KR20130033733A - Silicon oxide coated with graphine-carbon complex and method for manufacturing the same - Google Patents

Silicon oxide coated with graphine-carbon complex and method for manufacturing the same Download PDF

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KR20130033733A
KR20130033733A KR1020110097596A KR20110097596A KR20130033733A KR 20130033733 A KR20130033733 A KR 20130033733A KR 1020110097596 A KR1020110097596 A KR 1020110097596A KR 20110097596 A KR20110097596 A KR 20110097596A KR 20130033733 A KR20130033733 A KR 20130033733A
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graphene
silicon oxide
carbon
manufacturing
carbon complex
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KR101819042B1 (en
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강윤규
이철
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주식회사 예일전자
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/182—Graphene
    • 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
    • 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

PURPOSE: Silicon oxide coated with a grapheme-carbon complex and a manufacturing method thereof are provided to have a cathode active material which secures stable electric capacity by minimizing a volume expansion of the cathode material and to be applied to a highly efficient lithium secondary battery. CONSTITUTION: A manufacturing method of silicon oxide coated with a grapheme-carbon complex comprises the following steps: a step of manufacturing the graphene-carbon complex by mixing graphene and carbon; and a step of coating the silicon oxide particle surface with the graphene-carbon complex. The graphene and carbon are mixed at a 8:2 weight ratio. In the coating step, the graphene-carbon complex and the silicon oxide are mixed in a 1:9-2:8 weight ratio and coated by using a drying method.

Description

그래핀-탄소 복합체로 코팅된 실리콘산화물 및 그 제조방법{SILICON OXIDE COATED WITH GRAPHINE-CARBON COMPLEX AND METHOD FOR MANUFACTURING THE SAME}Silicon oxide coated with graphene-carbon composites and a method of manufacturing the same {SILICON OXIDE COATED WITH GRAPHINE-CARBON COMPLEX AND METHOD FOR MANUFACTURING THE SAME}

본 발명은 리튬 이차전지의 음극재에 관한 것으로서, 보다 상세하게는 그래핀과 탄소 복합체로 코팅된 실리콘산화물(SiOX)에 관한 것이다.The present invention relates to a negative electrode material of a lithium secondary battery, and more particularly, to a silicon oxide (SiO X ) coated with graphene and a carbon composite.

21세기에 들어서면서 IT산업기술은 기타 과학기술 분야에 비해 비약적인 발전은 계속하고 있고, 이들은 노트북, 휴대전화, PDA등 휴대가 가능하고 간편한 모바일기기를 중심으로 많은 상품개발이 주축을 이루어왔으며, 최근에는 모바일 기기의 성능 다양화와 가정, 회사, 사회 등을 연결하는 유비쿼터스 네트워크가 급속도로 진행되고 있다.
Entering the 21st century, IT industry technology has continued to make rapid leap compared to other science and technology fields, and many of them have been focusing on product development mainly on portable and simple mobile devices such as laptops, mobile phones, PDAs, etc. In recent years, ubiquitous networks connecting the performance of mobile devices with homes, businesses, and societies are rapidly progressing.

특히 환경문제 및 에너지 문제에 대한 관심 및 연구개발이 집중되면서, 전기자동차용 리튬이차전지와 에너지저장용 리튬이차전지에 관한 기술선점 욕구는 전 세계적으로 매우 치열한 경쟁이 진행되고 있고 이를 위한 활발한 연구가 진행되고 있다.
Particularly, as interest and research and development on environmental and energy issues are concentrated, the desire to occupy the technology for lithium secondary batteries for electric vehicles and lithium secondary batteries for energy storage is intensifying competition all over the world. It's going on.

리튬이차전지에 있어서, 특히 음극재료에 대한 기술이 부각되고 있다. 리튬이차전지의 음극 활물질은 흑연이 지속적으로 사용되어 왔으며, 용량 증가에 대한 요구로 인해 다른 탄소계 물질이나, 리튬 금속 화합물 등이 연구되어 왔다. 그러나 음극재료는 초기 비가역용량이 존재하고 부피변화가 심하게 발생되며, 수명 특성이 크게 떨어지는 문제가 있어, 아직까지는 흑연을 대체하여 상용화할 수 있는 물질을 찾아보기 어렵다.
BACKGROUND OF THE INVENTION In lithium secondary batteries, technology for negative electrode materials is particularly highlighted. Graphite is continuously used as a negative electrode active material of a lithium secondary battery, and other carbon-based materials, lithium metal compounds, and the like have been studied due to a demand for increasing capacity. However, the negative electrode material has an initial irreversible capacity, a severe volume change occurs, and has a problem of significantly deteriorating the lifetime characteristics. Thus, it is difficult to find a material that can be commercialized by replacing graphite.

