JP2004063141A - Nano-composite compound of oxide and carbon, and battery using it - Google Patents
Nano-composite compound of oxide and carbon, and battery using it Download PDFInfo
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- Y02E60/10—Energy storage using 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
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- Y02E60/13—Energy storage using capacitors
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Abstract
Description
【０００１】
【産業の属する技術分野】
本発明は、電池工学上有用な材料として利用できる金属酸化物と炭素との複合化合物の製造法とそれを用いた電池に関するものである。
【０００２】
【従来の技術】
小形携帯電子機器、電気自動車の電源等には、高エネルギー密度化かつ高出力密度化が望まれる。現在、金属酸化物を電極材料として用いた電気化学キャパシタと呼ばれる新しいタイプのエネルギーデバイスが注目されている。金属酸化物系材料には一連の貴金属・弁金属・遷移金属・リチウム遷移金属の酸化物がエネルギー貯蔵材料として用いられている。これらのうちで弁金属は電解キャパシタ材料として使用され、その他の金属は電気化学キャパシタや種々の電池の電極材料として使用されている。
【０００３】
金属酸化物を電池に用いた場合には、電極の導電性を保つためには、通常炭素と均一に混ぜて製膜する必要がある。現在の技術としては、通常機械的な混合方法が使われている。この場合、炭素材や金属酸化物の凝集により、特に微細粒子に対して均一な混合は難しいのである。本発明者らは、水溶液とマンガン化合物とを共沈することによって均一化合物を生成する方法を報告している（特開２００１−３１６２００、発明の名称「マンガン酸化物単結晶粒子およびその製造法」）。
【０００４】
【発明が解決しようとする課題】
本発明は、炭素と混合した金属化合物の熱分解反応を利用して、金属酸化物と炭素との均一ナノサイズ複合化合物の調製法、また製造した複合化合物を電池などのデバイスに用いる技術の提供を目的としている。
【０００５】
【課題を解決するための手段】
本発明は、金属化合物、その水和物、またはその溶液と炭素とを混合し加熱することによって生成する酸化物と炭素のナノ複合化合物を要旨としている。
【０００６】
二種類以上の金属化合物、その水和物、またはその溶液を用いたものであり、その場合、本発明は、二種類以上の金属化合物、その水和物、またはその溶液と炭素とを混合し加熱することによって生成する酸化物と炭素のナノ複合化合物である。
【０００７】
目的の化合物によって加熱する際の雰囲気を制御しており、その場合、本発明は、金属化合物、必要に応じ二種類以上の金属化合物、その水和物、またはその溶液と炭素とを混合し、目的の化合物によって加熱する際の雰囲気を制御して加熱することによって生成する酸化物と炭素のナノ複合化合物である。
【０００８】
比表面積の異なった炭素材を用いることによって組成、形状および／または粒子サイズが制御されており、その場合、本発明は、金属化合物、必要に応じ二種類以上の金属化合物、その水和物、またはその溶液と炭素とを混合し加熱する、好ましくは目的の化合物によって加熱する際の雰囲気を制御して加熱することによって、比表面積の異なった炭素材を用いることによって組成、形状および／または粒子サイズが制御されることによって生成する酸化物と炭素のナノ複合化合物である。
【０００９】
また、本発明は、上記のいずれかのナノ複合化合物を用いたリチウム二次電池やキャパシタなどのデバイスを要旨としている。
【００１０】
【発明の実施の形態】
本発明は、ナノサイズの金属酸化物と炭素との複合化合物、およびこの複合化合物を用いる電池やキャパシタに関するものである。
