JP2002350330A - Method and apparatus for measuring adhesion of thin film - Google Patents

Method and apparatus for measuring adhesion of thin film

Info

Publication number
JP2002350330A
JP2002350330A JP2001160690A JP2001160690A JP2002350330A JP 2002350330 A JP2002350330 A JP 2002350330A JP 2001160690 A JP2001160690 A JP 2001160690A JP 2001160690 A JP2001160690 A JP 2001160690A JP 2002350330 A JP2002350330 A JP 2002350330A
Authority
JP
Japan
Prior art keywords
thin film
rubbing
measuring
load
support
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.)
Pending
Application number
JP2001160690A
Other languages
Japanese (ja)
Inventor
Yukiyasu Nakao
之泰 中尾
Yasuhiro Yoshida
育弘 吉田
Tetsuyuki Kurata
哲之 蔵田
Sadaji Takahashi
貞治 高橋
Mikako Maeda
美佳子 前田
Masaru Fujii
優 藤井
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Mitsubishi Electric Corp
Original Assignee
Mitsubishi Electric Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Mitsubishi Electric Corp filed Critical Mitsubishi Electric Corp
Priority to JP2001160690A priority Critical patent/JP2002350330A/en
Priority to TW090121558A priority patent/TW505785B/en
Priority to KR1020010055144A priority patent/KR20020090835A/en
Publication of JP2002350330A publication Critical patent/JP2002350330A/en
Pending legal-status Critical Current

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Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N19/00Investigating materials by mechanical methods
    • G01N19/04Measuring adhesive force between materials, e.g. of sealing tape, of coating
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/227Measuring photoelectric effect, e.g. photoelectron emission microscopy [PEEM]
    • G01N23/2273Measuring photoelectron spectrum, e.g. electron spectroscopy for chemical analysis [ESCA] or X-ray photoelectron spectroscopy [XPS]

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  • 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)
  • Spectroscopy & Molecular Physics (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)
  • Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)

Abstract

PROBLEM TO BE SOLVED: To provide a measuring method and a measuring apparatus used for the method which are not limited by composition of a thin film, types of substrates and a mechanical vibration during measurement, etc., and can mea sure adhesion of the thin film having a thickness of the order of nanometers. SOLUTION: A base fixed to a support and having the thin film on a surface is placed in the vicinity of a scratching member attached to a lower face of a load adding mechanism. A loading member is mounted on an upper face of the load adding mechanism. The thin film and the scratching member are in a closely contacting state. The support or the load adding mechanism moves in the horizontal direction of the base. The thin film is scratched by the scratching member. The scratched surface of the thin film is analyzed. The adhesion of the thin film to the base is measured.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は、薄膜の基板に対す
る付着力の測定方法及びその測定方法に用いる測定装置
に関し、より詳しくは膜厚がナノメータオーダである薄
膜の基板に対する付着力の測定方法及びその測定方法に
用いる測定装置に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for measuring the adhesion of a thin film to a substrate and a measuring apparatus used for the method. The present invention relates to a measuring device used for the measuring method.

【0002】[0002]

【従来の技術】表面反射防止膜,表面帯電防止膜等の機
能性無機薄膜を有するデバイスに対し、その表面の防汚
や傷防止を目的として、シランカップリング剤、アルミ
ニウム型カップリング剤、そしてチタネート系カップリ
ング剤等のカップリング剤が塗布されている。カップリ
ング剤は、上記の無機薄膜と単分子レベルで化学結合を
形成し、数nm程度の厚さの薄膜からなる保護層を形成
する。この保護層の上記の無機薄膜に対する付着力は、
保護層の形成条件の影響を受ける。したがって、高い付
着力を得るためには、保護層の付着力を定量的に評価
し、その結果を保護層の形成条件にフィードバックして
いく必要がある。
2. Description of the Related Art For devices having a functional inorganic thin film such as a surface anti-reflection film and a surface anti-static film, a silane coupling agent, an aluminum-type coupling agent, A coupling agent such as a titanate-based coupling agent is applied. The coupling agent forms a chemical bond with the above-mentioned inorganic thin film at a monomolecular level, and forms a protective layer composed of a thin film having a thickness of about several nm. The adhesion of the protective layer to the inorganic thin film is
It is affected by the conditions for forming the protective layer. Therefore, in order to obtain a high adhesion, it is necessary to quantitatively evaluate the adhesion of the protective layer and feed back the result to the conditions for forming the protective layer.

【0003】薄膜の付着力測定方法としては、ひっかき
法がよく知られている。ひっかき法は,硬い針等の圧子
を薄膜にある荷重下で押し付けた状態で動かし、ひっか
きによって薄膜を基板から引き剥がす方法であり、薄膜
表面にひっかき傷を形成する荷重、あるいは摩擦係数の
急激な上昇が生じる荷重(臨界荷重値)を薄膜と基板間
の密着力としている。例えば、特開昭64−31036
号公報には、薄膜/基板間の界面における破壊や剥離に
伴う薄膜内部のアコースティク・エミッション信号を測
定して薄膜の付着力を測定する方法が提案されている。
また、特開平7−325028号公報には、薄膜の剥離
部を透過若しくは反射する光を測定して薄膜の剥離を検
出する方法が提案されている。
[0003] As a method for measuring the adhesive force of a thin film, a scratch method is well known. The scratching method is a method in which an indenter such as a hard needle is moved while being pressed against a thin film under a certain load, and the thin film is peeled off from the substrate by scratching. The load that forms a scratch on the thin film surface or the sharp friction coefficient The load at which the rise occurs (critical load value) is defined as the adhesion between the thin film and the substrate. For example, JP-A-64-31036
Japanese Patent Application Laid-Open Publication No. H11-163873 proposes a method for measuring the adhesion force of a thin film by measuring an acoustic emission signal inside the thin film due to destruction or peeling at the interface between the thin film and the substrate.
Further, Japanese Patent Application Laid-Open No. 7-325028 proposes a method of measuring the light transmitted or reflected at a peeling portion of a thin film to detect the peeling of the thin film.

【0004】[0004]

【発明が解決しようとする課題】しかしながら、ひっか
き法は、測定可能な薄膜の膜厚がミクロンオーダあるい
はサブミクロンオーダに限定され、ナノメータオーダの
膜厚の薄膜には適用できないという問題がある。また、
延性材料からなる薄膜に対しては、ひっかき針の前方に
形成される隆起により摩擦係数が増大して測定が困難で
あり、測定対象が酸化膜、窒化膜及び炭化膜等の硬質膜
に限定されるという問題もある。また、密着力の算出に
必要な臨界荷重値は,基板硬度と膜厚に複雑に依存する
ため,異なるサンプル間で密着力を比較する場合,同ー
硬度の基板及び同ー膜厚の薄膜のサンプルに限定される
という問題もある。また、測定時の機械的振動により薄
膜の剥離を検出する手段の感度が低下し、測定の精度が
低下するという問題もあった。
However, the scratching method has a problem that the thickness of a measurable thin film is limited to a micron order or a submicron order, and cannot be applied to a thin film having a thickness of a nanometer order. Also,
For a thin film made of a ductile material, the coefficient of friction increases due to the bulge formed in front of the scratching needle, making measurement difficult, and the measurement target is limited to hard films such as oxide films, nitride films, and carbide films. There is also a problem that. Also, the critical load value required for calculating the adhesion force depends on the substrate hardness and the film thickness in a complicated manner. Therefore, when comparing the adhesion force between different samples, when comparing the adhesion force between a substrate having the same hardness and a thin film having the same thickness, There is also the problem of being limited to samples. In addition, there is a problem that the sensitivity of the means for detecting the peeling of the thin film due to mechanical vibration during measurement decreases, and the accuracy of measurement decreases.

