JP2012132876A - Thickness evaluation method and apparatus for carbon thin film - Google Patents

Thickness evaluation method and apparatus for carbon thin film Download PDF

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JP2012132876A
JP2012132876A JP2010287251A JP2010287251A JP2012132876A JP 2012132876 A JP2012132876 A JP 2012132876A JP 2010287251 A JP2010287251 A JP 2010287251A JP 2010287251 A JP2010287251 A JP 2010287251A JP 2012132876 A JP2012132876 A JP 2012132876A
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JP5565298B2 (en
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寛 ▲宝▼来
Hiroshi Horai
Hiroshi Nakai
宏 中井
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Abstract

PROBLEM TO BE SOLVED: To provide a thickness evaluation method for a carbon thin film by which a thickness of a carbon thin film of diamond-like carbon or the like may be simply evaluated.SOLUTION: A thickness evaluation method for a carbon thin film with a thickness of 100 nm or less formed on a substrate, comprises the steps of: obtaining correlation between a thickness of a carbon thin film and brightness of the carbon thin film measured by a brightness measuring device; measuring, by the brightness measuring device, brightness of a carbon thin film to be evaluated; and evaluating, from the measured brightness of the carbon thin film to be evaluated, a thickness of the carbon thin film to be evaluated on the basis of the correlation precedently obtained.

Description

本発明は、カーボン薄膜の膜厚評価方法及びカーボン薄膜の膜厚評価装置に関する。   The present invention relates to a carbon thin film thickness evaluation method and a carbon thin film thickness evaluation apparatus.

近年、カーボン膜としてダイヤモンド性を付与したもの、すなわちダイヤモンドライクカーボン(Diamond Like Carbon:DLC)膜が提供されており、各種の用途で実用化が進められている。例えば、磁気記録媒体の磁性層の保護膜として用いられたり(特許文献1参照)、金型や治具の表面皮膜などとして用いられている。   In recent years, diamond films having a diamond property, that is, diamond-like carbon (DLC) films, have been provided and are being put to practical use in various applications. For example, it is used as a protective film for a magnetic layer of a magnetic recording medium (see Patent Document 1), or as a surface film for a mold or a jig.

ところで、このダイヤモンドライクカーボンは、通常は薄膜に形成されて用いられるが、その膜厚の管理や評価が非常に困難になっている。例えば、前記特許文献1ではダイヤモンドライクカーボン薄膜の膜質を評価する方法については提案されているが、膜厚の評価については示されていない。   By the way, this diamond-like carbon is usually formed and used in a thin film, but it is very difficult to manage and evaluate the film thickness. For example, Patent Document 1 proposes a method for evaluating the film quality of a diamond-like carbon thin film, but does not show the evaluation of the film thickness.

一般に、1μm以下の薄膜の膜厚測定には段差計やカロテスターなどが使用されるが、これら段差計やカロテスターなどの機械的な測定の下限は300nm程度であり、例えば100nm以下の薄膜の膜厚を機械的に測定することは、現状では極めて困難である。
そのため、100nm程度以下の膜厚を測定しようとした場合、X線回折(X−ray diffraction:XRD)や走査型電子顕微鏡(Scanning Electron Microscope:SEM)によって行うのが一般的である。
In general, a step gauge, a carotester, or the like is used for measuring a film thickness of a thin film having a thickness of 1 μm or less. However, the lower limit of the mechanical measurement of the step gauge, the carotester, or the like is about 300 nm. It is extremely difficult to measure the film thickness mechanically at present.
Therefore, when a film thickness of about 100 nm or less is to be measured, it is generally performed by X-ray diffraction (XRD) or a scanning electron microscope (SEM).

特開平8−7257号公報JP-A-8-7257

しかしながら、このようなX線回折や走査型電子顕微鏡によって膜厚を測定する手法では、測定に要する処理が煩雑であるため、例えば被測定物が多数ある場合には測定に長時間を要してしまい、極めて効率が悪いといった問題がある。さらに、このような測定を行うための機器は非常に高価であるといった問題もある。   However, in such a method of measuring the film thickness by X-ray diffraction or scanning electron microscope, the processing required for the measurement is complicated, and for example, when there are a large number of objects to be measured, a long time is required for the measurement. Therefore, there is a problem that the efficiency is extremely low. Furthermore, there is a problem that an apparatus for performing such a measurement is very expensive.

特に、品質管理の一環として膜厚を調べたい場合などでは、測定に長時間をかけるのは効率の面でもコストの面でも極めて不利になる。したがって、特に品質管理の場合のように、膜厚の絶対値を求める必要が無い場合などでは、簡易な手法によって膜厚を評価することのできる方法が求められている。   In particular, when it is desired to check the film thickness as a part of quality control, it is extremely disadvantageous in terms of efficiency and cost to take a long time for measurement. Accordingly, there is a need for a method that can evaluate the film thickness by a simple method, particularly when the absolute value of the film thickness does not need to be obtained as in the case of quality control.

