JPH0914946A - Method for measuring thickness of film utilizing x-ray diffraction - Google Patents
Method for measuring thickness of film utilizing x-ray diffractionInfo
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- JPH0914946A JPH0914946A JP16332595A JP16332595A JPH0914946A JP H0914946 A JPH0914946 A JP H0914946A JP 16332595 A JP16332595 A JP 16332595A JP 16332595 A JP16332595 A JP 16332595A JP H0914946 A JPH0914946 A JP H0914946A
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Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、Ｘ線回折を利用した膜
厚測定方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a film thickness measuring method using X-ray diffraction.
【０００２】[0002]
【従来の技術】近年、品質管理上或いは研究開発上、各
種蒸着法，メッキ等により基板上に形成された皮膜の膜
厚を測定することが要求されている。膜厚測定方法とし
ては、破壊式のもの，非破壊式のものがあり、例えば破
壊式のものとして顕微鏡断面法や電解式厚さ測定法等が
あり、また、例えば非破壊式のものとして蛍光Ｘ線によ
る方法，β線による方法，渦電流法等が知られている。2. Description of the Related Art In recent years, for quality control or research and development, it is required to measure the film thickness of a film formed on a substrate by various vapor deposition methods, plating and the like. There are destructive and non-destructive film thickness measuring methods. For example, destructive methods include a microscopic cross-section method and electrolytic thickness measuring method. X-ray method, β-ray method, eddy current method and the like are known.
【０００３】非破壊式の膜厚測定方法として、蛍光Ｘ線
による膜厚測定方法は精度，操作の簡便性等の利点が多
く代表的なものとされている。この蛍光Ｘ線による膜厚
測定方法は金属の皮膜試料の一定面積にＸ線を照射し、
発生する蛍光Ｘ線の強度が金属の皮膜の厚さに比例する
ことを原理とするもので、予め厚さが既知の標準膜厚板
を用いて厚みと蛍光Ｘ線の強度の関係を検量線として記
憶しておき、未知の厚みの試料から得られる蛍光Ｘ線の
強度と検量線によって膜厚を測定するものである。As a non-destructive film thickness measuring method, a film thickness measuring method using a fluorescent X-ray is typical because it has many advantages such as accuracy and easiness of operation. This fluorescent X-ray film thickness measuring method irradiates a certain area of a metal coating sample with X-rays,
The principle is that the intensity of the fluorescent X-rays generated is proportional to the thickness of the metal film. Using a standard thickness plate whose thickness is known in advance, the relationship between the thickness and the intensity of the fluorescent X-rays is calibrated. The thickness of the film is measured by the intensity of a fluorescent X-ray obtained from a sample having an unknown thickness and a calibration curve.
【０００４】[0004]
【発明が解決しようとする課題】ところが、蛍光Ｘ線に
よる膜厚測定方法で試料の膜厚を測定するためには、専
用機としての蛍光Ｘ線膜厚装置が必要とされるが、この
蛍光Ｘ線膜厚装置は膜厚測定の専用機としての機能に限
定されるため、分析装置を、精度良く、簡易に測定でき
る膜厚装置としても使用し、蛍光Ｘ線膜厚装置に代える
ことが求められている。However, in order to measure the film thickness of the sample by the film thickness measuring method using fluorescent X-rays, a fluorescent X-ray film thickness device as a dedicated machine is required. Since the X-ray film thickness device is limited in its function as a dedicated device for film thickness measurement, it is possible to replace the fluorescent X-ray film thickness device by using the analyzer also as a film thickness device capable of measuring accurately and easily. It has been demanded.
