JP2002042809A - Non-aqueous secondary battery - Google Patents
Non-aqueous secondary batteryInfo
- Publication number
- JP2002042809A JP2002042809A JP2000230470A JP2000230470A JP2002042809A JP 2002042809 A JP2002042809 A JP 2002042809A JP 2000230470 A JP2000230470 A JP 2000230470A JP 2000230470 A JP2000230470 A JP 2000230470A JP 2002042809 A JP2002042809 A JP 2002042809A
- Authority
- JP
- Japan
- Prior art keywords
- siox
- active material
- electrode active
- value
- secondary battery
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
【０００１】[0001]
【発明の属する技術分野】本発明は、電解液に非水系電
解液を用い、負極及び／又は正極にリチウムイオンを吸
蔵・放出可能な材料を用いた非水系二次電池及びそれに
用いられる電極活物質に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a non-aqueous secondary battery using a non-aqueous electrolytic solution as an electrolytic solution and a material capable of occluding and releasing lithium ions for a negative electrode and / or a positive electrode, and an electrode active material used therefor. About the substance.
【０００２】[0002]
【従来の技術】近年、ノートパソコンや携帯電話の普及
に伴い、小型の二次電池に対する需要が高まっている。
正極活物質に複合酸化物を、また負極活物質に黒鉛など
の炭素質材料又は金属酸化物を用いたリチウムイオン二
次電池は、その優れた特性、安全性により、活発な研究
が行われている。2. Description of the Related Art In recent years, with the spread of notebook personal computers and mobile phones, demand for small secondary batteries has been increasing.
Active research has been conducted on lithium ion secondary batteries using composite oxides for the positive electrode active material and carbonaceous materials such as graphite or metal oxides for the negative electrode active material due to their excellent properties and safety. I have.
【０００３】[0003]
【発明が解決しようとする課題】負極活物質に黒鉛など
の炭素質材料を用いた二次電池の最大充放電容量は、３
７２ｍＡｈ／ｇであり、金属リチウムを用いた場合に比
較して小さい。そこで、リチウムと金属合金を形成する
金属を含有する金属酸化物が提案されており（特開平１
０−２８４０５６号参照）、これによって炭素質材料と
比較して高い充放電容量を発現するようになった。The maximum charge / discharge capacity of a secondary battery using a carbonaceous material such as graphite as the negative electrode active material is 3
It is 72 mAh / g, which is smaller than the case where lithium metal is used. Therefore, a metal oxide containing a metal that forms a metal alloy with lithium has been proposed (Japanese Patent Laid-Open Publication No. HEI 1-1990).
No. 0-284056), thereby exhibiting a higher charge / discharge capacity as compared with a carbonaceous material.
【０００４】一方、本発明者らはこれまでの実験を通
じ、ＳｉＯｘのｘ値が小さいほど充放電容量が高くなる
傾向を理解していた。しかし、上記において開示されて
いるＳｉＯｘは気相法を用いて製造されているので、ｘ
値が１．００未満になることは起こりにくく、ｘ値が
１．００未満のＳｉＯｘを電極活物質とすることは実現
できていなかった。On the other hand, the present inventors have understood through experiments so far that the smaller the x value of SiOx, the higher the charge / discharge capacity. However, since the SiOx disclosed above is manufactured using a vapor phase method, x
It is unlikely that the value becomes less than 1.00, and it has not been possible to use SiOx having an x value of less than 1.00 as the electrode active material.
【０００５】本発明は上記に鑑みてなされたものであ
り、その目的は、非水系二次電池用電極活物質を提供す
ることである。またその電極活物質を用いて充放電容量
が極めて大である非水系二次電池を提供することであ
る。[0005] The present invention has been made in view of the above, and an object of the present invention is to provide an electrode active material for a non-aqueous secondary battery. Another object of the present invention is to provide a non-aqueous secondary battery having a very large charge / discharge capacity using the electrode active material.
【０００６】[0006]
【課題を解決するための手段】すなわち、本発明はｘ値
が１．００未満であるＳｉＯｘからなることを特徴とす
るリチウムイオンを吸蔵・放出可能な電極活物質であ
り、特に該ＳｉＯｘがフッ酸処理法によって得られるこ
とを特徴とするものである。また本発明は上記の電極活
物質が用いられてなることを特徴とする電極あるいは非
水系二次電池である。さらに、本発明は上記の電極活物
質の製造に適用できる、ｘ値が１．００未満のＳｉＯｘ
の製造方法である。That is, the present invention relates to an electrode active material capable of occluding and releasing lithium ions, characterized in that the electrode active material is made of SiOx having an x value of less than 1.00. It is characterized by being obtained by an acid treatment method. Further, the present invention provides an electrode or a non-aqueous secondary battery using the above-mentioned electrode active material. Further, the present invention can be applied to the production of the above-mentioned electrode active material.
