JP3441765B2 - Method for forming positive electrode active material layer - Google Patents
Method for forming positive electrode active material layerInfo
- Publication number
- JP3441765B2 JP3441765B2 JP16530293A JP16530293A JP3441765B2 JP 3441765 B2 JP3441765 B2 JP 3441765B2 JP 16530293 A JP16530293 A JP 16530293A JP 16530293 A JP16530293 A JP 16530293A JP 3441765 B2 JP3441765 B2 JP 3441765B2
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- JP
- Japan
- Prior art keywords
- active material
- positive electrode
- electrode active
- material layer
- aqueous solution
- Prior art date
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Classifications
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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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- Cell Electrode Carriers And Collectors (AREA)
- Battery Electrode And Active Subsutance (AREA)
Description
【発明の詳細な説明】Detailed Description of the Invention
【０００１】[0001]
【産業上の利用分野】本発明は電池の正極活物質層を形
成する方法に関するものである。TECHNICAL FIELD The present invention relates to a method for forming a positive electrode active material layer of a battery.
【０００２】[0002]
【従来の技術】リチウム電池等の薄型電池では、非プロ
トン溶媒等を電解液として用い、Ｖ２Ｏ５ ・ｎＨ２
Ｏ等のキセロゲルを正極活物質層として用いている。こ
の種の電池の正極活物質層は、Ｖ２ Ｏ５ 等の水溶性
活物質を溶解した水溶液を正極集電体に塗布してから、
これを乾燥して形成する。図４はこのようにして形成さ
れた正極活物質層の部分断面図である。この図に示すよ
うに正極活物質層は、活物質相互の結合力の強い部分
（層）１と結合力の弱い部分即ち層間部２とが規則的に
交互に現れる多層構造を有している。結合力の弱い層間
部２からリチウムイオン等の負極活物質イオンが侵入し
て正極活物質と反応することにより放電が行われる。2. Description of the Related Art In thin batteries such as lithium batteries, an aprotic solvent or the like is used as an electrolytic solution, and V 2 O 5 .nH 2
Xerogel such as O is used as the positive electrode active material layer. For the positive electrode active material layer of this type of battery, after applying an aqueous solution in which a water-soluble active material such as V 2 O 5 is dissolved onto the positive electrode current collector,
It is dried to form. FIG. 4 is a partial cross-sectional view of the positive electrode active material layer thus formed. As shown in this figure, the positive electrode active material layer has a multi-layer structure in which portions (layers) 1 having a strong bonding force between active materials and portions having a weak bonding force, that is, interlayer portions 2 regularly appear. . Discharge is performed by the negative electrode active material ions such as lithium ions penetrating from the interlayer portion 2 having a weak bonding force and reacting with the positive electrode active material.
【０００３】[0003]
【発明が解決しようとする課題】しかしながら従来の方
法で形成された正極活物質層では、結合力の弱い層間部
２の大部分は面方向に延びており、正極活物質層の厚み
方向に延びる層間部２の長さまたは面積は少ない。その
ために負極活物質イオンは正極活物質層内部に十分に拡
散できず、正極活物質の利用率を上げることができない
という問題があった。またこのような正極活物質層で
は、電池の充放電により正極活物質が膨脹、収縮する際
に生じる応力が一つの方向に集中しやすいため、活物質
層内に比較的大きな応力が発生する。そのため、電池に
充放電か繰り返されると、この応力により正極活物質層
が崩壊して電池のサイクル寿命が短くなるという問題が
あった。特に放電の深度が深くなると大幅にサイクル寿
命は短くなる。However, in the positive electrode active material layer formed by the conventional method, most of the interlayer portion 2 having a weak bonding force extends in the plane direction, and extends in the thickness direction of the positive electrode active material layer. The length or area of the interlayer portion 2 is small. Therefore, there is a problem that the negative electrode active material ions cannot be sufficiently diffused into the positive electrode active material layer, and the utilization rate of the positive electrode active material cannot be increased. Further, in such a positive electrode active material layer, the stress generated when the positive electrode active material expands and contracts due to charge and discharge of the battery is likely to concentrate in one direction, so that a relatively large stress occurs in the active material layer. Therefore, when the battery is repeatedly charged and discharged, there is a problem that the positive electrode active material layer collapses due to this stress and the cycle life of the battery is shortened. In particular, the cycle life is significantly shortened as the depth of discharge increases.