【０００５】蛍光Ｘ線による膜厚測定方法では、予め実
験的に蛍光Ｘ線の強度と膜厚の関係を検量線として求め
ておくことが必要で、依然として、操作の簡便性を満足
することができなかった。また、膜厚の時々刻々の変化
を捉える動的測定法として、水晶振動子法が用いられて
いる。この水晶振動子法は水晶振動子の固有振動がその
質量の変化によって変化することを利用したものであ
る。即ち、水晶振動子に薄膜が蒸着されると、水晶振動
子の質量に比べてその薄膜の質量が充分に小さければ、
単に水晶振動子の質量或いは厚さが増加したのと同じ効
果が生じ、質量変化に比例した固有振動の変化が生じる
ことを利用したものである。この水晶振動子法で例えば
真空蒸着法による薄膜作成時の膜厚が測定される。In the method of measuring the film thickness by the fluorescent X-ray, it is necessary to experimentally obtain the relationship between the intensity of the fluorescent X-ray and the film thickness as a calibration curve in advance, and still the easiness of the operation can be satisfied. could not. Further, a quartz oscillator method is used as a dynamic measurement method for catching a momentary change in film thickness. This crystal oscillator method utilizes the fact that the natural vibration of the crystal oscillator changes according to the change in its mass. That is, when a thin film is deposited on a crystal unit, if the mass of the thin film is sufficiently smaller than the mass of the crystal unit,
This is because the same effect as that of increasing the mass or thickness of the crystal unit occurs, and the change of natural vibration in proportion to the change of mass occurs. With this crystal oscillator method, for example, the film thickness at the time of forming a thin film by the vacuum evaporation method is measured.
【０００６】ところが、この水晶振動子法により成膜中
に膜厚を測定すると、間接的に膜厚を測定することにな
り、水晶振動子のセッティングの方法，成膜状態等の条
件によって測定された膜厚が実際の膜厚と相違すること
があり、膜厚の測定データに誤差を含む可能性がある。
本発明は、上述の問題点を解決するためになされたもの
で、その目的は、蛍光Ｘ線膜厚装置に代えて精度良く、
検量線を必要としないで簡易に膜厚を測定でき、しか
も、成膜中に膜厚を測定することができるＸ線回折を利
用した膜厚測定方法を提供することである。However, if the film thickness is measured during film formation by the crystal oscillator method, the film thickness is indirectly measured, and the film thickness is measured according to the setting method of the crystal oscillator, the film forming state and the like. The film thickness may differ from the actual film thickness, and the measurement data of the film thickness may include an error.
The present invention has been made to solve the above-mentioned problems, and its purpose is to replace the fluorescent X-ray film thickness device with high accuracy,
It is an object of the present invention to provide a film thickness measuring method using X-ray diffraction, which can easily measure the film thickness without requiring a calibration curve and can measure the film thickness during film formation.
【０００７】[0007]
【課題を解決するための手段】請求項１記載の発明は、
基板上に形成された皮膜の膜厚を測定するに際し、皮膜
上に照射されたＸ線が回折して生じた回折Ｘ線の強度を
測定するＸ線強度検出器を、基板からの回折Ｘ線のみを
検出する位置に固定し、照射されるＸ線の入射角度を０
度から変化させて、Ｘ線強度検出器により、Ｘ線の入射
角度に対応する基板からの回折Ｘ線の強度を測定し、Ｘ
線の入射角度に対応する基板からの回折Ｘ線の強度の関
係図を作り、測定された回折Ｘ線の強度の零値から増加
傾向に変化する立上り点を生じさせるＸ線の入射角度の
値を入射深さに換算して皮膜の膜厚を求めることを特徴
とする。According to the first aspect of the present invention,
When measuring the film thickness of the film formed on the substrate, an X-ray intensity detector for measuring the intensity of the diffracted X-ray generated by diffracting the X-ray irradiated on the film is used. Fix the position to detect only the X-ray incident angle to 0
X-ray intensity detector measures the intensity of the diffracted X-ray from the substrate corresponding to the incident angle of X-ray,
X-ray incident angle value that creates a rising point that changes from zero value of the measured diffracted X-ray intensity to an increasing tendency by making a relational diagram of the intensity of the diffracted X-ray from the substrate corresponding to the incident angle of the X-ray Is converted into the incident depth, and the film thickness of the film is obtained.
