JP2003307477A - Method for three-point bending test for sheet-type test piece and apparatus used for the same - Google Patents
Method for three-point bending test for sheet-type test piece and apparatus used for the sameInfo
- Publication number
- JP2003307477A JP2003307477A JP2002114396A JP2002114396A JP2003307477A JP 2003307477 A JP2003307477 A JP 2003307477A JP 2002114396 A JP2002114396 A JP 2002114396A JP 2002114396 A JP2002114396 A JP 2002114396A JP 2003307477 A JP2003307477 A JP 2003307477A
- Authority
- JP
- Japan
- Prior art keywords
- sheet
- bending
- test piece
- shaped
- point bending
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
-
- 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
Landscapes
- Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)
- Secondary Cells (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、シート状試験片の
３点曲げ試験方法およびそれに使用する装置に関し、さ
らに詳しくは、プラスチック材料あるいはプラスチック
を含む複合材料などのように、曲げ変形しやすく反発力
の小さいシート状材料からなるシート状試験片の曲げ反
力を高精度に測定できるシート状試験片の３点曲げ試験
方法およびそれに使用する装置に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a three-point bending test method for a sheet-shaped test piece and an apparatus used therefor, and more specifically, it is easily repelled by bending, such as a plastic material or a composite material containing plastic. TECHNICAL FIELD The present invention relates to a three-point bending test method for a sheet-shaped test piece and a device used therefor capable of highly accurately measuring a bending reaction force of a sheet-shaped test piece made of a sheet-shaped material having a small force.
【０００２】[0002]
【従来の技術】従来、シート状材料の曲げ試験方法とし
ては、一般にオートグラフを用いた３点折り曲げ試験方
法が採用されていた。この方式の試験方法において、曲
げ角度に関して、平らなシート状材料の曲げ角を０°と
し、そこから変形して曲げられた角度を曲げ角θにした
場合に、曲げ角θが１８０°に至る大きな変形と曲げ半
径ｒを規制できる試験方法としては、ＪＩＳ Ｚ ２２
４８に規定されているシート状金属材料の曲げ試験方法
が一般的に採用されている。この試験方法は、シート状
試験片を一定距離（Ｌ）離して設けられた２個の円筒状
支えに載せ、その中央部に先端部が半円柱状（半径ｒ）
に形成された押し金具を当て、徐々に押し込んで上記シ
ート状試験片を所定の曲げ角度（θ）にまで曲げること
によってシート状試験片の曲げ反力を測定する試験方法
であって、シート状試験片の曲げ耐久性に関する評価
は、該試験片を取り外した後、湾曲部の外側の裂け、キ
ズ、その他の欠点の有無を観察することによって行って
いる。そして、このＪＩＳ Ｚ２２４８では、ｒ≧１０
ｍｍで、Ｌ＝ｒ＋３×試料厚と規定されている。2. Description of the Related Art Conventionally, as a bending test method for a sheet-shaped material, a three-point bending test method using an autograph has been generally adopted. In the test method of this system, regarding the bending angle, when the bending angle of the flat sheet-shaped material is 0 ° and the angle bent by being deformed from the bending angle is the bending angle θ, the bending angle θ reaches 180 °. As a test method capable of controlling large deformation and bending radius r, JIS Z 22
The bending test method for a sheet-shaped metal material specified in 48 is generally adopted. In this test method, a sheet-shaped test piece is placed on two cylindrical supports provided at a constant distance (L) apart, and the tip portion is semi-cylindrical (radius r) at the center thereof.
It is a test method for measuring the bending reaction force of a sheet-shaped test piece by applying a pressing metal fitting formed on the sheet and gradually pushing it to bend the sheet-shaped test piece to a predetermined bending angle (θ). The bending durability of the test piece is evaluated by removing the test piece and then observing the presence of tears, scratches, and other defects on the outside of the curved portion. And in this JIS Z2248, r ≧ 10
In mm, it is defined as L = r + 3 × sample thickness.
【０００３】この３点曲げ試験用の上記部材は、通常、
オートグラフの試験用治具の一つとして一式で販売され
ている〔例えば、島津製作所社製小型万能試験機 ＥＺ
Ｔｓｅｔｅｒ、同ＡＧ−Ｉいずれも、（商品名）があ
る〕。この場合、上記２個の円筒状支えをオートグラフ
のクロスバー（可動部）に取り付け、上記押し金具をロ
ードセルを介して支持体に取り付け、クロスバーの上下
動によって曲げ試験が行われる。そのほか、これに近い
ものとして、曲げ角が小さい場合に採用されるＪＩＳ
Ｋ ６９１１に規定の熱可塑性プラスチック曲げ強さ試
験方法や、ＪＩＳ Ｒ １６０１に規定のセラミック曲
げ試験方法などがある。これらの試験方法では、試験片
の曲げ反力の変化を上記ロードセルで測定することが可
能であるが、曲げ反力の垂直分力しか測定できず、した
がって、曲げ角θが小さい範囲でのみ有効で、曲げ角θ
が３０°程度より大きくなると、曲げ耐久性の評価には
使用することができない。The member for the three-point bending test is usually
It is sold as a set as one of the test jigs for the autograph [eg, small universal testing machine EZ manufactured by Shimadzu Corporation
Both Tsetter and AG-I have (brand name)]. In this case, the two cylindrical supports are attached to a crossbar (movable part) of the autograph, the push fitting is attached to a support through a load cell, and a bending test is performed by moving the crossbar up and down. In addition, JIS that is adopted when the bending angle is small is similar to this.
K 6911 includes a thermoplastic plastic bending strength test method, and JIS R 1601 includes a ceramic bending test method. With these test methods, it is possible to measure the change in the bending reaction force of the test piece with the above load cell, but only the vertical component force of the bending reaction force can be measured, so it is effective only in the range where the bending angle θ is small. And the bending angle θ
Is larger than about 30 °, it cannot be used for evaluation of bending durability.
