JPS60196644A - Adhesion evaluating method - Google Patents
Adhesion evaluating methodInfo
- Publication number
- JPS60196644A JPS60196644A JP59052312A JP5231284A JPS60196644A JP S60196644 A JPS60196644 A JP S60196644A JP 59052312 A JP59052312 A JP 59052312A JP 5231284 A JP5231284 A JP 5231284A JP S60196644 A JPS60196644 A JP S60196644A
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- JP
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- Prior art keywords
- thin film
- adhesion
- area
- stage
- substrate
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Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N19/00—Investigating materials by mechanical methods
- G01N19/04—Measuring adhesive force between materials, e.g. of sealing tape, of coating
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
- Testing Or Measuring Of Semiconductors Or The Like (AREA)
Abstract
Description
【発明の詳細な説明】 の程度から付着力を評価する付着力評価方法に関する。[Detailed description of the invention] This invention relates to an adhesion evaluation method for evaluating adhesion from the degree of adhesion.
薄膜の基板に対する付着力は、薄膜の耐久性。 The adhesion of the thin film to the substrate is the durability of the thin film.
耐摩耗性に大きく影響するために従来から付着力のいろ
いろな評価方法が試みられている。たとえば、粘着性の
接着テープを薄膜の表面に貼シつけ。Various evaluation methods have been tried for adhesion since it has a large effect on wear resistance. For example, apply sticky adhesive tape to the surface of a thin film.
テープをはがしたときに薄膜が基板に残るかまたはテー
プにくっつくかをみて、薄膜の基板に対する付着の強さ
の程度を調べる引きはがし法がある。There is a peel-off method that examines the strength of the thin film's adhesion to the substrate by checking whether the thin film remains on the substrate or sticks to the tape when the tape is removed.
また、薄膜の表面に平らな円板を接着し、基板を固定し
た上でその円板を面に垂直方向に引張って薄膜をはく離
させ、そのときに加えられた力を測定する引張り法があ
る。また、硬い小さな圧子を薄膜に押しつけ、いろいろ
々荷重によって圧子を動かし、薄膜にはく離を生じたと
きの荷重を測定するひっかき法がある。Another method is the tensile method, in which a flat disk is glued to the surface of a thin film, the substrate is fixed, and the disk is pulled perpendicularly to the surface to separate the thin film, and the force applied at that time is measured. . There is also a scratching method in which a small, hard indenter is pressed against a thin film, the indenter is moved under various loads, and the load when the thin film peels is measured.
しかるに、接着テープをはがしたときに、薄膜が基板に
残るかテープにくっつくかをみて付着力の強さの程度を
調べる引きはがし法は、きわめて簡便で広く用いられて
いるが、いわゆる付着力のおおざっばな合否の判定がで
きるのみであり、正確な評価は困難である。また、薄膜
に接着した円板を垂直方向に引張って付着力を評価する
引張り法は１円板と薄膜の確実な接着が難しく、また薄
膜を基板から引きはがすのに要した力以外に、薄膜が円
板の縁のところから裂けてしまうことが多いため、測定
値に大きなばらつきを生じ、すこぶる不便である。まだ
、薄膜のはく離したときのひっかき荷重を測定すること
により付着力を評価するひっかき法は、異なる大きさの
荷重により数多くのひっかきを必要とするだめすこぶる
不便であシ、シかもはく離したか否かの判定が難しく、
また、はく離時のひっかき荷重を検出するための専用装
置が必要となり、容易にかつ安価に試験機を製作できな
い不都合があった。However, the peel-off method, which tests the strength of the adhesive force by checking whether a thin film remains on the substrate or sticks to the tape when the adhesive tape is removed, is extremely simple and widely used, but the so-called adhesive strength Only a rough pass/fail judgment can be made, and accurate evaluation is difficult. In addition, the tensile method, in which a disk adhered to a thin film is pulled vertically to evaluate the adhesion force, is difficult to ensure reliable adhesion between a disk and the thin film, and in addition to the force required to peel the thin film from the substrate, The disc is often torn from the edge, causing large variations in the measurements and being extremely inconvenient. However, the scratching method, which evaluates the adhesion force by measuring the scratching load when the thin film is peeled off, is extremely inconvenient as it requires numerous scratches due to loads of different magnitudes, and it is difficult to determine whether the thin film has been peeled off or not. It is difficult to determine whether
In addition, a special device is required to detect the scratching load during peeling, and there is an inconvenience that a testing machine cannot be easily and inexpensively manufactured.