【0005】そこで、本発明は上記課題を解決し、薄膜
の組成や基板の種類、そして測定時の機械的振動等に限
定されることなく、膜厚がナノメータオーダの薄膜の付
着力の測定が可能な測定方法及びその方法に用いる測定
装置を提供することを目的とした。
Accordingly, the present invention solves the above-mentioned problems, and is not limited to the composition of the thin film, the type of the substrate, and the mechanical vibration at the time of measurement, and can measure the adhesive force of a thin film having a thickness of the order of nanometers. An object of the present invention is to provide a possible measuring method and a measuring device used for the method.

【0006】[0006]

【課題を解決するための手段】上記課題を解決するた
め、本発明の薄膜の付着力測定方法は、支持体上に固定
され表面に薄膜を有する基体と、前記支持体上に支持さ
れ前記薄膜を擦過する荷重付加機構の下面に取り付けら
れた擦過部材とを近接させ、前記荷重付加機構の上面に
荷重部材を搭載して前記薄膜と前記擦過部材とを密着状
態とし、前記支持体又は荷重付加機構を基体の水平方向
に進退運動せしめて擦過部材により薄膜を擦過し、擦過
された薄膜の表面分析を行い、薄膜の基体に対する付着
力を測定することを特徴とする。
In order to solve the above-mentioned problems, a method for measuring the adhesion of a thin film according to the present invention comprises a substrate fixed on a support and having a thin film on the surface; A rubbing member attached to the lower surface of the load applying mechanism for rubbing is brought into close proximity, a load member is mounted on the upper surface of the load applying mechanism to bring the thin film and the rubbing member into close contact with each other, and the support or the load The mechanism is characterized by moving the mechanism forward and backward in the horizontal direction of the substrate, rubbing the thin film with a rubbing member, analyzing the surface of the rubbed thin film, and measuring the adhesion of the thin film to the substrate.

【0007】本発明の付着力測定方法によれば、下面に
擦過部材を有し、上面に荷重部材を有する荷重付加機構
を用い、荷重部材からの荷重が擦過部材に加わるように
したので、擦過部材を常に薄膜と密着した状態で薄膜を
擦過することができる。これにより、膜厚がナノメータ
オーダの薄膜であっても、その薄膜の表面を擦過するこ
とができる。また、薄膜を擦過後、擦過により変化した
薄膜表面の組成や状態を分析するようにしたので、薄膜
の基板からの剥離を検出する必要がなく、剥離検出用の
アコースティック・エミッション装置や光検出装置等の
薄膜の剥離検出手段が不要となる。これにより、付着力
の測定が、薄膜の組成や基板の種類、そして擦過時の機
械的振動等に影響されることがないので、サンプルの種
類に限定されることがない。また、擦過した薄膜を高感
度の表面分析方法を用いて分析することができるので、
より精度の高い測定が可能となる。
According to the adhesive force measuring method of the present invention, the load from the load member is applied to the rubbing member by using the load applying mechanism having the rubbing member on the lower surface and the load member on the upper surface. The thin film can be rubbed with the member always in close contact with the thin film. Thus, even if the thickness of the thin film is on the order of nanometers, the surface of the thin film can be rubbed. In addition, after the thin film is rubbed, the composition and state of the thin film surface changed by the rubbing are analyzed, so there is no need to detect the peeling of the thin film from the substrate, and an acoustic emission device or a light detecting device for detecting the peeling. This eliminates the need for thin film peeling detecting means such as the above. Thus, the measurement of the adhesive force is not affected by the composition of the thin film, the type of the substrate, the mechanical vibration at the time of rubbing, and the like, and is not limited to the type of the sample. In addition, the rubbed thin film can be analyzed using a highly sensitive surface analysis method,
Higher precision measurement is possible.

【0008】また、本発明の付着力測定方法は、荷重付
加機構を支持体の垂直方向に昇降可能に支持させ、荷重
付加機構を降下せしめて擦過部材を薄膜とを近接させ、
薄膜を擦過した後、荷重付加機構を上昇せしめて擦過部
材を薄膜から離間させることができる。
In the method for measuring an adhesive force according to the present invention, the load applying mechanism is supported so as to be able to move up and down in the vertical direction of the support, and the load applying mechanism is lowered to bring the scraping member close to the thin film.
After rubbing the thin film, the load applying mechanism can be raised to separate the rubbing member from the thin film.

【0009】また、本発明の付着力測定方法には、擦過
部材として布材を用いることができる。
Further, in the method for measuring adhesive force according to the present invention, a cloth material can be used as the rubbing member.

【0010】また、本発明の付着力測定方法には、表面
分析として表面接触角測定法を用いることができる。
In the method for measuring adhesive force according to the present invention, a surface contact angle measuring method can be used as a surface analysis.

【0011】また、本発明の付着力測定方法には、表面
分析として光電子分光法を用いることができる。
In the method for measuring adhesive force according to the present invention, photoelectron spectroscopy can be used for surface analysis.

【0012】本発明の薄膜の付着力測定装置は、基体上
に形成された薄膜の前記基体に対する付着力の測定に使
用される薄膜の付着力測定装置であって、基体上に形成
された薄膜の前記基体に対する付着力の測定に使用され
る薄膜の付着力測定装置であって、基体を固定する支持
体と、前記支持体上に配置され、下面には擦過部材を有
し、上面には前記擦過部材を前記薄膜に密着させる着脱
自在の荷重部材を有する荷重付加機構と、前記支持体又
は前記荷重付加機構を基体の水平方向に移動可能に支持
し、薄膜と擦過部材とを密着させた状態で、支持した支
持体又は荷重付加機構を基体の水平方向に進退運動せし
める駆動機構と、前記駆動機構に固着されてなり、前記
荷重付加機構を基体の垂直方向に移動可能に支持する摺
動支持機構と、前記駆動機構又は前記支持体を基体の垂
直方向に移動可能に支持し、薄膜と擦過部材とを近接又
は離間させる昇降機構と、前記荷重付加機構と連動して
薄膜と擦過部材とを密着させるように昇降機構を作動さ
せ、薄膜と擦過部材とを密着させた状態で支持体又は荷
重付加機構を基体の水平方向に進退運動せしめるように
駆動機構を作動させる制御手段と、を有する薄膜擦過部
と、該薄膜擦過部により擦過された薄膜の表面状態を測
定する表面分析部と、から成ることを特徴とする。
An apparatus for measuring the adhesion of a thin film according to the present invention is an apparatus for measuring the adhesion of a thin film formed on a substrate to a substrate, wherein the apparatus for measuring the adhesion of the thin film formed on the substrate is used. An adhesive force measuring device for a thin film used for measuring the adhesive force to the substrate, wherein a support for fixing the substrate, disposed on the support, a lower surface has a scraping member, and an upper surface A load applying mechanism having a detachable load member for bringing the rubbing member into close contact with the thin film, and the support or the load applying mechanism movably supported in the horizontal direction of the base, and the thin film and the rubbing member were brought into close contact with each other. A driving mechanism for moving the supported support or the load applying mechanism in the horizontal direction of the base in the state, and a slide fixed to the drive mechanism and supporting the load applying mechanism movably in the vertical direction of the base. Support mechanism and front A drive mechanism or the supporter is supported so as to be movable in the vertical direction of the base, and an elevating mechanism for moving the thin film and the rubbing member close to or away from each other, and the thin film and the rubbing member in close contact with the load applying mechanism. Activating the elevating mechanism, a control means for operating a driving mechanism to cause the support or the load applying mechanism to move forward and backward in the horizontal direction of the base in a state where the thin film and the scraping member are in close contact with each other, And a surface analysis unit for measuring a surface state of the thin film rubbed by the thin film rubbing unit.

【0013】また、本発明の付着力測定装置は、荷重部
材に積層可能な1以上の板材を用いることができる。そ
の1以上の板材を荷重付加機構の上面に積層することに
より、擦過部材へ付加される荷重を調整することができ
る。
Further, the adhesive force measuring device of the present invention can use one or more plate members that can be laminated on the load member. By laminating the one or more plate members on the upper surface of the load applying mechanism, the load applied to the rubbing member can be adjusted.

