JP2013115028A - Molecular cluster ion positive electrode material - Google Patents

Molecular cluster ion positive electrode material Download PDF

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JP2013115028A
JP2013115028A JP2011263333A JP2011263333A JP2013115028A JP 2013115028 A JP2013115028 A JP 2013115028A JP 2011263333 A JP2011263333 A JP 2011263333A JP 2011263333 A JP2011263333 A JP 2011263333A JP 2013115028 A JP2013115028 A JP 2013115028A
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positive electrode
electrode material
periodic table
secondary battery
lithium
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Noriyuki Sonoyama
範之 園山
Shinya Uematsu
信也 上松
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Nagoya Institute of Technology NUC
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Abstract

PROBLEM TO BE SOLVED: To provide a positive electrode material such as a lithium ion secondary battery which is low-cost and has high energy density and furthermore which has superior cycle characteristics.SOLUTION: A positive electrode material contains polyoxometalate represented by chemical formula: A(XMOH)(A: elements in second to fourth periods of group 1 in the periodic table, X: elements in second to fifth periods of group 13 in the periodic table, and M: elements in fourth to sixth periods of groups 5 to 6 in the periodic table).

Description

本発明は、リチウムイオン二次電池等に利用され得る正極材料に関する。   The present invention relates to a positive electrode material that can be used in lithium ion secondary batteries and the like.

近年、携帯電話、ノートパソコン、デジタルカメラ等のポータブル機器用電源として二次電池が広く使用されている。なかでも、コバルト酸リチウム、ニッケル酸リチウム、あるいはマンガン酸リチウム等のリチウム遷移金属酸化物を正極材、黒鉛等の炭素材料を負極材、そしてリチウム化合物を液体有機化合物に溶解した電解質を用いたリチウム二次電池が急速に普及している。 In recent years, secondary batteries have been widely used as power sources for portable devices such as mobile phones, notebook computers, and digital cameras. In particular, lithium using lithium transition metal oxides such as lithium cobaltate, lithium nickelate, or lithium manganate as a positive electrode material, a carbon material such as graphite as a negative electrode material, and an electrolyte in which a lithium compound is dissolved in a liquid organic compound. Secondary batteries are rapidly spreading.

前記リチウムイオン二次電池は、充電時には正極活物質であるリチウム遷移金属酸化物中のリチウムがリチウムイオンとなり負極の炭素層間に入り込み、放電時にはリチウムイオンが炭素層間から離脱して正極に移動して元のリチウム遷移金属酸化物になることにより充放電反応が進行する。このリチウムイオン二次電池は高出力電圧、高エネルギー密度、さらにはメモリー効果がない等、従来のニッケルカドミウム等の二次電池にはない優れた特徴を有している。 In the lithium ion secondary battery, lithium in the lithium transition metal oxide, which is a positive electrode active material, becomes lithium ions during charging and enters the carbon layer of the negative electrode. The charge / discharge reaction proceeds by becoming the original lithium transition metal oxide. This lithium ion secondary battery has excellent features not found in conventional secondary batteries such as nickel cadmium, such as high output voltage, high energy density, and no memory effect.

しかし、リチウムイオン二次電池は、充放電を繰り返すことが可能な回数、すなわち、サイクル寿命については十分なものではなかった。特にエネルギー貯蔵用や電気自動車用の電源としてはサイクル寿命をさらに長くすることが必要であり、高温特性の改善、低コスト化も望まれていた。 However, the lithium ion secondary battery has not been sufficient in terms of the number of times that charge and discharge can be repeated, that is, the cycle life. In particular, as a power source for energy storage and electric vehicles, it is necessary to further increase the cycle life, and improvement in high temperature characteristics and cost reduction have been desired.

特開２００６−１７２７５３号公報JP 2006-172753 A 特開２００７−３３５３３１号公報JP 2007-335331 A 特開２０１１−０２８９９９号公報JP2011-028999A

本発明の課題は、低コストで、高エネルギー密度、さらには優れたサイクル特性を有するリチウムイオン二次電池等の二次電池用正極材を提供することである。 An object of the present invention is to provide a positive electrode material for a secondary battery such as a lithium ion secondary battery that has low cost, high energy density, and excellent cycle characteristics.

本発明者らは鋭意検討を重ねた結果、上記課題を解決する、分子性クラスタ−イオンを有する正極材を見出した。すなわち、本発明によれば以下の正極材が提供される。 As a result of intensive studies, the present inventors have found a positive electrode material having molecular cluster ions that solves the above problems. That is, according to the present invention, the following positive electrode material is provided.