【０００４】本発明の目的は、正極活物質の利用率を高
め、しかも正極活物質が膨脹、収縮する際に生じる応力
を緩和して電池のサイクル寿命を延ばすことができる正
極活物質層の形成方法を提供することにある。An object of the present invention is to form a positive electrode active material layer capable of increasing the utilization rate of the positive electrode active material and relaxing the stress generated when the positive electrode active material expands and contracts to extend the cycle life of the battery. To provide a method.
【０００５】[0005]
【課題を解決するための手段】請求項１の発明では、乾
燥するとキセロゲルになる水溶性活物質を含む水溶液を
基体に塗布した後に乾燥して正極活物質層を形成する方
法を対象にして、基体に塗布した水溶性活物質を含む水
溶液が乾燥して規則的な多層構造が形成される前に、該
水溶液に振動を加えて不規則な層構造を形成する。According to a first aspect of the present invention, there is provided a method for forming a positive electrode active material layer by applying an aqueous solution containing a water-soluble active material that becomes a xerogel when dried to a substrate and then drying the applied solution. before the aqueous solution containing the coated water-soluble active material to the substrate is regular multilayer structure by drying is formed, that to form a disordered layer structure by adding a vibration to the <br/> solution.
【０００６】請求項２の発明では、超音波振動により水
溶液に振動を加える。According to the second aspect of the invention, vibration is applied to the aqueous solution by ultrasonic vibration.
【０００７】請求項３の発明では、水溶性活物質として
非晶質五酸化バナジウムを用いる場合に請求項１の発明
の形成方法を適用する。According to the third aspect of the invention, the formation method of the first aspect of the invention is applied when amorphous vanadium pentoxide is used as the water-soluble active material.
【０００８】[0008]
【作用】請求項１の発明によれば、水溶液が乾燥して規
則的な多層構造が形成される前に、水溶液に振動を加え
るので、活物質相互の結合力の強い部分（層）様々な方
向を向いて形成され、その結果、不規則な層構造が形成
される。そのため結合力の弱い層間部が正極活物質層の
厚み方向に延びる率が高くなり、負極活物質イオンの正
極活物質層内部への拡散性が向上する。またこのように
不規則な層構造が形成されると、電池の充放電で正極活
物質層内に生じる応力が分散しやすくなり、電池の充放
電の繰り返しによる正極活物質層の崩壊を抑制すること
ができる。According to the invention of claim 1, since the aqueous solution is vibrated before the aqueous solution is dried to form a regular multilayer structure, various portions (layers) having a strong binding force between the active materials are formed. Formed in a direction, resulting in an irregular layered structure. Therefore, the interlayer portion having a weak bonding force has a high rate of extending in the thickness direction of the positive electrode active material layer, and the diffusion of the negative electrode active material ions into the positive electrode active material layer is improved. Further, when such an irregular layer structure is formed, the stress generated in the positive electrode active material layer during charging and discharging of the battery is easily dispersed, and the collapse of the positive electrode active material layer due to repeated charging and discharging of the battery is suppressed. be able to.
【０００９】請求項２の発明のように超音波振動により
水溶液に振動を加えれば、正極活物質層全体に不規則な
層構造を簡単に形成できる。By vibrating the aqueous solution by ultrasonic vibration as in the second aspect of the invention, an irregular layer structure can be easily formed on the entire positive electrode active material layer.
