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KR20040082803A - Negative active material for lithium secondary battery and method of preparing same - Google Patents

Negative active material for lithium secondary battery and method of preparing same Download PDF

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Publication number
KR20040082803A
KR20040082803A KR1020030017486A KR20030017486A KR20040082803A KR 20040082803 A KR20040082803 A KR 20040082803A KR 1020030017486 A KR1020030017486 A KR 1020030017486A KR 20030017486 A KR20030017486 A KR 20030017486A KR 20040082803 A KR20040082803 A KR 20040082803A
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active material
negative electrode
electrode active
lithium secondary
secondary battery
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KR1020030017486A
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Korean (ko)
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김영준
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삼성에스디아이 주식회사
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Publication of KR20040082803A publication Critical patent/KR20040082803A/en

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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
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • 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
    • 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
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

PURPOSE: A negative electrode active material for a lithium secondary battery and a preparation method thereof are provided to improve the charge-discharge potential and capacity, and the discharge voltage. CONSTITUTION: The negative electrode active material for a lithium secondary battery comprises a core containing a crystalline carbon and an amorphous shell where C-Si-O is mixed, in which the amount of Si is 1-20wt% based on the total weight of the negative electrode active material. The method for preparing negative electrode active material comprises mixing Si oxides such as SiO or SiO2 with a crystalline carbon and heating the mixture at 600-1800deg.C.

Description

리튬 이차 전지용 음극 활물질 및 그의 제조 방법{NEGATIVE ACTIVE MATERIAL FOR LITHIUM SECONDARY BATTERY AND METHOD OF PREPARING SAME}Negative active material for lithium secondary battery and manufacturing method thereof {NEGATIVE ACTIVE MATERIAL FOR LITHIUM SECONDARY BATTERY AND METHOD OF PREPARING SAME}

[산업상 이용 분야][Industrial use]

본 발명은 리튬 이차 전지용 음극 활물질 및 그의 제조 방법에 관한 것으로서, 보다 상세하게는 향상된 고율 특성 및 높은 방전 전압 특성을 나타내는 리튬 이차 전지용 음극 활물질 및 그의 제조 방법에 관한 것이다.The present invention relates to a negative electrode active material for a lithium secondary battery and a method of manufacturing the same, and more particularly, to a negative electrode active material for a lithium secondary battery showing improved high rate characteristics and high discharge voltage characteristics and a method of manufacturing the same.

[종래 기술][Prior art]

리튬 이차 전지의 음극 활물질로서 리튬 금속이 처음 사용되었으나, 충방전 과정에서 용량이 급격히 감소되고, 리튬이 석출되어 덴드라이트 상을 형성함에 따라 세퍼레이터가 파괴되므로 전지의 수명이 단축되는 문제점이 있었다. 이를 해결하기 위해 리튬 금속 대신 리튬 합금이 사용되었으나 리튬 금속을 사용할 때의 문제점을 크게 개선하지는 못하였다.Lithium metal was first used as a negative electrode active material of a lithium secondary battery, but the capacity of the lithium secondary battery was rapidly decreased, and the separator was destroyed as lithium precipitates to form a dendrite phase, thereby reducing the battery life. To solve this problem, a lithium alloy was used instead of lithium metal, but it did not significantly improve the problem of using lithium metal.

이후, 음극 활물질로서 리튬 이온을 인터칼레이션하고 디인터칼레이션할 수 있는 탄소계 물질이 주로 사용되고 있다. 이러한 탄소계 물질로는 결정질 탄소와 비정질 탄소가 있다. 그 중 주로 사용하고 있는 결정질 탄소는 다시 인조 흑연과 천연 흑연으로 분류할 수 있다.Since, a carbon-based material capable of intercalating and deintercalating lithium ions is mainly used as a negative electrode active material. Such carbonaceous materials include crystalline carbon and amorphous carbon. Among them, crystalline carbon mainly used can be classified into artificial graphite and natural graphite.