本発明は前記事情に鑑みてなされたもので、その目的とするところは、特にダイヤモンドライクカーボンについて、その膜厚を簡易な手法で評価できるようにした、カーボン薄膜の膜厚評価方法及びカーボン薄膜の膜厚評価装置を提供することにある。   The present invention has been made in view of the above circumstances, and its object is to evaluate the film thickness of a carbon thin film and the carbon thin film, in particular, so that the film thickness can be evaluated by a simple method for diamond-like carbon. It is in providing the film thickness evaluation apparatus.

本発明者は前記目的を達成すべく鋭意検討した結果、評価対象となる薄膜が同一材質の場合、膜厚の変化に対応して薄膜の色も変化するとの知見を得た。そして、このような知見に基づきさらに検討を重ねた結果、本発明を完成した。   As a result of intensive studies to achieve the above object, the present inventor has found that when the thin film to be evaluated is the same material, the color of the thin film also changes in accordance with the change in the film thickness. As a result of further studies based on such knowledge, the present invention was completed.

すなわち、本発明のカーボン膜の膜厚評価方法は、基材上に形成された厚さ100nm以下のカーボン薄膜の膜厚評価方法であって、
前記カーボン薄膜の膜厚と明度計測装置で計測した前記カーボン薄膜の明度との相関を求める工程と、
明度計測装置によって被評価膜となるカーボン薄膜の明度を計測する工程と、
計測した被評価膜となるカーボン薄膜の明度から前記相関に基づき、被評価膜となるカーボン薄膜の膜厚を評価する工程と、を備えることを特徴としている。
That is, the carbon film thickness evaluation method of the present invention is a film thickness evaluation method of a carbon thin film having a thickness of 100 nm or less formed on a substrate,
Obtaining a correlation between the thickness of the carbon thin film and the brightness of the carbon thin film measured by a brightness measuring device;
A step of measuring the lightness of the carbon thin film as the film to be evaluated by a lightness measuring device;
And a step of evaluating the film thickness of the carbon thin film to be evaluated based on the correlation based on the measured brightness of the carbon thin film to be evaluated.

また、本発明のカーボン膜の膜厚評価装置は、基材上に形成された厚さ100nm以下のカーボン薄膜の膜厚評価装置であって、
前記カーボン薄膜の膜厚と明度計測装置で計測した前記カーボン薄膜の明度との相関を記憶する記憶手段と、
被評価膜となるカーボン薄膜の明度を計測する明度計測装置と、
明度計測装置によって計測された被評価膜となるカーボン薄膜の明度から、前記記憶手段に記憶した前記相関に基づき、被評価膜となるカーボン薄膜の膜厚を評価する評価手段と、を備えることを特徴としている。
The carbon film thickness evaluation apparatus of the present invention is a carbon film thickness evaluation apparatus having a thickness of 100 nm or less formed on a substrate,
Storage means for storing a correlation between the thickness of the carbon thin film and the brightness of the carbon thin film measured by a brightness measuring device;
A lightness measuring device for measuring the lightness of the carbon thin film to be evaluated;
An evaluation means for evaluating the film thickness of the carbon thin film to be evaluated based on the correlation stored in the storage means from the lightness of the carbon thin film to be evaluated film measured by the brightness measuring device. It is a feature.

また、前記明度計測手段が、分光測色計であるのが好ましい。
また、前記カーボン薄膜はダイヤモンドライクカーボンであってもよい。
The lightness measuring means is preferably a spectrocolorimeter.
The carbon thin film may be diamond-like carbon.

本発明のカーボン膜の膜厚評価方法及びカーボン膜の膜厚評価装置によれば、以下の効果を奏する。
ダイヤモンドライクカーボン等の厚さ100nm以下のカーボン薄膜は、その膜厚が例えば分光測色計などの明度計測装置で計測したカーボン薄膜の明度と相関を有する。したがって、予めこの相関を求めておくことにより、明度計測装置で計測して得られたカーボン薄膜の明度から、このカーボン薄膜の膜厚を評価することができる。
よって、例えばこの評価装置や評価方法を品質管理の一環としての膜厚管理に適用した場合に、この膜厚管理を短時間でかつ低コストで行うことができる。
The carbon film thickness evaluation method and the carbon film thickness evaluation apparatus of the present invention have the following effects.
A carbon thin film having a thickness of 100 nm or less such as diamond-like carbon has a correlation with the lightness of the carbon thin film measured by a lightness measuring device such as a spectrocolorimeter. Therefore, by obtaining this correlation in advance, the film thickness of the carbon thin film can be evaluated from the lightness of the carbon thin film obtained by measurement with a lightness measuring device.
Therefore, for example, when this evaluation apparatus and evaluation method are applied to film thickness management as part of quality control, this film thickness management can be performed in a short time and at low cost.