【０００４】[0004]
【発明が解決しようとする課題】ところで、パソコン、
携帯電話などの小型精密電子機器には、その部品にプラ
スチック材料あるいはプラスチックを含む複合材料が多
く用いられている。これらの材料で小型精密電子機器用
の部品を作製する際には、上記材料をシート状に成形
し、さらに適当に曲げ加工を施すことが頻繁に行われて
いる。そして、そのような目的で用いられるシート状材
料の曲げ耐久性を試験するため、所定の曲げ半径に規制
でき、かつ曲げ角θが１８０°に至る深い曲げを行うこ
とができるという理由で、前記シート状金属材料の３点
曲げ試験方法を適用すると、シート状材料と２個の円筒
状の支えとの間で生じる摩擦力のため、曲げ反力を正確
に測定することができず、そのため、曲げ耐久性が評価
できないという問題があった。By the way, a personal computer,
A small precision electronic device such as a mobile phone is often made of a plastic material or a composite material containing plastic as its component. When manufacturing parts for small precision electronic devices with these materials, it is often the case that the above materials are formed into a sheet shape and further appropriately bent. Then, in order to test the bending durability of the sheet-like material used for such a purpose, the bending radius can be restricted to a predetermined value, and the bending angle θ can be deeply bent to 180 °. When the three-point bending test method for sheet metal material is applied, the bending reaction force cannot be accurately measured due to the frictional force generated between the sheet material and the two cylindrical supports, and therefore, There was a problem that the bending durability could not be evaluated.
【０００５】しかるに、携帯電話やノート型パソコンな
どのポータブル電子機器の二次電池として用いられるこ
とが多くなってきたリチウムイオン二次電池では、機器
収納時のスペース効率を高めることができる角形電池の
実現が強く要望されている。そして、その角形電池の構
成部材である電極は、正極活物質にバインダー、導電助
剤などと溶剤を加え、分散、攪拌して調製した塗料を集
電体となる導電性の基材の片面または両面に塗布し、乾
燥して正極活物質含有塗膜を形成することによって作製
したシート状正極と、同様に負極活物質にバインダーと
溶剤を加え、分散、攪拌して調製した塗料を集電体とな
る導電性の基材の片面または両面に塗布し、乾燥して負
極活物質含有塗膜を形成することによって作製したシー
ト状負極とをセパレータを介して対向させ、渦巻状に巻
回して巻回構造の電極体にしている。しかも、このよう
な角形電池用の巻回電極体では、角形の電池ケースに収
納するのに適するようにするため、両端部が半円状で中
央部が扁平状の長円形巻回電極体にする必要がある。However, the lithium ion secondary battery, which has been increasingly used as a secondary battery for portable electronic devices such as mobile phones and notebook computers, is a prismatic battery which can improve space efficiency when storing the device. Realization is strongly demanded. Then, the electrode, which is a constituent member of the prismatic battery, has a binder, a conductive additive, and a solvent added to the positive electrode active material, and the coating material prepared by dispersing and stirring the conductive material is used as a current collector on one side or A sheet-shaped positive electrode prepared by coating on both sides and drying to form a positive electrode active material-containing coating film, and a paint prepared by adding a binder and a solvent to the negative electrode active material, dispersing and stirring the same. The sheet-shaped negative electrode prepared by applying the negative electrode active material-containing coating on one or both sides of a conductive base material to be dried and facing the sheet-shaped negative electrode via a separator, and wound in a spiral shape. The electrode body has a spiral structure. Moreover, in such a spirally wound electrode body for a prismatic battery, in order to be suitable for being housed in a prismatic battery case, an elliptical spirally wound electrode body having a semicircular shape at both ends and a flat center portion is used. There is a need to.
【０００６】この長円形巻回電極体を作製するとき、そ
の最内周部では、シート状正極またはシート状負極（シ
ート状正極とシート状負極のいずれかを指す場合または
両者を合わせて「シート状電極」という）を半径０．５
ｍｍ程度の小さい曲率半径で折り曲げざるを得ないた
め、あらかじめ、このシート状電極の厳しい曲げでの耐
久性を評価しておくことが必要になる。When this elliptical spirally wound electrode body is manufactured, the innermost peripheral portion thereof is a sheet-shaped positive electrode or a sheet-shaped negative electrode (either a sheet-shaped positive electrode or a sheet-shaped negative electrode, or both are referred to as a "sheet"). "Shaped electrode") radius 0.5
Since there is no choice but to bend it with a small radius of curvature of about mm, it is necessary to evaluate beforehand the durability of this sheet electrode in severe bending.
【０００７】ところが、上記従来の３点曲げ試験方法を
シート状電極の曲げ耐久性評価に適用すると、２個の円
筒状支えとシート状電極から作製されたシート状試験片
の接点で生じる摩擦力が曲げ反力に大きな誤差を生じさ
せてしまう。また、シート状試験片の曲げ反力はその面
垂直方向に働く一方、上記従来の曲げ試験方法では押し
金具の移動方向（例えば、垂直方向）のみの分力しか測
定できないため、曲げ角θの増加に伴って測定値が低下
し、特にθ≧３０°では前記摩擦力に基づく誤差が無視
できない程度に大きくなり、さらにθ≧９０°では評価
に使えなくなる。しかも、市販の３点曲げ試験機では、
ＪＩＳ Ｚ ２２４８に準拠しているためにｒが１０ｍ
ｍ以上の押し金具しか入手できず、目的とする厳しい曲
げでの評価を行うことができなかった。However, when the above-mentioned conventional three-point bending test method is applied to the bending durability evaluation of the sheet electrode, the frictional force generated at the contact point of the sheet test piece made from the two cylindrical supports and the sheet electrode. Causes a large error in the bending reaction force. Further, while the bending reaction force of the sheet-shaped test piece acts in the direction perpendicular to the surface thereof, the conventional bending test method described above can measure only the component force only in the moving direction (for example, the vertical direction) of the pressing metal fitting, so that the bending angle θ The measured value decreases with an increase, and particularly when θ ≧ 30 °, the error based on the frictional force becomes too large to be ignored, and when θ ≧ 90 °, it cannot be used for evaluation. Moreover, with a commercially available 3-point bending tester,
R is 10 m because it conforms to JIS Z 2248
Only a metal fitting having a length of m or more was available, and it was not possible to carry out an evaluation in the target severe bending.
