JP4225639B2 - Spiral lithium battery - Google Patents

Spiral lithium battery Download PDF

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Publication number
JP4225639B2
JP4225639B2 JP22331399A JP22331399A JP4225639B2 JP 4225639 B2 JP4225639 B2 JP 4225639B2 JP 22331399 A JP22331399 A JP 22331399A JP 22331399 A JP22331399 A JP 22331399A JP 4225639 B2 JP4225639 B2 JP 4225639B2
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negative electrode
spiral
lithium
sheet
electrode sheet
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JP2001052720A (en
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伸泰 稲吉
千洋 村田
廣彦 太田
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FDK Corp
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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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Description

【０００１】
【発明が属する技術分野】
この発明は、スパイラル形電極構造のリチウム電池に関し、特に電池ケースを兼ねた負極缶とリチウム負極との接続構造の改良に関する。
【０００２】
【従来の技術】
従来の代表的なスパイラル形リチウム電池の内部構造を図１に示す。有底円筒形の負極缶２にスパイラル形電極体７と非水電解液が収容されている。缶開口部２ａにはガスケット４を介して封口体６がはめ込まれ、缶開口部２ａを封口体に対してかしめることにより缶内部を密閉している。封口体６外面には正極端子６ａが突出形成されている。
【０００３】
スパイラル形電極体７は、帯状のリチウム負極シート１０・正極シート８・セパレータ１２の積層物をスパイラル状に巻回して円筒状に成形して製作される。その巻芯部には中心孔１７が形成されている。その下面にはドーナツ円板形の絶縁板１８が配設されている。リチウム負極シート１０は金属リチウムを薄く形成したものである。正極シート８は二酸化マンガンなどの正極活物質を集電体である多孔性金属シートの両面に一体的に塗布して形成されている。セパレータ１２はポリプロピレン、ポリエチレンなどのポリオレフィン系不織布からなる。
【０００４】
スパイラル形電極体７の上端面および下端面からはそれぞれ金属製で帯状のリードタブ１４、１６が突出している。各リードタブ１４、１６は電極７内部でそれぞれリチウム負極シート１０と正極シート８に溶接接合されている。電極上端の正極リードタブ１４の先端部は封口体６の内面６ｂに溶接接合され、正極シート８と正極体を兼ねた封口体６とを電気的に接続している。電極下端の負極リードタブ１６は、絶縁板１８により正極シート８と隔離されながら電極中心孔１７方向へ折り曲げられ、その先端部が缶内底部２ｂ中央で溶接接合されている。これにより、リチウム負極シート１０と負極缶２とは電気的に接続されている。
【０００５】
負極リードタブ１６と負極缶２との溶接作業は次のようにして行われている。まず、負極リードタブ１６を電極収容前に径方向内側に折り曲げておく。このときリードタブ１６は中心孔１７の真下を横切るようにする。リードタブ１６が電極の中心孔１７の真下からズレないようにしながら電極７を缶内部に挿入する。電極７挿入後、電極上方から中心孔１７にスポット溶接棒を差し込み、その先端部をリードタブ１６先端に上から押し当て、これを缶内底部２ｂ中央に溶接接合する。
【０００６】
【発明が解決しようとする課題】
前述した溶接作業は工程が多く複雑できわめて煩雑な作業であった。つまり、負極リードタブ折曲時には電極中心孔１７の真下にくるようにしなければならないとともに、電極挿入時にはリードタブ１６の位置ズレに注意しなければならない。また、スポット溶接棒と中心孔１７との位置合わせに高い精度が要求されるとともに、リードタブ１６が位置ズレしていたときにはスポット溶接棒の先端部とリードタブ１６との間で微調節が必要であった。このように十分に注意を払いながら溶接作業を行っても溶接不良を確実に防ぐことはできず、例えば特開平６−１７６７７０号で代表されるような複雑な検査を実施せざるを得なかった。リードタブ１６の長さを長くすれば、缶収容前の電極を負極缶に接続でき、溶接作業がやりやすくなるが、リードタブを缶内部に収容したとき、リードタブの体積が大きくなり、活物質を入れるスペースが小さくなる。つまり、放電性能が悪化するので採用できない。