本発明に係る被評価体を模式的に示す側断面図である。It is a sectional side view which shows typically the to-be-evaluated body which concerns on this invention. (a)は成膜時間とDLC薄膜の明度(L)との関係を示すグラフであり、(b)は成膜時間とDLC薄膜の膜厚との関係を示すグラフであり、(c)はDLC薄膜の膜厚とDLC薄膜の明度(L)との関係(相関)を示すグラフである。(A) is a graph which shows the relationship between film-forming time and the brightness (L * ) of a DLC thin film, (b) is a graph which shows the relationship between film-forming time and the film thickness of a DLC thin film, (c) These are graphs showing the relationship (correlation) between the film thickness of the DLC thin film and the brightness (L * ) of the DLC thin film. 本発明に係るカーボン薄膜の膜厚評価装置の一実施形態を示す概略構成図である。It is a schematic block diagram which shows one Embodiment of the film thickness evaluation apparatus of the carbon thin film which concerns on this invention.

以下、本発明を詳しく説明する。
まず、本発明に係るカーボン膜の膜厚評価方法を説明する。
図1は、本発明に係る被評価体を模式的に示す図であり、図1中符号1は被評価体である。この被評価体1は、基材2上に下地金属層3を形成し、さらにこの下地金属層3上にダイヤモンドライクカーボン薄膜(以下、DLC薄膜と記す)4を形成したものである。
The present invention will be described in detail below.
First, the carbon film thickness evaluation method according to the present invention will be described.
FIG. 1 is a diagram schematically showing an object to be evaluated according to the present invention, and reference numeral 1 in FIG. 1 is an object to be evaluated. In this evaluation object 1, a base metal layer 3 is formed on a substrate 2, and a diamond-like carbon thin film (hereinafter referred to as DLC thin film) 4 is further formed on the base metal layer 3.

基材2は、被評価体1の種類や形態に応じて適宜に選択されるもので、例えばアルミニウム等の金属や合金によって形成されたものである。ただし、基材2の表面2a、すなわちDLC薄膜4を形成する側の面は、後述するように100nm以下と非常に薄いDLC薄膜4を形成するため、このDLC薄膜4を均一な膜厚の薄膜にするべく、平滑面である必要がある。したがって、この基材2の表面2aについては、例えば研磨処理を行っておき、平滑化しておくのが好ましい。   The base material 2 is appropriately selected according to the type and form of the evaluation object 1 and is formed of a metal such as aluminum or an alloy, for example. However, the surface 2a of the base material 2, that is, the surface on the side where the DLC thin film 4 is formed forms a very thin DLC thin film 4 of 100 nm or less, as will be described later. Therefore, the surface must be smooth. Accordingly, it is preferable that the surface 2a of the substrate 2 is polished and smoothed, for example.

下地金属層3は、基材2の材質等に応じて適宜に選択され、形成されるもので、例えばCrやTi等からなるものである。また、前記したようにこの下地金属層3上にDLC薄膜4を均一な膜厚で形成する必要上、この下地金属層3も平滑である必要があり、したがって平滑化された基材2の表面2aの平滑性を損なわないよう、下地金属層3は十分に薄く形成されているのが好ましい。具体的には、100nm〜300nm程度に形成されているのが好ましい。   The base metal layer 3 is appropriately selected and formed according to the material of the base 2 and is made of, for example, Cr or Ti. Further, as described above, it is necessary to form the DLC thin film 4 with a uniform film thickness on the base metal layer 3, and the base metal layer 3 also needs to be smooth. The underlying metal layer 3 is preferably formed sufficiently thin so as not to impair the smoothness of 2a. Specifically, it is preferably formed to be about 100 nm to 300 nm.

DLC薄膜4は、本発明における被評価膜となるもので、前記したダイヤモンド状カーボン、すなわちダイヤモンドに近い特性をもつ非結晶(アモルファス)のカーボンの薄膜であり、厚さが100nm以下の非常に薄い膜である。このようなDLC薄膜4は、硬いため耐摩耗性が高く、耐薬品性に優れ、低摩擦性であり、ガス遮断性を有するなど、優れた性質を有している。   The DLC thin film 4 is a film to be evaluated in the present invention. The DLC thin film 4 is a diamond-like carbon, that is, an amorphous carbon thin film having characteristics similar to diamond, and is very thin with a thickness of 100 nm or less. It is a membrane. Since such a DLC thin film 4 is hard, it has excellent properties such as high wear resistance, excellent chemical resistance, low friction and gas barrier properties.

このDLC薄膜4の形成方法としては、熱CVD法、プラズマCVD法等のCVD法(化学気相成長法)や、真空蒸着法、イオンプレーティング法、スパッタ法、レーザーアブレーション法等のPVD法(物理気相成長法)が採用される。例えば、ArガスにCH4 などを混合したガス雰囲気中でカーボンをスパッタ成膜し、膜中に水素を含有させてダイヤモンド性を付与し、DLC薄膜4を形成する、といった手法が採用可能である。 As a method for forming the DLC thin film 4, a CVD method (chemical vapor deposition method) such as a thermal CVD method or a plasma CVD method, or a PVD method (such as a vacuum deposition method, an ion plating method, a sputtering method, a laser ablation method) Physical vapor deposition method) is adopted. For example, it is possible to employ a technique in which carbon is sputtered in a gas atmosphere in which CH 4 or the like is mixed in Ar gas, hydrogen is contained in the film to impart diamond properties, and the DLC thin film 4 is formed. .