本発明の目的は、上記事情を参酌してなされたもので、
ひっかき法によって薄膜を基板からはく離させ、そのは
く離した面積の大きさから薄膜の付着力の強さの程度を
高能率かつ高精度で評価することの可能な付着力評価方
法を提供することにある。The purpose of the present invention was achieved in consideration of the above circumstances, and
An object of the present invention is to provide an adhesion evaluation method that allows a thin film to be peeled off from a substrate using a scratching method, and the strength of the adhesion of the thin film to be evaluated with high efficiency and accuracy based on the size of the peeled area. .
〔発明の概要〕
本発明は、基板に付着した薄ｊ■迄のある一定面積内を
錐状の圧子により、疎部から密部へ連続的に変化する格
子状にひつかき、」二記一定面積とはく離した面積との
割合に基づいて薄膜の基板に対する付着力の強さの程度
を評価しようとしたものである。[Summary of the Invention] The present invention is based on the invention, in which a conical indenter is applied to a certain area of a thin film adhered to a substrate in a lattice shape that changes continuously from a sparse area to a dense area. This is an attempt to evaluate the strength of the adhesion of a thin film to a substrate based on the ratio of the area to the peeled area.
以下１本発明を図面を参照して、実施例に基づいて詳述
する。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described below in detail based on embodiments with reference to the drawings.
第１図は、本発明の一実施例の付着力評価方法に用いら
れる付着力評価装置を示している。Ｘステージ（１）は
、このＸステージ（１）に連設されたＸマイクロメータ
（２）のつまみ（２ａ）の回動によりＸ方向（第１図紙
面垂直方向）に移動できるように設けられている。この
Ｘステージ（１）上には、Ｘステージ（３）が、とのＸ
ステージ（３）に連設されたＸマイクロメータ（４）の
つまみ（４ａ）の回動によ！ｌｌ第１図矢印（５）のＹ
方向に摺接して移動できるように載設されている。そし
てＸステージ（１）とＸステージ（３）とは。FIG. 1 shows an adhesion force evaluation device used in an adhesion force evaluation method according to an embodiment of the present invention. The X stage (1) is provided so that it can be moved in the X direction (perpendicular to the paper in Figure 1) by rotating the knob (2a) of the X micrometer (2) connected to the X stage (1). ing. On this X stage (1), there is an X stage (3) with
By rotating the knob (4a) of the X micrometer (4) connected to the stage (3)! llY of arrow (5) in Figure 1
It is mounted so that it can be moved by sliding in the direction. And what are X stage (1) and X stage (3)?
基板（６ａ）と薄Ｍ （６ｂ）とから成る試料（６）を
載置するためのＸＸステージ（７）を構成している。一
方、このＸＸステージ（７）の上方には、レバー（８）
がレバー軸（９）に軸支され、矢印（ｉｏａ）、 （ｔ
ａｂ）方向に回動自在となっている。そして、レバー（
８）の一端部には。It constitutes an XX stage (7) on which a sample (6) consisting of a substrate (6a) and a thin M (6b) is placed. On the other hand, above this XX stage (7) is a lever (8).
is pivoted on the lever shaft (9), and arrows (ioa), (t
It is rotatable in the ab) direction. And the lever (
8) At one end.
先端がダイヤモンド製の円錐状の圧子（ＩＩ）が取材け
られている。また、圧子（１１）の上面には円環状の周
壁部αりに載置したおもり（１３）が設けられている。A conical indenter (II) with a diamond tip has been reported. Further, a weight (13) placed on the annular peripheral wall portion α is provided on the upper surface of the indenter (11).