【０００８】請求項２記載の発明は、基板上に形成され
た皮膜の膜厚を測定するに際し、皮膜上に照射されたＸ
線が回折して生じた回折Ｘ線の強度を測定するＸ線強度
検出器を、皮膜からの回折Ｘ線のみを検出する位置に固
定し、照射されるＸ線の入射角度を０度から変化させ
て、Ｘ線強度検出器により、Ｘ線の入射角度に対応する
皮膜からの回折Ｘ線の強度を測定し、Ｘ線の入射角度に
対応する皮膜からの回折Ｘ線の強度の関係図を作り、測
定された回折Ｘ線の強度の増加傾向から減少傾向に変化
する変位点を生じさせるＸ線の入射角度の値を入射深さ
に換算して皮膜の膜厚を求めることを特徴とする。According to a second aspect of the present invention, when the film thickness of the film formed on the substrate is measured, X irradiated on the film is measured.
The X-ray intensity detector, which measures the intensity of the diffracted X-rays generated by diffracted rays, is fixed at a position that detects only the diffracted X-rays from the film, and the incident angle of the irradiated X-rays is changed from 0 degrees. Then, the intensity of the diffracted X-ray from the film corresponding to the incident angle of the X-ray is measured by the X-ray intensity detector, and the relationship diagram of the intensity of the diffracted X-ray from the film corresponding to the incident angle of the X-ray is shown. It is characterized in that the film thickness of the film is obtained by converting the value of the incident angle of the X-ray that causes the displacement point where the measured diffracted X-ray intensity changes from the increasing tendency to the decreasing tendency to the incident depth. .
【０００９】[0009]
【作用】請求項１記載の発明においては、Ｘ線の入射角
度αが０度（皮膜の表面と平行な方向）から増加され
る。この変化に伴い、Ｘ線は徐々に皮膜より内部に深く
入るようになる。 （１）Ｘ線の入射角度が小さいと、Ｘ線は皮膜のみに入
り、皮膜によるＸ線回折は生じるが、基板には到達せ
ず、基板によるＸ線回折は生じない。According to the first aspect of the invention, the incident angle α of X-rays is increased from 0 degree (direction parallel to the surface of the film). With this change, X-rays gradually enter deeper inside the film. (1) When the incident angle of X-rays is small, X-rays enter only the film and X-ray diffraction occurs by the film, but does not reach the substrate and X-ray diffraction by the substrate does not occur.
【００１０】そして、Ｘ線強度検出器の位置が特定され
た位置にあるので、皮膜に照射されて回折した回折Ｘ線
の強度は、Ｘ線強度検出器により零値として検出され
る。 （２）Ｘ線の入射角度が大きくなり、所定の角度以上に
なると、Ｘ線は皮膜と基板の両方に入る。Ｘ線の入射角
度の増加に伴って、Ｘ線は基板の表面から基板の内部に
深く入る。Ｂｒａｇｇの式を満たす場合、Ｘ線は基板表
面及び基板の内部で回折されて回折Ｘ線が種々の方向に
向けて生じる。Since the position of the X-ray intensity detector is at the specified position, the intensity of the diffracted X-rays which are irradiated on the film and diffracted is detected as a zero value by the X-ray intensity detector. (2) When the incident angle of X-rays becomes large and exceeds a predetermined angle, X-rays enter both the film and the substrate. As the incident angle of X-rays increases, the X-rays penetrate deep into the inside of the substrate from the surface of the substrate. When the Bragg equation is satisfied, X-rays are diffracted on the surface of the substrate and inside the substrate, and diffracted X-rays are generated in various directions.
【００１１】Ｘ線強度検出器と同角度の回折Ｘ線の強度
はＸ線強度検出器により検出される。Ｘ線強度検出器に
より基板からの回折Ｘ線のみが測定される。ここで、皮
膜に照射されて回折した回折Ｘ線の強度はＸ線強度検出
器の位置が特定された位置にあるので、Ｘ線強度検出器
により検出されない。次に、請求項１記載の発明に係わ
るＸ線回折を利用した膜厚測定方法の原理について説明
する。The intensity of diffracted X-rays at the same angle as the X-ray intensity detector is detected by the X-ray intensity detector. Only the diffracted X-rays from the substrate are measured by the X-ray intensity detector. Here, the intensity of the diffracted X-rays which are applied to the film and diffracted are not detected by the X-ray intensity detector because the position of the X-ray intensity detector is specified. Next, the principle of the film thickness measuring method using X-ray diffraction according to the first aspect of the present invention will be described.