また、本発明は、炭素材と金属化合物とを混合し、炭素材分解しない温度下で金属化合物を分解させて生成する金属酸化物と炭素材の製造法、及びこの複合化合物を用いた電極を使用する電池の製造技術である。
【００１１】
低温で分解する金属塩が硝酸塩や炭酸塩、水酸化物、又はこれらの混合塩であり、その場合、本発明は、これらの化合物を炭素材と混合し、炭素材を分解せず、用いた金属硝酸塩や炭酸塩、水酸化物またはその混合物を分解し金属酸化物に相変化することによって、金属酸化物と炭素材との複合化合物の製造法である。さらに、この複合化合物を製膜することによって作成する電池の製造法である。
【００１２】
炭素化合物を分解せず金属化合物を分解するには、炭素材の種類にもよるが一般に６００℃以下の温度を制御することができるが、真空や不活性ガス雰囲気の制御下で進行することができる。その場合、本発明は、低温で分解する金属塩、より具体的には硝酸マンガン、硝酸コバルトや硝酸ニッケル、硝酸クロムなどと炭素材たとえばアセチレンブラックと混合した後空気中あるいは雰囲気制御した環境化でこれらの金属塩の分解反応を進行させる製造法である。
【００１３】
二種類以上の塩を使用する場合には、予め金属硝酸塩や炭酸塩、水酸化物やその水和物、あるいは溶液を混合し作成した混合物と炭素材とを混合し、又は金属硝酸塩や炭酸塩、水酸化物やその水和物、あるいは溶液と炭素材とを所定量で混合し、反応場に導入することによって金属酸化物と炭素との複合化合物を生成させており、その場合、本発明は、二種類以上の分解性金属塩と炭素材とを、４５０℃以下、又は雰囲気制御した反応場に導入して分解反応を進行させて複合化合物を生成させる金属酸化物と炭素材との複合化合物製造法である。
【００１４】
〔原料化合物〕
原料化合物としての金属化合物は、いずれも公知のものが使用できるが、低温や不活性ガス環境で分解する塩でなければならない。例えば、リチウム、マンガン、コバルトなどの硝酸塩や炭酸塩、水酸化物などが挙げられる。
【００１５】
〔生成物の組成や形態制御〕
生成物の組成は原料化合物の種類を選択することによって制御できる他、加熱温度や雰囲気などのコントロールで制御できるたとえば、Ｍｎ（ＮＯ３）２を用いてＭｎＯ２と炭素との複合化合物を調製する場合には、４５０℃以下の比較的に低温が好ましいことに対して、同様な系で真空下で分解反応を進行させるとより低温化で進行することができる。反応場または炭素の選択によって微細のナノサイズ粒子からミクロオーダサイズの結晶までの調製が可能になる。
【００１６】
〔加熱温度〕
複合化合物を得るためには、金属塩あるいは十分に混合したそれらの混合物を加熱すればよい。加熱温度は用いる金属塩の分解温度以上と炭素材を分解する温度以下の間にすればよいが、マンガン、鉄などの遷移金属酸化物の場合には、金属の原子価が温度に大きく影響されるために温度の設定が重要である。
【００１７】
〔雰囲気〕
複合化合物を得るためには、空気中における反応も可能であるが、特定の酸化物を得るためには酵素分圧を制御するのが重要である。雰囲気を制御するには、酸素ガス、窒素ガス、あるいはその混合ガスなどの導入で制御できるが、反応場に酸化−還元性の試薬を添加することによって制御することも可能になる。
【００１８】
【作用】
金属硝酸塩や炭酸塩、水酸化物やその水和物、あるいは溶液を加熱すると、これらの化合物は分解し、酸化物になることが分かっているが、ほとんどの場合には、数十ミクロン以上のサイズの粒子や塊を生成する。
本発明は、金属硝酸塩や炭酸塩、水酸化物やその水和物、あるいは溶液と炭素材とを混合し、これらの化合物を炭素材表面に付着する。その後、加熱分解することによって金属酸化物・炭素材ナノ複合体が得られる。
したがって、使用される炭素材の表面積は重要である。より小さいナノ粒子を得るためには、高い表面積の炭素材を用いることが適当である。
【００１９】
マンガンやコバルト、クロムの硝酸塩は３００℃以下の低温で分解することが知られている。この温度では炭素材の分解がおこらない。したがって、両者の混合物を適当な温度や雰囲気で加熱すると、金属酸化物と炭素材との複合化合物が生成できる。
例えば、マンガンの硝酸塩は２００℃以上加熱すると分解し、二酸化マンガンが生成する。他方の炭素材のアセチレンブラックは４６０℃以上分解するので、２００−４６０℃の間で加熱すると、二酸化マンガン・アセチレンブラックの複合体が得られる。反応場の酸素圧力によっては硝酸マンガンはＭｎ２Ｏ３、Ｍｎ３Ｏ４に分解することができるため、この場合にはＭｎ２Ｏ３、Ｍｎ３Ｏ４とアセチレンブラックの複合体がえられる。