【0014】また、本発明の付着力測定装置は、荷重付
加機構が駆動機構に固着されたものを用いることができ
る。昇降機構により荷重付加機構を昇降させて、薄膜と
擦過部材とを近接させることができる。
Further, as the adhesive force measuring device of the present invention, a device in which a load applying mechanism is fixed to a driving mechanism can be used. The thin film and the scraping member can be brought close to each other by raising and lowering the load applying mechanism by the lifting mechanism.

【0015】また、本発明の付着力測定装置は、荷重付
加機構を基体の水平方向に進退運動させたときに生じる
摩擦力を測定する摩擦力測定手段を支持体に取付けるこ
とができる。
Further, in the adhesive force measuring device of the present invention, a frictional force measuring means for measuring a frictional force generated when the load applying mechanism is moved in the horizontal direction of the base can be attached to the support.

【0016】また、本発明の付着力測定装置は、表面分
析部に表面接触角計を用いることができる。
Further, in the adhesive force measuring device of the present invention, a surface contact angle meter can be used in the surface analyzing section.

【0017】また、本発明の付着力測定装置は、表面分
析部に光電子分光器を用いることができる。
Further, in the adhesive force measuring device of the present invention, a photoelectron spectrometer can be used in the surface analyzing section.

【0018】[0018]

【発明の実態の形態】以下、図面を用いて、本発明の実
施の形態について説明する。図1及び2は、本発明に係
る薄膜の付着力測定装置に用いる薄膜擦過部の1例の構
成を示す模式図であり、図1は側面図、図2は図1のI
I−II′線における断面図を含む正面図である。
Embodiments of the present invention will be described below with reference to the drawings. 1 and 2 are schematic diagrams showing the configuration of an example of a thin film rubbing unit used in the thin film adhesion measuring device according to the present invention. FIG. 1 is a side view, and FIG.
FIG. 2 is a front view including a cross-sectional view taken along line I-II ′.

【0019】薄膜擦過部50は、表面に薄膜36を有す
る基体35を固定する支持体1と、支持体1を架台37
に固定する固定部材2と、支持体1上に配置され、下面
に擦過部材10を有し上面に荷重部材6を有する荷重付
加機構5と、荷重付加機構5を基体35の垂直方向に移
動可能に支持する摺動支持機構25と、摺動支持機構2
5が固着され荷重付加機構を基体35の水平方向に進退
移動させる駆動機構15と、駆動機構15を基体35の
垂直方向に移動させる昇降機構20とから成る擦過機構
40と、昇降機構20と駆動機構15の動作を制御する
制御機構(図示せず)と、から成っている。
The thin film scraping section 50 comprises a support 1 for fixing a base 35 having a thin film 36 on its surface, and a support 37
And a load applying mechanism 5 disposed on the support 1 and having a scraping member 10 on the lower surface and a load member 6 on the upper surface, and the load applying mechanism 5 can be moved in the vertical direction of the base 35. Sliding support mechanism 25 for supporting on
5, a rubbing mechanism 40 including a driving mechanism 15 for moving the load applying mechanism forward and backward in the horizontal direction of the base 35, and a lifting mechanism 20 for moving the driving mechanism 15 in the vertical direction of the base 35; A control mechanism (not shown) for controlling the operation of the mechanism 15.

【0020】荷重付加機構5は、下面側から、擦過部材
10と、擦過部材10を着脱可能に固定する擦過部材固
定手段9と、擦過部材固定手段9と連結部8aを介して
一体的に形成された荷重部材用ステージ8と、下端が荷
重部材用ステージ8の上端部に螺合され上端が荷重部材
用ステージ8の上方に伸びる荷重部材用固定ロッド7
と、荷重部材用固定ロッド7が摺動可能な貫通するガイ
ド穴(図示せず)を有する1以上の板材からなる荷重部
材6と、から成っている。荷重部材用固定ロッド7にガ
イド穴を貫通させて板材を嵌め込み、板材を荷重部材用
ステージ8上に固定する。
The load applying mechanism 5 is integrally formed from the lower surface side through the rubbing member 10, the rubbing member fixing means 9 for detachably fixing the rubbing member 10, and the rubbing member fixing means 9 and the connecting portion 8a. And a load member fixing rod 7 whose lower end is screwed to the upper end of the load member stage 8 and whose upper end extends above the load member stage 8.
And a load member 6 made of one or more plates having a guide hole (not shown) through which the load member fixing rod 7 can slide. The plate material is fitted into the load member fixing rod 7 by penetrating the guide hole, and the plate material is fixed on the load member stage 8.

【0021】摺動支持機構25は、荷重部材用ステージ
8の連結部8aを摺動可能に支持する摺動手段27と、
摺動手段の一端に設けられた接続手段26と、から成
り、接続手段26は駆動機構15に固着されている。摺
動手段27は、連結部8aの周囲に嵌め込まれる一対の
着脱自在の嵌め込み部材29,31を有している。一方
の嵌め込み部材31は枠体28に嵌め込まれて使用され
る。他方の嵌め込み部材29を連結部8aを介して嵌め
込み部材31及び枠体28と当接させ、固定部材30を
嵌め込み部材29及び枠体28に螺合させることによ
り、連結部8aを嵌め込み部材29,31に摺動可能に
挟持させる。
The sliding support mechanism 25 includes sliding means 27 for slidably supporting the connecting portion 8a of the load member stage 8,
Connecting means 26 provided at one end of the sliding means, and the connecting means 26 is fixed to the drive mechanism 15. The sliding means 27 has a pair of detachable fitting members 29 and 31 fitted around the connecting portion 8a. One fitting member 31 is used by being fitted into the frame 28. The other fitting member 29 is brought into contact with the fitting member 31 and the frame 28 via the connecting portion 8a, and the fixing member 30 is screwed to the fitting member 29 and the frame 28, thereby connecting the connecting portion 8a to the fitting member 29, 31 so as to be slidable.

【0022】駆動機構15は、可動手段17と、可動手
段17を基体の水平方向に移動させる移動用レール18
を有する駆動手段16と、から成っている。可動手段1
7には摺動支持機構25の接続手段26が固着されてい
るので、可動手段17を移動させることにより、荷重付
加機構5を基体の水平方向に移動させることができる。
The driving mechanism 15 includes a movable means 17 and a moving rail 18 for moving the movable means 17 in the horizontal direction of the base.
And driving means 16 having Movable means 1
Since the connecting means 26 of the sliding support mechanism 25 is fixed to the, the moving means 17 can be moved to move the load applying mechanism 5 in the horizontal direction of the base.

【0023】昇降機構20は、ネジ機構により駆動機構
15を介して重量付加機構5を基体35の水平方向に移
動させるハンドル21と、擦過部材10を基体35上の
所望の高さに保持するロック22と、から成っている。
The lifting mechanism 20 includes a handle 21 for moving the weight adding mechanism 5 in the horizontal direction of the base 35 via a driving mechanism 15 by a screw mechanism, and a lock for holding the rubbing member 10 at a desired height on the base 35. 22.

【0024】次に、図2により、薄膜擦過部50の動作
を説明する。表面に薄膜36を有する基体35が支持体
1上に固定されている。ここで、支持体1は、ワイヤ3
により両端を釣り下げられ、基体35の水平方向に移動
可能な状態で支持されている。さらに、支持体の両端部
にはそれぞれ摩擦力測定手段としてのロードセル4が取
付けられ、擦過部材10と薄膜36との間に生じる摩擦
力を測定することが可能な構成となっている。
Next, the operation of the thin film scraping section 50 will be described with reference to FIG. A base 35 having a thin film 36 on the surface is fixed on the support 1. Here, the support 1 is a wire 3
Thus, both ends are hung down, and the base 35 is supported so as to be movable in the horizontal direction. Further, load cells 4 as frictional force measuring means are attached to both ends of the support, respectively, so that the frictional force generated between the rubbing member 10 and the thin film 36 can be measured.