このおもり（Ｉ３）の重さを任意に設定することにより
、圧子（１υによるひりかき条痕の大きさを変化させる
ことができる。０・っかき条痕の大きさ及びはく離面積
は、薄膜（６ｂ）の表面に対して任意に傾いた光軸（１
つをもつ顕微鏡（１（１）によって観６１すされる。By arbitrarily setting the weight of this weight (I3), it is possible to change the size of scratch marks caused by the indenter (1υ). The optical axis (1
Viewed using a microscope (1(1)) with two
つぎに、上ｆＱ ４’４′成の付着力評価装置を力］い
た付着力評価方法について説明する。まず、ＸＸステー
ジ（７）上面上に基板（６ａ）と薄膜（６ｂ）とから成
る板状試料（６）を載置する。つぎに、圧子（Ｉｔ）加
圧用の任意のおもり（１３１を周壁部（１４に裁置し、
レバー軸（９）を矢印（１０ａ）の方向に回転させるこ
とにより、圧子αυを？！７−膜（６ｂ）の第２図に示
す顕微鏡視野部（（６）の始点σ優に押しつける。つぎ
に、Ｘマイクロメータ（４）のつまみ（４ａ）を一定速
度、例えばＯ，１１１１ｍ７秒で回動し。Next, an explanation will be given of an adhesion force evaluation method using an adhesion force evaluation apparatus having the above fQ 4'4' configuration. First, a plate-shaped sample (6) consisting of a substrate (6a) and a thin film (6b) is placed on the upper surface of the XX stage (7). Next, an arbitrary weight (131) for pressurizing the indenter (It) is placed on the peripheral wall (14,
By rotating the lever shaft (9) in the direction of the arrow (10a), the indenter αυ can be moved ? ! 7-Press the membrane (6b) onto the starting point σ of the microscope field of view ((6) shown in Figure 2).Next, press the knob (4a) of the X micrometer (4) at a constant speed, e.g. Rotate.
Ｘステージ（３）を第１図の左から右方向に１２０μｍ
移動させ、条痕（ｉ７ａ）をＮ膜（６ｂ）の表面に形成
する。Move the X stage (3) 120 μm from left to right in Figure 1.
The N film (6b) is moved to form streaks (i7a) on the surface of the N film (6b).
条痕（１７ａ）形成後、第１図のレバー軸（９）を矢印
（１０ｂ）の方向に回転させることによシ、圧子（１１
）を薄膜（６ｂ）の条痕（１７ａ）の終点（２＠から離
間させる。つぎＫ。After forming the striations (17a), by rotating the lever shaft (9) in the direction of the arrow (10b) in FIG.
) is separated from the end point (2@) of the streak (17a) of the thin film (6b). Next, K.
Ｘマイクロメータ（２）のつ１み（２ａ）の回動によシ
Ｘ方向第１図紙面の裏から表方向に３０μｍ（１００μ
ｍ ｘ Ｌｏｐ２）移動させ、前と同様にして条痕（１
７ａ）に平行な条痕（１７ｂ）を形成する。以下同様に
して、始点（１１からＸ方向に１００μｍｘＬｏｙｎ
（ここでｎは、ひっかきの本数）の間隔で１０本の条痕
（１７Ｃ）、 （１７ｄ）、・・・を形成する。ついで
、Ｙ方向の条痕（１７ａ）、〜、（１７ｊ）と同様の手
順により、１００μ＋ｎｘＪｏｙｎ（ここで、ｎはひっ
かきの本数）間隔でＸ方向の条痕（１８ａ）、〜、（１
８ｊ）を１０本形成する。このようＫして得られたＸＹ
方向の条痕（１７ａ）、・・・、（１７ｊ ）、 （１
８ａ）、・・・、（Ｉｓｊ ）は、第２図の顕微鏡視野
部αＱに示すように、１００μｍＸ１００μｍの面積の
簿膜（６ｂ）表面を８１区画に分割している。この場合
、格子面積の小さな部分は格子面積の大きな部分よりも
、ひっかきによって生じた内部応力の影響により、薄膜
にはく離が生じ易い傾向をもっている。また、このよう
なはく離の大きさは。By rotating the knob (2a) of the X micrometer (2), the distance is 30 μm (100 μm) in the
m x Lop2) and create a streak (1
A streak (17b) parallel to 7a) is formed. Similarly, from the starting point (11 to 100 μm x Loyn in the X direction)
Ten streaks (17C), (17d), . . . are formed at intervals of (where n is the number of scratches). Next, by the same procedure as the Y-direction striations (17a), ~, (17j), X-direction striations (18a), ~, (1
Form 10 pieces of 8j). XY obtained by K in this way
Directional streaks (17a), ..., (17j), (1
8a), . . . , (Isj), the surface of the book membrane (6b) with an area of 100 μm×100 μm is divided into 81 sections, as shown in the microscope field of view αQ in FIG. In this case, parts with a small lattice area are more likely to cause peeling of the thin film than parts with a large lattice area due to the influence of internal stress caused by scratching. Also, what is the size of such peeling?
付着力の強い薄膜では、はく離面積が小さく、逆に、弱
い薄膜では、はく離面積が大きくなる。したがって、付
着力の強さの程度を比較するだめのはく離面積比ａを次
式で定義することができる。A thin film with strong adhesion has a small peeling area, and a weakly adhesive thin film has a large peeling area. Therefore, the peeling area ratio a for comparing the strength of adhesion can be defined by the following equation.