【００２０】
本発明のリチウム二次電池において上記複合化合物を正極活物質として使用する。正極の作成は、従来法と同様であるが、本複合化合物には炭素材が含んでいるため、導電材の添加は不要である。
一方、負極は活物質としては、リチウムイオンを吸蔵、放出しうる物質であれば特に制限されず、例えば、金属リチウム、リチウム−アルミニウム、リチウム−水銀、リチウム−鉛、リチウム−錫、ウッド合金などのリチウム合金、ポリアセチレン、グラファイトなどの炭素化合物とリチウムの複合体などが上げることができる。
さらに、電解質としては、従来リチウム電池に使用されるものであれば特に制限はない。
【００２１】
【実施例】
本願発明の詳細を実施例で説明する。本願発明はこれら実施例によって何ら限定されるものではない。
【００２２】
実施例１
Ｍｎ（ＮＯ３）２・６Ｈ２Ｏ（液体状、１１．５ｇ）と１ｇのアセチレンブラックとをよく混合し、３２０℃で８時間加熱した。加熱終了後、複合化合物が得られる。
得られる複合化合物は、１００ｎｍ程度以下のの粒子である（図１）。炭素材とマンガン酸化物粒子の区別がつかない。ＴＥＭ観察から、アセチレンブラックとマンガン酸化物との結合は確認できる。
【００２３】
実施例２
実施例１で得られた複合化合物とテフロン（登録商標）繊維との混合した後、成型し正極を作成した。リチウム金属を負極にし、電解質として１Ｍ ＬｉＰＦ６／ＥＣ＋ＤＥＣ（１：１）を用いてコイン型電池を作成した。電池の充放電は４．９−１．２Ｖで行った。
一回目の放電は３２０ｍＡｈ／ｇの高い容量を得た（図２）。また２０までは安定なサイクル特性を示した。
【００２４】
比較例１
Ｍｎ（ＮＯ３）２・６Ｈ２Ｏを３２０℃で８時間加熱した。得られた生成物はβ−ＭｎＯ２であり、ＳＥＭ写真から５マイクロメーター以上の粒子であることが分かる（図３）。
【００２５】
【発明の効果】
電池工学上有用な材料として利用できるマンガン酸化物・アセチレンブラックナノ複合化合物を提供することができる。
【図面の簡単な説明】
【図１】ＭｎＯ２・アセチレンブラック複合化合物
【図２】一回目の放電曲線と２０回目までの充放電曲線
【図３】Ｍｎ（ＮＯ３）２・６Ｈ２Ｏの熱分解で得られた二酸化マンガン[0001]
[Technical field to which industry belongs]
The present invention relates to a method for producing a composite compound of metal oxide and carbon, which can be used as a useful material in battery engineering, and a battery using the same.
[0002]
[Prior art]
2. Description of the Related Art High power density and high output density are desired for power supplies of small portable electronic devices and electric vehicles. At present, a new type of energy device called an electrochemical capacitor using a metal oxide as an electrode material has attracted attention. A series of noble metal, valve metal, transition metal, and lithium transition metal oxides are used as energy storage materials as metal oxide-based materials. Of these, valve metals are used as electrolytic capacitor materials, and other metals are used as electrode materials for electrochemical capacitors and various batteries.