【0025】荷重付加機構5は荷重部材6を取り外した
状態で、基体35上の所定の待機位置に保持され、昇降
機構20のハンドル21を回転させて、荷重付加機構5
を所定の近接位置まで降下させる。次いで、荷重部材固
定手段8上に荷重部材6を搭載して固定し、荷重部材6
の荷重を擦過部材10に付加して、擦過部材10を薄膜
36に密着させる。ここで、連結部8aは嵌め込み部材
29,31により摺動可能に支持されており、荷重部材
6の荷重により降下する。
The load applying mechanism 5 is held at a predetermined standby position on the base 35 with the load member 6 removed, and the handle 21 of the lifting / lowering mechanism 20 is rotated to cause the load applying mechanism 5 to rotate.
Is lowered to a predetermined proximity position. Next, the load member 6 is mounted and fixed on the load member fixing means 8.
Is applied to the rubbing member 10 to bring the rubbing member 10 into close contact with the thin film 36. Here, the connecting portion 8 a is slidably supported by the fitting members 29 and 31, and is lowered by the load of the load member 6.

【0026】擦過部材10を薄膜36に密着させた状態
で、可動手段17を移動レール18上で基体5の水平方
向に進退運動せしめることにより、擦過部材10により
薄膜36を擦過することができる。擦過回数、擦過距離
そして擦過速度等は、制御機構45により可動手段17
の進退回数、進退移動距離及び進退移動速度を制御して
変化させることができる。
The thin film 36 can be rubbed by the rubbing member 10 by moving the movable means 17 on the moving rail 18 in the horizontal direction while the rubbing member 10 is in close contact with the thin film 36. The number of times of rubbing, the rubbing distance, the rubbing speed, and the like are controlled by
The number of forward / backward movements, forward / backward moving distance and forward / backward moving speed can be controlled and changed.

【0027】次いで、進退運動を繰り返して薄膜36を
所定の回数擦過した後、可動手段17の進退運動を停止
させ、荷重部材6を取り外し、荷重付加機構5を上昇さ
せて擦過部材10と基体35とを離間させる。次いで、
基体35を支持体1から取り外し、所定の表面分析部
(図示せず)を用い擦過された薄膜の表面状態の分析を
行う。
Next, after the thin film 36 is rubbed a predetermined number of times by repeating the forward and backward movements, the forward and backward movement of the movable means 17 is stopped, the load member 6 is removed, the load applying mechanism 5 is raised, and the rubbing member 10 and the base 35 are lifted. And separated. Then
The substrate 35 is removed from the support 1, and the surface state of the rubbed thin film is analyzed using a predetermined surface analysis unit (not shown).

【0028】本発明の付着力測定方法に適用可能な基板
は、表面が平坦であれば良く、金属や、無機固体、そし
て有機物等の固体物からなる基板を使用することができ
る。
The substrate applicable to the adhesive force measuring method of the present invention only needs to have a flat surface, and a substrate made of a solid such as a metal, an inorganic solid, and an organic material can be used.

【0029】また、本発明の付着力測定方法に適用可能
な薄膜は、一層であっても、複数の層が積層された多層
膜であっても良い。また、薄膜の膜厚は、1nm以上で
あれば良く、好ましくは1nm〜1μm、より好ましく
は1nm〜0.1μmである。また、擦過部材に加える
荷重を大きくすることにより軟質膜でも擦過可能であ
り、薄膜の材質の影響を受けることがない。
The thin film applicable to the adhesion measuring method of the present invention may be a single film or a multilayer film in which a plurality of layers are laminated. The thickness of the thin film may be 1 nm or more, preferably 1 nm to 1 μm, and more preferably 1 nm to 0.1 μm. Also, by increasing the load applied to the rubbing member, it is possible to rub even a soft film without being affected by the material of the thin film.

【0030】また、本発明の付着力測定方法では、基板
と薄膜との間の付着力の大きさによって、擦過部材に付
加する荷重を調整することが好ましい。荷重部材固定ス
テージ上に搭載する板材の重量あるいは枚数を増減させ
ることにより、擦過部材に付加する荷重を容易に調整す
ることができる。好ましい荷重の範囲は、98Pa〜9
80kPaである。例えば、シリカ基板上のシランカッ
プリング剤から成る薄膜の場合、1.96kPa〜98
kPaの範囲とすることが好ましい。
In the method for measuring an adhesive force according to the present invention, it is preferable to adjust the load applied to the rubbing member according to the magnitude of the adhesive force between the substrate and the thin film. By increasing or decreasing the weight or the number of plate members mounted on the load member fixing stage, the load applied to the rubbing member can be easily adjusted. The preferable range of the load is 98 Pa-9.
It is 80 kPa. For example, in the case of a thin film composed of a silane coupling agent on a silica substrate, 1.96 kPa to 98
It is preferable to be in the range of kPa.

【0031】また、本発明の付着力測定方法に用いる擦
過部材には、織布や不織布等の布材や、ゴム材、高分子
パッド材等を用いることができるが、布材が好ましい。
布材は、柔軟なため基板を傷付けることがなく、また、
表面の凹凸により薄膜を容易にかきとることができる。
布材の材質としては、ポリエステル、ポリプロピレン、
ビニロン、アクリル、ポリエチレンテレフタレート、レ
ーヨン、ナイロン等の化学繊維、ウールやシルク等の動
物繊維、そして麻や木綿等の植物繊維が挙げられるが、
木綿が好ましい。
The rubbing member used in the adhesive force measuring method of the present invention may be a cloth material such as a woven or nonwoven fabric, a rubber material, a polymer pad material, etc., but a cloth material is preferable.
The cloth material is flexible and does not damage the substrate.
The thin film can be easily scraped off by the unevenness on the surface.
Polyester, polypropylene,
Vinylon, acrylic, polyethylene terephthalate, rayon, chemical fibers such as nylon, animal fibers such as wool and silk, and plant fibers such as hemp and cotton,
Cotton is preferred.

【0032】また、擦過部材の厚さは、薄膜に十分に密
着させるために、0.1〜5.0mm、より好ましくは
0.5〜2.0mmである。また、擦過部材の面積は1
〜50cmが好ましい。
The thickness of the rubbing member is 0.1 to 5.0 mm, more preferably 0.5 to 2.0 mm, in order to sufficiently adhere to the thin film. The area of the rubbing member is 1
~50cm 2 is preferred.

【0033】また、擦過部材の擦過速度と擦過回数は、
それぞれ、1cm・sec−1〜10cm・sec−1
と1回〜10000回の範囲が好ましい。
The rubbing speed and the number of times of rubbing of the rubbing member are as follows:
1 cm · sec -1 to 10 cm · sec −1
And the range of 1 to 10000 times is preferable.

【0034】また、本発明の付着力測定方法では、擦過
した薄膜の表面分析方法として、表面接触角測定、光電
子分光測定、赤外線分光法、そして可視紫外分光法等を
用いて、擦過による薄膜の表面組成の変化を調べること
ができる。複数の試料について、擦過回数毎に表面組成
の変化を測定することにより、薄膜の基板に対する付着
力の試料間の相対比較が可能となる。
In the method for measuring the adhesive force according to the present invention, the surface of the abraded thin film is analyzed by surface contact angle measurement, photoelectron spectroscopy, infrared spectroscopy, visible ultraviolet spectroscopy, or the like. Changes in surface composition can be examined. By measuring the change in the surface composition of each of the plurality of samples for each number of times of rubbing, it becomes possible to make a relative comparison between the samples on the adhesive force of the thin film to the substrate.