최근에 리튬이차전지의 음극 활물질로 금속 Si 나노와이어(nanowire)가 개발되었으나, 고가의 가격 경쟁력을 극복하지 못하고 있는 실정이다. 또한, 다른 금속 또는 금속 산화물을 이용하여 복합 전극을 제조하는 기술이 등장하고 있으나, 첨가된 금속이나 금속 산화물이 용량을 발현하지 못하고, 낮은 에너지 밀도를 보이는 단점이 존재한다.
Recently, metal Si nanowires (nanowires) have been developed as negative electrode active materials for lithium secondary batteries, but they do not overcome expensive price competitiveness. In addition, a technique for manufacturing a composite electrode using other metals or metal oxides has emerged, but there is a disadvantage in that the added metal or metal oxide does not express a capacity and shows a low energy density.

한편, 음극 활물질로 SiO-C 복합체를 제조하는 기술이 등장하고 있으나, 이러한 SiO-C복합체는 출발물질(precursor)로 SiO를 사용하여 고온(약 700~1000℃)의 열처리를 필요로 하고, 다시 기계적, 물리적으로 파쇄를 통해 입자크기를 줄여야 하는 기술적 난점을 가지고 있다.
On the other hand, there is a technology for producing a SiO-C composite as a negative electrode active material, such a SiO-C composite requires a high temperature (about 700 ~ 1000 ℃) heat treatment using SiO as a starting material (precursor), again There is a technical difficulty to reduce the particle size through mechanical and physical crushing.

따라서, 전지 효율이 우수하고, 장시간 사용할 수 있는 음극 활물질이 절실히 요구되고 있으며, 이러한 음극 활물질을 경제적이고, 용이하게 제조할 수 있는 방법이 요구되고 있다.Therefore, there is an urgent need for a negative electrode active material that is excellent in battery efficiency and can be used for a long time, and a method for economically and easily manufacturing such a negative electrode active material is required.

본 발명의 일측면은 효율이 우수하고, 부피변화가 심하지 않아 장기간 사용이 가능한 그래핀-탄소 복합체로 코팅된 실리콘 산화물과 이를 용이하게 제조할 수 있는 방법을 제공하고자 하는 것이다.One aspect of the present invention is to provide a silicon oxide coated with a graphene-carbon composite that can be used for a long time because the efficiency is excellent, and the volume change is not so severe.

본 발명은 그래핀과 흑연을 혼합하여 그래핀-탄소 복합체를 제조하는 단계; 및The present invention is to prepare a graphene-carbon composite by mixing graphene and graphite; And

상기 그래핀-탄소 복합체를 실리콘 산화물 입자 표면에 코팅하는 단계를 포함하는 그래핀-탄소 복합체로 코팅된 실리콘 산화물의 제조방법
Method for producing a silicon oxide coated with a graphene-carbon composite comprising the step of coating the graphene-carbon composite on the surface of the silicon oxide particles

또한, 본 발명은 상기 방법으로 제조된 실리콘 산화물을 제공한다.The present invention also provides a silicon oxide prepared by the above method.

본 발명은 음극재의 부피팽창을 최소화를 통해, 안정적인 전기 용량을 확보할 수 있는 음극활물질을 제공한다. 이를 통해, 고성능 리튬 이차전지로의 활용을 기대할 수 있는 장점이 있다.The present invention provides a negative electrode active material that can secure a stable electric capacity through minimizing the volume expansion of the negative electrode material. Through this, there is an advantage that can be expected to be utilized as a high performance lithium secondary battery.

도 1(a)는 발명예를 관찰한 SEM 사진이고, (b)는 상기 (a)를 확대한 사진임
도 2는 본 발명 실시예의 결과를 나타낸 그래프임.Figure 1 (a) is an SEM photograph observing the invention example, (b) is an enlarged photograph of (a).
Figure 2 is a graph showing the results of the embodiment of the present invention.

이하, 본 발명에 대해 상세히 설명한다.Hereinafter, the present invention will be described in detail.

먼저, 본 발명의 실리콘 산화물의 제조방법에 대해서 상세히 설명한다.
First, the manufacturing method of the silicon oxide of this invention is demonstrated in detail.

그래핀(graphine)과 흑연을 혼합하여 그래핀-탄소 복합체를 제조한다. 상기 그래핀과 흑연은 중량비 8:2의 비율로 준비하고 건식방법을 통해 혼합함으로서, 그래핀-탄소 복합체를 제조한다.
Graphene and graphite are mixed to prepare a graphene-carbon composite. The graphene and graphite are prepared in a weight ratio of 8: 2 and mixed by a dry method to prepare a graphene-carbon composite.

상기 그래핀은 높은 전기전도도를 가지며, 탄소재 표면에 미세한 탄소층을 형성하고, 후술하는 그래핀-탄소 복합체가 코팅된 실리콘 산화물의 제조시에 실리콘의 확산을 억제하고 산소와의 결함력을 약화시켜, 실리카(SiO2)의 형성을 억제하여 용량을 비약적으로 확대시킬 수 있다.
The graphene has a high electrical conductivity, forms a fine carbon layer on the surface of the carbon material, inhibits diffusion of silicon and weakens defects with oxygen during the production of the graphene-carbon composite-coated silicon oxide described below. In this way, the formation of silica (SiO 2 ) can be suppressed to significantly increase the capacity.