It is a manufacturing method of.
【０００７】[0007]
【発明の実施の形態】以下、本発明について更に詳しく
説明する。BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in more detail.
【０００８】本発明で使用される電極活物質は、ｘ値が
１．００未満のＳｉＯｘである。[0008] The electrode active material used in the present invention is SiOx having an x value of less than 1.00.
【０００９】本発明のＳｉＯｘとは粉末のＳｉとＯとの
質量比を、例えば、ＦＥＳＥＭ／ＥＤＳ（エネルギー分
散型エックス線検出器、例えば、日本電子社製）を用い
て測定し、それをモル比に換算し、組成式ＳｉＯｘの化
合物であると見なしたときに、そのｘ値が０．１０〜
１．００であり、しかもＥＳＣＡ分析（Ｘ線光電子分光
法、例えば島津製作所作製「ＥＳＣＡ７５０」）を行っ
たときに、Ｓｉ及びＳｉＯ2とは異なる位置にピークを
有する物質であると定義される。The SiOx of the present invention is obtained by measuring the mass ratio between Si and O in a powder using, for example, a FESEM / EDS (energy dispersive X-ray detector, manufactured by JEOL Ltd.), and measuring the molar ratio. When considered as a compound of the composition formula SiOx, the x value is 0.10 to 0.10.
It is defined as a substance having a peak at a position different from Si and SiO 2 when subjected to ESCA analysis (X-ray photoelectron spectroscopy, for example, “ESCA750” manufactured by Shimadzu Corporation).
【００１０】本発明のＳｉＯｘの合成方法としては、特
に制約はないが、例えばｘ値が１．００以上のＳｉＯｘ
をフッ酸で処理する方法が挙げられる。すなわち、特公
平３−７２００８号公報、特公平４−２９６０３号公報
に開示されているように、固体状ＳｉＯ、ＳｉＯ2、Ｓ
ｉを単独あるいは混合して反応器内に充填し、１４００
℃以上に加熱しつつ、Ａｒのような不活性ガスやＨ2の
ような還元性ガスを供給してＳｉＯガスを発生させ、そ
れを冷却して生成した粒子を捕集したＳｉＯｘ（ｘ値が
２．００未満）あるいは市販のＳｉＯｘを二次処理する
ことによって得られる。The method for synthesizing SiOx of the present invention is not particularly limited, but for example, SiOx having an x value of 1.00 or more is used.
Is treated with hydrofluoric acid. That is, as disclosed in Japanese Patent Publication No. 3-72008 and Japanese Patent Publication No. 4-29603, solid SiO, SiO 2 , S
i alone or mixed and charged into the reactor,
While heating the mixture to a temperature of not less than 0 ° C., an inert gas such as Ar or a reducing gas such as H 2 is supplied to generate a SiO gas, which is cooled to collect particles generated by SiOx (x value: (Less than 2.00) or by secondary treatment of commercially available SiOx.
【００１１】二次処理としてフッ酸で処理する方法とし
ては、ＳｉＯｘ（ｘ値が２．００未満）に対し、フッ酸
水溶液をフッ酸質量で０．１〜１０倍量添加し、１〜１
２０分間攪拌した後、濾過する。濾紙上の残留物を濾液
が中性を示すまでよく洗浄し、ｘ値が１．００未満のＳ
ｉＯｘが得られる。フッ酸添加量が０．１倍未満の場
合、又は攪拌時間が１分未満ではｘ値が１．００未満の
ＳｉＯｘが得られない。一方、フッ酸添加量が１０倍量
を超える場合、又は撹拌時間が１２０分を超える過剰な
処理を行うと、目的とするｘ値のＳｉＯｘの収率が著し
く低下する。As a secondary treatment, a treatment with hydrofluoric acid is performed by adding an aqueous solution of hydrofluoric acid to SiOx (x value is less than 2.00) in an amount of 0.1 to 10 times by mass of hydrofluoric acid,
After stirring for 20 minutes, filter. The residue on the filter paper is thoroughly washed until the filtrate shows neutrality, and the X value is less than 1.00.
iOx is obtained. When the addition amount of hydrofluoric acid is less than 0.1 times, or when the stirring time is less than 1 minute, SiOx having an x value less than 1.00 cannot be obtained. On the other hand, when the addition amount of hydrofluoric acid exceeds 10 times or when the stirring time is excessively longer than 120 minutes, the yield of SiOx having the desired x value is significantly reduced.