このようなDLC薄膜4は、特に100nm以下と非常に薄い膜厚であるため、この10nm以下の膜厚範囲において、膜厚が明度計測装置で計測されたカーボン薄膜の明度と相関を有する。ここで、明度計測装置としては分光測色計が好適に用いられる。分光測色計は、色ごと(正確には光の波長ごと)の強さを測定するものであり、本実施形態では、基準光源から被評価体1のDLC薄膜4に向けて光を照射し、このDLC薄膜4で反射した光の色の明度(L)を計測するようにしている。 Since such a DLC thin film 4 has a very thin film thickness, particularly 100 nm or less, the film thickness has a correlation with the brightness of the carbon thin film measured by the lightness measuring device in the film thickness range of 10 nm or less. Here, a spectrocolorimeter is preferably used as the lightness measuring device. The spectrocolorimeter measures the intensity for each color (precisely, for each wavelength of light). In this embodiment, light is irradiated from the reference light source toward the DLC thin film 4 of the object 1 to be evaluated. The lightness (L * ) of the color of light reflected by the DLC thin film 4 is measured.

この色の明度(L)は、CIE(国際照明委員会)が1976年に定めた均等色空間のひとつである、三次元直交座標を用いる色空間(L色空間)を用いたL表色系における、明度(明度指数)(L)である。このL表色系は、日本でも「JIS Z 8729」において採用されている。 The lightness (L * ) of this color is a color space (L * a * b * color space) using three-dimensional Cartesian coordinates, which is one of the uniform color spaces established by the CIE (International Lighting Commission) in 1976. It is the lightness (lightness index) (L * ) in the L * a * b * color system used. This L * a * b * color system is also adopted in “JIS Z 8729” in Japan.

このような明度(L)を計測する分光測色計として、本実施形態ではコニカミノルタ社製の「CM−2002」を用いている。ただし、分光測色計としてはこれに限定されることなく、前記明度(L)を計測することのできる公知の分光測色計は、全て使用可能である。
このような分光測色計を用い、DLC薄膜4の色に対応した波長域を選択しておき、この波長域の反射光の明度(L)を計測する。なお、明度(L)は、100に近づくと白に近づき(明るくなり)、0に近づくと黒に近づく(暗くなる)。
In this embodiment, “CM-2002” manufactured by Konica Minolta is used as a spectrocolorimeter for measuring such lightness (L * ). However, the spectrocolorimeter is not limited to this, and any known spectrocolorimeter that can measure the lightness (L * ) can be used.
Using such a spectrocolorimeter, a wavelength region corresponding to the color of the DLC thin film 4 is selected, and the lightness (L * ) of reflected light in this wavelength region is measured. The lightness (L * ) approaches white (becomes brighter) as it approaches 100, and approaches black (becomes dark) as it approaches 0.

本実施形態の膜厚評価方法では、DLC薄膜の膜厚と分光測色計(明度計測装置)で計測したDLC薄膜の明度(L)との相関を求めるべく、まず、前記分光測色計を用いて、被評価体1と同じ構成からなる試料のDLC薄膜4の明度(L)を計測する。
前記試料として、DLC薄膜の成膜時間を変え、それ以外は同じ条件で成膜を行ったものを3つ用意した。また、DLC薄膜の成膜を行わず、したがって下地金属層3が露出している試料も用意した。なお、DLC薄膜の形成方法としては、公知のスパッタ法によって行った。
In the film thickness evaluation method of the present embodiment, in order to obtain the correlation between the film thickness of the DLC thin film and the lightness (L * ) of the DLC thin film measured by the spectrocolorimeter (lightness measuring device), first, the spectrocolorimeter Is used to measure the lightness (L * ) of the DLC thin film 4 of the sample having the same configuration as the object 1 to be evaluated.
Three samples were prepared under the same conditions except that the DLC thin film deposition time was changed. A sample was also prepared in which the DLC thin film was not formed, and therefore the underlying metal layer 3 was exposed. The DLC thin film was formed by a known sputtering method.

DLC薄膜の成膜を行わなかったもの(すなわちDLC薄膜の膜厚が0nmのもの)、及び成膜時間を12分、18分、24分としたものを試料とし、これら試料について、前記分光測色計(コニカミノルタ社製「CM−2002」)を用いてそれぞれDLC薄膜(DLC薄膜の膜厚が0nmのものでは下地金属層)の明度(L)を計測した。成膜時間と得られた明度(L)との関係を図2(a)のグラフに示す。 Samples in which the DLC thin film was not formed (that is, those having a DLC thin film thickness of 0 nm) and those in which the film formation time was 12 minutes, 18 minutes, and 24 minutes were used as samples. The lightness (L * ) of each DLC thin film (underlying metal layer when the DLC thin film has a thickness of 0 nm) was measured using a colorimeter ("CM-2002" manufactured by Konica Minolta). The relationship between the film formation time and the obtained brightness (L * ) is shown in the graph of FIG.