【０００８】したがって、本発明は、上記のような従来
の３点曲げ試験方法における問題点を解決し、プラスチ
ック材料あるいはシート状電極のようなプラスチック材
料を含む複合材料などからなるシート状試験片に対して
も、高精度に曲げ試験を行うことができ、厳しい曲げで
の耐久性を評価できる試験方法とそれに使用する装置を
提供することを目的とする。Therefore, the present invention solves the problems in the conventional three-point bending test method as described above, and provides a sheet-shaped test piece made of a plastic material or a composite material containing a plastic material such as a sheet-shaped electrode. On the other hand, it is an object of the present invention to provide a test method that can perform a bending test with high accuracy and can evaluate durability in severe bending, and an apparatus used for the testing method.
【０００９】[0009]
【課題を解決するための手段】本発明は、シート状試験
片を一定距離離して設けられた２個の円筒状支えに載
せ、その中央部に先端部が半円柱状に形成された押し金
具を当て、この押し金具を上記シート状試験片に徐々に
押し込んで所定の曲げ角度にまで曲げることによってシ
ート状試験片の曲げ反力を測定する３点曲げ試験方法に
おいて、円筒状支えをローラで構成し、かつ上記シート
状試験片の面垂直方向の曲げ反力を測定するロードセン
サー測定系を有するように構成することによって、上記
課題を解決したものである。SUMMARY OF THE INVENTION According to the present invention, a sheet metal test piece is placed on two cylindrical supports provided at a fixed distance from each other, and a pressing member having a semi-cylindrical tip at the center thereof. In the three-point bending test method for measuring the bending reaction force of the sheet-shaped test piece by gradually pushing the metal fitting into the sheet-shaped test piece and bending the sheet-shaped test piece to a predetermined bending angle, the cylindrical support is supported by a roller. The above-mentioned problems are solved by configuring the above-mentioned sheet-shaped test piece and having a load sensor measuring system for measuring the bending reaction force in the direction perpendicular to the plane.
【００１０】すなわち、本発明においては、円筒状支え
をローラで構成するので、２個の円筒状支えとシート状
試験片との接点で摩擦力が発生せず、したがって、上記
摩擦力に基づく誤差が生じず、また、シート状試験片の
面垂直方向に働く曲げ反力を測定できるので、曲げ角θ
の増加に伴う測定値の低下がなく、θ≧３０°でもシー
ト状電極の耐久性評価を行うことができる。That is, in the present invention, since the cylindrical support is composed of the rollers, no frictional force is generated at the contact points between the two cylindrical supports and the sheet-shaped test piece, and therefore an error based on the frictional force is generated. And the bending reaction force acting in the direction perpendicular to the plane of the sheet-shaped test piece can be measured.
It is possible to evaluate the durability of the sheet-shaped electrode even if θ ≧ 30 ° without decreasing the measured value with the increase of
【００１１】[0011]
【発明の実施の形態】本発明において、３点曲げ試験を
行うための押し金具の先端部は半円柱状に形成されてい
るが、その半円柱状先端部の半径ｒは、試験目的にあわ
せて適切に選ぶことができる。ＪＩＳ Ｚ ２２４８で
は、この半径ｒが１０ｍｍ以上と規定されているが、本
発明では、円筒状支えとしてのローラとロードセンサー
測定系を有する装置で試験を行うので、それ以下でも可
能である。例えば、前述したシート状電極の巻回時にお
ける半径０．５ｍｍ程度の厳しい曲げでの耐久性を評価
するために、ｒを同じ値の０．５ｍｍとすることができ
る。BEST MODE FOR CARRYING OUT THE INVENTION In the present invention, the tip of a pressing member for conducting a three-point bending test is formed in a semi-cylindrical shape, and the radius r of the semi-cylindrical shape of the tip depends on the purpose of the test. Can be selected appropriately. According to JIS Z 2248, this radius r is specified to be 10 mm or more, but in the present invention, since the test is carried out with a device having a roller as a cylindrical support and a load sensor measurement system, it is possible to use a radius less than that. For example, in order to evaluate the durability of the above-mentioned sheet-like electrode in a severe bending with a radius of about 0.5 mm when wound, r can be set to the same value of 0.5 mm.
【００１２】本発明において、３点曲げ試験を行う際の
２個の円筒状支えとなるローラは、例えば、その両端に
ミニチュアベアリングを介して支持部材に取り付けられ
る。その２個のローラ間の距離Ｌは、ＪＩＳ Ｚ ２２
４８に記載されているように、Ｌ＝ｒ＋３×シート状試
験片厚を目安に適宜調整すればよい。In the present invention, the two rollers that serve as the cylindrical supports for performing the three-point bending test are attached to the support member via, for example, miniature bearings at both ends thereof. The distance L between the two rollers is JIS Z 22
As described in No. 48, it may be appropriately adjusted with L = r + 3 × sheet-shaped test piece thickness as a guide.