그러나 이러한 탄소계 물질을 사용하였을 경우에는 리튬 금속을 사용한 경우에 비해서 용량이 다소 낮아 최근에 리튬 금속을 사용하였을 경우와 유사한 용량을 내는 새로운 음극 활물질에 관한 연구가 진행되고 있으며, 미국 특허 제 6,051,340호에 충전시 형성되는 리튬과 합금이 가능한 제 1 금속을 포함하는 전류 집전체와 이 전류 집전체에 형성되고, 상기 제 1 금속과 충전시 형성되는 리튬과 합금이 가능함 제 2 금속을 포함하는 층을 포함하며, 초기 충전 공정 전에 리튬이 포함되어 있지 않은 음극이 기술되어 있다. 상기 제 1 금속은 Ni, Ti, Cu, Ag, AU, Pt, Fe, Co, Cr, W 및 Mo으로 이루어진 군에서 선택되며, 상기 제 2 금속은 Al, Mg, K, Na, Ca, Sr, Ba, Si, Ge, Sb, Pb, In 및 Zn으로 이루어진 군에서 선택된다.However, when the carbon-based material is used, a study is conducted on a new negative electrode active material having a capacity lower than that of lithium metal, and having a capacity similar to that of lithium metal recently. US Pat. No. 6,051,340 A current collector comprising a first metal capable of alloying with lithium formed during charging, and a layer comprising a second metal formed in the current collector, capable of alloying with lithium formed during charging with the first metal. And negative electrodes that do not contain lithium prior to the initial charging process. The first metal is selected from the group consisting of Ni, Ti, Cu, Ag, AU, Pt, Fe, Co, Cr, W and Mo, and the second metal is Al, Mg, K, Na, Ca, Sr, Ba, Si, Ge, Sb, Pb, In and Zn.

또한 미국 특허 제 6,022,642 호에는 고용량 리튬 이차 전지를 제조하기 위해서 음극 표면에 절연막(insulative layer)를 형성하는 내용이 기술되어 있다.In addition, U.S. Patent No. 6,022,642 describes the formation of an insulative layer on the surface of a negative electrode to manufacture a high capacity lithium secondary battery.

그러나 상술한 기술들은 여전히 만족할만한 수준의 물성을 나타내는 음극을 형성하지는 못하고 있는 실정이다.However, the above-described techniques still do not form a cathode exhibiting satisfactory levels of physical properties.

본 발명은 상술한 문제점을 해결하기 위한 것으로서, 본 발명의 목적은 향상된 고율 특성 및 높은 방전 전압을 나타내는 리튬 이차 전지용 음극 활물질을 제공하는 것이다.SUMMARY OF THE INVENTION The present invention has been made to solve the above problems, and an object of the present invention is to provide a negative electrode active material for a lithium secondary battery exhibiting improved high rate characteristics and high discharge voltage.

본 발명의 또 다른 목적은 상술한 물성을 갖는 리튬 이차 전지용 음극 활물질의 제조 방법을 제공하는 것이다.Another object of the present invention is to provide a method for producing a negative electrode active material for a lithium secondary battery having the above-described physical properties.

도 1은 본 발명의 실시예 1 및 비교예 2의 음극 활물질의 충방전 특성을 나타낸 그래프.1 is a graph showing the charge and discharge characteristics of the negative electrode active material of Example 1 and Comparative Example 2 of the present invention.

상기 목적을 달성하기 위하여, 본 발명은 결정질 탄소를 포함하는 코어; 및 C-Si-O가 혼재된 비정질 쉘을 포함하는 리튬 이차 전지용 음극 활물질을 제공한다본 발명은 또한 SiO 또는 SiO2의 Si 산화물을 결정질 탄소와 혼합하고; 상기 혼합물을 600 내지 1800℃로 열처리하는 공정을 포함하는 리튬 이차 전지용 음극 활물질의 제조 방법을 제공한다.In order to achieve the above object, the present invention comprises a core containing crystalline carbon; And an amorphous shell in which C-Si-O is mixed. The present invention also relates to mixing a Si oxide of SiO or SiO 2 with crystalline carbon; It provides a method for producing a negative electrode active material for a lithium secondary battery comprising the step of heat-treating the mixture at 600 to 1800 ℃.

이하 본 발명을 보다 상세하게 설명한다.Hereinafter, the present invention will be described in more detail.

본 발명은 고율 특성 및 방전 전압 특성이 향상된 리튬 이차 전지용 음극 활물질을 제조할 수 있는 방법에 관한 것으로서, 본 발명의 제조 방법은 먼저 SiO 또는 SiO2의 Si 산화물을 결정질 탄소와 혼합한다. 이때, Si 산화물과 결정질 탄소와의 혼합 비율은 1 내지 20 : 99 내지 80 중량비가 바람직하다. Si 산화물의 양이 1 중량%보다 작을 경우에는 표면에 비정질상 형성이 안되며, 20 중량%를 초과할 경우에는 비가역 용량이 커져 충방전 효율이 안 좋아지고 탄소 수율이 저하되어 바람지하지 않다.The present invention relates to a method capable of manufacturing a negative electrode active material for a lithium secondary battery having improved high rate characteristics and discharge voltage characteristics, and the manufacturing method of the present invention first mixes Si or Si oxide of SiO 2 with crystalline carbon. At this time, the mixing ratio of Si oxide and crystalline carbon is preferably 1 to 20:99 to 80 weight ratio. When the amount of Si oxide is less than 1% by weight, no amorphous phase is formed on the surface. When the amount of Si oxide is more than 20% by weight, the irreversible capacity is increased, resulting in poor charging and discharging efficiency and low carbon yield.