なお、分光測色計(コニカミノルタ社製「CM−2002」)による明度(L)の計測については、計測面積(スポット面積)を約1cm程度として、試料面上の異なる3箇所で計測を行った。そして、その結果については平均値を採用した。
図2(a)より、成膜時間と明度(L)とはリニア(直線的)な関係にあることが確認された。
For lightness (L * ) measurement using a spectrocolorimeter (“CM-2002” manufactured by Konica Minolta, Inc.), the measurement area (spot area) is about 1 cm 2 and is measured at three different locations on the sample surface. Went. And the average value was employ | adopted about the result.
From FIG. 2A, it was confirmed that the film formation time and the lightness (L * ) have a linear relationship.

また、DLC薄膜の膜厚は、その成膜時間に正比例すると考えられる。そこで、その確認のため、前記試料と同様にして作製した試料(または同じ試料)の成膜時間と、DLC薄膜の膜厚との関係を調べた。得られた関係を図2(b)のグラフに示す。なお、DLC薄膜の膜厚については、簡易的にX線反射率測定で求めた。ただし、DLC薄膜の膜厚をより正確に測定するためには、TEM(透過型電子顕微鏡)等の電子顕微鏡によって試験片の断面を観察することで行うのが好ましい。   The thickness of the DLC thin film is considered to be directly proportional to the film formation time. In order to confirm this, the relationship between the film formation time of a sample (or the same sample) produced in the same manner as the above sample and the film thickness of the DLC thin film was examined. The relationship obtained is shown in the graph of FIG. In addition, about the film thickness of the DLC thin film, it calculated | required by the X-ray reflectivity measurement simply. However, in order to more accurately measure the thickness of the DLC thin film, it is preferable to observe the cross section of the test piece with an electron microscope such as a TEM (transmission electron microscope).

図2(b)より、成膜時間と膜厚とはリニア(直線的)な関係にあることが確認された。すなわち、成膜時間が0分のときには、当然DLC薄膜の膜厚は0nmとなるが、実際に膜厚を測定した試料から得られた直線は、図2(b)中二点鎖線で示すように原点(成膜時間が0分、DLC薄膜の膜厚が0nmの点)を通る。よって、試料の膜厚測定から得られた線形(直線)は、成膜時間と膜厚との関係を正確に表していると考えられる。   From FIG. 2B, it was confirmed that the film formation time and the film thickness were in a linear relationship. That is, when the film formation time is 0 minutes, the DLC thin film naturally has a film thickness of 0 nm, but the straight line obtained from the sample for which the film thickness was actually measured is shown by a two-dot chain line in FIG. Pass through the origin (the point at which the film formation time is 0 minute and the thickness of the DLC thin film is 0 nm). Therefore, the line (straight line) obtained from the film thickness measurement of the sample is considered to accurately represent the relationship between the film formation time and the film thickness.

図2(a)、図2(b)に示した結果より、DLC薄膜の膜厚はその成膜時間に正比例し(図2(b))、成膜時間とDLC薄膜の明度(L)とはリニア(直線的)な関係(相関)にある(図2(a))ことから、DLC薄膜の膜厚とその明度(L)とは、有意な相関があると考えられる。
そこで、試料のDLC薄膜の膜厚と、これら試料のDLC薄膜を前記分光測色計で計測して得られた明度(L)との相関を求めた。なお、DLC薄膜の膜厚については、前記したようにX線回折(XRD)法で求めた。得られた相関を図2(c)のグラフに示す。
From the results shown in FIGS. 2A and 2B, the film thickness of the DLC thin film is directly proportional to the film formation time (FIG. 2B), and the film formation time and the brightness of the DLC thin film (L * ). Is a linear relationship (correlation) (FIG. 2 (a)), it is considered that there is a significant correlation between the film thickness of the DLC thin film and its brightness (L * ).
Therefore, the correlation between the thickness of the DLC thin film of the sample and the lightness (L * ) obtained by measuring the DLC thin film of the sample with the spectrocolorimeter was obtained. The film thickness of the DLC thin film was determined by the X-ray diffraction (XRD) method as described above. The obtained correlation is shown in the graph of FIG.

図2(c)より、DLC薄膜の膜厚が薄くなると、DLC薄膜の明度(L)は高くなり、逆に膜厚が厚くなると、DLC薄膜の明度(L)は低くなることが分かった。したがって、DLC薄膜は、膜厚が厚くなるほど明度が低くなり、黒に近づく(暗くなる)傾向にあることが分かった。すなわち、DLC薄膜の膜厚と、分光測色計で計測したDLC薄膜の明度とは、図2(c)に示す相関を有していることが求められた。 2 from (c), the film thickness of the DLC film becomes thinner, the DLC thin film lightness (L *) is high, the film thickness becomes thicker Conversely, the DLC thin film lightness (L *) is found to be lower It was. Accordingly, it was found that the DLC thin film has a tendency to become lighter and darker as the film thickness increases. That is, the DLC thin film thickness and the brightness of the DLC thin film measured with a spectrocolorimeter were required to have a correlation shown in FIG.