【００１３】本発明において、３点曲げ試験時の面垂直
方向に働く曲げ反力を測定するロードセンサー測定系
は、ロードセル、増幅器（アンプ）、変換器および解析
用パソコンなどの記録・表示手段で構成され、例えば、
押し金具をロードセルを介してオートグラフの支持体に
取り付け、上記ロードセルの測定出力変化を下記に述べ
る変換器に入力して、出力変化を記録し、表示すること
ができるように構成されている。In the present invention, the load sensor measuring system for measuring the bending reaction force acting in the direction perpendicular to the surface during the three-point bending test is a recording / display means such as a load cell, an amplifier, a converter and a personal computer for analysis. Configured, for example,
The push metal fitting is attached to the support of the autograph through the load cell, and the change in the measured output of the load cell is input to the converter described below so that the change in the output can be recorded and displayed.
【００１４】上記ロードセンサー測定系を構成する変換
器としては、例えば、ロードセルの直接測定値をＦとす
ると、入力Ｆに対して「Ｆ／（２×Ｃｏｓθ）」変換し
出力する機能を有するものが使用される。The converter constituting the load sensor measuring system has a function of converting "F / (2 × Cosθ)" to the input F when the direct measurement value of the load cell is F and outputting the converted value. Is used.
【００１５】上記変換器に必要な変数θは、例えば、シ
ート状試験片の曲げ状態を横からカメラで観察して画像
解析で測定するという直接的な測定方法を採用して求め
てもよいが、オートグラフの標準的な機能であるクロス
バーの移動距離測定出力、すなわち、押し金具の押し込
む距離（深さ）ｄの測定値を用い、以下の近似式（１）
のような計算式から求めると新たなセンサー、試験機構
を追加しなくてすむ。The variable θ required for the converter may be obtained by adopting a direct measuring method in which the bending state of the sheet-shaped test piece is observed from the side by a camera and measured by image analysis. , The standard function of the autograph, using the measured output of the crossbar movement distance, that is, the measured value of the pushing distance (depth) d of the metal fitting, the following approximate expression (1)
It is not necessary to add a new sensor or test mechanism if the calculation formula is used.
【００１６】
θ＝２×ｔａｎ-1〔（Ｍ／２）／（Ｒ＋ｒ−ｄ）−ｔａｎ-1（Ｊ／（Ｒ＋ｒ）〕
…（１）
ここで、Ｊ＝〔（Ｍ／２）2 ＋（Ｒ＋ｒ−ｄ）2 −（Ｒ
＋ｒ）2 〕1/2
Ｍ＝Ｌ＋２×Ｒ
Ｒはローラの半径Θ = 2 × tan -1 [(M / 2) / (R + rd) -tan -1 (J / (R + r)] (1) Here, J = [(M / 2) 2 + (R + r-d) 2- (R
+ R) 2 ] 1/2 M = L + 2 × RR where R is the radius of the roller
【００１７】また、本発明の３点曲げ試験装置において
面垂直方向の曲げ反力を測定するロードセンサー測定系
では、円筒状支えとしてのローラとシート状試験片との
接点が曲げ試験の進行に伴って変化するため、テコの原
理で曲げ反力が変化する。そこで、例えば「上記接点が
押し金具と接点より１単位離れた位置での曲げ反力Ｔ」
を測定値にするように、テコの原理による補正を行うこ
とが好ましい。この補正は、例えば、上記変換器を次の
近似式（２）を適用することによって可能である。Further, in the load sensor measuring system for measuring the bending reaction force in the direction perpendicular to the plane in the three-point bending test apparatus of the present invention, the contact point between the roller as the cylindrical support and the sheet-shaped test piece is used for the progress of the bending test. Since it changes with the change, the bending reaction force changes according to the lever principle. Therefore, for example, "the bending reaction force T at the position where the above contact is 1 unit away from the push fitting and the contact"
It is preferable to perform the correction based on the lever principle so that This correction is possible, for example, by applying the following approximation formula (2) to the converter.
【００１８】Ｔ＝Ｊ×Ｆ／（２×Ｃｏｓθ）…（２）T = J × F / (2 × Cosθ) (2)
【００１９】上記変換器はアナログ方式でもデジタル方
式でもよいが、例えば、デジタル方式を採用すると、ロ
ードセルの出力を増幅器（アンプ）を通してＡ／Ｄ変換
器（アナログ／デジタル変換器）に入力し、その出力信
号をデジタル回線を通して解析用パソコンで処理するこ
とが可能であり、同一パソコンにて測定結果の記録・表
示を行うことができる。The converter may be of an analog type or a digital type. For example, if a digital type is adopted, the output of the load cell is inputted to an A / D converter (analog / digital converter) through an amplifier and the The output signal can be processed by a personal computer for analysis through a digital line, and the measurement results can be recorded and displayed on the same personal computer.
【００２０】本発明の３点曲げ試験装置におけるオート
グラフは、シート状試験片の材料、シートの厚さに応じ
て適当なものを選ぶことが可能であり、例えば、上記シ
ート状電極では小型オートグラフを用いることができ
る。このとき用いるロードセルとしては最大荷重１ｋｇ
程度の高感度センサーが好ましく、クロスバーの移動速
度は５ｍｍ／ｍｉｎ以下に設定することが好ましく、ク
ロスバーの移動距離測定器は分解能が０．００５ｍｍ以
下のものが好ましい。As the autograph in the three-point bending test apparatus of the present invention, an appropriate one can be selected according to the material of the sheet-shaped test piece and the thickness of the sheet. Graphs can be used. The load cell used at this time has a maximum load of 1 kg.
A high-sensitivity sensor is preferable, the moving speed of the crossbar is preferably set to 5 mm / min or less, and the resolution of the crossbar moving distance measuring device is preferably 0.005 mm or less.