【００１２】一般に、Ｘ線の入射条件がＢｒａｇｇの式
を満たす場合に回折現象を起こし、Ｂｒａｇｇの式が以
下のように成立する。 ｎλ＝２ｄ・ｓｉｎθ ここで、λはＸ線の波長，ｄは格子面間隔，θはＸ線の
回折角度である。ｎは回折の次数で、一般に１として扱
われる。Generally, when the X-ray incidence condition satisfies the Bragg equation, a diffraction phenomenon occurs, and the Bragg equation is established as follows. nλ = 2d · sin θ where λ is the wavelength of X-rays, d is the lattice spacing, and θ is the diffraction angle of X-rays. n is the order of diffraction and is generally treated as 1.
【００１３】即ち、Ｂｒａｇｇの式を満たすＸ線の入射
角度に対して強い回折があり、回折Ｘ線の強度が大きく
なる。格子面間隔ｄは個々の材料が有する物性値で、Ｘ
線の波長が分かれば、Ｂｒａｇｇの式に、Ｘ線の回折強
度が得られる回折角度θを代入することで求められる。
これは、材料を決めれば、Ｘ線の回折角度θが決定され
ることを意味している。That is, there is strong diffraction with respect to the incident angle of the X-ray that satisfies the Bragg equation, and the intensity of the diffracted X-ray increases. The lattice spacing d is a physical property value of each material, and X
If the wavelength of the line is known, it can be obtained by substituting the diffraction angle θ for obtaining the X-ray diffraction intensity into the Bragg equation.
This means that if the material is determined, the diffraction angle θ of the X-ray is determined.
【００１４】従って、皮膜，基板の材料を特定すれば、
Ｘ線の回折角度θが決定され、材料を特定したＸ線の入
射角度αに対して、強い回折があり、回折Ｘ線の強度が
大きくなることを意味している。しかも、Ｘ線強度検出
器が、基板からの回折Ｘ線のみを検出する位置に固定さ
れているので、Ｘ線強度検出器により、基板からの回折
Ｘ線は検出されるが、皮膜からの回折Ｘ線は検出されな
い。Therefore, if the materials of the film and the substrate are specified,
The diffraction angle θ of the X-ray is determined, which means that there is strong diffraction with respect to the incident angle α of the X-ray that specifies the material, and the intensity of the diffracted X-ray increases. Moreover, since the X-ray intensity detector is fixed at a position that detects only the diffracted X-rays from the substrate, the X-ray intensity detector detects the diffracted X-rays from the substrate, but the diffraction from the film. No X-rays are detected.
【００１５】上述のようにＸ線の入射角度αを０度（皮
膜の表面と平行な方向）から増加させると、所定の角度
までは、Ｘ線は皮膜のみに入り、基板には到達しない。
所定の角度になると、Ｘ線は基板で回折されて回折Ｘ線
が生じる。Ｘ線の入射角度がさらに増加されると、Ｘ線
が基板の内部に深く入り、基板による回折Ｘ線の回折量
が多くなることから、Ｘ線強度検出器により検出される
基板からの回折Ｘ線の強度が増加する。As described above, when the incident angle α of X-rays is increased from 0 degree (direction parallel to the surface of the film), the X-rays enter only the film and do not reach the substrate up to a predetermined angle.
At a predetermined angle, the X-rays are diffracted by the substrate to generate diffracted X-rays. When the incident angle of the X-rays is further increased, the X-rays penetrate deep inside the substrate, and the diffraction amount of the diffracted X-rays by the substrate increases, so that the diffraction X-rays from the substrate detected by the X-ray intensity detector are detected. The strength of the line increases.