[0003]
When a metal oxide is used for a battery, it is usually necessary to uniformly mix it with carbon to form a film in order to maintain the conductivity of the electrode. Current technology usually employs a mechanical mixing method. In this case, it is difficult to uniformly mix fine particles in particular due to aggregation of the carbon material and the metal oxide. The present inventors have reported a method for producing a homogeneous compound by coprecipitating an aqueous solution and a manganese compound (Japanese Patent Application Laid-Open No. 2001-316200, entitled "Mn Manganese Oxide Single Crystal Particles and Method for Producing the Same"). ).
[0004]
[Problems to be solved by the invention]
The present invention provides a method for preparing a uniform nanosized composite compound of a metal oxide and carbon by utilizing a thermal decomposition reaction of a metal compound mixed with carbon, and a technique for using the manufactured composite compound for a device such as a battery. It is an object.
[0005]
[Means for Solving the Problems]
The gist of the present invention is a nanocomposite compound of oxide and carbon generated by mixing and heating a metal compound, a hydrate thereof, or a solution thereof and carbon.
[0006]
Two or more metal compounds, hydrates thereof, or a solution thereof is used.In this case, the present invention provides a method of mixing two or more metal compounds, hydrates, or solutions thereof with carbon. This is a nanocomposite compound of oxide and carbon generated by heating.
[0007]
The atmosphere at the time of heating by the target compound is controlled, in which case, the present invention, a metal compound, two or more kinds of metal compounds as required, a hydrate thereof, or a solution thereof and a mixture of carbon, This is a nanocomposite compound of oxide and carbon generated by heating while controlling the atmosphere when heating with a target compound.
[0008]
The composition, shape and / or particle size are controlled by using carbon materials having different specific surface areas. In this case, the present invention relates to a metal compound, if necessary, two or more metal compounds, a hydrate thereof, Or by mixing and heating the solution and carbon, preferably by controlling and heating the atmosphere when heating with the target compound, by using carbon materials having different specific surface areas, by using compositions, shapes and / or particles. This is a nanocomposite compound of oxide and carbon generated by controlling the size.
[0009]
The present invention also provides a device such as a lithium secondary battery or a capacitor using any of the above nanocomposite compounds.
[0010]
BEST MODE FOR CARRYING OUT THE INVENTION
The present invention relates to a composite compound of a nano-sized metal oxide and carbon, and a battery and a capacitor using the composite compound.
Further, the present invention provides a method for producing a metal oxide and a carbon material produced by mixing a carbon material and a metal compound and decomposing the metal compound at a temperature at which the carbon material does not decompose, and an electrode using the composite compound. This is the battery manufacturing technology to be used.
[0011]
The metal salt that decomposes at a low temperature is nitrate, carbonate, hydroxide, or a mixed salt thereof.In this case, the present invention uses these compounds by mixing these compounds with a carbon material without decomposing the carbon material. This is a method for producing a composite compound of a metal oxide and a carbon material by decomposing a metal nitrate, a carbonate, a hydroxide or a mixture thereof and changing the phase to a metal oxide. Further, the present invention relates to a method for producing a battery formed by forming a film of the composite compound.
[0012]
In order to decompose the metal compound without decomposing the carbon compound, it is generally possible to control a temperature of 600 ° C. or lower depending on the type of the carbon material, but it is possible to proceed under control of a vacuum or an inert gas atmosphere. it can. In this case, the present invention provides a method of mixing a metal salt that decomposes at a low temperature, more specifically, manganese nitrate, cobalt nitrate, nickel nitrate, chromium nitrate, and the like with a carbon material such as acetylene black, and then in an air or atmosphere-controlled environment. This is a production method in which the decomposition reaction of these metal salts proceeds.
[0013]
When using two or more kinds of salts, a metal nitrate or carbonate, a hydroxide or a hydrate thereof, or a mixture prepared by mixing a solution and a carbon material are mixed, or a metal nitrate or carbonate is used. A composite compound of metal oxide and carbon is produced by mixing a predetermined amount of a hydroxide or a hydrate thereof, or a solution and a carbon material, and introducing the mixture into a reaction field. Is a composite of a metal oxide and a carbon material, in which two or more types of decomposable metal salts and a carbon material are introduced into a reaction field at 450 ° C. or lower, or in an atmosphere-controlled state, and the decomposition reaction proceeds to form a composite compound. This is a method for producing a compound.