상기 결정질 탄소로는 천연 흑연 또는 인조 흑연을 사용할 수 있다.As the crystalline carbon, natural graphite or artificial graphite may be used.

상기 혼합물을 600 내지 1800℃의 온도로 열처리한다. 열처리 온도가 600℃보다 낮으면 반응이 진행이 안되는 문제점이 있고, 1800℃보다 높으면, Si와 C가 반응하여 SiC 등의 카바이드가 형성되고 또한 비정질 쉘에서 산소 성분이 탄소와 반응하여 CO나 CO2등의 가스로 모두 소실될 우려가 있어 바람직하지 않다.The mixture is heat treated to a temperature of 600 to 1800 ° C. If the heat treatment temperature is lower than 600 ℃, there is a problem that the reaction does not proceed, if higher than 1800 ℃, Si and C reacts to form carbides such as SiC, and the oxygen component reacts with carbon in the amorphous shell, CO or CO 2 It is not preferable because all of them may be lost by such gases.

상기 열처리 공정은 질소나 아르곤 분위기에서 실시하는 것이 부반응을 유발하지 않으므로 바람직하다.The heat treatment step is preferably performed in a nitrogen or argon atmosphere because it does not cause side reactions.

상기 열처리 공정에 따라 결정질 탄소 표면 구조가 비정질 상으로 변화되어 결정질 탄소의 표면에 C-Si-O가 혼재된 비정질 상, 즉 결정질 탄소 코어와 Si, O 및 C를 포함하는 비정질 쉘 구조를 갖는 음극 활물질이 제조된다. 상기 음극 활물질은 Si을 음극 활물질 전체 중량에 대하여 1 내지 20 중량%로 포함한다.According to the heat treatment process, the crystalline carbon surface structure is changed to an amorphous phase, and thus the anode having an amorphous shell structure containing a C-Si-O mixed on the surface of the crystalline carbon, that is, a crystalline carbon core and Si, O and C An active material is prepared. The negative electrode active material contains Si in an amount of 1 to 20% by weight based on the total weight of the negative electrode active material.

상기 비정질 쉘은 리튬 이온의 출입을 용이하게 하여 탄소의 반응성을 높이며, 표면 피막 안정성에도 기여한다. 또한 산소가 포함됨에 따라 음극 활물질의 화학적인 안전성을 향상시킬 수 있다. 또한 제조된 음극 활물질은 상술한 바와 같이 표면 구조를 개선시킴에 따라 고율 특성을 향상시키고 방전 전압을 높일 수 있다. 특히 방전 전압의 상승은 전력(power)의 개념이 중요한 원통형에서 큰 위력을 발휘할 것으로 보이며, 각형의 경우도 유효 사용 용량의 증가 효과를 기대할 수 있다.The amorphous shell facilitates the entry and exit of lithium ions, increases carbon reactivity, and contributes to surface film stability. In addition, as oxygen is included, chemical safety of the negative electrode active material may be improved. In addition, the prepared negative active material may improve high rate characteristics and increase discharge voltage as the surface structure is improved as described above. In particular, the increase in the discharge voltage is expected to exert great power in the cylindrical shape, in which the concept of power is important, and in the case of a square shape, an increase in the effective use capacity can be expected.

이하 본 발명의 바람직한 실시예 및 비교예를 기재한다. 그러나 하기 실시예는 본 발명의 바람직한 일 실시예일 뿐 본 발명이 하기한 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 1)(Example 1)

SiO와 천연 흑연을 1 : 9 중량비로 혼합하였다. 이 혼합물을 1000℃의 온도로 질소 분위기에서 열처리하여 천연 흑연 코어와 Si, O 및 C를 포함하는 비정질 쉘을 갖는 리튬 이차 전지용 음극 활물질을 제조하였다.SiO and natural graphite were mixed in a 1: 9 weight ratio. The mixture was heat-treated at a temperature of 1000 ° C. in a nitrogen atmosphere to prepare a negative active material for a lithium secondary battery having a natural graphite core and an amorphous shell containing Si, O, and C.

(실시예 2)(Example 2)

SiO 대신 SiO2를 사용한 것을 제외하고는 상기 실시예 1과 동일하게 실시하였다.The same process as in Example 1 was carried out except that SiO 2 was used instead of SiO.