【００１０】[0010]
【実施例】以下、図面を参照して本発明の形成方法をリ
チウム電池に用いる正極板の五酸化バナジウムキセロゲ
ルからなる正極活物質層を形成する方法に適用した実施
例を詳細に説明する。EXAMPLES Hereinafter, examples in which the forming method of the present invention is applied to a method of forming a positive electrode active material layer made of vanadium pentoxide xerogel of a positive electrode plate used in a lithium battery will be described in detail with reference to the drawings.
【００１１】まず非晶質五酸化バナジウム（Ｖ２ Ｏ
５ ）からなる水溶性活物質３重量％を水に溶解したゾ
ル状またはゲル状の水溶液を作った。次に、この水溶液
をニッケル箔からなる正極集電体（基体）に塗布してか
ら水溶液が乾燥して規則的な多層構造が形成される前
に、該水溶液に超音波発生機の焦点を合わせて該水溶液
に２３ＫＨｚの超音波振動を２５分間加えて不規則な層
構造を形成しながら２５℃の温度で水溶液を乾燥した。
なお、本実施例では２０Ｋ〜２５ＫＨｚの超音波振動を
２０〜３０時間加えながら水溶液を乾燥するのが好まし
い。そして厚み約２０μm の五酸化バナジウムキセロゲ
ル（Ｖ２ Ｏ５ ・ｎＨ２ Ｏ）からなる正極活物質層
を形成した。First, amorphous vanadium pentoxide (V 2 O
5 %) was dissolved in water to prepare a sol-like or gel-like aqueous solution. Next, this aqueous solution is applied to a positive electrode current collector (base) made of nickel foil, and then the aqueous solution is dried to form a regular multilayer structure.
Then, the ultrasonic generator is focused on the aqueous solution, and ultrasonic vibration of 23 KHz is applied to the aqueous solution for 25 minutes to form an irregular layer.
The aqueous solution was dried at a temperature of 25 ° C while forming the structure .
In this example, it is preferable to dry the aqueous solution while applying ultrasonic vibration of 20 K to 25 KHz for 20 to 30 hours. Then, a positive electrode active material layer made of vanadium pentoxide xerogel (V 2 O 5 .nH 2 O) having a thickness of about 20 μm was formed.
【００１２】図１は本実施例の方法で形成した正極活物
質層の部分断面図である。この図に示すように本実施例
の方法で正極活物質層を形成すると層１０…が不規則に
形成され、正極活物質層の厚み方向に延びる層間部２０
…が多数形成される。FIG. 1 is a partial sectional view of a positive electrode active material layer formed by the method of this embodiment. As shown in this figure, when the positive electrode active material layer is formed by the method of this embodiment, the layers 10 are irregularly formed, and the interlayer portion 20 extending in the thickness direction of the positive electrode active material layer.
Many are formed.
【００１３】次に二種類の正極活物質層を用いた電池
Ａ，Ｂを製造して試験を行い、本実施例の方法で形成し
た正極活物質層の特性を調べた結果について説明する。Next, the results of examining the characteristics of the positive electrode active material layer formed by the method of this embodiment by producing and testing batteries A and B using two kinds of positive electrode active material layers will be described.