【００１２】実際に、ＳｉＯｘのｘ値を１．００未満と
することで、これまでにない大きな充放電容量が得られ
た。ｘ値は小さいほど放充電容量の向上には望ましい。
ＳｉＯｘの電極活物質としてのＬｉイオンの吸蔵・放出
機構はよくわからないが、初期の充放電時にＳｉＯｘが
Ｓｉに還元され、そのＳｉとＬｉとの間においてＬｉの
可逆的な反応が起こると推定され、本発明のＳｉＯｘで
は、ｘ値が１．００以上のＳｉＯｘと比較して、ＳｉＯ
ｘにおける相対的なＳｉの含有量が増加したためではな
いかと推察している。Actually, by setting the x value of SiOx to less than 1.00, an unprecedentedly large charge / discharge capacity was obtained. The smaller the value of x is, the more desirable it is to improve the discharge capacity.
Although the mechanism of insertion and extraction of Li ions as the electrode active material of SiOx is not well understood, it is assumed that SiOx is reduced to Si during the initial charge and discharge, and a reversible reaction of Li occurs between the Si and Li. According to the SiOx of the present invention, as compared with SiOx having an x value of 1.00 or more,
It is speculated that this may be due to an increase in the relative content of Si in x.
【００１３】本発明の電極活物質は正極又は負極のいず
れの活物質としても用いることができるが、負極活物質
として用いることがより好ましい。The electrode active material of the present invention can be used as either a positive electrode or a negative electrode active material, but is more preferably used as a negative electrode active material.
【００１４】負極活物質として用いた場合、正極活物質
としては、一般的なＴｉＳ2、ＭｏＳ2、ＮｂＳｅ2、Ｖ2
Ｏ5等のリチウムを含有しない金属硫化物又は金属酸化
物や、ＬｉｘＭＯ2（但し、Ｍは一種類以上の遷移金属
であり、通常、ｘ値は０．０５〜１．０である。）を主
体とするリチウム複合酸化物、具体的にはコバルト酸リ
チウム、マンガン酸リチウム等が使用される。When used as a negative electrode active material, common positive electrode active materials include TiS 2 , MoS 2 , NbSe 2 , V 2
Lithium-free metal sulfides or metal oxides such as O 5 , or LixMO 2 (where M is one or more transition metals, and the x value is usually 0.05 to 1.0). A lithium composite oxide as a main component, specifically, lithium cobalt oxide, lithium manganate, or the like is used.
【００１５】本発明の活物質を正極活物質として用いた
場合、負極活物質としては、一般的にＬｉなどの卑金属
を用いることができる。When the active material of the present invention is used as a positive electrode active material, a base metal such as Li can generally be used as the negative electrode active material.
【００１６】本発明の非水系二次電池に用いる電極は、
上記ＳｉＯｘ粉末からなる負極活物質又は正極活物質と
導電剤との混合物を、結着剤を含む液体に分散してスラ
リーを調製し、それを金属箔からなる集電板に塗布・乾
燥することによって、製造することができる。The electrodes used in the non-aqueous secondary battery of the present invention are:
Dispersing a mixture of the negative electrode active material or the positive electrode active material composed of the SiOx powder and a conductive agent in a liquid containing a binder to prepare a slurry, and applying the slurry to a current collector plate composed of a metal foil and drying the slurry. Can be manufactured.
【００１７】本発明の非水系二次電池の電極に用いられ
る結着剤としては、ポリエチレン、ニトリルゴム、ポリ
ブタジエン、ブチルゴム、ポリスチレン、スチレン・ブ
タジエンゴム、多硫化ゴム、ニトロセルロース、四フッ
化エチレン樹脂、ポリフッ化ビニリデン、ポリフッ化ク
ロロプレン等が用いられる。The binder used for the electrode of the non-aqueous secondary battery of the present invention includes polyethylene, nitrile rubber, polybutadiene, butyl rubber, polystyrene, styrene / butadiene rubber, polysulfide rubber, nitrocellulose, and tetrafluoroethylene resin. , Polyvinylidene fluoride, polyvinyl chloroprene, or the like.
【００１８】本発明の非水系二次電池の電極に用いられ
る集電板としては、特に限定されるものではないが、
金、銀、銅、白金、アルミニウム、鉄、ニッケル、クロ
ム、マンガン、鉛、タングステン、チタン等、ないしは
これらを成分とする合金の金属箔が使用される。金属箔
の厚みは、薄いほうが好ましい。取り扱いの容易さから
正極にはアルミニウムが、負極には銅が好まれて用いら
れる。The current collector plate used for the electrode of the non-aqueous secondary battery of the present invention is not particularly limited.