【００１６】従って、例えば横軸にＸ線の入射角度を取
り、縦軸に回折Ｘ線の強度を取った関係図を作成すれ
ば、Ｘ線の入射角度が所定の角度の範囲までは基板から
の回折Ｘ線の強度は零で、Ｘ線の入射角度が所定の角度
より大きくなるに従い、基板からの回折Ｘ線の強度が増
加することになる。即ち、回折Ｘ線の強度が零値から増
加傾向に変化する立上り点（Ｘ線の入射角度）を横軸上
で読むことにより、所定の角度が求められる。この所定
の角度が皮膜の膜厚に対応しており、次の式で所定の角
度が入射深さに換算され、入射深さが皮膜の膜厚とな
る。Therefore, for example, if a relational diagram is created in which the horizontal axis represents the incident angle of X-rays and the vertical axis represents the intensity of diffracted X-rays, from the substrate, the incident angle of X-rays is within a predetermined angle range. The intensity of the diffracted X-ray is zero, and the intensity of the diffracted X-ray from the substrate increases as the incident angle of the X-ray becomes larger than a predetermined angle. That is, the predetermined angle is obtained by reading the rising point (incident angle of X-ray) where the intensity of the diffracted X-ray changes from zero value to the increasing tendency on the horizontal axis. This predetermined angle corresponds to the film thickness of the film, and the predetermined angle is converted into the incident depth by the following formula, and the incident depth becomes the film thickness of the film.
【００１７】ｔ＝（４．６／μ）・ｓｉｎα ここで、ｔはＸ線の入射深さ、μは線吸収係数、αはＸ
線の入射角度（所定の角度）である。T = (4.6 / μ) · sin α where t is the incident depth of X-rays, μ is the linear absorption coefficient, and α is X.
It is the incident angle (predetermined angle) of the line.
【００１８】請求項２記載の発明においては、Ｘ線の入
射角度αが０度（皮膜の表面と平行な方向）から増加さ
れる。この変化に伴い、Ｘ線は徐々に皮膜より内部に深
く入るようになる。 （１）Ｘ線の入射角度が小さいと、Ｘ線は皮膜のみに入
り、基板には到達せず、基板によるＸ線の回折は起こら
ない。皮膜に入ったＸ線は、皮膜で回折して回折Ｘ線が
種々の方向に向けて生じる。Ｘ線強度検出器と同角度の
回折Ｘ線はＸ線強度検出器により検出され、Ｘ線の入射
角度が増加するに従って増加する。即ち、Ｘ線の入射角
度に対応する皮膜からの回折Ｘ線の強度の関係図を作
り、関係図上で、測定された回折Ｘ線の強度は増加傾向
となる。According to the second aspect of the invention, the incident angle α of X-rays is increased from 0 degree (direction parallel to the surface of the film). With this change, X-rays gradually enter deeper inside the film. (1) When the incident angle of X-rays is small, the X-rays enter only the film, do not reach the substrate, and the X-ray diffraction by the substrate does not occur. The X-rays that have entered the film are diffracted by the film, and diffracted X-rays are generated in various directions. Diffracted X-rays at the same angle as the X-ray intensity detector are detected by the X-ray intensity detector and increase as the incident angle of X-rays increases. That is, a relational diagram of the intensity of the diffracted X-ray from the film corresponding to the incident angle of the X-ray is created, and the intensity of the measured diffracted X-ray tends to increase on the relational diagram.
【００１９】（２）Ｘ線の入射角度が大きくなり、所定
の角度以上になると、Ｘ線は皮膜と基板の両方に入る。
Ｘ線は皮膜，基板で回折されて回折Ｘ線が生じる。Ｘ線
の入射角度の増加に伴って、所定の角度以上になると、
Ｘ線が基板に入り、基板からも回折Ｘ線が生じるが、基
板にＸ線が照射されても、Ｘ線強度検出器が特定された
位置にあるので、皮膜からの回折Ｘ線の強度はＸ線強度
検出器で計測される回折Ｘ線の強度から基板で回折して
生じた回折Ｘ線の強度を差し引いた値となり、減少傾向
となる。(2) When the incident angle of X-rays becomes large and exceeds a predetermined angle, X-rays enter both the film and the substrate.
X-rays are diffracted by the film and the substrate to generate diffracted X-rays. As the incident angle of X-rays increases, when the angle exceeds a predetermined angle,
X-rays enter the substrate, and diffracted X-rays are also generated from the substrate. Even if the substrate is irradiated with X-rays, the intensity of the diffracted X-rays from the film is still high because the X-ray intensity detector is located at the specified position. The value becomes a value obtained by subtracting the intensity of the diffracted X-ray generated by diffracting on the substrate from the intensity of the diffracted X-ray measured by the X-ray intensity detector, and the value tends to decrease.