【００１４】ここで電池Ａは本実施例の方法で形成した
正極活物質層を用いた固体電解質リチウム電池であり、
図２に示すような断面を有している。固体電解質リチウ
ム電池Ａは次のようにして製造した。まず厚み２０μm
のニッケル箔からなる正極集電体３の一方の表面３ａの
中央部分に本実施例の方法で厚み２０μm の五酸化バナ
ジウムキセロゲル（Ｖ２ Ｏ５ ・ｎＨ２ Ｏ）からな
る正極活物質層４を形成した。次にポリフォスファゼン
誘導体の一種である分子量約２００万のメトキシオリゴ
エチレンオキシポリフォスファゼン（ＭＥＰ７）と該Ｍ
ＥＰ７に対して８重量％のＬｉＣｌＯ４ とを１、２−
ジメトキシエタン（ＤＭＥ）中に２０重量％溶かして高
分子固体電解質用溶液を作り、この溶液を正極活物質層
４を全体的に覆うようにして正極活物質層４上に塗布し
た。そして、これを乾燥してＤＭＥを揮発するキャステ
ィングにより厚み１００μm の固体電解質層５を作っ
た。次に固体電解質層５の上に厚み４０μm のＬｉ箔か
らなる負極活物質層６を載置し、正極集電体３の外周端
部３ｂの上にホットメルト７を載置した。そして、負極
活物質層６とホットメルト７とを覆うようにして正極集
電体３と同寸法のステンレスからなる負極集電体８を載
置した。次に加熱によりホットメルト７を集電体３及び
８の外周端部３ｂ及び８ｂに完全に接続して固体電解質
リチウム電池Ａを製造した。Here, the battery A is a solid electrolyte lithium battery using the positive electrode active material layer formed by the method of this embodiment,
It has a cross section as shown in FIG. The solid electrolyte lithium battery A was manufactured as follows. First, the thickness is 20 μm
A positive electrode active material layer 4 made of vanadium pentoxide xerogel (V 2 O 5 .nH 2 O) having a thickness of 20 μm was formed on the central portion of one surface 3 a of the positive electrode current collector 3 made of nickel foil by the method of this embodiment. Formed. Next, methoxyoligoethyleneoxypolyphosphazene (MEP7) having a molecular weight of about 2,000,000, which is a kind of polyphosphazene derivative, and M
8% by weight of LiClO 4 with respect to EP7 and 1,2-
A solution for a polymer solid electrolyte was prepared by dissolving 20% by weight in dimethoxyethane (DME), and this solution was applied onto the positive electrode active material layer 4 so as to cover the positive electrode active material layer 4 entirely. Then, this was dried to form a solid electrolyte layer 5 having a thickness of 100 μm by casting to volatilize DME. Next, the negative electrode active material layer 6 made of Li foil having a thickness of 40 μm was placed on the solid electrolyte layer 5, and the hot melt 7 was placed on the outer peripheral end portion 3b of the positive electrode current collector 3. Then, a negative electrode current collector 8 made of stainless steel and having the same size as the positive electrode current collector 3 was placed so as to cover the negative electrode active material layer 6 and the hot melt 7. Next, the hot melt 7 was completely connected to the outer peripheral end portions 3b and 8b of the current collectors 3 and 8 by heating to manufacture a solid electrolyte lithium battery A.
【００１５】電池Ｂは従来の方法で形成した正極活物質
層を用い、その他は電池Ａと同様の方法で製造した固体
電解質リチウム電池である。なお、電池Ｂに用いた正極
活物質層は超音波振動を加えずに２５℃で水溶液を乾燥
し、その他は本実施例と同様の方法で形成した。Battery B is a solid electrolyte lithium battery manufactured by the same method as Battery A, except that the positive electrode active material layer formed by the conventional method is used. The positive electrode active material layer used in Battery B was formed by the same method as in this example except that the aqueous solution was dried at 25 ° C. without applying ultrasonic vibration.
【００１６】次に電池Ａ，Ｂを電流密度２５μA/cm２
で終止電圧２．０Ｖまで放電した後に電流密度２５μA/
cm２ で終止電圧４．２Ｖまで充電する充放電を繰り返
し各電池のサイクル寿命特性を調べた。図３はその測定
結果を示している。本図より本実施例の方法で形成した
正極活物質層を用いると活物質利用率を高めて、電池の
容量を高く維持でき、しかも電池のサイクル寿命を延ば
せるのが判る。Next, the batteries A and B were charged with a current density of 25 μA / cm 2
Current density 25μA /
The cycle life characteristics of each battery were examined by repeating charge and discharge charging to a final voltage of 4.2 V at cm 2 . FIG. 3 shows the measurement result. From this figure, it can be seen that by using the positive electrode active material layer formed by the method of this embodiment, the utilization rate of the active material can be increased, the capacity of the battery can be maintained high, and the cycle life of the battery can be extended.