Metal foil of gold, silver, copper, platinum, aluminum, iron, nickel, chromium, manganese, lead, tungsten, titanium, or the like, or an alloy containing these components is used. The thickness of the metal foil is preferably thin. Aluminum is preferably used for the positive electrode and copper is preferably used for the negative electrode because of ease of handling.
【００１９】本発明の非水系二次電池を作製するには、
従来の正極と負極と電解液からなる構成されている電池
において、負極及び／又は正極のかわりに、本発明に係
わるＳｉＯｘ粉末含有の負極及び／又は正極を用いれば
よく、特別なことは必要でない。To manufacture the non-aqueous secondary battery of the present invention,
In a conventional battery comprising a positive electrode, a negative electrode, and an electrolytic solution, the negative electrode and / or the positive electrode containing the SiOx powder according to the present invention may be used instead of the negative electrode and / or the positive electrode, and no special matter is required. .
【００２０】電解液としては、プロピレンカーボネー
ト、エチレンカーボネート、γ−ブチルラクトン、Ｎ−
メチルピロリドン、アセトニトリル、Ｎ，Ｎ−ジメチル
ホルムアミド、ジメチルスルフォキシド、テトラヒドロ
フラン、１，３−ジオキソラン、ギ酸メチル、スルホラ
ン、オキソゾリドン、塩化チオニル、１，２，−ジメト
キシエタン、ジエチレンカーボネートや、これらの誘導
体等が用いられている。また、電解質としてはリチウム
のハロゲン化物、リチウムの過塩素酸塩、リチウムのチ
オシアン塩、リチウムのホウフッ化塩、リチウムのリン
フッ化塩、リチウムの砒素フッ化塩、リチウムのアルミ
ニウムフッ化塩、リチウムのトリフルオロメチル硫酸塩
等が使用される。必要に応じて、セパレーター、端子、
絶縁板等の部品が取り付けられる。As the electrolyte, propylene carbonate, ethylene carbonate, γ-butyl lactone, N-
Methylpyrrolidone, acetonitrile, N, N-dimethylformamide, dimethylsulfoxide, tetrahydrofuran, 1,3-dioxolane, methyl formate, sulfolane, oxozolidone, thionyl chloride, 1,2-dimethoxyethane, diethylene carbonate, and derivatives thereof Etc. are used. Examples of the electrolyte include lithium halide, lithium perchlorate, lithium thiocyanate, lithium borofluoride, lithium phosphorus fluoride, lithium arsenic fluoride, lithium aluminum fluoride, lithium aluminum fluoride, and lithium lithium fluoride. Trifluoromethyl sulfate is used. If necessary, separators, terminals,
Parts such as an insulating plate are attached.
【００２１】本発明の非水系二次電池の形状は、コイン
型、箱型、ペーパー型、カード型等とすることができ、
また用途としては、ビデオカメラ、パソコン、ワープ
ロ、携帯電話等の携帯用小型電子機器などである。The shape of the non-aqueous secondary battery of the present invention can be coin type, box type, paper type, card type, etc.
Applications include small portable electronic devices such as video cameras, personal computers, word processors, and mobile phones.
【００２２】[0022]
【実施例】以下、実施例、比較例をあげて更に具体的に
本発明を説明する。The present invention will be described more specifically with reference to examples and comparative examples.
【００２３】〔実施例１〜３〕〔比較例１〕 市販のＳｉＯ2粉末と金属Ｓｉ粉末の混合物を反応器内
に充填し、１４００℃以上に加熱しつつ、Ａｒを供給し
てＳｉＯガスを発生させ、そのガスを冷却して生成した
粉末を捕集し、ｘ値が１．０７のＳｉＯｘを得た。得ら
れたＳｉＯｘ粉末を表１に示す量を秤とり、それに対し
て５％フッ酸水溶液を表１に示す容量を添加し、それぞ
れ１５分間攪拌した後濾過した。濾紙上の残留物を純水
１５０ｍｌで濾液が中性を示すまでよく洗浄した。得ら
れた試料の物性を表１に示す。なお、フッ酸処理処理を
行わないものを、比較例１として用いた。[Examples 1 to 3] [Comparative Example 1] A commercially available mixture of SiO 2 powder and metal Si powder was filled in a reactor, and heated to 1400 ° C or more while supplying Ar to supply SiO gas. The generated gas was cooled and the generated powder was collected to obtain SiOx having an x value of 1.07. The obtained SiOx powder was weighed in the amount shown in Table 1, and a 5% aqueous hydrofluoric acid solution was added to the volume shown in Table 1, stirred for 15 minutes and filtered. The residue on the filter paper was thoroughly washed with 150 ml of pure water until the filtrate became neutral. Table 1 shows the physical properties of the obtained sample. In addition, the thing which did not perform the hydrofluoric acid treatment process was used as Comparative Example 1.