【０００７】
一方、リードタブを使わずにスパイラル形電極体の電極と外側の電極缶とを接続する構造の電池が知られている（特開昭５４−７６９２９号公報・特開昭５４−７６９３０号公報参照）。スパイラル形電極体の最外周に存在する正極シートを電極缶内周面に圧接して接続するのである。しかし、正極シート内部の集電体と缶内周とは直接接続されないため、集電体で大電流を取り出すことができず、性能的に問題があった。
【０００８】
本発明は、前記事情に鑑みてなされたものであって、その目的は、従来と同様の性能を確保でき、かつ電極と電極缶との接続を容易に行うことができるスパイラル形リチウム電池を提供することにある。
【０００９】
【課題を解決するための手段】
そこで、本発明では、リチウム負極シートと正極シートとセパレータとの積層物をスパイラル状に巻回して円筒形に成形したスパイラル形電極体を非水電解液とともに有底円筒形の負極缶に収容し、この負極缶の開口部を封口体とガスケットで密閉した構造のスパイラル形リチウム電池において、前記正極シートと前記封口体の端子板とをリードタブで接続し、前記スパイラル形電極体の最外周部分に１周以上にわたって前記リチウムシートを存在させるとともに該リチウムシートを前記負極缶の内周面に直接に圧接させた。
【００１０】
また、好ましくは、前記スパイラル形電極体の最外周部分に、前記正極シートと対向しない前記リチウム負極シートを２周以上存在させることである。
【００１１】
【発明の実施の形態】
本発明にかかるスパイラル形リチウム電池の一実施形態を図２に示し、そのスパイラル形電極体を図３に示す。この電池は、３つのシートの巻回状態と、負極リードタブがない点以外は、前述した従来例と同じ構成である。なお、従来と同一の構成要素には同一の符号を付してある。
【００１２】
３種類のシートはリチウム負極シート１０が一番外側にくるように巻回されている。セパレータ１２は正極シート８とリチウム負極シート１０とを確実に遮断するために若干幅広くかつ正極シート８よりも若干長く形成されている。正極シート８には従来と同様リードタブ１４が設けられ電極体上端から延出される。
【００１３】
この発明の特徴は３種類のシートのうちリチウム負極シート１０が電極体巻回端部において正極シート８及びセパレータ１２よりもとび抜けて長い点である。リチウム負極シート１０は正極シート８よりも長さＬ分だけ長くなっている。長さＬは、リチウム負極シート１０がそれに対向する正極シート８が存在しなくなってから電極体外周に１周以上余分に巻き付けられるように設定されている。従って、電極体７の最外周部分には、正極シート８と対向しないリチウム負極シートが１周以上、好ましくは後述する理由から２周以上存在する。
【００１４】
図４にスパイラル形電極体７を収容したときの負極缶断面を示す。電極体７は缶に収容されると巻回拘束力が若干ゆるむ。このとき、リチウム負極シート１０がその弾性復元力で径方向へと広がり、その最外周の巻回部が負極缶内周面に密着される。リチウム負極シート１０は金属リチウムがむき出しの状態であるため、リチウム負極シート１０と負極缶２とは直接電気的に接続され、リチウム負極シート１０が生成した電気エネルギーを負極缶２に良好に伝えることができる。従って、リチウム負極シート１０と負極缶２との接続にリードタブを使用する必要がない。なお、正極シート８の集電体として、好ましくは径方向外側への弾発力を有する多孔性金属シート１３を使用することである。
【００１５】
リチウム負極シート１０と正極シート８との間で放電反応が進み、リチウム負極シート１０が消費されたとしても、スパイラル形電極体７の最外周部分には正極シート８と対向していないリチウム負極シート１０が存在するから、これが消費されずに残り、負極缶２とリチウム負極シート１０との接続状態に悪影響が出ることはない。
【００１６】
スパイラル形電極体の正極シートを越えて延長するリチウム負極シートの好ましい長さＬを調べるために、正極シートと対向しない負極リチウムシートの最外周部における巻数と電池の性能との関係について比較試験を行った。前記巻数をそれぞれ１．０周、１．５周、２．０周、３．０周とした単二形電池を製作し、各電池についてそれぞれ温度−２０℃の環境下において放電負荷４０Ωで放電試験を行い、そのときの放電時間を測定して結果を以下の表１にまとめた。なお、放電時間は、負極リードタブを用いた従来の電池の場合を１００として示してある。
【００１７】
【表１】

Figure 0004225639
【００１８】
この比較試験から、リチウム負極シートは、スパイラル形電極体の最外周部分に、正極シートと対向することなく２周以上存在させるのが好ましいことがわかった。
【００１９】
リチウム負極シート１０と負極缶２の密着性を高めるためには、電極体７の中心孔１７やリチウム負極シート１０の負極缶２内周面に対向する部分の裏側に適当なスペーサを詰め込み、リチウム負極シート１０を内側から径方向外側へ圧迫するようにするとよい。
【００２０】