[１]二次電池用正極材であって、化学式がＡ３（ＸＭＯ２４Ｈ６）（Ａ：周期律表第１族の第２〜４周期の元素、Ｘ：周期律表第１３族第２〜５周期の元素、Ｍ：周期律表第５〜６族の第４〜６周期の元素）からなるポリオキソメタレートを含む正極材。 [1] A positive electrode material for a secondary battery, the chemical formula of which is A 3 (XMO 24 H 6 ) (A: elements in groups 2 to 4 of group 1 of the periodic table, X: group 13 of periodic table) A positive electrode material comprising a polyoxometalate composed of an element having 2 to 5 periods, M: an element having 4 to 6 periods in Groups 5 to 6 of the periodic table.

[２]前記化学式において、ＡがＬｉ、Ｎａ、Ｋのいずれか一であり、ＸがＡｌあるいはＧａであり、ＭがＶ、Ｍｏ，Ｎｂのいずれか一である、請求項１に記載の正極材。 [2] The positive electrode according to claim 1, wherein, in the chemical formula, A is any one of Li, Na, and K, X is Al or Ga, and M is any one of V, Mo, and Nb. Wood.

[３]前記二次電池がＬｉイオン二次電池である請求項１または２に記載の正極材。 [3] The positive electrode material according to claim 1 or 2, wherein the secondary battery is a Li ion secondary battery.

本発明のポリオキソメタレートのクラスタ−イオン構造を模式的に示す図である。It is a figure which shows typically the cluster-ion structure of the polyoxometalate of this invention. 本発明の一実施例であるＮａ３ＡｌＭｏ６Ｏ２４Ｈ６のリートベルト解析結果である。A Rietveld analysis result of the Na 3 AlMo 6 O 24 H 6 is one embodiment of the present invention. 本発明の一実施例である、正極にＮａ３ＡｌＭｏ６Ｏ２４Ｈ６を用いた電池の充放電曲線を示す。Which is an embodiment of the present invention, showing a charge-discharge curve of a battery using Na 3 AlMo 6 O 24 H 6 in the positive electrode. 本発明の一実施例である、正極にＮａ３ＧａＭｏ６Ｏ２４Ｈ６を用いた電池の充放電曲線を示す。Which is an embodiment of the present invention, showing a charge-discharge curve of a battery using Na 3 GaMo 6 O 24 H 6 in the positive electrode. 本発明の、正極にＮａ３ＡｌＭｏ６Ｏ２４Ｈ６あるいはＮａ３ＧａＭｏ６Ｏ２４Ｈ６を用いた電池の充放電サイクル特性を示す。The charge / discharge cycle characteristics of a battery using Na 3 AlMo 6 O 24 H 6 or Na 3 GaMo 6 O 24 H 6 for the positive electrode of the present invention are shown.

以下、図面を参照しつつ本発明の実施の形態について説明する。本発明は、以下の実施形態に限定されるものではなく、発明の範囲を逸脱しない限りにおいて、変更、修正、改良を加え得るものである。   Hereinafter, embodiments of the present invention will be described with reference to the drawings. The present invention is not limited to the following embodiments, and changes, modifications, and improvements can be added without departing from the scope of the invention.

本発明のポリオキソメタレート（ＰＯＭ）は周期律表第５族あるいは第６族の遷移金属Ｍ（Ｍ＝Ｖ、Ｍｏ、Ｎｂ等）が形成する分子性クラスターイオンである。ポリオキソメタレートは、第５族あるいは第６族の遷移金属の酸化力を利用した酸化触媒として従来から知られているが、一方では、溶液中で分子単体として安定に存在するため、分子単位でリチウムが脱挿入する機能を有すると考えられ、リチウムイオン二次電池電極材料として期待される。 The polyoxometalate (POM) of the present invention is a molecular cluster ion formed by a transition metal M (M = V, Mo, Nb, etc.) of Group 5 or Group 6 of the periodic table. Polyoxometalates are conventionally known as oxidation catalysts that utilize the oxidizing power of Group 5 or Group 6 transition metals. On the other hand, polyoxometalates are stably present as single molecules in solution. Therefore, it is considered to have a function of removing and inserting lithium, and is expected as a lithium ion secondary battery electrode material.