【００２１】[0021]
【実施例】つぎに、実施例を挙げて本発明をより具体的
に説明する。ただし、本発明はそれらの実施例のみに限
定されるものではない。EXAMPLES Next, the present invention will be described more specifically with reference to examples. However, the present invention is not limited to only those examples.
【００２２】実施例１
この実施例１ではリチウムイオン二次電池用のシート状
正極の破断ダメージ（損傷）に対する耐久性評価に本発
明を適用した例について示す。なお、本実施例１におい
て、シート状試験片となるシート状正極を下記のように
作製した。なお、濃度などを示す％は特にその基準を付
記しない限り質量％である。Example 1 This Example 1 shows an example in which the present invention is applied to the durability evaluation of a sheet positive electrode for a lithium ion secondary battery against breakage damage (damage). In addition, in Example 1, a sheet-shaped positive electrode to be a sheet-shaped test piece was produced as follows. In addition,% indicating concentration and the like is mass% unless otherwise specified.
【００２３】（１）シート状正極の作製
まず、正極活物質含有塗膜形成用塗料を下記の組成で調
製した。(1) Preparation of Sheet-shaped Positive Electrode First, a coating material for forming a coating film containing a positive electrode active material was prepared with the following composition.
【００２４】正極活物質含有塗膜形成用塗料の組成： リチウムコバルト酸化物 ９２質量部 鱗片状黒鉛 ５質量部 ポリビニリデンフルオライド ３質量部 Ｎ−メチル−２−ピロリドン ３４質量部Composition of coating composition for forming coating film containing positive electrode active material: Lithium cobalt oxide 92 parts by mass Flake graphite 5 parts by mass Polyvinylidene fluoride 3 parts by mass N-methyl-2-pyrrolidone 34 parts by mass
【００２５】上記塗料の調製は次に示すように行った。
まず、上記Ｎ−メチル−２−ピロリドンの一部にポリビ
ニリデンフルオライドを溶解して１２％バインダー溶液
を調製した。次に、このバインダー溶液に正極活物質の
リチウムコバルト酸化物と電子伝導助剤としての鱗片状
黒鉛を加え、さらに上記Ｎ−メチル−２−ピロリドンの
残りの部分を加えて混合することによって塗料を調製し
た。The above coating composition was prepared as follows.
First, polyvinylidene fluoride was dissolved in a part of the N-methyl-2-pyrrolidone to prepare a 12% binder solution. Next, a lithium cobalt oxide as a positive electrode active material and scaly graphite as an electron conduction aid are added to this binder solution, and the rest of the N-methyl-2-pyrrolidone is further added and mixed to form a paint. Prepared.
【００２６】そして、得られた塗料を厚さ１５μｍのア
ルミニウム箔からなる基材にアプリケータを用いて所定
量塗布し、１１０℃に設定したホットプレート上で２０
分間乾燥して正極活物質含有塗膜を形成した。同様に、
上記アルミニウム箔からなる基材の裏面側にも上記塗料
を所定量塗布し、１１０℃に設定したホットプレート上
で２０分間乾燥した後、１００℃で８時間真空乾燥して
正極活物質含有塗膜を形成した。そして、この塗膜形成
後の電極体をロールプレスして、下記表１に示す厚みの
異なるシート状正極ａ〜ｄを作製した。なお、このシー
ト状正極ａ〜ｄの塗膜密度はすべて３．３ｇ／ｃｍ3 で
あった。そして、このシート状正極ａ〜ｄを幅１０ｍ
ｍ、長さ２０ｍｍの長方形に切り出してシート状試験片
とした。Then, a predetermined amount of the obtained coating material was applied to a base material made of aluminum foil having a thickness of 15 μm using an applicator, and the coating material was applied on a hot plate set at 110 ° C. for 20 minutes.
After drying for a minute, a positive electrode active material-containing coating film was formed. Similarly,
A predetermined amount of the coating material is applied to the back side of the base material made of the aluminum foil, dried on a hot plate set at 110 ° C. for 20 minutes, and then vacuum dried at 100 ° C. for 8 hours to form a positive electrode active material-containing coating film. Was formed. Then, the electrode body after the coating film formation was roll-pressed to produce sheet-like positive electrodes a to d having different thicknesses shown in Table 1 below. The coating densities of the sheet-shaped positive electrodes a to d were all 3.3 g / cm 3 . Then, the sheet-shaped positive electrodes a to 10
A sheet-shaped test piece was obtained by cutting out a rectangle having a length of m and a length of 20 mm.
【００２７】[0027]
【表１】 [Table 1]
【００２８】つぎに、この実施例１において用いる３点
曲げ試験装置を図１〜２に基づいて説明する。図１はこ
の実施例１の３点曲げ試験を実施するための試験装置を
模式的に示す概略図であり、Ａ部はその要部拡大図であ
る。ただし、このＡ部では押し金具をシート状試験片に
押し込んだ状態でかつ特定部位についてのみ示してい
る。そして、図２は図１に示す押し金具を拡大して示す
ものであり、（ａ）はその正面図で、この（ａ）は図１
に示す場合と同じ面から見た図であり、（ｂ）はその側
面図である。まず、部材と参照符号との関係について説
明すると、図１のＡ部において、１は押し金具であり、
２は円筒状支えとしてのローラである。上記押し金具１
は、図２に示すように、その本体部１ａは板状で〔図２
の（ｂ）参照〕、その先端部１ｂは半円柱状をしてい
て、その半円柱状先端部１ｂの半径ｒは０．５ｍｍであ
り、その本体部１ａの厚みは１ｍｍである。上記ローラ
２は一定距離Ｌ離れて２個設けられていて、それぞれ直
径４ｍｍのミニュチュアベアリングを内蔵して構成され
ている。Next, the three-point bending test apparatus used in the first embodiment will be described with reference to FIGS. FIG. 1 is a schematic view schematically showing a test apparatus for carrying out the three-point bending test of this Example 1, and part A is an enlarged view of a main part thereof. However, in the section A, only the specific portion is shown in a state in which the push fitting is pushed into the sheet-shaped test piece. 2 is an enlarged view of the push fitting shown in FIG. 1. FIG. 2A is a front view thereof, and FIG.
