agent.
제조된 리튬전지를 사용하여 화성 충방전과 표준충방전 과정 후 4.2V 만충전 상태에서 고온(80℃, 10일) 부풀림 실험을 하였으며, 그 결과를 표 1에 나타내었다. 한편 수명(표준충방전)특성(50 사이클)을 측정하여 이를 도 1에 나타낸다. 한편, 테트로닉산이 1.0중량% 첨가된 전해액(실시예) 및 첨가되지 않은 전해액(비교예)의 전기화학적 특성을 측정하여 이를 도 2에 나타내었다.Using the manufactured lithium battery, the experiment was performed at high temperature (80 ° C., 10 days) inflation in 4.2V full charge state after the process of chemical charge and discharge and standard charge and discharge, and the results are shown in Table 1. Meanwhile, life (standard charge and discharge) characteristics (50 cycles) were measured and shown in FIG. 1. On the other hand, the electrochemical characteristics of the electrolytic solution (example) and the non-added electrolyte solution (example) added 1.0% by weight of tetronic acid was measured and shown in FIG.
△IR(mΩ): 고온 방치 전-후의 내부저항 변화△ IR (mΩ): Internal resistance change before and after high temperature
△V(volt): 고온 방치 전-후의 전압 변화ΔV (volt): voltage change before and after high temperature
△T(mm): 고온 방치 전-후의 두께 변화ΔT (mm): thickness change before and after high temperature standing
(고온방치 조건: 80℃±0.2℃, 10일)(High temperature leaving condition: 80 ℃ ± 0.2 ℃, 10 days)
본 발명에 의해 고온 방치시에도 전지의 두께 증가율이 현저히 감소되고 고온에서의 용량 저장 특성이 향상된 신규 리튬 전지용 비수 전해액을 제공할 수 있다.The present invention can provide a novel nonaqueous electrolyte solution for lithium batteries, in which the rate of increase in thickness of the battery is significantly reduced and the capacity storage characteristics at high temperatures are improved even when left at high temperature.
도 1은 본 발명의 실시예에서 제조된 리튬전지의 충번전 특성을 나타내는 그래프이고,1 is a graph showing charge and discharge characteristics of a lithium battery prepared in an embodiment of the present invention,
도 2는 본 발명의 실시예에서 제조된 비수전해액의 전기화학적 특성을 나타내는 그래프이다.Figure 2 is a graph showing the electrochemical characteristics of the non-aqueous electrolyte prepared in the embodiment of the present invention.
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| WO2006046785A1 (en) * | 2004-10-27 | 2006-05-04 | Cheil Industries Inc. | Nonaqueous electrolyte for battery |
| US11424483B2 (en) | 2017-04-28 | 2022-08-23 | Samsung Sdi Co., Ltd. | Electrolyte for lithium secondary battery, and lithium secondary battery comprising same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2006046785A1 (en) * | 2004-10-27 | 2006-05-04 | Cheil Industries Inc. | Nonaqueous electrolyte for battery |
| US11424483B2 (en) | 2017-04-28 | 2022-08-23 | Samsung Sdi Co., Ltd. | Electrolyte for lithium secondary battery, and lithium secondary battery comprising same |
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