代表的なポリオキソメタレートとしては、Ｋｅｇｇｉｎ型ポリオキソメタレートが知られているが、クラスタ−イオンユニットの構造安定性が低く、例えばＫｅｇｇｉｎ型ポリオキソモリブデイトであるＫ３ＰＭｏ１２Ｏ４０を正極材とするリチウム二次電池正極特性では急速に容量劣化を生じる。 As a typical polyoxometalate, a Keggin type polyoxometalate is known, but the structural stability of the cluster-ion unit is low. For example, K 3 PMo 12 O 40 which is a Keggin type polyoxomolybdate is used. The positive electrode characteristics of the lithium secondary battery used as the positive electrode material cause rapid capacity deterioration.

本発明では、クラスタ−イオンユニットが密な構造を有し、共有結合性が高く、分子ユニット中の非反応元素割合が高いＡｎｄｅｒｓｏｎ型ポリオキソメタレートが好ましい。ポリオキソメタレートの化学式は、[ＸＭ６Ｏ２４]ｙ−（Ｘは周期律第１５族〜第１６族の第４〜第６周期の元素であり、より具体的には、Ｔｅ５＋、Ｓｂ５＋等である）あるいは[Ｘ’Ｍ６Ｏ２４Ｈ６]Ｚ−（Ｘ’は周期律表第１３族第２〜５周期の元素であり、より具体的にはＡｌ、Ｇａである）。より好ましくは、[Ｘ’Ｍ６Ｏ２４Ｈ６]Ｚ−（Ｘ’は周期律表第１３族第２〜５周期の元素であり、より具体的にはＡｌ、Ｇａである）。なお、Ｍは周期律表第５〜６族の第４〜６周期の元素、より具体的にはＶ、Ｍｏ，Ｎｂである。 In the present invention, an Anderson type polyoxometalate having a dense structure of cluster-ion units, high covalent bonding, and a high proportion of non-reactive elements in the molecular unit is preferable. The chemical formula of polyoxometalate is [XM 6 O 24 ] y− (X is an element of groups 4 to 6 of groups 15 to 16 of the periodic rule, and more specifically, Te 5+ , Sb 5 ), or [X′M 6 O 24 H 6 ] Z− (X ′ is an element of Group 13 to Group 5 of the periodic table, and more specifically, Al and Ga). More preferably, [X′M 6 O 24 H 6 ] Z— (X ′ is an element of Group 13 to Group 2 to Period 5 of the periodic table, and more specifically, Al and Ga). Note that M is an element in the 4th to 6th periods of the 5th to 6th groups of the periodic table, more specifically, V, Mo, Nb.

＜粉末合成＞
Ａｎｄｅｒｓｏｎ型ポリオキソメタレートの粉末合成、および比較としてＫｅｇｇｉｎ型ポリオキソメタレートの粉末合成は以下の様に行った。
（実施例１：Na3[AlMo6O24H6]・7H2Oの合成）
モリブデン酸ナトリウム3.5 gと塩化アルミニウム0.8290 gを25 mlの水に溶解させ、pH=1.8になるまでHClを加えた。その後、しばらく加熱撹拌を行い、脱水させることで結晶を得た。その結晶をろ過、洗浄し、80℃で乾燥させた。
（実施例２：Li3[AlMo6O24H6]・7H2Oの合成）
モリブデン酸リチウム5 gと塩化アルミニウム0.4592 gを30 mlの水に溶解させ、pH=3.5になるまでHClを滴下した。しばらく加熱撹拌を行い、水を蒸発させることで結晶を得た。
（比較例：K3PMo12O40の合成）
ケギン型ポリオキソメタレートK3PMo12O40の合成には、市販のH3PMo12O40を蒸留水に溶解させ、塩化カリウムを過剰に加え、析出した沈殿をろ過した。得られた沈殿は、未反応の塩化カリウムを除去するために蒸留水で洗浄し、その後120℃で乾燥させた。 <Powder synthesis>
The powder synthesis of Anderson type polyoxometalate and, as a comparison, the powder synthesis of Keggin type polyoxometalate were carried out as follows.
(Example 1: Synthesis of Na 3 [AlMo 6 O 24 H 6 ] · 7H 2 O)
3.5 g of sodium molybdate and 0.8290 g of aluminum chloride were dissolved in 25 ml of water, and HCl was added until pH = 1.8. Thereafter, the mixture was heated and stirred for a while and dehydrated to obtain crystals. The crystals were filtered, washed and dried at 80 ° C.
(Example 2: Synthesis of Li 3 [AlMo 6 O 24 H 6 ] · 7H 2 O)
5 g of lithium molybdate and 0.4592 g of aluminum chloride were dissolved in 30 ml of water, and HCl was added dropwise until pH = 3.5. Crystals were obtained by heating and stirring for a while and evaporating water.
(Comparative example: Synthesis of K 3 PMo 12 O 40 )
For the synthesis of Keggin type polyoxometalate K 3 PMo 12 O 40 , commercially available H 3 PMo 12 O 40 was dissolved in distilled water, potassium chloride was added in excess, and the deposited precipitate was filtered. The resulting precipitate was washed with distilled water to remove unreacted potassium chloride and then dried at 120 ° C.