ａ ＝ Ａ ／ Ａｏ
ただし、この式において、Ａは、はくｈ１１面積（μｍ
２）。a = A / Ao However, in this formula, A is the area of the wall (μm
2).
及び、Ａｏは、格子総面積（μｎ］２）である。ちなみ
に、本実施例においては、Ａｏは、１００μｍ ｘ １
００μｍ＝ １００００μｍ２である。かくして、はく
離面積比ａが小さい場合は、付着力が強く、逆に、大き
い場合は、付着力が弱いと評価する。And Ao is the total lattice area (μn] 2). Incidentally, in this example, Ao is 100 μm x 1
00μm=10000μm2. Thus, when the peeled area ratio a is small, the adhesive force is evaluated to be strong, and conversely, when it is large, the adhesive force is evaluated to be weak.
以上のように、本実施例の（＝Ｊ着力評価方法ｔ」、。As described above, (=J adhesion evaluation method t) of this embodiment.
条痕（１７ａ）、・・・、（１７ｊ ）、 （１８ａ）
、・・・、（１ｓｊ ）を両対数目盛状に形成したので
、はく離の生じた部分と生じていない部分の見分けが容
易につくとともに１面積計数が容易となり、はく離した
面積の大きさから薄膜の付着力の程度を、能率的にしか
も関精度で評価することが可能となる。Streaks (17a),..., (17j), (18a)
, ..., (1sj) are formed in a double-logarithmic scale, so it is easy to distinguish between areas where peeling has occurred and areas where no peeling has occurred, and it is also easy to count one area. It becomes possible to efficiently and accurately evaluate the degree of adhesion.
なお、上記実施例においては、圧子αυの先端形状を円
錐状としたが、四角錐状であってもよい。In the above embodiments, the tip of the indenter αυ has a conical shape, but it may also have a square pyramid shape.
また、格子間隔は、上記実施例では対数目盛間隔とした
が、その間隔に制約されることはなく、要するに、ある
一定面積内においてはく離の生じた部分と生じていない
部分の見分けがつくように格子間隔を疎部から密部へ連
続的に変化させたものであればよく、例えば等比間隔で
もよい。のみならず、ＸＹ方向の条痕は必ずしも１ケ交
の必要はなく、格子内部形状が菱形、つ寸りＸ方向とＹ
方向の交差角が鋭角であってもよい。さらに、と記党施
例においては、顕微鐘（１４）をはく離面積の測定用に
用いたが、 ＩＴＶカメラを用いた画像解析装置を用い
るとよシ便利である。In addition, although the grid spacing was set to a logarithmic scale spacing in the above embodiment, it is not limited to that spacing, and in short, it is designed so that it is possible to distinguish between areas where peeling has occurred and areas where no peeling has occurred within a certain area. It is sufficient if the lattice spacing is continuously changed from a sparse portion to a dense portion, for example, a geometric spacing may be used. In addition, it is not necessary that only one striation in the X and Y directions intersects, and the internal shape of the grid is rhombic, and the dimensions are in the X and Y directions.
The intersecting angle of the directions may be an acute angle. Furthermore, in the present example, a microscope bell (14) was used to measure the peeling area, but it would be more convenient to use an image analysis device using an ITV camera.
発明の付着力評価方法は、高能率かつ高１’ｉ７度で付
着力の評価が可能となり、測定能率及び測定精度が向上
する。また、はく離時のひっかき荷重測定法に比べて、
安価に、かつ簡便に装置を製作できる利点を有している
。The adhesion force evaluation method of the invention enables evaluation of adhesion force with high efficiency and high 1'i7 degrees, improving measurement efficiency and measurement accuracy. In addition, compared to the scratch load measurement method during peeling,
It has the advantage that the device can be manufactured easily and at low cost.
第１図は本発明の一実施例の付着力評価方法に用いられ
る付着力評価装置の要部構成図、第２図は第１回に示す
ｆづ着力計測装置を用いたけ漬方評価方法の説明図であ
る。
（６）：試料（被測定物） 、 （６ｂ） ：薄膜。
α１）：圧子。
（１７ａ）、・・・、（１７ｊ）、 （１８ａ）、・・
・、（ＩＵ） ：条痕。
代理人 弁理士 則 近 憲 （ｈ
（Ｉ−１か１名）
第 １ 図Fig. 1 is a block diagram of the main parts of an adhesion evaluation device used in the adhesion evaluation method according to an embodiment of the present invention, and Fig. 2 is a diagram of the immersion evaluation method using the f-adhesion measurement device shown in Part 1. It is an explanatory diagram. (6): Sample (object to be measured), (6b): Thin film. α1): Indenter. (17a),..., (17j), (18a),...