【0035】ここで、表面分析に表面接触角測定法を用
いた場合の、付着力の測定方法について説明する。図3
は、擦過回数に対する表面接触角の変化の1例を示すグ
ラフである。薄膜の表面被覆率をX、薄膜が基板全体を
覆った場合の接触角をθ1、基板表面の表面接触角をθ2
とおくと、擦過部分の表面接触角θは、以下の式(1)
で示される。 cosθ=X・cosθ1+(1−X)・cosθ2 ・・・・(1) したがって、被覆率Xは、以下の式(2)で表わされ
る。 X=(cosθ-cosθ2)/(cosθ1-cosθ2) ・・・・(2) 擦過回数毎に表面接触角の測定を行い、上記の式(2)
を用いて被覆率を算出する。擦過回数毎の被覆率の変化
を測定することにより、付着力の試料間の相対的な評価
が可能となる。
Here, a method for measuring the adhesive force when the surface contact angle measuring method is used for the surface analysis will be described. FIG.
Is a graph showing an example of a change in a surface contact angle with respect to the number of times of rubbing. The surface coverage of the thin film is X, the contact angle when the thin film covers the entire substrate is θ 1 , and the surface contact angle of the substrate surface is θ 2
In other words, the surface contact angle θ of the rubbed portion is given by the following equation (1).
Indicated by cos θ = X · cos θ 1 + (1−X) · cos θ 2 (1) Therefore, the coverage X is expressed by the following equation (2). X = (cos θ−cos θ 2 ) / (cos θ 1 −cos θ 2 ) (2) The surface contact angle is measured every number of times of rubbing, and the above equation (2) is obtained.
Is used to calculate the coverage. By measuring the change in the covering ratio for each number of times of rubbing, it becomes possible to evaluate the adhesion force between the samples.

【0036】また、光電子分光測定、赤外線分光法、そ
して可視紫外分光法等の接触角測定以外の方法を用いる
場合においても、それら各測定方法において得られる薄
膜に起因するピークの面積の相対比較により被覆率Xを
算出できるので、薄膜の付着力の相対的な評価が可能と
なる。
Also, when using methods other than contact angle measurement, such as photoelectron spectroscopy, infrared spectroscopy, and visible-ultraviolet spectroscopy, the relative areas of the peaks attributable to the thin films obtained in each of these methods are compared. Since the coverage X can be calculated, the relative evaluation of the adhesive force of the thin film becomes possible.

【0037】本実施の形態では、摩擦力測定手段4を支
持体1に取付けた例を示したが、摩擦力測定手段4を荷
重付加機構5に取付けても、同様の効果が得られる。こ
の場合、支持体1を駆動機構15に固着して、昇降機構
20により駆動機構15を介して支持体1を昇降させれ
ば良い。
In this embodiment, the example in which the frictional force measuring means 4 is attached to the support 1 is shown. However, the same effect can be obtained by attaching the frictional force measuring means 4 to the load applying mechanism 5. In this case, the support 1 may be fixed to the drive mechanism 15, and the support 1 may be moved up and down by the lift mechanism 20 via the drive mechanism 15.

【0038】[0038]

【実施例】以下に本発明を実施例によって詳細に説明す
るが、これによって限定されるものではない。以下の実
施例は、CRTの表面コート用フィルムの最表面に形成
される防汚コートの付着力を測定した例である。防汚コ
ートに傷が入ると、その部分の透湿性が増加して、ゴー
ストグリッダーと呼ばれる不良が発生する。この不良
は,防汚コートの剥離と相関があることが知られてい
る。本発明に付着力測定方法を用いて防汚コートの付着
力を測定し、得られた付着力とゴーストグリッダーの発
生し易さとの相関を調べた。
EXAMPLES The present invention will be described below in detail with reference to Examples, but it should not be construed that the invention is limited thereto. The following examples are examples in which the adhesion of an antifouling coat formed on the outermost surface of a surface coating film of a CRT was measured. When the antifouling coat is damaged, the moisture permeability of the portion increases, and a defect called ghost gridder occurs. It is known that this defect has a correlation with the peeling of the antifouling coat. The adhesive force of the antifouling coat was measured using the adhesive force measuring method according to the present invention, and the correlation between the obtained adhesive force and the susceptibility of ghost gridder to occurrence was examined.

【0039】実施例1.基体にはCRTの表面コート用
フィルムを用い、そのフィルムの表面に組成と形成条件
の異なる膜厚5nmの3種類の防汚コートを形成して、
試料フィルムA,B,Cを調製した。試料フィルムをガ
ラス板に張り合わせて支持体上に水平に固定した。縦
7.6cm、横5.2cmの木綿さらし布を擦過部材と
し、重量1.0kgの錘を荷重部材として擦過部材へ荷
重を加えてフィルム表面に密着させた。この状態で、擦
過部材を試料フィルムに対して水平方向に10cm・s
ec −1の速度で進退運動させて試料フィルムの表面を
擦過させた。
Embodiment 1 Substrate for surface coating of CRT
Using a film, the composition and forming conditions on the surface of the film
Forming three types of antifouling coats with different thicknesses of 5 nm,
Sample films A, B, and C were prepared. Remove the sample film
The substrate was fixed horizontally on a support by laminating on a lath plate. Vertical
7.6cm, 5.2cm width cotton bleached cloth with rubbing member
And load the weight of 1.0 kg as a load member onto the scraping member.
A weight was added to adhere to the film surface. In this state,
10cm · s horizontal member to sample film
ec -1Forward and backward at the speed of
Scratched.

【0040】擦過した後、試料フィルムを支持体から取
り外し、フィルム表面の擦過箇所のイオン交換水に対す
る表面接触角を、協和界面科学製modelPD−Xを
用いて測定した。図6に試料フィルムA,B,Cの表面
を10回擦過した後の表面接触角を示す。擦過後の表面
接触角の大きさは,A<B<Cの順であった。フィルム
に対する付着力の小さい防汚コートは擦過によりフィル
ムから剥離するので、表面接触角は小さくなる。したが
って、試料フィルムCの防汚コートが最も付着力が大き
く、試料フィルムAが最も付着力が小さく、試料フィル
ムBがその中間であるという結果が得られた。また、こ
れらの試料フィルムは、別途行った試験によれば、A>
B>Cの順で、ゴーストグリッダーが発生しやすいとい
う結果が得られた。以上の結果より、擦過した試料フィ
ルムの表面接触角が小さくなると、すなわち、防汚コー
トの付着力の小さいフィルムほど、ゴーストグリッダー
が発生し易くなることがわかった。
After rubbing, the sample film was removed from the support, and the surface contact angle of the rubbed portion of the film surface with ion-exchanged water was measured using Kyowa Interface Science model PD-X. FIG. 6 shows the surface contact angles after rubbing the surfaces of the sample films A, B and C ten times. The magnitude of the surface contact angle after rubbing was in the order of A <B <C. Since the antifouling coat having a small adhesive force to the film is peeled off from the film by abrasion, the surface contact angle becomes small. Therefore, the result was obtained that the antifouling coat of the sample film C had the highest adhesion, the sample film A had the lowest adhesion, and the sample film B was intermediate. In addition, according to a test performed separately, these sample films show that A>
In the order of B> C, the result that a ghost gridder is easily generated was obtained. From the above results, it was found that the smaller the surface contact angle of the rubbed sample film, that is, the smaller the adhesive force of the antifouling coat, the more easily ghost gridder is generated.

【0041】実施例2.擦過回数を320回まで変化さ
せ、所定回数毎に表面接触角を測定した以外は、実施例
1と同様の方法により試料フィルムについて付着力の測
定を行なった。図7に、試料フィルムA,B,Cの、擦
過回数と表面接触角の関係を示す。いずれのフィルムに
おいても、擦過回数が150回程度を超えると表面接触
角は一定値に収束した。試料フィルムA,B,Cの表面
接触角の収束値の大きさは、それぞれ、70度、95
度、108度であった。試料フィルムAは試料フィルム
B,Cに比べ、擦過回数の増加に伴う表面接触角の低下
が大きく、防汚コートの付着力が他の試料フィルムに比
べかなり小さいことがわかった。
Example 2 The adhesive force of a sample film was measured in the same manner as in Example 1 except that the number of times of rubbing was changed up to 320 times and the surface contact angle was measured every predetermined number of times. FIG. 7 shows the relationship between the number of times of rubbing and the surface contact angle of the sample films A, B, and C. In any of the films, when the number of times of rubbing exceeded about 150, the surface contact angle converged to a constant value. The magnitudes of the convergence values of the surface contact angles of the sample films A, B, and C are 70 degrees and 95 degrees, respectively.
Degrees, 108 degrees. It was found that the sample film A had a larger decrease in the surface contact angle with the increase in the number of times of rubbing than the sample films B and C, and the adhesion of the antifouling coat was considerably smaller than the other sample films.