상기 그래핀-탄소 복합체를 실리콘 산화물(SiOX) 입자에 코팅시켜 그래핀-탄소 복합체가 코팅된 실리콘 산화물을 제조한다.
The graphene-carbon composite is coated on silicon oxide (SiO X ) particles to prepare silicon oxide coated with graphene-carbon composite.

이하, 본 발명의 실시예에 대하여 상세히 설명한다.Hereinafter, embodiments of the present invention will be described in detail.

(실시예)(Example)

입자크기 150㎛의 인조흑연과 층간간격이 0.45~0.8㎚인 그래핀(알드리치사)을 준비하였다. 상기 그래핀과 흑연을 중량비 8:2로 100~200rpm으로 약 2~5시간 동안 건식 혼합방식을 통해 그래핀-탄소 복합체를 제조하였다.Artificial graphite having a particle size of 150 μm and graphene (Aldrich) having an interlayer spacing of 0.45 to 0.8 nm were prepared. Graphene and graphite were prepared in a graphene-carbon composite by dry mixing for about 2 to 5 hours at 100 to 200 rpm with a weight ratio of 8: 2.

또한, 실리콘 산화물(SiOX)(알드리치사)를 준비하고, 상기 그래핀-탄소 복합체와 상기 실리콘 산화물을 1:9~2:8의 중량비로 200~500rpm으로 건식방법을 통해, 상기 그래핀-탄소 복합체가 코팅된 실리콘 산화물을 제조하였다.In addition, silicon oxide (SiO X ) (Aldrich Co., Ltd.) was prepared, and the graphene-carbon composite and the silicon oxide were dried at 200 to 500 rpm at a weight ratio of 1: 9 to 2: 8, and the graphene- A silicon oxide coated with a carbon composite was prepared.

이렇게 제조된 실리콘 산화물을 전자현미경인 SEM으로 분석하여 그 결과를 도 1에 나타내었다. 도 1의 (a) 및 (b)에 나타난 바와 같이, 탄소내에 그래핀이 균일하게 위치하여 있음을 알 수 있다.
The silicon oxide thus prepared was analyzed by SEM, which is shown in FIG. 1. As shown in (a) and (b) of Figure 1, it can be seen that the graphene is uniformly located in the carbon.

한편, 본 발명의 그래핀-탄소 복합체가 코팅된 실리콘 산화물(발명예)과 통상의 탄소 코팅 실리콘 산화물(비교예)의 수명특성을 평가하고 그 결과를 도 2에 나타내었다. 도 2에 나타난 바와 같이, 비교예에 비해, 발명예는 50cycle까지도 500mAh/g의 용량을 확보하여 안정적인 용량을 확보할 수 있다. 이는 상기 그래핀-탄소 복합체가 Si의 확산과 산화를 억제하여 부피팽창을 최소화하기 때문이다.Meanwhile, the life characteristics of the graphene-carbon composite coated silicon oxide of the present invention (invention example) and the conventional carbon coated silicon oxide (comparative example) were evaluated and the results are shown in FIG. 2. As shown in Figure 2, compared to the comparative example, the invention can ensure a stable capacity by securing a capacity of 500mAh / g even up to 50 cycles. This is because the graphene-carbon composite inhibits diffusion and oxidation of Si to minimize volume expansion.

Claims (4)

그래핀과 흑연을 혼합하여 그래핀-탄소 복합체를 제조하는 단계; 및
상기 그래핀-탄소 복합체를 실리콘 산화물 입자 표면에 코팅하는 단계
를 포함하는 그래핀-탄소 복합체로 코팅된 실리콘 산화물의 제조방법.
Preparing a graphene-carbon composite by mixing graphene and graphite; And
Coating the graphene-carbon composite on a surface of silicon oxide particles
Method for producing a silicon oxide coated with a graphene-carbon composite comprising a.
청구항 1에 있어서,
상기 그래핀과 흑연은 중량비 8:2의 비율로 혼합하는 그래핀-탄소 복합체로 코팅된 실리콘 산화물의 제조방법.
The method according to claim 1,
The graphene and graphite is a method of producing a silicon oxide coated with a graphene-carbon composite in a ratio of 8: 2 by weight.
청구항 1에 있어서,
상기 코팅은 그래핀-탄소 복합체와 실리콘 산화물을 중량비 1:9~2:8비율로 혼합한 후, 건식방법을 통해 코팅하는 그래핀-탄소 복합체로 코팅된 실리콘 산화물의 제조방법.
The method according to claim 1,
The coating is a method of producing a silicon oxide coated with a graphene-carbon composite after the graphene-carbon composites and silicon oxide mixed in a weight ratio 1: 9 ~ 2: 8 ratio, and coated by a dry method.
청구항 1 내지 3 중 어느 하나의 방법으로 제조된 그래핀-탄소 복합체로 코팅된 실리콘 산화물.Silicon oxide coated with a graphene-carbon composite prepared by the method of any one of claims 1 to 3.
KR1020110097596A 2011-09-27 2011-09-27 Silicon oxide coated with graphine-carbon complex and method for manufacturing the same KR101819042B1 (en)

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KR20150128592A (en) 2014-05-09 2015-11-18 주식회사 엘지화학 Graphene-wrapped porous silicon-carbon composite and preparation method thereof
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