【００２０】即ち、Ｘ線の入射角度に対応する皮膜から
の回折Ｘ線の強度の関係図上で、測定された回折Ｘ線の
強度は変位点を境にして増加傾向から減少傾向に変化す
る。この変位点を生じさせる入射角度の値が入射深さに
換算されて、皮膜の膜厚が求められる。なお、請求項２
記載の発明に係わるＸ線回折を利用した膜厚測定方法の
原理については、請求項１記載の発明に係わるＸ線回折
を利用した膜厚測定方法の原理と基本的に同様なので説
明を省略する。That is, in the relationship diagram of the intensity of the diffracted X-ray from the film corresponding to the incident angle of the X-ray, the measured intensity of the diffracted X-ray changes from the increasing tendency to the decreasing tendency at the displacement point. . The value of the incident angle that causes this displacement point is converted into the incident depth to obtain the film thickness of the coating. Claim 2
The principle of the film thickness measuring method using X-ray diffraction according to the described invention is basically the same as the principle of the film thickness measuring method using X-ray diffraction according to the invention of claim 1, and therefore the description thereof is omitted. .
【００２１】[0021]
【実施例】以下、図面により本発明の実施例について説
明する。図１ないし図３により請求項１記載の発明の実
施例に係わるＸ線回折を利用した膜厚測定方法について
説明する。図１において、符号１は試料で、この試料１
は基板２と、基板２上に形成された皮膜３とで構成され
ている。基板２，皮膜３の材料は結晶質で、例えば金
属，セラミックスが挙げられ、ガラス，アモルファス金
属のような非晶質の材料は含まれない。Embodiments of the present invention will be described below with reference to the drawings. 1 to 3, a film thickness measuring method using X-ray diffraction according to an embodiment of the present invention will be described. In FIG. 1, reference numeral 1 is a sample, and this sample 1
Is composed of a substrate 2 and a film 3 formed on the substrate 2. The material of the substrate 2 and the film 3 is crystalline, and examples thereof include metals and ceramics, and do not include amorphous materials such as glass and amorphous metal.
【００２２】４はＸ線照射装置で、図面上、試料１の上
方に配置され、また、Ｘ線強度検出器５が試料１の上方
に配置されている。Ｘ線強度検出器５は皮膜３上に照射
されたＸ線が回折して生じた基板２からの回折Ｘ線６の
強度を測定するもので、基板２からの回折Ｘ線６のみを
検出する位置に固定されている。かかるＸ線照射装置
４，Ｘ線強度検出器５の配置の下に、次のように皮膜３
の膜厚が求められる。An X-ray irradiation device 4 is arranged above the sample 1 in the drawing, and an X-ray intensity detector 5 is arranged above the sample 1. The X-ray intensity detector 5 measures the intensity of the diffracted X-rays 6 from the substrate 2 generated by diffracting the X-rays irradiated on the film 3, and detects only the diffracted X-rays 6 from the substrate 2. It is fixed in position. Under the arrangement of the X-ray irradiation device 4 and the X-ray intensity detector 5, the film 3 is formed as follows.
The film thickness of is required.
【００２３】先ず、Ｘ線照射装置４からＸ線が皮膜３に
照射される。照射されるＸ線の入射角度αが０度から増
加されると、回折現象が生じ、試料１から回折Ｘ線６が
回折し、この回折Ｘ線６の強度はＸ線強度検出器５によ
り測定される。回折Ｘ線６の強度はＸ線の入射角度に対
応しており、図２に示すように、横軸にＸ線の入射角
度，縦軸に基板２からの回折Ｘ線６の強度を取った関係
図が得られる。First, the coating 3 is irradiated with X-rays from the X-ray irradiation device 4. When the incident angle α of the irradiated X-ray is increased from 0 degree, a diffraction phenomenon occurs and the diffracted X-ray 6 is diffracted from the sample 1, and the intensity of this diffracted X-ray 6 is measured by the X-ray intensity detector 5. To be done. The intensity of the diffracted X-ray 6 corresponds to the incident angle of the X-ray. As shown in FIG. 2, the horizontal axis represents the incident angle of the X-ray and the vertical axis represents the intensity of the diffracted X-ray 6 from the substrate 2. A relationship diagram is obtained.