【0042】実施例3.擦過時にフィルムにかかる摩擦
力を、支持体の両端部に取り付けたロードセルで測定し
た以外は実施例2と同様の方法で、試料フィルムについ
て付着力の測定を行なった。図8に、試料フィルムA,
B,Cについて、接触角の変化から求めた被覆率と擦過
回数との関係を示す。被覆率は、擦過回数150回程度
以上で一定値に収束し、試料フィルムA,B,Cの被覆
率の収束値は、それぞれ、38%、80%、92%であ
った。これより、試料フィルムの付着力の大きさが、A
<B<Cの順であることがわかった。
Example 3 The adhesive force of a sample film was measured in the same manner as in Example 2 except that the frictional force applied to the film during rubbing was measured with load cells attached to both ends of the support. FIG. 8 shows sample films A,
For B and C, the relationship between the coverage obtained from the change in the contact angle and the number of times of rubbing is shown. The coverage converged to a constant value when the number of times of rubbing was about 150 or more, and the convergence values of the coverage of the sample films A, B, and C were 38%, 80%, and 92%, respectively. Thus, the magnitude of the adhesive force of the sample film is A
It turned out that <B <C.

【0043】実施例4.擦過した試料フィルムの表面
を、表面接触角測定に代えて光電子分光器(島津製作所
製ESCA-1000)により分析した以外は、実施例
2と同様の方法により試料フィルムの付着力の測定を行
なった。光電子スペクトルにおいて、防汚コート中のフ
ッ素原子に由来するF1sに帰属される689eV付近
のピーク面積と擦過回数との関係を調べた。いずれの試
料フィルムにおいても、689eV付近のピーク面積は
擦過回数ともに減少し、一定値に収束する傾向を示し
た。689eV付近のピーク面積の減少は防汚コートの
剥離の進行によるものであり、各試料フィルムの防汚コ
ートの付着力の大きさは、A<B<Cの順であり、実施
例2の場合と同様の結果が得られた。
Example 4 A sample film was prepared in the same manner as in Example 2 except that the surface of the rubbed sample film was analyzed using a photoelectron spectrometer (ESCA-1000 manufactured by Shimadzu Corporation) instead of measuring the surface contact angle. The adhesion was measured. In the photoelectron spectrum, the relationship between the peak area around 689 eV attributed to F1s derived from fluorine atoms in the antifouling coat and the number of times of rubbing was examined. In any of the sample films, the peak area around 689 eV decreased with the number of times of rubbing, and tended to converge to a constant value. The decrease in the peak area around 689 eV is due to the progress of the peeling of the antifouling coat, and the magnitude of the adhesion of the antifouling coat of each sample film is in the order of A <B <C. The same result was obtained.

【0044】[0044]

【発明の効果】以上説明したように、本発明の薄膜の付
着力測定方法は、下面に擦過部材を有し上面に荷重部材
を有する荷重付加機構を薄膜の直上に配置し、荷重部材
の荷重により擦過部材を薄膜と密着させた状態で、擦過
部材を薄膜の水平方向に移動させるようにして擦過し、
かつ、擦過後の薄膜を表面分析することにより付着力を
測定するようにしたので、膜厚がナノメータオーダの薄
膜について、サンプルの種類に限定されることなく、精
度の高い付着力の測定が可能となる。
As described above, according to the method for measuring the adhesive force of a thin film of the present invention, a load applying mechanism having a rubbing member on the lower surface and a load member on the upper surface is disposed immediately above the thin film, With the rubbing member in close contact with the thin film, rubbing the rubbing member so as to move the thin film in the horizontal direction,
In addition, since the adhesive force is measured by analyzing the surface of the thin film after rubbing, it is possible to measure the adhesive force with high accuracy regardless of the type of sample for a thin film with a thickness of nanometer order Becomes

【0045】また、本発明の付着力測定方法は、荷重付
加機構を支持体の垂直方向に昇降可能としたので、擦過
部材の位置決めを簡便に行うことができる。
In the method for measuring the adhesive force according to the present invention, the load applying mechanism can be moved up and down in the vertical direction of the support, so that the positioning of the rubbing member can be performed easily.

【0046】また、本発明の付着力測定方法は、擦過部
材に布材を用いるようにしたので、基体を傷つけること
なく薄膜を擦過することができ、より精度の高い付着力
の測定が可能となる。
Further, in the method for measuring adhesive force according to the present invention, since a cloth material is used for the scraping member, it is possible to scrape the thin film without damaging the substrate, and it is possible to measure the adhesive force with higher accuracy. Become.

【0047】また、本発明の付着力測定方法は、表面分
析に表面接触角測定を用い、擦過に伴う接触角の変化か
ら薄膜の付着力を測定するようにしたので、膜厚がナノ
メータオーダの薄膜の付着力を簡便に測定できる。
In the method for measuring the adhesive force according to the present invention, the surface contact angle is measured for the surface analysis, and the adhesive force of the thin film is measured from the change in the contact angle due to the rubbing. The adhesive force of the thin film can be easily measured.

【0048】また、本発明の付着力測定方法は、表面分
析に光電子分光法を用い、擦過に伴う特定元素のピーク
面積の変化から薄膜の付着力を測定するようにしたの
で、膜厚がナノメータオーダの薄膜の付着力をより高精
度に測定できる。
In the adhesion measuring method of the present invention, photoelectron spectroscopy is used for surface analysis, and the adhesion of a thin film is measured from the change in the peak area of a specific element due to abrasion. The adhesive force of the thin film of the order can be measured with higher accuracy.

【0049】また、本発明の薄膜の付着力測定装置は、
薄膜を擦過する薄膜擦過部と擦過された薄膜の表面状態
を測定する表面分析部とから成り、さらに、薄膜擦過部
を、基体を固定する支持体と、支持体上に配置され、下
面には擦過部材を有し、上面には擦過部材を薄膜に密着
させる荷重部材を有する荷重付加機構と、支持体又は荷
重付加機構を支持し、薄膜と擦過部材とを密着させた状
態で、支持した支持体又は荷重付加機構を基体の水平方
向に進退運動せしめる駆動機構と、駆動機構に固着さ
れ、荷重付加機構を基体の垂直方向に移動可能に支持す
る摺動支持機構と、駆動機構又は支持体を基体の垂直方
向に移動可能に支持し、薄膜と擦過部材とを近接又は離
間させる昇降機構と、荷重付加機構と連動して薄膜と擦
過部材とを密着させるように昇降機構を作動させ、薄膜
と擦過部材とを密着させた状態で支持体又は荷重付加機
構を基体の水平方向に進退運動せしめるように駆動機構
を作動させる制御手段とで構成したので、膜厚がナノメ
ータオーダの薄膜について、サンプルの種類に限定され
ることなく、精度の高い付着力の測定が可能な測定装置
を提供できる。
Further, the apparatus for measuring the adhesive force of a thin film according to the present invention comprises:
Consists of a thin film rubbing part for rubbing the thin film and a surface analysis part for measuring the surface state of the rubbed thin film, and further, the thin film rubbing part, a support for fixing the base, and disposed on the support, A load applying mechanism having a rubbing member and having a load member on the upper surface having a load member for bringing the rubbing member into close contact with the thin film, supporting the support or the load applying mechanism, and supporting the thin film and the rubbing member in a state of being in close contact with the thin film. A drive mechanism for moving the body or the load applying mechanism forward and backward in the horizontal direction of the base, a sliding support mechanism fixed to the drive mechanism and supporting the load applying mechanism movably in the vertical direction of the base, and a drive mechanism or a support. An elevating mechanism that movably supports the substrate in the vertical direction, moves the thin film and the rubbing member close to or away from each other, and operates an elevating mechanism to make the thin film and the rubbing member adhere to each other in conjunction with the load applying mechanism. Close contact with scraping member Control means for operating the drive mechanism to move the support or the load applying mechanism forward and backward in the horizontal direction of the substrate in a state where the thin film having a thickness of the order of nanometers is limited to the sample type. A measuring device capable of measuring an adhesive force with high accuracy can be provided.