It is the figure seen from the same surface as the case shown in (b), and (b) is the side view. First, the relationship between the members and the reference numerals will be described. In the portion A of FIG. 1, 1 is a push fitting,
2 is a roller as a cylindrical support. The above push fitting 1
As shown in FIG. 2, the main body 1a has a plate shape [Fig.
(B)], the tip 1b has a semi-cylindrical shape, the radius r of the semi-cylindrical tip 1b is 0.5 mm, and the thickness of the main body 1a is 1 mm. The two rollers 2 are provided at a fixed distance L from each other, and each has a built-in miniature bearing having a diameter of 4 mm.
【００２９】そして、押し金具１はロードセル３を介し
てオートグラフ４の支持体５の天板部に取り付けられて
おり、ローラ２は２個のローラ間の間隔微調整機構を内
蔵した支持部材６によってクロスバー７に取り付けら
れ、２個のローラ２間の距離Ｌは、支持部材６によって
Ｌ＝ｒ＋３×シート状試験片の全厚となるように調整さ
れている。上記支持体５は２本の横軸部の上部に上記天
板部を配置した構成をしており、前記クロスバー７はこ
の支持体５の２本の横軸部の間に配置されていて、クロ
スバー７はその２本の横軸部の間で上下に移動ができる
構成になっている。そして、上記オートグラフ４の制御
用電子回路は操作部１２に組み込まれている。The push fitting 1 is attached to the top plate portion of the support 5 of the autograph 4 via the load cell 3, and the roller 2 is a support member 6 having a mechanism for finely adjusting the gap between the two rollers. Is attached to the crossbar 7 by means of the support member 6 and the distance L between the two rollers 2 is adjusted to be L = r + 3 × the total thickness of the sheet-shaped test piece. The support 5 has a configuration in which the top plate portion is arranged above two horizontal shaft portions, and the crossbar 7 is arranged between the two horizontal shaft portions of the support body 5. The crossbar 7 can move up and down between the two horizontal axis portions. The control electronic circuit of the autograph 4 is incorporated in the operation unit 12.
【００３０】シート状試験片８は、その両端部が２個の
ローラ２上に行き渡るようにしてローラ２に載せられて
いて、その中央部に押し金具１の先端部を当て、操作部
１２の指令により、クロスバー７を上方に移動すること
で徐々にシート状試験片８を押してシート状試験片８を
曲げ角θが最大１８０°まで折り曲げることができるよ
うに構成されている。そして、試験片８の曲げ反力はロ
ードセル３で測定され、そのロードセル３の出力は増幅
器（アンプ）９に入力され、増幅器９の出力はＡ／Ｄ変
換器１０に入力され、Ａ／Ｄ変換器１０の出力は解析用
パソコン１１に入力される。解析用パソコン１１には前
記近似式（２）による変換プログラムが組み込まれてお
り、３点曲げ試験中の曲げ反力が記録・表示されるよう
に構成されている。そして、この実施例１では、ロード
セル３は最大荷重１ｋｇの高感度型のものが用いられ、
クロスバー７の上昇時の速度は０．５ｍｍ／ｍｉｎに設
定されている。このクロスバー７の移動は支持体５に内
蔵された１μｍの分解能を持つマグネスケール測長器に
よって測定制御される。そして、この図１に示す３点曲
げ試験装置において、ロードセンサー系は、ロードセル
３、増幅器９、Ａ／Ｄ変換器１０および解析用パソコン
１１で構成される。The sheet-shaped test piece 8 is placed on the roller 2 so that both ends thereof are spread over the two rollers 2, and the tip of the pressing metal fitting 1 is applied to the central portion of the sheet-shaped test piece 8 so that the operation portion 12 is operated. According to the command, the sheet-shaped test piece 8 is gradually pushed by moving the crossbar 7 upward so that the sheet-shaped test piece 8 can be bent at a bending angle θ of up to 180 °. The bending reaction force of the test piece 8 is measured by the load cell 3, the output of the load cell 3 is input to the amplifier (amplifier) 9, the output of the amplifier 9 is input to the A / D converter 10, and the A / D conversion is performed. The output of the instrument 10 is input to the analysis personal computer 11. The analysis personal computer 11 incorporates a conversion program according to the approximate expression (2), and is configured to record and display the bending reaction force during the three-point bending test. In the first embodiment, the load cell 3 is a high sensitivity type with a maximum load of 1 kg,
The ascending speed of the crossbar 7 is set to 0.5 mm / min. The movement of the crossbar 7 is measured and controlled by a Magnescale length measuring device having a resolution of 1 μm built in the support 5. In the three-point bending test apparatus shown in FIG. 1, the load sensor system is composed of the load cell 3, the amplifier 9, the A / D converter 10 and the analysis personal computer 11.
【００３１】なお、この図１は本実施例１で使用する３
点曲げ試験装置が本発明に係る構成のものであることを
目的として概略的に図示したものであり、したがって、
この図１では本発明に係る３点曲げ試験装置の構成部材
のうち、特定のものしか図示していない。Incidentally, this FIG. 1 is used in the first embodiment 3
The point bending test apparatus is schematically illustrated for the purpose of having a configuration according to the present invention, and therefore,
FIG. 1 shows only specific ones of the constituent members of the three-point bending test apparatus according to the present invention.