[0014]
(Raw material compound)
As the metal compound as a raw material compound, any known metal compound can be used, but it must be a salt that decomposes at low temperature or in an inert gas environment. For example, nitrates, carbonates, hydroxides and the like of lithium, manganese, cobalt and the like can be mentioned.
[0015]
(Product composition and morphology control)
The composition of the product can be controlled by selecting the type of the raw material compound, and can be controlled by controlling the heating temperature, atmosphere, and the like. For example, a composite compound of MnO 2 and carbon is prepared using Mn (NO 3 ) 2. In such a case, a relatively low temperature of 450 ° C. or lower is preferable, whereas the decomposition reaction can be performed at a lower temperature by performing the decomposition reaction in a similar system under vacuum. The choice of reaction field or carbon allows the preparation of fine nano-sized particles to micro-ordered crystals.
[0016]
〔Heating temperature〕
In order to obtain a composite compound, the metal salt or a sufficiently mixed mixture thereof may be heated. The heating temperature may be between the decomposition temperature of the metal salt used and the temperature at which the carbon material is decomposed, but in the case of transition metal oxides such as manganese and iron, the valence of the metal is greatly affected by the temperature. Therefore, setting the temperature is important.
[0017]
〔atmosphere〕
In order to obtain a composite compound, a reaction in air is possible, but in order to obtain a specific oxide, it is important to control the partial pressure of the enzyme. The atmosphere can be controlled by introducing oxygen gas, nitrogen gas, or a mixture thereof, but can also be controlled by adding an oxidizing / reducing reagent to the reaction field.
[0018]
[Action]
Heating metal nitrates and carbonates, hydroxides and their hydrates, or solutions has been shown to decompose these compounds into oxides, but in most cases, these compounds are tens of microns or larger. Generates particles and clumps of size.
According to the present invention, a metal nitrate or carbonate, a hydroxide or a hydrate thereof, or a solution is mixed with a carbon material, and these compounds are attached to the surface of the carbon material. Thereafter, the resultant is thermally decomposed to obtain a metal oxide / carbon material nanocomposite.
Therefore, the surface area of the carbon material used is important. In order to obtain smaller nanoparticles, it is appropriate to use a carbon material having a high surface area.
[0019]
It is known that manganese, cobalt, and chromium nitrates decompose at a low temperature of 300 ° C. or less. At this temperature, decomposition of the carbon material does not occur. Therefore, when a mixture of the two is heated at an appropriate temperature or atmosphere, a composite compound of a metal oxide and a carbon material can be produced.
For example, manganese nitrate decomposes when heated to 200 ° C. or higher, producing manganese dioxide. Acetylene black, which is the other carbon material, decomposes at 460 ° C. or higher, so that when heated between 200 and 460 ° C., a manganese dioxide / acetylene black composite is obtained. Manganese nitrate can be decomposed into Mn 2 O 3 and Mn 3 O 4 depending on the oxygen pressure in the reaction field. In this case, a composite of Mn 2 O 3 , Mn 3 O 4 and acetylene black is obtained.
[0020]
The composite compound is used as a positive electrode active material in the lithium secondary battery of the present invention. The preparation of the positive electrode is the same as that of the conventional method, but since the composite compound contains a carbon material, it is not necessary to add a conductive material.
On the other hand, the negative electrode is not particularly limited as an active material as long as it can absorb and release lithium ions, and examples thereof include metal lithium, lithium-aluminum, lithium-mercury, lithium-lead, lithium-tin, and wood alloy. And a composite of lithium with a carbon compound such as a lithium alloy, polyacetylene, and graphite.
Further, the electrolyte is not particularly limited as long as it is conventionally used for lithium batteries.