これら実施例１、実施例２、および比較例の粉末結晶の同定は、Ｘ線回折（ＸＲＤ）、フーリエ変換赤外線分光硬度計（ＦＴ−ＩＲ）、およびＲａｍａｎ分光法により行った。 The identification of the powder crystals of Example 1, Example 2, and Comparative Example was performed by X-ray diffraction (XRD), Fourier transform infrared spectroscopic hardness meter (FT-IR), and Raman spectroscopy.

<電池作成・評価>
次にポリオキソメタレートの粉末試料を導電材であるアセチレングラックと重量比１：２の割合で混合して外径10 ｍｍ、厚み1 ｍｍの正極合材を用い、負極に外径8 ｍｍ、厚み0.5 ｍｍの金属リチウムから成る負極材、電解液として１Ｍ ＬｉＰＦ６を含むエチレンカーボネート（ＥＣ）とジエチルカーボネート（ＤＥＣ）との混合溶媒（ＥＣ：ＤＥＣ＝３：７体積比）を用いてコイン型電池を作成し、電気化学測定を行った。５０μＡの定電流にて充電あるいは放電した場合の、正極試料の単位重量あたりの電気容量と電池電圧を測定した。 <Battery creation and evaluation>
Next, a powder sample of polyoxometalate was mixed with acetylene rack as a conductive material at a weight ratio of 1: 2, and a positive electrode mixture having an outer diameter of 10 mm and a thickness of 1 mm was used. Coin type using a negative electrode material made of metallic lithium having a thickness of 0.5 mm, and a mixed solvent (EC: DEC = 3: 7 volume ratio) of ethylene carbonate (EC) and diethyl carbonate (DEC) containing 1M LiPF 6 as an electrolyte. A battery was prepared and subjected to electrochemical measurements. The electric capacity and battery voltage per unit weight of the positive electrode sample when charged or discharged at a constant current of 50 μA were measured.

（実施例１）
Ａｎｄｅｒｓｏｎ型ポリオキソメタレートとしてＮａ３ＡｌＭｏ６Ｏ２４Ｈ６粉末を用い、アセチレンブラックとの混合を５００ｒｐｍで１時間、外径５５ｍｍのボールミルで直径１０mmと５mmの2種類のボールを使った混合と、比較として手混ぜ混合を行った。充放電結果を図３に示す。この結果から手混ぜ混合の場合はボールミル混合に比して、充電容量が小さく、また放電時の電圧降下が早いことがわかる。ボールミル混合では充電容量は２８０ｍＡｈ／ｇ以上の大きな値を示した。 Example 1
Using Na 3 AlMo 6 O 24 H 6 powder as Anderson type polyoxometalate, mixing with acetylene black for 1 hour at 500 rpm, mixing using two types of balls of 10 mm and 5 mm in diameter with a 55 mm outer diameter ball mill As a comparison, hand mixing was performed. The charge / discharge results are shown in FIG. From this result, it can be seen that the manual mixing is smaller in charge capacity and the voltage drop during discharging is faster than in the ball mill mixing. In the ball mill mixing, the charging capacity showed a large value of 280 mAh / g or more.

（実施例２）
Ａｎｄｅｒｓｏｎ型ポリオキソメタレートとしてＮａ３ＧａＭｏ６Ｏ２４Ｈ６粉末を用い、アセチレンブラックとの混合を５００ｒｐｍで１時間、外径５５ｍｍのボールミルで直径１０mmと５mmの２種類のボールを使った混合と、比較として手混ぜ混合を行った。充放電結果を図４に示す。実施例２は実施例１とほぼ同様の結果となった。 (Example 2)
Using Na 3 GaMo 6 O 24 H 6 powder as Anderson type polyoxometalate, mixing with acetylene black for 1 hour at 500 rpm, mixing using two types of balls of 10 mm and 5 mm in diameter with a 55 mm outer diameter ball mill As a comparison, hand mixing was performed. The charge / discharge results are shown in FIG. The result of Example 2 was almost the same as that of Example 1.