次に、本実施形態の膜厚評価方法では、実際の膜厚評価を行うための被評価体1について、前記分光測色計を用いてそのDLC薄膜4(被評価膜)の明度(L)を計測する。計測条件は、図2(c)に示す相関を求めたときと同じ条件で行う。計測箇所については、例えばDLC薄膜4上の3〜5箇所程度を計測し、その平均値を計測値として採用する。 Next, in the film thickness evaluation method of the present embodiment, the brightness (L * ) of the DLC thin film 4 (film to be evaluated) is measured using the spectrocolorimeter for the object to be evaluated 1 for actual film thickness evaluation . ). The measurement conditions are the same as when the correlation shown in FIG. About a measurement location, about 3-5 location on the DLC thin film 4 is measured, for example, and the average value is employ | adopted as a measured value.

その後、得られた計測値(DLC薄膜4(被評価膜)の明度(L))から、先に求めた相関に基づき、被評価膜となるDLC薄膜4の膜厚を評価する。すなわち、得られた計測値(明度(L))を図2(c)のグラフに示す相関にあてはめ、被評価膜となるDLC薄膜4の膜厚を推定し評価する。 Thereafter, the film thickness of the DLC thin film 4 serving as the film to be evaluated is evaluated from the obtained measurement value (lightness (L * ) of the DLC thin film 4 (film to be evaluated)) based on the previously obtained correlation. That is, the obtained measurement value (lightness (L * )) is applied to the correlation shown in the graph of FIG. 2C, and the film thickness of the DLC thin film 4 serving as the film to be evaluated is estimated and evaluated.

このように、DLC薄膜の膜厚と明度(L)との相関を予め求めておくことで、分光測色計で計測して得られた被評価膜となるDLC薄膜4の明度(L)から、前記相関に基づいてその膜厚を推定し、評価することができる。
したがって、例えばこの評価方法を品質管理の一環としての膜厚管理に適用した場合に、この膜厚管理を短時間でかつ低コストで行うことができる。
In this way, by obtaining the correlation between the film thickness of the DLC thin film and the lightness (L * ) in advance, the lightness (L * ) of the DLC thin film 4 to be evaluated is obtained by measuring with a spectrocolorimeter . ), The film thickness can be estimated and evaluated based on the correlation.
Therefore, for example, when this evaluation method is applied to film thickness management as part of quality control, this film thickness management can be performed in a short time and at low cost.

すなわち、品質管理の一環としての膜厚管理では、通常は形成したDLC薄膜4(カーボン薄膜)の絶対値は必要でなく、予め規定された管理範囲内にあるか否かが問題になる。したがって、このような管理範囲の膜厚に対応する明度(L)を図2(c)のグラフから求めておくことにより、被評価膜、すなわち被検査品の膜厚管理を、前記分光測色計によって簡易的に行うことができる。 That is, in the film thickness control as a part of quality control, the absolute value of the formed DLC thin film 4 (carbon thin film) is usually not necessary, and it is a problem whether it is within a predetermined control range. Therefore, by obtaining the lightness (L * ) corresponding to the film thickness in such a management range from the graph of FIG. 2 (c), the film thickness management of the film to be evaluated, that is, the inspected product, can be controlled by the spectroscopic measurement. This can be done easily with a color meter.

よって、本実施形態の膜厚評価方法によれば、X線回折を行うための装置や走査型電子顕微鏡に比べて格段に安価な分光測色計により、DLC薄膜の膜厚を簡易な手法で推定し評価することができるので、例えばこの膜厚評価方法を適用したDLC薄膜の膜厚管理などを、短時間でかつ低コストで行うことができる。   Therefore, according to the film thickness evaluation method of this embodiment, the film thickness of the DLC thin film can be reduced by a simple method using a spectrocolorimeter that is much cheaper than an apparatus for performing X-ray diffraction or a scanning electron microscope. Since estimation and evaluation can be performed, for example, film thickness management of a DLC thin film to which this film thickness evaluation method is applied can be performed in a short time and at low cost.

次に、このような膜厚評価方法を実施し得るカーボン薄膜の膜厚評価装置について説明する。
図3は、本発明のカーボン薄膜の膜厚評価装置の一実施形態を示す図であり、図3中符号10はカーボン薄膜の膜厚評価装置である。この膜厚評価装置10は、基材上に形成された厚さ100nm以下のカーボン薄膜の膜厚を評価する装置であって、例えば図1に示した被評価体1におけるDLC薄膜4の膜厚を評価する装置である。
Next, a carbon thin film thickness evaluation apparatus capable of implementing such a film thickness evaluation method will be described.
FIG. 3 is a diagram showing an embodiment of a carbon thin film thickness evaluation apparatus according to the present invention, and reference numeral 10 in FIG. 3 denotes a carbon thin film thickness evaluation apparatus. This film thickness evaluation apparatus 10 is an apparatus for evaluating the film thickness of a carbon thin film having a thickness of 100 nm or less formed on a substrate, and for example, the film thickness of the DLC thin film 4 in the evaluation object 1 shown in FIG. It is a device that evaluates.