【００３２】上記の３点曲げ試験装置を用いてシート状
正極から作製されたシート状試験片の曲げ試験を行い、
その曲げ反力の測定を行った。その際、曲げ角θは０か
ら１００°に至るまでの間で行った。その結果を図３に
示す。A bending test of a sheet-shaped test piece prepared from the sheet-shaped positive electrode was conducted by using the above-mentioned three-point bending tester.
The bending reaction force was measured. At that time, the bending angle θ was from 0 to 100 °. The result is shown in FIG.
【００３３】図３に示す結果から明らかなように、シー
ト状正極の曲げ半径が０．５ｍｍという厳しい曲げに対
し、正極の全厚が厚いほどその曲げ反力が大きいが、全
厚１６９μｍのシート状正極は曲げ角θが約１００°前
に急激な曲げ反力の低下が現れ、全厚１８１μｍのシー
ト状正極は曲げ角θが約５０°前で急激な曲げ反力の低
下が現れた。これに対して、全厚が１５１μｍのシート
正極や全厚が１６０μｍのシート状正極では試験した範
囲内では、急激な曲げ反力の低下が認められなかった。As is clear from the results shown in FIG. 3, the sheet-like positive electrode has a bending radius of 0.5 mm, and the bending reaction force increases as the total thickness of the positive electrode increases, but the total thickness of the sheet is 169 μm. The sheet-shaped positive electrode with a total thickness of 181 μm showed a sharp decrease in the bending reaction force before the bending angle θ was about 50 °. On the other hand, in the case of the sheet positive electrode having a total thickness of 151 μm and the sheet positive electrode having a total thickness of 160 μm, no rapid decrease in bending reaction force was observed within the range tested.
【００３４】次に、シート状正極ｃ、ｄについて、再度
同様の曲げ試験を行い、それぞれ、１００°、５０°曲
げたときの曲げ湾曲部の外周部について、内周側から観
察光を当てながら顕微鏡観察してそのダメージ（損傷）
を観察した。その結果、図４に示すように、全厚が１６
９μｍのシート状正極ｃでは部分的にクラックが発生し
ていることが認められ、また、図５に示すように、全厚
が１８１μｍのシート状正極ｄでは基材が完全に破断し
ていることがわかった。すなわち、内周側（つまり、裏
側）から観察光を当てているので、クラックの発生して
いるところは白くなり、クラックの発生していないとこ
ろは黒っぽくなるが、全厚が１６９μｍのシート状正極
では、図４に示すように、一部が白くなり、大部分は黒
っぽいままなので、部分的にクラックが発生しているこ
とがわかる。これに対して、全厚が１８１μｍのシート
状正極ｄでは、図５に示すように、幅方向の中央部の全
体が白くなっているので、基材が完全に破断しているこ
とがわかる。Next, the sheet-shaped positive electrodes c and d were again subjected to the same bending test, and the outer peripheral portions of the bent curved portions when bent at 100 ° and 50 ° were irradiated with observation light from the inner peripheral side. The damage (damage) under the microscope
Was observed. As a result, as shown in FIG. 4, the total thickness is 16
It was confirmed that the sheet-shaped positive electrode c having a thickness of 9 μm was partially cracked, and as shown in FIG. 5, the substrate was completely broken in the sheet-shaped positive electrode d having a total thickness of 181 μm. I understood. That is, since the observation light is applied from the inner peripheral side (that is, the back side), the place where the crack is generated becomes white and the place where the crack is not generated becomes dark, but the total thickness of the sheet-shaped positive electrode is 169 μm. Then, as shown in FIG. 4, it can be seen that a part is white and most is blackish, so that a crack is partially generated. On the other hand, in the sheet-shaped positive electrode d having a total thickness of 181 μm, as shown in FIG. 5, the entire central portion in the width direction is white, so it can be seen that the base material is completely broken.
【００３５】以上の結果から明らかなように、図３に示
すような曲げ反力変化曲線の急激な低下が図５に示すよ
うなシート状正極の破断に対応しており、本発明の３点
曲げ試験方法によれば、シート状正極の破断に至るダメ
ージが発生しない限界の曲げ角が得られ、その結果か
ら、曲げ耐久性を評価することができる。例えば、全厚
が１６９μｍのシート状正極ｃでは曲げ角θが９２°で
割れが発生し、全厚が１８１μｍのシート状正極ｄでは
曲げ角θが４８°で割れが発生するので、それに至る前
の曲げ角θを知ることができ、それによって、曲げ耐久
性を評価することができる。As is clear from the above results, the sharp decrease in the bending reaction force change curve as shown in FIG. 3 corresponds to the breakage of the sheet positive electrode as shown in FIG. 5, and the three points of the present invention. According to the bending test method, a limit bending angle at which damage leading to breakage of the sheet-shaped positive electrode does not occur can be obtained, and the bending durability can be evaluated from the result. For example, a sheet-shaped positive electrode c having a total thickness of 169 μm cracks at a bending angle θ of 92 °, and a sheet-shaped positive electrode d having a total thickness of 181 μm cracks at a bending angle θ of 48 °. It is possible to know the bending angle θ of, and thereby the bending durability can be evaluated.
【００３６】[0036]
【発明の効果】以上説明したように、本発明によれば、
プラスチック材料あるいはシート状電極のようなプラス
チックを含む複合材料からなるシート状試験片に対して
も、高精度に曲げ試験を行うことができ、その耐久性を
評価することができる。As described above, according to the present invention,
A bending test can be performed with high accuracy even on a sheet-shaped test piece made of a plastic material or a composite material containing a plastic such as a sheet-shaped electrode, and its durability can be evaluated.