また、このようなスパイラル形電極７を径方向に押し潰して断面長円形状にすれば、これを角筒状の負極缶に収容して、その負極缶との密着性を高めることができる。
【００２１】
【発明の効果】
本発明では、スパイラル形電極体の最も外側に存在するリチウム負極シートが負極缶内周面に圧接されるから、リードタブで使わずにリチウム負極シートと負極缶との電気的な接続を図ることができる。従来必要であった負極リードタブと負極缶との溶接作業を不要にでき、組立にかかる手間を軽減できる。とくに、この接続はリチウム負極シートの長さを正極シート及びセパレータに対して長くするだけ良いから、特別な作業を必要とせず、従来に比べ電極接続工程を削減でき、作業も簡単になって、それだけ生産性が向上する。
また、前記スパイラル形電極体の最外周部分に、前記正極シートと対向しない前記リチウム負極シートを２周以上存在させることにより、リチウム負極シートの放電が進行しても負極リチウムと負極缶との電気的接続が損なわれず、従来と同様に性能の優れた電池が得られる。
【図面の簡単な説明】
【図１】従来の代表的なスパイラル形リチウム電池の内部構造を示した縦断面図である。
【図２】本発明のスパイラル形リチウム電池の内部構造を示した縦断面図である。
【図３】本発明のスパイラル形リチウム電池のスパイラル形電池複合体の巻回端部を開放して示した斜視図である。
【図４】本発明のスパイラル形リチウム電池の外周部を拡大して示した部分拡大横断面図である。
【符号の説明】
２ 負極缶
４ ガスケット
６ 封口体
７ スパイラル形電極体
８ リチウム負極シート
１０ 正極シート
１２ セパレータ
１４ 正極リードタブ
１６ 負極リードタブ
１７ 中心孔
１８ 絶縁板[0001]
[Technical field to which the invention belongs]
The present invention relates to a lithium battery having a spiral electrode structure, and more particularly to improvement of a connection structure between a negative electrode can also serving as a battery case and a lithium negative electrode.
[0002]
[Prior art]
The internal structure of a typical typical spiral lithium battery is shown in FIG. A spiral-shaped electrode body 7 and a non-aqueous electrolyte are accommodated in a bottomed cylindrical negative electrode can 2. A sealing body 6 is fitted into the can opening 2a via a gasket 4, and the inside of the can is sealed by caulking the can opening 2a against the sealing body. A positive electrode terminal 6 a is formed on the outer surface of the sealing body 6 so as to protrude.
[0003]
The spiral electrode body 7 is manufactured by winding a belt-like laminate of a lithium negative electrode sheet 10, a positive electrode sheet 8, and a separator 12 in a spiral shape to form a cylindrical shape. A center hole 17 is formed in the winding core. A donut disk-shaped insulating plate 18 is disposed on the lower surface thereof. The lithium negative electrode sheet 10 is formed by thinly forming metallic lithium. The positive electrode sheet 8 is formed by integrally applying a positive electrode active material such as manganese dioxide on both surfaces of a porous metal sheet as a current collector. Separator 12 consists of polyolefin nonwoven fabrics, such as polypropylene and polyethylene.