この膜厚評価装置10は、DLC薄膜4(カーボン薄膜)の膜厚と明度計測装置で計測した前記DLC薄膜4の明度との相関を記憶する記憶手段11と、被評価膜となるDLC薄膜4の明度を計測する明度計測装置12と、前記明度計測装置12によって計測された被評価膜となるDLC薄膜4の明度から、前記記憶手段11に記憶した前記相関に基づき、被評価膜となるDLC薄膜4(カーボン薄膜)の膜厚を評価する評価手段13と、を備えたものである。   This film thickness evaluation apparatus 10 includes a storage means 11 for storing the correlation between the film thickness of the DLC thin film 4 (carbon thin film) and the lightness of the DLC thin film 4 measured by the lightness measuring device, and the DLC thin film 4 serving as the film to be evaluated. Based on the correlation stored in the storage means 11 based on the brightness of the brightness measuring device 12 for measuring the brightness of the DLC thin film 4 that is the evaluated film measured by the brightness measuring device 12, the DLC that is the evaluated film Evaluation means 13 for evaluating the film thickness of the thin film 4 (carbon thin film).

記憶手段11は、例えばコンピューターのハードディスクや、その他公知のメモリ装置、またはメモリ媒体などからなっている。そして、この記憶手段11には、先の評価方法で述べたように、予め求めた、DLC薄膜4の膜厚と明度計測装置(分光測色計)で計測したDLC薄膜の明度(L)との相関、すなわち図2(c)に示したような相関が、記憶(記録)されている。なお、この記憶手段11は、図3に示すようにコンピューター等の制御装置14に内蔵されあるいは外付けされた、ハードディスク等のメモリ装置からなっている。 The storage means 11 is composed of, for example, a computer hard disk, other known memory devices, or memory media. In the storage means 11, as described in the previous evaluation method, the film thickness of the DLC thin film 4 and the lightness (L * ) of the DLC thin film measured with a lightness measuring device (spectral colorimeter) are obtained in advance. , That is, the correlation as shown in FIG. 2C is stored (recorded). The storage means 11 comprises a memory device such as a hard disk, which is built in or externally attached to a control device 14 such as a computer as shown in FIG.

明度計測装置12は、前記したように分光測色計からなるものである。ただし、分光測色計以外にも、DLC薄膜4の明度を計測できるものであれば、使用可能である。
評価手段13は、前記記憶手段11とともに前記制御装置14に設けられたもので、記憶手段11に記憶した前記相関に基づき、DLC薄膜4(カーボン薄膜)の膜厚を評価する評価ソフトを有したものである。なお、この評価手段13も、記憶手段11と同様に、ハードディスクや、その他公知のメモリ装置、またはメモリ媒体などからなっている。
The lightness measuring device 12 is composed of a spectrocolorimeter as described above. However, other than the spectrocolorimeter, any device that can measure the brightness of the DLC thin film 4 can be used.
The evaluation means 13 is provided in the control device 14 together with the storage means 11 and has evaluation software for evaluating the film thickness of the DLC thin film 4 (carbon thin film) based on the correlation stored in the storage means 11. Is. The evaluation unit 13 is also composed of a hard disk, other known memory device, or memory medium, as with the storage unit 11.

また、制御装置14は、CPU(中央演算処理装置)を有し、前記記憶手段11及び前記評価手段13の動作を制御するとともに、前記明度計測装置12の動作も制御するようになっている。すなわち、被評価体1が明度計測装置12にセットされたら、その後制御装置14は明度計測装置12にDLC薄膜4(カーボン薄膜)の明度を計測させる。そして、得られた計測値(明度)と、予め記憶手段11に記憶(記録)された前記相関とに基づき、前記評価手段13の評価ソフトを実行させて演算処理させ、DLC薄膜4(カーボン薄膜)の膜厚を評価する。そして、評価結果をモニターに表示し、またはプリンターで紙等に記録させるといった出力動作を行わせる。   The control device 14 includes a CPU (Central Processing Unit), and controls the operations of the storage unit 11 and the evaluation unit 13 and also controls the operation of the lightness measurement device 12. That is, when the evaluation object 1 is set in the lightness measuring device 12, the control device 14 causes the lightness measuring device 12 to measure the lightness of the DLC thin film 4 (carbon thin film). Then, based on the obtained measured value (brightness) and the correlation stored (recorded) in the storage unit 11 in advance, the evaluation software of the evaluation unit 13 is executed to perform arithmetic processing, and the DLC thin film 4 (carbon thin film) ) Is evaluated. Then, an output operation is performed such that the evaluation result is displayed on a monitor or recorded on paper or the like by a printer.

このような構成からなるカーボン薄膜の膜厚評価装置10にあっても、前述した膜厚評価方法と同様に、被評価膜となるDLC薄膜4の膜厚管理を簡易的に行うことができる。よって、X線回折を行うための装置や走査型電子顕微鏡に比べて格段に安価な明度計測装置(分光測色計)により、DLC薄膜の膜厚を簡易に評価することができるので、例えばこの膜厚評価装置を用いたDLC薄膜の膜厚管理などを、短時間でかつ低コストで行うことができる。   Even in the carbon thin film thickness evaluation apparatus 10 having such a configuration, it is possible to easily manage the film thickness of the DLC thin film 4 serving as the film to be evaluated, as in the above-described film thickness evaluation method. Therefore, the film thickness of the DLC thin film can be easily evaluated by a brightness measuring device (spectral colorimeter) that is much cheaper than an apparatus for performing X-ray diffraction or a scanning electron microscope. The film thickness management of the DLC thin film using the film thickness evaluation apparatus can be performed in a short time and at a low cost.