【００２４】図２に示す関係図において、測定された回
折Ｘ線６の強度は零値から立上り点Ｗを境として増加傾
向に変化する。Ｘ線の入射角度αがＸ線の入射角度α
（ｋ１）より小さく、例えば入射角度αがα（１）の時
には回折Ｘ線６の強度は零値となる。Ｘ線の入射角度α
がＸ線の入射角度α（ｋ１）より大きく、例えば入射角
度αがα（２）の時には回折Ｘ線６の強度は増加傾向と
なる。In the relationship diagram shown in FIG. 2, the measured intensity of the diffracted X-ray 6 changes from a zero value to an increasing tendency with the rising point W as a boundary. X-ray incident angle α is X-ray incident angle α
The intensity of the diffracted X-ray 6 becomes zero when the incident angle α is smaller than (k1), for example, α (1). X-ray incident angle α
Is larger than the incident angle α (k1) of the X-ray, and for example, when the incident angle α is α (2), the intensity of the diffracted X-ray 6 tends to increase.
【００２５】図２に示す関係図から立上り点Ｗ（Ｘ線の
入射角度）を横軸上で読むことにより、入射角度α（ｋ
１）が求められる。次の式で入射角度α（ｋ１）がＸ線
の入射深さに換算され、Ｘ線の入射深さが皮膜３の膜厚
となる。このように、入射角度α（ｋ１）に対応して皮
膜３の膜厚が求められる。 ｔ＝（４．６／μ）・ｓｉｎα・・・（１） ここで、ｔは入射深さ，μは線吸収係数，αはＸ線の入
射角度である。By reading the rising point W (incident angle of X-ray) on the horizontal axis from the relationship diagram shown in FIG. 2, the incident angle α (k
1) is required. The incident angle α (k1) is converted into the X-ray incident depth by the following formula, and the X-ray incident depth becomes the film thickness of the film 3. In this way, the film thickness of the film 3 is obtained corresponding to the incident angle α (k1). t = (4.6 / μ) · sin α (1) where t is the depth of incidence, μ is the linear absorption coefficient, and α is the incident angle of X-rays.
【００２６】この式はＸ線の浸透深さを示すもので、以
下のように求められる。安東和人著「薄膜Ｘ線回折法」
（日本電子株式会社発行のＪＥＯＬ ａｐｐｌｉｃａｔ
ｉｏｎ ｎｏｔｅ ＸＲ２２）のＰ６〜Ｐ７によれば、
入射角度α（ｋ１）に対応して皮膜３の膜厚を求める式
として ｔ＝｛ｌｎ（１／（１−ＧX））｝／｛μ（１／ｓｉｎα）｝・・・（２） が記載されている。This equation shows the penetration depth of X-rays and is obtained as follows. Kazuto Ando "Thin Film X-ray Diffraction Method"
(JEOL apply published by JEOL Ltd.
According to P6 to P7 of ion note XR22),
As an expression for obtaining the film thickness of the film 3 corresponding to the incident angle α (k1), t = {ln (1 / (1-G X ))} / {μ (1 / sin α)} (2) Have been described.
【００２７】ここで、ＧXは、試料に強度ＩPのＸ線が入
射した時、強度ＩPに対して、試料の表面から所定の深
さでのＸ線回折強度の比率で、精度測定上からＧXは実
験的に９９％が適切な値と確認され、この値を（２）式
に代入すると、（１）式が得られる。また、線吸収係数
μは次のように求められる。Ｘ線は物質を透過すると減
衰し、波長一定のＸ線が物質を一定方向にｘｃｍだけ透
過したとき、強度がＩ0からＩに減衰したとすれば、 Ｉ＝Ｉ0・ｅｘｐ（−μｘ） と表され、μ（ｃｍ-1）が線吸収係数と呼ばれている。[0027] Here, G X, when X-ray intensity I P is incident on the sample, with respect to the intensity I P, the ratio of X-ray diffraction intensity at a given depth from the surface of the sample, accuracy measurement From the above, 99% of G X is experimentally confirmed to be a proper value, and by substituting this value into the equation (2), the equation (1) is obtained. Further, the linear absorption coefficient μ is obtained as follows. X-rays are attenuated when they pass through a substance, and when X-rays having a constant wavelength pass through the substance by xcm in a certain direction, assuming that the intensity is attenuated from I 0 to I, I = I 0 · exp (−μx) And μ (cm −1 ) is called the linear absorption coefficient.
