JP4365071B2 - Nanocomposite compound of oxide and carbon, and battery using the same - Google Patents
Nanocomposite compound of oxide and carbon, and battery using the same Download PDFInfo
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- JP4365071B2 JP4365071B2 JP2002216926A JP2002216926A JP4365071B2 JP 4365071 B2 JP4365071 B2 JP 4365071B2 JP 2002216926 A JP2002216926 A JP 2002216926A JP 2002216926 A JP2002216926 A JP 2002216926A JP 4365071 B2 JP4365071 B2 JP 4365071B2
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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
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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
- Y02E60/13—Energy storage using capacitors
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 that can be used as a material useful in battery engineering, and a battery using the same.
[0002]
[Prior art]
High energy density and high output density are desired for power sources of small portable electronic devices and electric vehicles. Currently, 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 for metal oxide materials. Among 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 in a battery, it is usually necessary to form a film that is uniformly mixed with carbon in order to maintain the conductivity of the electrode. As the current technology, a mechanical mixing method is usually used. In this case, due to the aggregation of the carbon material and the metal oxide, it is particularly difficult to uniformly mix the fine particles. The present inventors have reported a method for producing a homogeneous compound by coprecipitation of an aqueous solution and a manganese compound (Japanese Patent Laid-Open No. 2001-316200, title of invention “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 nano-sized composite compound of metal oxide and carbon using a thermal decomposition reaction of a metal compound mixed with carbon, and a technique for using the manufactured composite compound in a device such as a battery. It is an object.
[0005]
[Means for Solving the Problems]
The gist of the present invention is an oxide-carbon nanocomposite compound produced by mixing and heating a metal compound, a hydrate thereof, or a solution thereof and carbon.
[0006]
Two or more types of metal compounds, hydrates thereof, or solutions thereof are used, and in this case, the present invention mixes two or more types of metal compounds, hydrates thereof, or solutions thereof with carbon. It is a nanocomposite compound of oxide and carbon produced by heating.
[0007]
The atmosphere at the time of heating is controlled by the target compound, and in this case, the present invention mixes a metal compound, if necessary, two or more kinds of metal compounds, hydrates thereof, or a solution thereof and carbon, It is an oxide and carbon nanocomposite compound produced by controlling the atmosphere when heated by the 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 provides a metal compound, two or more kinds of metal compounds as necessary, hydrates thereof, Alternatively, by mixing and heating the solution and carbon, preferably by controlling the atmosphere when heating with the target compound, the composition, shape and / or particles are obtained by using carbon materials having different specific surface areas. It is an oxide and carbon nanocomposite compound produced by controlling the size.
[0009]
In addition, the gist of the present invention is a device such as a lithium secondary battery or a capacitor using any one of the above nanocomposite compounds.
[0010]
DETAILED DESCRIPTION OF THE INVENTION
The present invention relates to a composite compound of nano-sized metal oxide and carbon, and a battery and a capacitor using the composite compound.
In addition, 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 is not decomposed, and an electrode using the composite compound. This is the manufacturing technology of the battery 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 was used without mixing the carbon material and 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, carbonate, hydroxide or a mixture thereof and changing the phase into a metal oxide.
Furthermore, it is a manufacturing method of the battery produced by forming this complex compound into a film.
[0012]
In order to decompose the metal compound without decomposing the carbon compound, although it can be controlled generally at a temperature of 600 ° C. or less depending on the type of the carbon material, it may proceed under the control of a vacuum or an inert gas atmosphere. it can. In that case, the present invention is a metal salt that decomposes at a low temperature, more specifically, in an environment controlled in air or atmosphere after mixing with manganese nitrate, cobalt nitrate, nickel nitrate, chromium nitrate, etc. and a carbon material such as acetylene black. This is a production method in which the decomposition reaction of these metal salts proceeds.
[0013]
When two or more kinds of salts are used, 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 mixed. In addition, a composite compound of a 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 kinds of decomposable metal salts and a carbon material are introduced into a reaction field of 450 ° C. or lower, or an atmosphere is controlled, and a decomposition reaction proceeds to generate a composite compound. It is a compound manufacturing method.
[0014]
[Raw compound]
Any known metal compound can be used as the raw material compound, but it must be a salt that decomposes at a low temperature or in an inert gas environment. For example, nitrates, carbonates, hydroxides, etc. of lithium, manganese, cobalt, etc. are mentioned.