次に、上記実施例１と２について、１８回の充放電サイクルを行い、容量低下を調べた。比較のため、Ｋｅｇｇｉｎ型ポリオキソメタレートであるＫ３ＰＭｏ１２Ｏ４０を正極材に用いた電池も評価した。Ｋ３ＰＭｏ１２Ｏ４０を正極材に用いると、数サイクルで３０％という大きな容量低下が見られたが、実施例１および実施例２のＡｎｄｅｒｓｏｎ型ポリオキソメタレートを正極に用いた電池では大きな容量低下は見られなかった。 Next, about the said Example 1 and 2, the charging / discharging cycle of 18 times was performed and the capacity | capacitance fall was investigated. For comparison, a battery using K 3 PMo 12 O 40 , which is a Keggin type polyoxometalate, as a positive electrode material was also evaluated. When K 3 PMo 12 O 40 was used as the positive electrode material, a large capacity reduction of 30% was observed in several cycles, but the battery using the Anderson type polyoxometalate of Example 1 and Example 2 as the positive electrode was large. There was no decrease in capacity.

本発明のＡｎｄｅｒｓｏｎ型ポリオキソメタレートは二次電池正極材に利用することができる。
The Anderson type polyoxometalate of the present invention can be used for a positive electrode material for a secondary battery.

Claims (3)

二次電池用正極材であって、化学式がＡ３（ＸＭＯ２４Ｈ６）（Ａ：周期律表第１族の第２〜４周期の元素、Ｘ：周期律表第１３族第２〜５周期の元素、Ｍ：周期律表第５〜６族の第４〜６周期の元素、）からなるポリオキソメタレートを含む正極材。 A positive electrode material for a secondary battery, the chemical formula of which is A 3 (XMO 24 H 6 ) (A: Elements in Groups 2 to 4 of Group 1 of the Periodic Table, X: Groups of Groups 13 to 5 in Periodic Table) A positive electrode material comprising a polyoxometalate comprising a periodic element, M: an element of the 4th to 6th period of the 5th to 6th groups of the periodic table. 前記化学式において、ＡがＬｉ，Ｎａ、Ｋのいずれか一であり、ＸがＡｌあるいはＧａであり、ＭがＶ、Ｍｏ，Ｎｂのいずれか一である、請求項１に記載の正極材。 The positive electrode material according to claim 1, wherein in the chemical formula, A is any one of Li, Na, and K, X is Al or Ga, and M is any one of V, Mo, and Nb. 前記二次電池がＬｉイオン二次電池である請求項１または２に記載の正極材。 The positive electrode material according to claim 1, wherein the secondary battery is a Li ion secondary battery.
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CN106159257A (en) * 2015-04-13 2016-11-23 惠州市豪鹏科技有限公司 A kind of positive electrode active materials and preparation method thereof, positive plate and lithium ion battery
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Publication number Priority date Publication date Assignee Title
CN106159257A (en) * 2015-04-13 2016-11-23 惠州市豪鹏科技有限公司 A kind of positive electrode active materials and preparation method thereof, positive plate and lithium ion battery
CN106159261A (en) * 2015-04-13 2016-11-23 惠州市豪鹏科技有限公司 The preparation method of a kind of positive electrode active materials, positive plate and lithium ion battery
CN106159257B (en) * 2015-04-13 2018-08-17 惠州市豪鹏科技有限公司 A kind of positive electrode active materials and preparation method thereof, positive plate and lithium ion battery
CN105957995A (en) * 2016-06-18 2016-09-21 清华大学 Potassium polyoxometalate ceramic membrane for lithium-ion battery
CN106099016A (en) * 2016-06-18 2016-11-09 清华大学 A kind of lithium ion battery multi-metal oxygen acid sodium-salt ceramic diaphragm
CN112582611A (en) * 2019-09-29 2021-03-30 中国科学院大连化学物理研究所 Application of polyacid oxide NVO in positive electrode of lithium-sulfur battery
CN112582611B (en) * 2019-09-29 2021-10-15 中国科学院大连化学物理研究所 Application of polyacid oxide NVO in positive electrode of lithium-sulfur battery

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