[0021]
【Example】
Examples of the present invention will be described in detail. The present invention is not limited by these examples.
[0022]
Example 1
Mn (NO 3 ) 2 .6H 2 O (liquid, 11.5 g) and 1 g of acetylene black were mixed well and heated at 320 ° C. for 8 hours. After the completion of the heating, a composite compound is obtained.
The resulting composite compound is particles having a size of about 100 nm or less (FIG. 1). Indistinguishable between carbon material and manganese oxide particles. From the TEM observation, the bond between acetylene black and manganese oxide can be confirmed.
[0023]
Example 2
After mixing the composite compound obtained in Example 1 with Teflon (registered trademark) fiber, the mixture was molded to form a positive electrode. A coin-type battery was prepared using lithium metal as a negative electrode and 1M LiPF 6 / EC + DEC (1: 1) as an electrolyte. The battery was charged and discharged at 4.9-1.2V.
The first discharge obtained a high capacity of 320 mAh / g (FIG. 2). Up to 20, stable cycle characteristics were exhibited.
[0024]
Comparative Example 1
Mn (NO 3 ) 2 .6H 2 O was heated at 320 ° C. for 8 hours. The obtained product is β-MnO 2 , and it can be seen from the SEM photograph that the product is particles of 5 micrometers or more (FIG. 3).
[0025]
【The invention's effect】
A manganese oxide / acetylene black nanocomposite compound that can be used as a useful material in battery engineering can be provided.
[Brief description of the drawings]
FIG. 1 is a MnO 2 .acetylene black composite compound. FIG. 2 is a first discharge curve and a charge / discharge curve up to 20 times. FIG. 3 is a dioxide obtained by thermal decomposition of Mn (NO 3 ) 2 .6H 2 O. manganese
Claims (5)
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| JP2002216926A JP4365071B2 (en) | 2002-07-25 | 2002-07-25 | Nanocomposite compound of oxide and carbon, and battery using the same |
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| JP2002216926A JP4365071B2 (en) | 2002-07-25 | 2002-07-25 | Nanocomposite compound of oxide and carbon, and battery using the same |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005260006A (en) * | 2004-03-11 | 2005-09-22 | Kri Inc | Capacitor and its manufacturing method |
| JP2012006821A (en) * | 2010-06-24 | 2012-01-12 | Samsung Electro-Mechanics Co Ltd | Lithium manganese oxide-carbon nanocomposite, and method for producing the same |
| JP2012209032A (en) * | 2011-03-29 | 2012-10-25 | Toray Ind Inc | Metal compound-conductive agent complex, lithium secondary battery using the same, and metal compound-conductive agent complex manufacturing method |
| JP2013537358A (en) * | 2010-09-20 | 2013-09-30 | エルジー・ケム・リミテッド | High capacity positive electrode active material with improved conductivity and non-aqueous electrolyte secondary battery including the same |
-
2002
- 2002-07-25 JP JP2002216926A patent/JP4365071B2/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005260006A (en) * | 2004-03-11 | 2005-09-22 | Kri Inc | Capacitor and its manufacturing method |
| JP2012006821A (en) * | 2010-06-24 | 2012-01-12 | Samsung Electro-Mechanics Co Ltd | Lithium manganese oxide-carbon nanocomposite, and method for producing the same |
| JP2013537358A (en) * | 2010-09-20 | 2013-09-30 | エルジー・ケム・リミテッド | High capacity positive electrode active material with improved conductivity and non-aqueous electrolyte secondary battery including the same |
| US9214664B2 (en) | 2010-09-20 | 2015-12-15 | Lg Chem, Ltd. | Cathode active material with high capacity and improved conductivity and non-aqueous electrolyte secondary battery comprising the same |
| JP2012209032A (en) * | 2011-03-29 | 2012-10-25 | Toray Ind Inc | Metal compound-conductive agent complex, lithium secondary battery using the same, and metal compound-conductive agent complex manufacturing method |
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| JP4365071B2 (en) | 2009-11-18 |
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