【００１７】なお、本実施例では、リチウム電池に用い
る正極板の正極活物質層を形成する場合に本発明を適用
したものであるが、多層構造になる正極活物質層であれ
ば、他の電池に用いる正極板の正極活物質層を形成する
方法に本発明を適用できるのはもちろんである。In the present embodiment, the present invention is applied to the case of forming the positive electrode active material layer of the positive electrode plate used in the lithium battery, but other positive electrode active material layers having a multi-layer structure can be used. Of course, the present invention can be applied to a method of forming a positive electrode active material layer of a positive electrode plate used in a battery.
【００１８】[0018]
【発明の効果】請求項１の発明によれば、水溶液が乾燥
して規則的な多層構造が形成される前に、水溶液に振動
を加えるので、不規則な層構造が形成される。そのため
結合力の弱い層間部が正極活物質層の厚み方向に延びる
率が高くなり、負極活物質イオンの正極活物質層内部へ
の拡散性が向上する。またこのように不規則な層構造が
形成されると、電池の充放電で正極活物質層内に生じる
応力が分散しやすくなり、電池の充放電の繰り返しによ
る正極活物質層の崩壊を抑制することができる。したが
って本発明の正極活物質を用いれば活物質利用率を高め
て、電池の容量を高く維持でき、しかも電池のサイクル
寿命を延ばすことができる。According to the invention of claim 1, vibration is applied to the aqueous solution before the aqueous solution is dried to form a regular multilayer structure, so that an irregular layer structure is formed. Therefore, the interlayer portion having a weak bonding force has a high rate of extending in the thickness direction of the positive electrode active material layer, and the diffusion of the negative electrode active material ions into the positive electrode active material layer is improved. Further, when such an irregular layer structure is formed, the stress generated in the positive electrode active material layer during charging and discharging of the battery is easily dispersed, and the collapse of the positive electrode active material layer due to repeated charging and discharging of the battery is suppressed. be able to. Therefore, by using the positive electrode active material of the present invention, the utilization rate of the active material can be increased, the capacity of the battery can be maintained high, and the cycle life of the battery can be extended.
【００１９】請求項２の発明によれば、超音波振動によ
り水溶液に振動を加えるので、正極活物質層全体に不規
則な層構造を簡単に形成できる。According to the second aspect of the invention, since the aqueous solution is vibrated by the ultrasonic vibration, an irregular layer structure can be easily formed on the entire positive electrode active material layer.
【図１】 本実施例の方法で形成した正極活物質層の部
分断面図である。FIG. 1 is a partial cross-sectional view of a positive electrode active material layer formed by the method of this example.
【図２】 本実施例の方法で形成した正極活物質層を用
いた固体電解質リチウム電池の断面図である。FIG. 2 is a cross-sectional view of a solid electrolyte lithium battery using a positive electrode active material layer formed by the method of this example.
【図３】 試験に用いた電池のサイクル寿命特性を示す
図である。FIG. 3 is a diagram showing cycle life characteristics of a battery used in a test.
【図４】 従来の方法で形成した正極活物質層の部分断
面図である。FIG. 4 is a partial cross-sectional view of a positive electrode active material layer formed by a conventional method.