[0004]
From the upper end surface and the lower end surface of the spiral electrode body 7, metal-made strip-like lead tabs 14 and 16 protrude, respectively. The lead tabs 14 and 16 are welded to the lithium negative electrode sheet 10 and the positive electrode sheet 8, respectively, inside the electrode 7. The tip of the positive electrode lead tab 14 at the upper end of the electrode is welded to the inner surface 6b of the sealing body 6 to electrically connect the positive electrode sheet 8 and the sealing body 6 also serving as the positive electrode body. The negative electrode lead tab 16 at the lower end of the electrode is bent in the direction of the electrode center hole 17 while being separated from the positive electrode sheet 8 by the insulating plate 18, and the tip thereof is welded and joined at the center of the inner bottom 2b of the can. Thereby, the lithium negative electrode sheet 10 and the negative electrode can 2 are electrically connected.
[0005]
The welding operation of the negative electrode lead tab 16 and the negative electrode can 2 is performed as follows. First, the negative electrode lead tab 16 is bent radially inward before accommodating the electrode. At this time, the lead tab 16 crosses directly below the center hole 17. The electrode 7 is inserted into the can while preventing the lead tab 16 from shifting from directly below the center hole 17 of the electrode. After the electrode 7 is inserted, a spot welding rod is inserted into the center hole 17 from above the electrode, and its tip is pressed against the tip of the lead tab 16 from above, and this is welded to the center of the bottom portion 2b of the can.
[0006]
[Problems to be solved by the invention]
The above-described welding work is a complicated and extremely complicated work with many processes. That is, when the negative electrode lead tab is bent, it must be positioned directly below the electrode center hole 17 and when the electrode is inserted, attention must be paid to the positional deviation of the lead tab 16. Further, high accuracy is required for alignment between the spot welding rod and the center hole 17, and when the lead tab 16 is misaligned, fine adjustment between the tip of the spot welding rod and the lead tab 16 is necessary. It was. Even if the welding operation is performed while paying sufficient attention in this way, it is impossible to reliably prevent welding failure, and for example, a complicated inspection represented by JP-A-6-176770 has to be performed. . If the length of the lead tab 16 is increased, the electrode before housing the can can be connected to the negative electrode can and the welding work can be easily performed. However, when the lead tab is housed inside the can, the volume of the lead tab becomes large and an active material is inserted. Space is reduced. In other words, it cannot be adopted because the discharge performance deteriorates.
[0007]
On the other hand, a battery having a structure in which an electrode of a spiral electrode body and an outer electrode can are connected without using a lead tab is known (see Japanese Patent Laid-Open Nos. 54-76929 and 54-76930). . The positive electrode sheet existing on the outermost periphery of the spiral electrode body is pressed and connected to the inner peripheral surface of the electrode can. However, since the current collector inside the positive electrode sheet and the inner periphery of the can are not directly connected, a large current cannot be taken out by the current collector, causing a problem in performance.
[0008]
The present invention has been made in view of the above circumstances, and an object of the present invention is to provide a spiral lithium battery that can ensure the same performance as the conventional one and can easily connect the electrode and the electrode can. There is to do.
[0009]
[Means for Solving the Problems]
Therefore, in the present invention, a spiral electrode body obtained by spirally winding a laminate of a lithium negative electrode sheet, a positive electrode sheet, and a separator into a cylindrical shape is accommodated in a bottomed cylindrical negative electrode can together with a non-aqueous electrolyte. In the spiral lithium battery having a structure in which the opening of the negative electrode can is sealed with a sealing body and a gasket, the positive electrode sheet and the terminal plate of the sealing body are connected by a lead tab, and the outermost peripheral portion of the spiral electrode body is connected. The lithium sheet was allowed to exist for at least one turn, and the lithium sheet was directly pressed against the inner peripheral surface of the negative electrode can.