【図１】本発明の３点曲げ試験を実施するための試験装
置の一例を模式的に示す概略図であり、Ａ部はその要部
拡大図である。ただし、このＡ部では押し金具をシート
状試験片に押し込んだ状態でかつ特定部位についてのみ
示している。FIG. 1 is a schematic view schematically showing an example of a test apparatus for carrying out a three-point bending test of the present invention, and an A part is an enlarged view of a main part thereof. However, in the section A, only the specific portion is shown in a state in which the push fitting is pushed into the sheet-shaped test piece.
【図２】図１に示す曲げ試験装置の押し金具を拡大して
示す図であり、（ａ）はその正面図で、（ｂ）はその側
面図である。2A and 2B are enlarged views of a push fitting of the bending test apparatus shown in FIG. 1, in which FIG. 2A is a front view thereof, and FIG. 2B is a side view thereof.
【図３】本発明の３点曲げ試験方法で測定した曲げ半径
０．５ｍｍのシート状正極の曲げ反力と曲げ角θとの関
係をシート状正極の厚みに応じて示した図である。FIG. 3 is a diagram showing a relationship between a bending reaction force and a bending angle θ of a sheet-shaped positive electrode having a bending radius of 0.5 mm measured by a three-point bending test method of the present invention according to the thickness of the sheet-shaped positive electrode.
【図４】全厚１６９μｍのシート状正極の曲げ湾曲部の
ダメージ状態を示す図である。FIG. 4 is a diagram showing a damaged state of a bending and bending portion of a sheet-shaped positive electrode having a total thickness of 169 μm.
【図５】全厚１８１μｍのシート状正極の曲げ湾曲部の
ダメージ状態を示す図である。FIG. 5 is a diagram showing a damaged state of a bending and bending portion of a sheet-shaped positive electrode having a total thickness of 181 μm.
１ 押し金具 １ａ 本体部 １ｂ 先端部 ２ ローラ ３ ロードセル ４ オートグラフ ５ 支持体 ６ 支持部材 ７ クロスバー ８ 試験片 ９ 増幅器（アンプ） １０ Ａ／Ｄ変換器 １１ 解析用パソコン １２ 操作部 1 push bracket 1a main body 1b Tip 2 rollers 3 load cell 4 Autograph 5 support 6 Support members 7 crossbar 8 test pieces 9 amplifier 10 A / D converter 11 Analysis personal computer 12 Operation part
Claims (4)
れた２個の円筒状支えに載せ、その中央部に先端部が半
円柱状に形成された押し金具を当て、その押し金具を上
記シート状試験片に徐々に押し込んで所定の曲げ角度に
まで曲げることによってシート状試験片の曲げ反力を測
定する３点曲げ試験方法であって、上記円筒状支えがロ
ーラで構成され、かつ上記シート状試験片の面垂直方向
の曲げ反力を測定するロードセンサー測定系を有する装
置でシート状試験片の３点曲げ試験をすることを特徴と
するシート状試験片の３点曲げ試験方法。1. A sheet-shaped test piece is placed on two cylindrical supports provided at a certain distance from each other, and a push fitting having a semi-cylindrical tip portion is applied to the center of the support, and the push fitting is set to the above-mentioned. A three-point bending test method for measuring a bending reaction force of a sheet-shaped test piece by gradually pushing it into a sheet-shaped test piece and bending it to a predetermined bending angle, wherein the cylindrical support is composed of rollers, and A three-point bending test method for a sheet-shaped test piece, which comprises performing a three-point bending test on the sheet-shaped test piece with an apparatus having a load sensor measuring system for measuring a bending reaction force in a direction perpendicular to the surface of the sheet-shaped test piece.
池のシート状電極からなるものであることを特徴とする
請求項１記載の３点曲げ試験方法。2. The three-point bending test method according to claim 1, wherein the sheet-shaped test piece comprises a sheet-shaped electrode of a lithium ion secondary battery.
れた２個の円筒状支えに載せ、その中央部に先端部が半
円柱状に形成された押し金具を当て、その押し金具を上
記シート状試験片に徐々に押し込んで所定の曲げ角度に
まで曲げることによってシート状試験片の曲げ反力を測
定する３点曲げ試験装置であって、上記円筒状支えがロ
ーラで構成され、かつ上記シート状試験片の面垂直方向
の曲げ反力を測定するロードセンサー測定系を有するこ
とを特徴とするシート状試験片の３点曲げ試験装置。3. A sheet-shaped test piece is placed on two cylindrical supports provided at a fixed distance from each other, and a push fitting having a semi-cylindrical tip is applied to the center of the support, and the push fitting is set as described above. A three-point bending tester for measuring a bending reaction force of a sheet-shaped test piece by gradually pushing it into a sheet-shaped test piece and bending it to a predetermined bending angle, wherein the cylindrical support is composed of rollers, and A three-point bending test apparatus for a sheet-shaped test piece, comprising a load sensor measuring system for measuring a bending reaction force of the sheet-shaped test piece in a direction perpendicular to the surface.
池のシート状電極からなるものであることを特徴とする
請求項３記載の３点曲げ試験装置。4. The three-point bending test apparatus according to claim 3, wherein the sheet-shaped test piece is composed of a sheet-shaped electrode of a lithium ion secondary battery.
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|---|---|---|---|
| JP2002114396A JP2003307477A (en) | 2002-04-17 | 2002-04-17 | Method for three-point bending test for sheet-type test piece and apparatus used for the same |
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|---|---|---|---|
| JP2002114396A JP2003307477A (en) | 2002-04-17 | 2002-04-17 | Method for three-point bending test for sheet-type test piece and apparatus used for the same |
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|---|---|
| JP2003307477A true JP2003307477A (en) | 2003-10-31 |
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|---|---|---|---|
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