・, (IU): Streak. Agent Patent attorney Ken Chika (h (I-1 or 1 person) Figure 1
Claims (2)
によシ間隔を規則的に変動させてひっかき、疎部から密
部へ連続的に変化する格子状の条痕を形成する方法と、
上記測定域の面積に対する上記ひっかきにより発生した
上記薄膜の上記被測定物からのはく雌部分の割合に基づ
き上記薄膜の上記被測定物に対する付着力を評価する方
法とを具備することを特徴とする付着力評価方法。(1) A conical indenter scratches the measurement area of the object to be measured to which a thin film is attached by regularly varying the pitch to form grid-like scratches that continuously change from sparse areas to dense areas. method and
A method for evaluating the adhesion force of the thin film to the object to be measured based on the ratio of the peeled portion of the thin film from the object to be measured caused by the scratching to the area of the measurement area. Adhesion evaluation method.
特許請求の範囲第１項記載の付着力評価方法。(2) The adhesion force evaluation method according to claim 1, characterized in that the streaks are formed in a logarithmic scale shape.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59052312A JPS60196644A (en) | 1984-03-21 | 1984-03-21 | Adhesion evaluating method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59052312A JPS60196644A (en) | 1984-03-21 | 1984-03-21 | Adhesion evaluating method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS60196644A true JPS60196644A (en) | 1985-10-05 |
Family
ID=12911260
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP59052312A Pending JPS60196644A (en) | 1984-03-21 | 1984-03-21 | Adhesion evaluating method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60196644A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02120645A (en) * | 1988-10-28 | 1990-05-08 | Shimadzu Corp | Apparatus for measuring surface characteristics |
| JPH0475952U (en) * | 1990-11-16 | 1992-07-02 | ||
| WO2003008938A3 (en) * | 2001-07-16 | 2003-05-22 | Siemens Ag | Method for determining the adhesiveness of a coating on a component |
| FR2848723A1 (en) * | 2002-12-16 | 2004-06-18 | Soitec Silicon On Insulator | Semiconductor substrate plates disintegrating tool for manufacturing semiconductor substrate, has control device relocating one handling unit with respect to another, and actuator inducing controlled flexion |
| US7187162B2 (en) | 2002-12-16 | 2007-03-06 | S.O.I.Tec Silicon On Insulator Technologies S.A. | Tools and methods for disuniting semiconductor wafers |
| WO2009040999A1 (en) * | 2007-09-27 | 2009-04-02 | Daikin Industries, Ltd. | Crosscut testing method, and cross-cut testing device |
-
1984
- 1984-03-21 JP JP59052312A patent/JPS60196644A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02120645A (en) * | 1988-10-28 | 1990-05-08 | Shimadzu Corp | Apparatus for measuring surface characteristics |
| JPH0549944B2 (en) * | 1988-10-28 | 1993-07-27 | Shimadzu Corp | |
| JPH0475952U (en) * | 1990-11-16 | 1992-07-02 | ||
| WO2003008938A3 (en) * | 2001-07-16 | 2003-05-22 | Siemens Ag | Method for determining the adhesiveness of a coating on a component |
| FR2848723A1 (en) * | 2002-12-16 | 2004-06-18 | Soitec Silicon On Insulator | Semiconductor substrate plates disintegrating tool for manufacturing semiconductor substrate, has control device relocating one handling unit with respect to another, and actuator inducing controlled flexion |
| US7187162B2 (en) | 2002-12-16 | 2007-03-06 | S.O.I.Tec Silicon On Insulator Technologies S.A. | Tools and methods for disuniting semiconductor wafers |
| US7740735B2 (en) | 2002-12-16 | 2010-06-22 | S.O.I.Tec Silicon On Insulator Technologies | Tools and methods for disuniting semiconductor wafers |
| WO2009040999A1 (en) * | 2007-09-27 | 2009-04-02 | Daikin Industries, Ltd. | Crosscut testing method, and cross-cut testing device |
| EP2204644A4 (en) * | 2007-09-27 | 2015-08-05 | Daikin Ind Ltd | Crosscut testing method, and cross-cut testing device |
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