[0010]
Preferably, the lithium negative electrode sheet that does not face the positive electrode sheet is present in the outermost peripheral portion of the spiral electrode body at least twice.
[0011]
DETAILED DESCRIPTION OF THE INVENTION
One embodiment of a spiral lithium battery according to the present invention is shown in FIG. 2, and the spiral electrode body is shown in FIG. This battery has the same configuration as the above-described conventional example except that the three sheets are wound and there is no negative electrode lead tab. In addition, the same code | symbol is attached | subjected to the component same as the past.
[0012]
The three types of sheets are wound so that the lithium negative electrode sheet 10 comes to the outermost side. The separator 12 is formed to be slightly wider and slightly longer than the positive electrode sheet 8 in order to reliably block the positive electrode sheet 8 and the lithium negative electrode sheet 10. The positive electrode sheet 8 is provided with a lead tab 14 as in the prior art and extends from the upper end of the electrode body.
[0013]
The feature of the present invention is that the lithium negative electrode sheet 10 out of the three types of sheets is far longer than the positive electrode sheet 8 and the separator 12 at the electrode body winding end. The lithium negative electrode sheet 10 is longer than the positive electrode sheet 8 by a length L. The length L is set so that the lithium negative electrode sheet 10 is wound around the outer periphery of the electrode body one or more times after the positive electrode sheet 8 that faces the lithium negative electrode sheet 10 no longer exists. Therefore, the outermost peripheral portion of the electrode body 7 has a lithium negative electrode sheet that is not opposed to the positive electrode sheet 8 for one or more rounds, and preferably for two or more rounds for reasons described later.
[0014]
FIG. 4 shows a cross section of the negative electrode can when the spiral electrode body 7 is accommodated. When the electrode body 7 is accommodated in the can, the winding restraining force is slightly loosened. At this time, the lithium negative electrode sheet 10 expands in the radial direction by the elastic restoring force, and the outermost winding part is in close contact with the inner peripheral surface of the negative electrode can. Since the lithium negative electrode sheet 10 is in a state in which metallic lithium is exposed, the lithium negative electrode sheet 10 and the negative electrode can 2 are directly electrically connected, and the electric energy generated by the lithium negative electrode sheet 10 can be transmitted well to the negative electrode can 2. Can do. Therefore, it is not necessary to use a lead tab for connecting the lithium negative electrode sheet 10 and the negative electrode can 2. In addition, as the current collector of the positive electrode sheet 8, it is preferable to use a porous metal sheet 13 having a resilient force toward the outside in the radial direction.
[0015]
Even if the discharge reaction proceeds between the lithium negative electrode sheet 10 and the positive electrode sheet 8 and the lithium negative electrode sheet 10 is consumed, the lithium negative electrode sheet that does not face the positive electrode sheet 8 at the outermost peripheral portion of the spiral electrode body 7 Since 10 exists, it remains without being consumed, and the connection state between the negative electrode can 2 and the lithium negative electrode sheet 10 is not adversely affected.
[0016]
In order to investigate the preferred length L of the lithium negative electrode sheet extending beyond the positive electrode sheet of the spiral electrode body, a comparative test was conducted on the relationship between the number of turns at the outermost periphery of the negative electrode lithium sheet not facing the positive electrode sheet and the battery performance. went. Manufactured single-cell batteries with the number of turns of 1.0, 1.5, 2.0, and 3.0, respectively, and each battery was discharged at a discharge load of 40Ω in an environment at a temperature of −20 ° C. The test was conducted, the discharge time at that time was measured, and the results are summarized in Table 1 below. The discharge time is shown as 100 for a conventional battery using a negative electrode lead tab.
[0017]
[Table 1]
Figure 0004225639
[0018]
From this comparative test, it was found that the lithium negative electrode sheet is preferably present in the outermost peripheral portion of the spiral electrode body at least twice without facing the positive electrode sheet.
[0019]
In order to improve the adhesion between the lithium negative electrode sheet 10 and the negative electrode can 2, an appropriate spacer is packed on the back side of the center hole 17 of the electrode body 7 or the portion of the lithium negative electrode sheet 10 facing the inner peripheral surface of the negative electrode can 2. The negative electrode sheet 10 may be pressed from the inside to the outside in the radial direction.