【0050】また、本発明の付着力測定装置は、荷重部
材に積層可能な1以上の板材を用いるようにしたので、
薄膜の付着力に応じて擦過部材への荷重を容易に調整す
ることでき、より精度の高い付着力の測定が可能とな
る。
Further, since the adhesion measuring device of the present invention uses one or more plate members which can be laminated on the load member,
The load on the rubbing member can be easily adjusted according to the adhesive force of the thin film, and more accurate measurement of the adhesive force can be performed.

【0051】また、本発明の付着力測定装置は、荷重付
加機構を駆動機構に固着し、昇降機構により荷重付加機
構を基体の垂直方向に移動できるようにしたので、基体
の垂直方向における擦過部材の位置決めを容易に行なう
ことができる。
Further, in the adhesive force measuring device of the present invention, the load applying mechanism is fixed to the drive mechanism, and the load applying mechanism can be moved in the vertical direction of the base by the elevating mechanism. Can be easily positioned.

【0052】また、本発明の付着力測定装置は、支持体
に摩擦力測定装置を取り付けるようにしたので、擦過時
の摩擦力を簡便に測定できる。
Further, in the adhesive force measuring device of the present invention, the friction force measuring device is attached to the support, so that the friction force at the time of rubbing can be easily measured.

【0053】また、本発明の付着力測定装置は、表面分
析部に表面接触角計を用いるようにしたので、膜厚がナ
ノメータオーダの薄膜の付着力を簡便に測定できる。
Further, since the adhesive force measuring device of the present invention uses a surface contact angle meter in the surface analyzing section, the adhesive force of a thin film having a thickness on the order of nanometers can be easily measured.

【0054】また、本発明の付着力測定装置は、表面分
析部に光電子分光器を用いるようにしたので、膜厚がナ
ノメータオーダの薄膜の付着力を高精度に測定できる。
Further, since the adhesive force measuring device of the present invention uses a photoelectron spectrometer in the surface analysis section, the adhesive force of a thin film having a thickness on the order of nanometer can be measured with high accuracy.

【図面の簡単な説明】[Brief description of the drawings]

【図1】 本発明の実施の形態に係る薄膜の付着力測定
装置の1例の構成を示す側面図である。
FIG. 1 is a side view showing a configuration of an example of a thin film adhesion measuring device according to an embodiment of the present invention.

【図2】 図1の付着力測定装置の、一部断面図を含む
正面図である。
FIG. 2 is a front view including a partial cross-sectional view of the adhesion measuring device of FIG. 1;

【図3】 図1の付着力測定装置を用いて得られた測定
結果の1例であり、表面接触角と擦過回数との関係を示
すグラフである。
FIG. 3 is a graph showing an example of measurement results obtained by using the adhesion measuring device of FIG. 1, and showing a relationship between a surface contact angle and the number of times of rubbing.

【図4】 本発明の実施例1における試料フィルムA,
B,Cの表面接触角を示すグラフである。
FIG. 4 shows sample films A and 1 according to the first embodiment of the present invention.
It is a graph which shows the surface contact angle of B and C.

【図5】 本発明の実施例2における試料フィルムA,
B,Cの、表面接触角と擦過回数との関係を示すグラフ
である。
FIG. 5 shows sample films A and 2 in Example 2 of the present invention.
It is a graph which shows the relationship between the surface contact angle of B and C, and the number of times of rubbing.

【図6】 本発明の実施例3における試料フィルムA,
B,Cの、被覆率と擦過回数との関係を示すグラフであ
る。
FIG. 6 shows sample films A, 3 in Example 3 of the present invention.
It is a graph which shows the relationship between the coverage and the number of times of rubbing of B and C.

【符号の説明】 1 支持体、 2 固定部材、 3 ワイヤ、 4 ロ
ードセル、 5 荷重付加機構、 6 荷重部材、 7
固定ロッド、 8 荷重部材用ステージ、8a 連結
部、 9 擦過部材用保持部材、 10 擦過部材、
15 駆動機構、 16 駆動手段、 17 可動手
段、 18 移動用レール、 20 昇降機構、 21
ハンドル、 22 ロック、 25 摺動支持機構、
26接続手段、 27 摺動手段、 28 枠体、
29 第1の嵌め込み部材、30 固定部材、 31
第2の嵌め込み部材、 35 基体、 36 薄膜、3
7 架台、 40 擦過機構、 45 制御機構、 5
0 薄膜擦過部。
[Description of Signs] 1 support, 2 fixing member, 3 wire, 4 load cell, 5 load applying mechanism, 6 load member, 7
Fixing rod, 8 stage for load member, 8a connecting portion, 9 holding member for scraping member, 10 scraping member,
Reference Signs List 15 drive mechanism, 16 drive means, 17 movable means, 18 moving rail, 20 lifting mechanism, 21
Handle, 22 lock, 25 sliding support mechanism,
26 connecting means, 27 sliding means, 28 frame,
29 first fitting member, 30 fixing member, 31
2nd fitting member, 35 base, 36 thin film, 3
7 gantry, 40 rubbing mechanism, 45 control mechanism, 5
0 Thin film rubbing part.

───────────────────────────────────────────────────── フロントページの続き (72)発明者 蔵田 哲之 東京都千代田区丸の内二丁目2番3号 三 菱電機株式会社内 (72)発明者 高橋 貞治 東京都千代田区丸の内二丁目2番3号 三 菱電機株式会社内 (72)発明者 前田 美佳子 東京都千代田区丸の内二丁目2番3号 三 菱電機株式会社内 (72)発明者 藤井 優 東京都千代田区丸の内二丁目2番3号 三 菱電機株式会社内 Fターム(参考) 2G001 AA01 BA08 CA03 KA03 LA06 MA05 RA08  ──────────────────────────────────────────────────続 き Continued on the front page (72) Inventor Tetsuyuki Kurata 2-3-2 Marunouchi, Chiyoda-ku, Tokyo Mitsui Electric Co., Ltd. (72) Inventor Sadaharu Takahashi 2-3-2 Marunouchi, Chiyoda-ku, Tokyo Rishi Electric Co., Ltd. (72) Inventor Mikako Maeda 2-3-2 Marunouchi, Chiyoda-ku, Tokyo Mitsui Electric Co., Ltd. (72) Inventor Yu Fujii 2-3-2 Marunouchi, Chiyoda-ku, Tokyo Mitsui Electric F term in the company (reference) 2G001 AA01 BA08 CA03 KA03 LA06 MA05 RA08

Claims (11)