１，１０ 層 ２，２０ 層間部 1,10 layers 2,20 Interlayer
───────────────────────────────────────────────────── フロントページの続き (72)発明者 早川 他▲く▼美 東京都新宿区西新宿二丁目１番１号 新 神戸電機株式会社内 (72)発明者 小牧 昭夫 東京都新宿区西新宿二丁目１番１号 新 神戸電機株式会社内 (72)発明者 犬伏 昭嘉 徳島県徳島市川内町加賀須野463番地 大塚化学株式会社 徳島研究所内 (72)発明者 中長 偉文 徳島県徳島市川内町加賀須野463番地 大塚化学株式会社 徳島研究所内 (72)発明者 笹岡 三千雄 徳島県徳島市川内町加賀須野463番地 大塚化学株式会社 徳島研究所内 (56)参考文献 特開 平４−169066（ＪＰ，Ａ) 特開 昭53−101764（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) H01M 4/66 H01M 4/04 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Hayakawa and others ▲ Ku ▼ Beauty, 2-1-1, Nishishinjuku, Shinjuku-ku, Tokyo Inside Kobe Electric Co., Ltd. (72) Inventor Akio Komaki Nishishinjuku, Shinjuku-ku, Tokyo 1-1-1 Shin Kobe Electric Co., Ltd. (72) Inventor Akiyoshi Inubushi 463 Kagasuno, Kawauchi Town, Tokushima City, Tokushima Prefecture Otsuka Chemical Co., Ltd. Tokushima Laboratory (72) Inventor, Weibun Kawauchi Town, Tokushima City, Tokushima Prefecture 463 Kagasuno Otsuka Chemical Co., Ltd. Tokushima Laboratory (72) Inventor Michio Sasaoka 463 Kagasuno Kawauchi-machi, Tokushima Prefecture Tokushima Laboratory (56) References JP-A-4-169066 (JP, A) ) JP-A-53-101764 (JP, A) (58) Fields investigated (Int.Cl. 7 , DB name) H01M 4/66 H01M 4/04
Claims (3)
質を含む水溶液を基体に塗布した後に乾燥して正極活物
質層を形成する方法において、 前記基体に塗布した前記水溶性活物質を含む水溶液が乾
燥して規則的な多層構造が形成される前に、前記水溶液
に振動を加えて不規則な層構造を形成することを特徴と
する正極活物質層の形成方法。1. A method for forming a positive electrode active material layer by applying an aqueous solution containing a water-soluble active material that becomes a xerogel when dried to a substrate and then drying the same to form a positive electrode active material layer, wherein the aqueous solution containing the water-soluble active material applied to the substrate is Dry
Before燥to regular multilayer structure is formed, the method of forming the positive electrode active material layer, characterized that you form an irregular layer structure by adding a vibration to the aqueous solution.
えることを特徴とする請求項１に記載の正極活物質層の
形成方法。2. The method for forming a positive electrode active material layer according to claim 1, wherein the aqueous solution is vibrated by ultrasonic vibration.
ウムであることを特徴とする請求項１に記載の正極活物
質層の形成方法。3. The method for forming a positive electrode active material layer according to claim 1, wherein the water-soluble active material is amorphous vanadium pentoxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16530293A JP3441765B2 (en) | 1993-07-05 | 1993-07-05 | Method for forming positive electrode active material layer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16530293A JP3441765B2 (en) | 1993-07-05 | 1993-07-05 | Method for forming positive electrode active material layer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0722030A JPH0722030A (en) | 1995-01-24 |
| JP3441765B2 true JP3441765B2 (en) | 2003-09-02 |
Family
ID=15809756
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16530293A Expired - Fee Related JP3441765B2 (en) | 1993-07-05 | 1993-07-05 | Method for forming positive electrode active material layer |
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| JP (1) | JP3441765B2 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100399053B1 (en) * | 2000-12-14 | 2003-09-26 | 한국전자통신연구원 | Organic-inorganic composite as positive electrode for rechargeable lithium battery and the preparation thereof |
| KR100424674B1 (en) * | 2001-05-19 | 2004-03-27 | 한국전자통신연구원 | Sonochemical preparation of VOPO4·2H2O and the use for cathode of rechargeable lithium battery |
| JP5105206B2 (en) * | 2009-12-18 | 2012-12-26 | トヨタ自動車株式会社 | Drying equipment |
| US9577261B2 (en) | 2011-03-18 | 2017-02-21 | Semiconductor Energy Laboratory Co., Ltd. | Lithium ion secondary battery and method for manufacturing the same |
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1993
- 1993-07-05 JP JP16530293A patent/JP3441765B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0722030A (en) | 1995-01-24 |
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