[0020]
Further, if such a spiral electrode 7 is crushed in the radial direction to have an oval cross section, it can be accommodated in a rectangular tube-shaped negative electrode can, and the adhesion to the negative electrode can can be enhanced.
[0021]
【The invention's effect】
In the present invention, since the lithium negative electrode sheet existing on the outermost side of the spiral electrode body is pressed against the inner peripheral surface of the negative electrode can, the lithium negative electrode sheet and the negative electrode can can be electrically connected without using the lead tab. it can. The welding operation of the negative electrode lead tab and the negative electrode can, which has been conventionally required, can be eliminated, and the labor required for assembly can be reduced. In particular, since this connection only requires the length of the lithium negative electrode sheet to be longer than that of the positive electrode sheet and the separator, no special work is required, the electrode connection process can be reduced compared to the prior art, and the work is simplified. As a result, productivity is improved.
In addition, since the lithium negative electrode sheet that does not face the positive electrode sheet is present in the outermost peripheral portion of the spiral electrode body at least two times, the electric discharge between the negative electrode lithium and the negative electrode can can be achieved even when the discharge of the lithium negative electrode sheet proceeds. As a result, a battery having excellent performance can be obtained as before.
[Brief description of the drawings]
FIG. 1 is a longitudinal sectional view showing an internal structure of a typical typical spiral lithium battery.
FIG. 2 is a longitudinal sectional view showing an internal structure of a spiral lithium battery according to the present invention.
FIG. 3 is a perspective view showing a spiral battery assembly of a spiral lithium battery according to the present invention with a winding end portion opened.
FIG. 4 is a partially enlarged cross-sectional view showing an enlarged outer peripheral portion of a spiral lithium battery of the present invention.
[Explanation of symbols]
2 Negative electrode can 4 Gasket 6 Sealing body 7 Spiral electrode body 8 Lithium negative electrode sheet 10 Positive electrode sheet 12 Separator 14 Positive electrode lead tab 16 Negative electrode lead tab 17 Center hole 18 Insulating plate

Claims (2)

リチウム負極シートと正極シートとセパレータとの積層物をスパイラル状に巻回して円筒形に成形したスパイラル形電極体を非水電解液とともに有底円筒形の負極缶に収容し、この負極缶の開口部を封口体とガスケットで密閉した構造のスパイラル形リチウム電池において、前記正極シートと前記封口体の端子板とをリードタブで接続し、前記スパイラル形電極体の最外周部分に１周以上にわたって前記リチウムシートを存在させるとともに該リチウムシートを前記負極缶の内周面に直接に圧接してなることを特徴とするスパイラル形リチウム電池。A spiral electrode body formed by spirally winding a laminate of a lithium negative electrode sheet, a positive electrode sheet, and a separator into a cylindrical shape is housed in a bottomed cylindrical negative electrode can together with a non-aqueous electrolyte, and the opening of the negative electrode can In a spiral lithium battery having a structure in which a portion is sealed with a sealing body and a gasket, the positive electrode sheet and a terminal plate of the sealing body are connected with a lead tab, and the lithium electrode is connected to the outermost peripheral portion of the spiral electrode body over one or more rounds. A spiral lithium battery characterized in that a sheet is present and the lithium sheet is directly pressed against the inner peripheral surface of the negative electrode can. 請求項１に記載のスパイラル形リチウム電池において、前記スパイラル形電極体の最外周部分に、前記正極シートと対向しない前記リチウム負極シートを２周以上存在させてなることを特徴とするスパイラル形リチウム電池。2. The spiral lithium battery according to claim 1, wherein the lithium negative electrode sheet that does not face the positive electrode sheet is present in the outermost peripheral portion of the spiral electrode body at least two times. 3. .
JP22331399A 1999-08-06 1999-08-06 Spiral lithium battery Expired - Fee Related JP4225639B2 (en)

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