[0015]
[Product composition and morphology control]
The composition of the product can be controlled by selecting the type of raw material compound, and can be controlled by controlling the heating temperature, atmosphere, etc. For example, a composite compound of MnO 2 and carbon is prepared using Mn (NO 3 ) 2 In some cases, a relatively low temperature of 450 ° C. or lower is preferable, but if the decomposition reaction is allowed to proceed in a similar system under vacuum, it can proceed at a lower temperature. The choice of reaction field or carbon allows the preparation of fine nano-sized particles to micro-order sized crystals.
[0016]
〔Heating temperature〕
In order to obtain a composite compound, a metal salt or a sufficiently mixed mixture may be heated. The heating temperature may be between the decomposition temperature of the metal salt used and the temperature below the decomposition temperature of the carbon material. In the case of transition metal oxides such as manganese and iron, the valence of the metal is greatly affected by the temperature. Therefore, the temperature setting is important.
[0017]
〔atmosphere〕
In order to obtain a complex compound, a reaction in air is possible, but in order to obtain a specific oxide, it is important to control the enzyme partial pressure. The atmosphere can be controlled by introducing oxygen gas, nitrogen gas, or a mixed gas 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, these compounds have been shown to decompose and become oxides, but in most cases they are several tens of microns or more. Generate particles and lumps of size.
In the present invention, a metal nitrate, carbonate, hydroxide or hydrate thereof, or a solution and a carbon material are mixed, and these compounds are attached to the surface of the carbon material. Then, a metal oxide / carbon material nanocomposite is obtained by thermal decomposition.
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 with a high surface area.
[0019]
It is known that nitrates of manganese, cobalt, and chromium are decomposed at a low temperature of 300 ° C. or lower. At this temperature, the carbon material does not decompose. Therefore, when the mixture of both is heated at an appropriate temperature or atmosphere, a composite compound of a metal oxide and a carbon material can be generated.
For example, manganese nitrate is decomposed when heated to 200 ° C. or more to produce manganese dioxide. Since the acetylene black of the other carbon material decomposes at 460 ° C. or higher, a composite of manganese dioxide and acetylene black is obtained when heated at 200-460 ° C. Depending on the oxygen pressure in the reaction field, manganese nitrate can be decomposed into Mn 2 O 3 and Mn 3 O 4. In this case, a complex of Mn 2 O 3 , Mn 3 O 4 and acetylene black is obtained.
[0020]
In the lithium secondary battery of the present invention, the composite compound is used as a positive electrode active material. The production of the positive electrode is the same as in 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 long as it is a material capable of occluding and releasing lithium ions. For example, metallic lithium, lithium-aluminum, lithium-mercury, lithium-lead, lithium-tin, wood alloy, etc. A lithium alloy, a polyacetylene, a carbon composite such as graphite, and a lithium complex can be raised.
Further, the electrolyte is not particularly limited as long as it is conventionally used for lithium batteries.
[0021]
【Example】
The details of the present invention will be described in Examples. The present invention is not limited to 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 completion of the heating, a composite compound is obtained.
The obtained composite compound is a particle of about 100 nm or less (FIG. 1). Indistinguishable between carbon and manganese oxide particles. From the TEM observation, the bond between acetylene black and manganese oxide can be confirmed.
[0023]
Example 2
The composite compound obtained in Example 1 and Teflon (registered trademark) fiber were mixed, and then molded to prepare 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 showed stable cycle characteristics.
[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 particles are 5 micrometers or more (FIG. 3).
[0025]
【The invention's effect】
It is possible to provide a manganese oxide / acetylene black nanocomposite compound that can be used as a material useful in battery engineering.
[Brief description of the drawings]
FIG. 1 MnO 2 .acetylene black composite compound FIG. 2 First discharge curve and charge / discharge curve up to 20th FIG. 3 Dioxide obtained by thermal decomposition of Mn (NO 3 ) 2 · 6H 2 O manganese
Claims (5)
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| KR101153480B1 (en) * | 2010-06-24 | 2012-06-11 | 연세대학교 산학협력단 | A lithium manganese oxide-carbon nano composite and a fabricating method thereof |
| KR101337365B1 (en) * | 2010-09-20 | 2013-12-05 | 주식회사 엘지화학 | Cathode Active Material with High Capacity and Improved Conductivity and Non-aqueous Electrolyte Secondary Battery Comprising the Same |
| JP5664404B2 (en) * | 2011-03-29 | 2015-02-04 | 東レ株式会社 | Metal compound-conductive agent composite, lithium secondary battery using the same, and method for producing metal compound-conductive agent composite |
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