(비교예 1)(Comparative Example 1)

열처리 공정을 1800℃에서 실시한 것을 제외하고는 상기 실시예 1과 동일하게 실시하였다.Except that the heat treatment step was carried out at 1800 ℃ was carried out in the same manner as in Example 1.

(비교예 2)(Comparative Example 2)

천연 흑연을 음극 활물질로 사용하였다.Natural graphite was used as the negative electrode active material.

(비교예 3)(Comparative Example 3)

SiO2를 콜타르 핏치와 2 : 8 중량비로 혼합하였다. 이 혼합물을 질소 분위기의 반응기에서 교반시키면서 300℃로 3시간 열처리하여 휘발 성분과 CO2등의 발생 가스를 제거한 후 재차 600℃로 열처리하여 코크스로 만들었다.SiO 2 was mixed with coal tar pitch in a 2: 8 weight ratio. The mixture was heat-treated at 300 ° C. for 3 hours with stirring in a nitrogen atmosphere reactor to remove volatile components and generated gases such as CO 2 , and then heat-treated again at 600 ° C. to obtain coke.

제조된 코크스를 1000℃로 2시간 동안 탄화시킨 후, 얻어진 탄화물을 2800℃의 비활성 분위기로 흑연화하여 리튬 이차 전지용 음극 활물질을 제조하였다.The prepared coke was carbonized at 1000 ° C. for 2 hours, and the obtained carbide was graphitized in an inert atmosphere of 2800 ° C. to prepare a negative active material for a lithium secondary battery.

상기 실시예 1 및 비교예 2의 음극 활물질을 이용하여 통상의 방법으로 전지를 제조한 후, 충방전 특성을 측정하여 그 결과를 도 1에 나타내었다. 도 1에 나타낸 것과 같이, 실시예 1의 음극 활물질이 비교예 1에 비하여 높은 충방전 전위와 용량을 나타내며, 우수한 충방전 특성을 나타냄을 알 수 있다.After the battery was manufactured by a conventional method using the negative electrode active materials of Example 1 and Comparative Example 2, the charge and discharge characteristics were measured and the results are shown in FIG. As shown in FIG. 1, it can be seen that the negative electrode active material of Example 1 exhibits higher charge / discharge potential and capacity than Comparative Example 1, and exhibits excellent charge / discharge characteristics.

상술한 바와 같이, 본 발명의 리튬 이차 전지용 음극 활물질은 우수한 고율 특성 및 높은 방전 전압을 나타내는 리튬 이차 전지를 제공할 수 있다.As described above, the negative electrode active material for a lithium secondary battery of the present invention can provide a lithium secondary battery exhibiting excellent high rate characteristics and high discharge voltage.

Claims (6)

결정질 탄소를 포함하는 코어; 및A core comprising crystalline carbon; And C-Si-O가 혼재된 비정질 쉘Amorphous Shell with C-Si-O 을 포함하는 리튬 이차 전지용 음극 활물질.A negative electrode active material for a lithium secondary battery comprising a. 제 1 항에 있어서, 상기 Si의 함량은 전체 음극 활물질 중량에 대하여 1 내지 20 중량%인 리튬 이차 전지용 음극 활물질.The negative active material of claim 1, wherein the Si content is 1 to 20 wt% based on the total weight of the negative electrode active material. 제 1 항에 있어서, 상기 결정질 탄소는 천연 흑연 또는 인조 흑연인 리튬 이차 전지용 음극 활물질.The negative active material of claim 1, wherein the crystalline carbon is natural graphite or artificial graphite. SiO 또는 SiO2의 Si 산화물을 결정질 탄소와 혼합하고;Si oxide of SiO or SiO 2 is mixed with crystalline carbon; 상기 혼합물을 600 내지 1800℃로 열처리하는Heat-treating the mixture at 600 to 1800 ° C. 공정을 포함하는 리튬 이차 전지용 음극 활물질의 제조 방법.The manufacturing method of the negative electrode active material for lithium secondary batteries containing a process. 제 4 항에 있어서, 상기 Si 산화물과 결정질 탄소의 혼합 비율은 중량비로 1 내지 20 : 99 내지 80인 리튬 이차 전지용 음극 활물질의 제조 방법.The method of claim 4, wherein the mixing ratio of the Si oxide and the crystalline carbon is 1 to 20:99 to 80 by weight. 제 4 항에 있어서, 상기 열처리 공정은 질소 또는 아르곤 분위기에서 실시하는 것인 리튬 이차 전지용 음극 활물질의 제조 방법.The method of claim 4, wherein the heat treatment step is performed in a nitrogen or argon atmosphere.
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