【００２４】得られたＳｉＯｘを活物質として用い、ア
セチレンブラック（導電剤）と混合した後、ＰＶＤＦ
（ポリフッ化ビニリデン：結着剤）を含む溶液に分散さ
せてＳｉＯｘ粉末と黒鉛とＰＶＤＦがそれぞれ４５％、
４０％、１５％になるようなスラリーを調製し、それを
銅箔（集電板）に塗布・乾燥して電極を作製した。After using the obtained SiOx as an active material and mixing it with acetylene black (conductive agent),
(Polyvinylidene fluoride: binder) dispersed in a solution containing 45% SiOx powder, graphite and PVDF, respectively.
A slurry was prepared so as to have a concentration of 40% or 15%, and the slurry was applied to a copper foil (current collector) and dried to prepare an electrode.
【００２５】正極として金属リチウムを用い、エチレン
カーボネート／ジメチルカーボネートを１／２の容積比
で混合した溶液に、ＬｉＰＦ6を１モル濃度溶解させた
ものを電解液とし、コイン型電池を作製し、充放電試験
を行った。Using lithium metal as a positive electrode, a solution obtained by dissolving LiPF 6 at a molar concentration of 1/2 of a mixture of ethylene carbonate / dimethyl carbonate at a volume ratio of 1/2 was used as an electrolyte to prepare a coin-type battery. A charge / discharge test was performed.
【００２６】試験条件は、金属リチウムに対し、０−
１．０Ｖ、定電流１．０６Ａ／ｇ（活物質に３ｍｇに対
して３．２ｍＡ）で行った。表１に最大放電容量を示
す。The test conditions were as follows: 0-
The test was performed at 1.0 V and a constant current of 1.06 A / g (3.2 mA for 3 mg of the active material). Table 1 shows the maximum discharge capacity.
【００２７】[0027]
【表１】 [Table 1]
【００２８】[0028]
【発明の効果】本発明によれば、Ｌｉイオンを吸蔵・放
出可能な電極活物質が提供され、さらに、その電極活物
質を用いることで充放電容量が大なる非水系二次電池が
提供される。According to the present invention, an electrode active material capable of occluding and releasing Li ions is provided, and a non-aqueous secondary battery having a large charge / discharge capacity by using the electrode active material is provided. You.
───────────────────────────────────────────────────── フロントページの続き Ｆターム(参考） 4G072 AA50 GG01 GG03 HH01 HH14 JJ18 UU30 5H029 AJ03 AK02 AK03 AK05 AL02 CJ11 HJ02 5H050 AA08 BA17 CA02 CA08 CA09 CA11 CB02 GA14 HA02 ──────────────────────────────────────────────────続 き Continued on the front page F term (reference) 4G072 AA50 GG01 GG03 HH01 HH14 JJ18 UU30 5H029 AJ03 AK02 AK03 AK05 AL02 CJ11 HJ02 5H050 AA08 BA17 CA02 CA08 CA09 CA11 CB02 GA14 HA02
Claims (5)
ることを特徴とするリチウムイオンを吸蔵・放出可能な
電極活物質。1. An electrode active material capable of occluding and releasing lithium ions, wherein the electrode active material comprises SiOx having an x value of less than 1.00.
処理して得られたものであることを特徴とする請求項１
記載の電極活物質。2. The method according to claim 1, wherein said SiOx (x value is less than 2.00) is obtained by hydrofluoric acid treatment.
The electrode active material according to the above.
処理する、ｘ値が１．００未満のＳｉＯｘの製造方法。3. A method for producing SiOx having an x value of less than 1.00, wherein the SiOx (x value is less than 2.00) is treated with hydrofluoric acid.
質が用いられてなることを特徴とする電極。4. An electrode comprising the electrode active material of SiOx according to claim 1 or 2.
を特徴とする非水系二次電池。5. A non-aqueous secondary battery using the electrode according to claim 4.
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| JP2000230470A JP2002042809A (en) | 2000-07-31 | 2000-07-31 | Non-aqueous secondary battery |
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|---|---|---|---|
| JP2000230470A JP2002042809A (en) | 2000-07-31 | 2000-07-31 | Non-aqueous secondary battery |
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