なお、本発明は前記実施形態に限定されることなく、本発明の主旨を逸脱しない範囲で種々の変更が可能である。
例えば、前記実施形態では本発明のカーボン薄膜をDLC薄膜としたが、アモルファスカーボン(a−C)薄膜や、グラファイト、カーボンナノチューブ、グラフェン、フラーレン、カーボンナノウオール等としてもよい。
The present invention is not limited to the above-described embodiment, and various modifications can be made without departing from the gist of the present invention.
For example, although the carbon thin film of the present invention is a DLC thin film in the above embodiment, it may be an amorphous carbon (a-C) thin film, graphite, carbon nanotube, graphene, fullerene, carbon nanowall, or the like.

また、前記実施形態では、被評価体1として基材2上に下地金属膜3を介してDLC薄膜4を形成したものを用いたが、例えば基材がクロム(Cr)やチタン(Ti)等のDLC薄膜形成に適した下地材料からなる場合には、この基材上に直接DLC薄膜4を形成してもよい。   Moreover, in the said embodiment, what formed the DLC thin film 4 on the base material 2 via the base metal film 3 as the to-be-evaluated object 1 was used, For example, a base material is chromium (Cr), titanium (Ti), etc. When the base material is suitable for forming a DLC thin film, the DLC thin film 4 may be formed directly on the base material.

1…被評価体、2…基材、3…下地金属層、4…ダイヤモンドライクカーボン薄膜(カーボン薄膜)、10…膜厚評価装置、11…記憶手段、12…明度計測手段、13…評価手段、14…制御装置 DESCRIPTION OF SYMBOLS 1 ... Evaluation object, 2 ... Base material, 3 ... Base metal layer, 4 ... Diamond-like carbon thin film (carbon thin film), 10 ... Film thickness evaluation apparatus, 11 ... Memory | storage means, 12 ... Lightness measurement means, 13 ... Evaluation means , 14 ... Control device

Claims (4)

基材上に形成された厚さ100nm以下のカーボン薄膜の膜厚評価方法であって、
前記カーボン薄膜の膜厚と明度計測装置で計測した前記カーボン薄膜の明度との相関を求める工程と、
明度計測装置によって被評価膜となるカーボン薄膜の明度を計測する工程と、
計測した被評価膜となるカーボン薄膜の明度から前記相関に基づき、被評価膜となるカーボン薄膜の膜厚を評価する工程と、を備えることを特徴とするカーボン薄膜の膜厚評価方法。
A film thickness evaluation method for a carbon thin film having a thickness of 100 nm or less formed on a substrate,
Obtaining a correlation between the thickness of the carbon thin film and the brightness of the carbon thin film measured by a brightness measuring device;
A step of measuring the lightness of the carbon thin film as the film to be evaluated by a lightness measuring device;
And a step of evaluating the film thickness of the carbon thin film as the film to be evaluated based on the correlation from the measured brightness of the carbon thin film as the film to be evaluated.
基材上に形成された厚さ100nm以下のカーボン薄膜の膜厚評価装置であって、
前記カーボン薄膜の膜厚と明度計測装置で計測した前記カーボン薄膜の明度との相関を記憶する記憶手段と、
被評価膜となるカーボン薄膜の明度を計測する明度計測装置と、
明度計測装置によって計測された被評価膜となるカーボン薄膜の明度から、前記記憶手段に記憶した前記相関に基づき、被評価膜となるカーボン薄膜の膜厚を評価する評価手段と、を備えることを特徴とするカーボン薄膜の膜厚評価装置。
A film thickness evaluation apparatus for a carbon thin film having a thickness of 100 nm or less formed on a substrate,
Storage means for storing a correlation between the thickness of the carbon thin film and the brightness of the carbon thin film measured by a brightness measuring device;
A lightness measuring device for measuring the lightness of the carbon thin film to be evaluated;
An evaluation means for evaluating the film thickness of the carbon thin film to be evaluated based on the correlation stored in the storage means from the lightness of the carbon thin film to be evaluated film measured by the brightness measuring device. A carbon thin film thickness evaluation device.
前記明度計測装置が、分光測色計であることを特徴とする請求項2記載のカーボン薄膜の膜厚評価装置。   3. The carbon thin film thickness evaluation apparatus according to claim 2, wherein the lightness measurement apparatus is a spectrocolorimeter. 前記カーボン薄膜はダイヤモンドライクカーボンであることを特徴とする請求項2又は3に記載のカーボン薄膜の膜厚評価装置。   The carbon thin film thickness evaluation apparatus according to claim 2, wherein the carbon thin film is diamond-like carbon.
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WO2018101306A1 (en) * 2016-12-02 2018-06-07 日産化学工業株式会社 Thin film, and undercoat foil for energy storage device electrode
JPWO2018101306A1 (en) * 2016-12-02 2018-11-29 日産化学株式会社 Undercoat foil for thin film and energy storage device electrodes

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