【特許請求の範囲】[Claims] 【請求項1】 支持体上に固定され表面に薄膜を有する
基体と、前記支持体上に支持され前記薄膜を擦過する荷
重付加機構の下面に取り付けられた擦過部材とを近接さ
せ、前記荷重付加機構の上面に荷重部材を搭載して前記
薄膜と前記擦過部材とを密着状態とし、前記支持体又は
荷重付加機構を基体の水平方向に進退運動せしめて擦過
部材により薄膜を擦過し、擦過された薄膜の表面分析を
行い、薄膜の基体に対する付着力を測定する薄膜の付着
力測定方法。
1. A substrate fixed on a support and having a thin film on its surface, and a rubbing member supported on said support and attached to a lower surface of a load applying mechanism for rubbing said thin film, are brought close to each other, and said load is applied. The thin film and the rubbing member were brought into close contact with each other by mounting a load member on the upper surface of the mechanism, and the thin film was rubbed and rubbed by the rubbing member by moving the support or the load applying mechanism forward and backward in the horizontal direction of the base. A method for measuring the adhesion of a thin film, in which the surface of the thin film is analyzed and the adhesion of the thin film to a substrate is measured.
【請求項2】 前記荷重付加機構は前記支持体の垂直方
向に昇降可能に支持されており、荷重付加機構を降下せ
しめて擦過部材を薄膜に近接させ、薄膜を擦過した後、
荷重付加機構を上昇せしめて擦過部材を薄膜から離間さ
せる請求項1記載の測定方法。
2. The load applying mechanism is supported so as to be able to move up and down in the vertical direction of the support. After the load applying mechanism is lowered to bring the scraping member close to the thin film and rub the thin film,
The measuring method according to claim 1, wherein the load applying mechanism is raised to separate the rubbing member from the thin film.
【請求項3】 前記擦過部材が布材である請求項1又は
2に記載の測定方法。
3. The measuring method according to claim 1, wherein the rubbing member is a cloth material.
【請求項4】 前記表面分析が表面接触角測定法である
請求項1から3のいずれか一つに記載の測定方法。
4. The measuring method according to claim 1, wherein the surface analysis is a surface contact angle measuring method.
【請求項5】 前記表面分析が光電子分光法である請求
項1から3のいずれか一つに記載の測定方法。
5. The measuring method according to claim 1, wherein the surface analysis is photoelectron spectroscopy.
【請求項6】 基体上に形成された薄膜の前記基体に対
する付着力の測定に使用される薄膜の付着力測定装置で
あって、 基体を固定する支持体と、 前記支持体上に配置され、下面には擦過部材を有し、上
面には前記擦過部材を前記薄膜に密着させる着脱自在の
荷重部材を有する荷重付加機構と、 前記支持体又は前記荷重付加機構を基体の水平方向に移
動可能に支持し、薄膜と擦過部材とを密着させた状態
で、支持した支持体又は荷重付加機構を基体の水平方向
に進退運動せしめる駆動機構と、 前記駆動機構に固着されてなり、前記荷重付加機構を基
体の垂直方向に移動可能に支持する摺動支持機構と、 前記駆動機構又は前記支持体を基体の垂直方向に移動可
能に支持し、薄膜と擦過部材とを近接又は離間させる昇
降機構と、 前記荷重付加機構と連動して薄膜と擦過部材とを密着さ
せるように昇降機構を作動させ、薄膜と擦過部材とを密
着させた状態で支持体又は荷重付加機構を基体の水平方
向に進退運動せしめるように駆動機構を作動させる制御
手段と、を有する薄膜擦過部と、 該薄膜擦過部により擦過された薄膜の表面状態を測定す
る表面分析部と、から成る薄膜の付着力測定装置。
6. An apparatus for measuring an adhesive force of a thin film formed on a substrate, which is used for measuring an adhesive force of the thin film on the substrate, comprising: a support for fixing the substrate; A load applying mechanism having a rubbing member on the lower surface and a detachable load member for bringing the rubbing member into close contact with the thin film on the upper surface; and allowing the support or the load applying mechanism to move in the horizontal direction of the base. A driving mechanism for moving the supported support or the load applying mechanism forward and backward in the horizontal direction of the base in a state in which the thin film and the rubbing member are in close contact with each other, and the load applying mechanism is fixed to the driving mechanism. A sliding support mechanism that movably supports the substrate in a vertical direction, an elevating mechanism that supports the driving mechanism or the support so as to be movable in a vertical direction of the substrate, and moves a thin film and a rubbing member close to or away from each other; Loading machine The lifting / lowering mechanism is operated so that the thin film and the rubbing member are brought into close contact with the structure, and the support or the load applying mechanism is driven to move forward and backward in the horizontal direction of the base with the thin film and the rubbing member in close contact with each other. A thin film adhesive force measuring device, comprising: a thin film rubbing part having a control means for operating a mechanism; and a surface analyzing part for measuring a surface state of the thin film rubbed by the thin film rubbing part.
【請求項7】 前記荷重部材が積層可能な1以上の板材
から成り、該1以上の板材を前記荷重付加機構の上面に
積層して、前記擦過部材へ荷重を付加する請求項6記載
の測定装置。
7. The measurement according to claim 6, wherein the load member is made of one or more stackable plate members, and the one or more plate members are stacked on an upper surface of the load applying mechanism to apply a load to the rubbing member. apparatus.
【請求項8】 前記荷重付加機構が前記駆動機構に固着
され、前記昇降機構により荷重付加機構を昇降させて薄
膜と擦過部材とを近接又は離間させる請求項6又は7に
記載の測定装置。
8. The measuring apparatus according to claim 6, wherein the load applying mechanism is fixed to the drive mechanism, and the load applying mechanism is moved up and down by the elevating mechanism to move the thin film and the rubbing member close to or away from each other.
【請求項9】 前記支持体が、前記荷重付加機構を基体
の水平方向に進退運動させたときに生じる摩擦力を測定
する摩擦力測定手段を有する請求項8記載の測定装置。
9. The measuring device according to claim 8, wherein the support has a frictional force measuring means for measuring a frictional force generated when the load applying mechanism is moved forward and backward in the horizontal direction of the base.
【請求項10】 前記表面分析部が表面接触角計である
請求項6から9のいずれか一つに記載の測定装置。
10. The measuring device according to claim 6, wherein the surface analysis unit is a surface contact angle meter.
【請求項11】 前記表面分析部が光電子分光器である
請求項6から9のいずれか一つに記載の測定装置。
11. The measurement device according to claim 6, wherein the surface analysis unit is a photoelectron spectroscope.
JP2001160690A 2001-05-29 2001-05-29 Method and apparatus for measuring adhesion of thin film Pending JP2002350330A (en)

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JP2001160690A JP2002350330A (en) 2001-05-29 2001-05-29 Method and apparatus for measuring adhesion of thin film
TW090121558A TW505785B (en) 2001-05-29 2001-08-31 Method and apparatus for measuring thin film adhesion force
KR1020010055144A KR20020090835A (en) 2001-05-29 2001-09-07 Method and apparatus for measuring an adhesive force of a thin film

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
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* Cited by examiner, † Cited by third party
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JP2006242765A (en) * 2005-03-03 2006-09-14 Sumitomo Chemical Co Ltd Adhesion measuring method and adhesion measuring device
KR101007997B1 (en) 2008-12-31 2011-01-14 엘아이지에이디피 주식회사 Testing equipment for adhesive pads of a adhesive chuck and testing method thereof
KR101762703B1 (en) 2017-03-03 2017-08-04 한국지질자원연구원 Method of measuring the hydrophobicity and hydrophilicity of specimen and apparatus therefor
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JP4611060B2 (en) * 2005-03-03 2011-01-12 住友化学株式会社 Adhesion force measuring method and adhesion force measuring device
KR101007997B1 (en) 2008-12-31 2011-01-14 엘아이지에이디피 주식회사 Testing equipment for adhesive pads of a adhesive chuck and testing method thereof
KR101762703B1 (en) 2017-03-03 2017-08-04 한국지질자원연구원 Method of measuring the hydrophobicity and hydrophilicity of specimen and apparatus therefor
WO2018159929A1 (en) * 2017-03-03 2018-09-07 한국지질자원연구원 Method for measuring hydrophobicity (hydrophilicity) of specimen and measurement device therefor
CN109406393A (en) * 2018-12-20 2019-03-01 浙江工业大学 A kind of film and the electric or hand measuring device of basal body binding force
CN109406393B (en) * 2018-12-20 2024-05-14 浙江工业大学 Electric or manual measuring device for binding force between film and substrate

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