【００２８】なお、上述の式はカリティ著「Ｘ線回折要
論」（アグネ出版）のＰ２６７にもＧXを求める式が記
載され、同様にして（１）式を求めることができる。次
に、本実施例の作用を説明する。Ｘ線の入射角度αが０
度（皮膜３の表面と平行な方向）から増加される。この
変化に伴い、Ｘ線は徐々は皮膜３から内部に深く入るよ
うになる。It should be noted, the above formula is described equation for G X to P267 of Kariti al "X-ray diffraction main theory" (Agne Publishing), it can be determined similarly to equation (1). Next, the operation of the present embodiment will be described. X-ray incidence angle α is 0
Degree (direction parallel to the surface of the film 3). With this change, X-rays gradually enter deep inside the film 3.
【００２９】（１）Ｘ線の入射角度が小さいと、例えば
入射角度αがα（１）の時には、Ｘ線は皮膜３のみに入
り、基板２には到達せず、基板２によるＸ線回折は生じ
ない。そして、Ｘ線強度検出器５が特定された位置にあ
るので、皮膜３に照射されて回折した回折Ｘ線６の強度
は、Ｘ線強度検出器５により零値として検出される。 （２）Ｘ線の入射角度が大きくなり、入射角度α（ｋ
１）以上になると、例えば入射角度αがα（２）の時に
は、Ｘ線は皮膜３と基板２の両方に照射される。(1) When the incident angle of X-rays is small, for example, when the incident angle α is α (1), the X-rays enter only the film 3 and do not reach the substrate 2, and the X-ray diffraction by the substrate 2 occurs. Does not occur. Then, since the X-ray intensity detector 5 is located at the specified position, the intensity of the diffracted X-ray 6 which is irradiated on the film 3 and diffracted is detected by the X-ray intensity detector 5 as a zero value. (2) The incident angle of X-ray becomes large, and the incident angle α (k
When 1) or more, for example, when the incident angle α is α (2), X-rays are applied to both the film 3 and the substrate 2.
【００３０】Ｘ線の入射角度の増加に伴って、Ｘ線は基
板２の表面から基板２の内部に深く入る。Ｘ線は基板２
の表面及び基板２の内部で回折されて回折Ｘ線６が種々
の方向に向けて生じる。Ｘ線強度検出器５と同角度の回
折Ｘ線６の強度はＸ線強度検出器５により検出される。
Ｘ線強度検出器５により基板２からの回折Ｘ線６のみが
測定される。As the incident angle of X-rays increases, the X-rays penetrate deep into the inside of the substrate 2 from the surface of the substrate 2. X-ray is substrate 2
X-rays 6 are generated in various directions by being diffracted on the surface of the substrate and inside the substrate 2. The intensity of the diffracted X-ray 6 having the same angle as the X-ray intensity detector 5 is detected by the X-ray intensity detector 5.
The X-ray intensity detector 5 measures only the diffracted X-rays 6 from the substrate 2.
【００３１】ここで、皮膜３に照射されて回折した回折
Ｘ線６の強度はＸ線強度検出器５が特定された位置にあ
るので、Ｘ線強度検出器５により検出されない。次に、
本実施例に係わるＸ線回折を利用した膜厚測定方法の原
理について説明する。一般に、結晶質の試料に入射され
たＸ線は、Ｂｒａｇｇの式を満たす角度で回折現象を起
こし、Ｂｒａｇｇの式が以下のように成立する。Here, the intensity of the diffracted X-rays 6 which are applied to the film 3 and diffracted are not detected by the X-ray intensity detector 5 because the X-ray intensity detector 5 is located at the specified position. next,
The principle of the film thickness measuring method using X-ray diffraction according to this embodiment will be described. Generally, an X-ray incident on a crystalline sample causes a diffraction phenomenon at an angle satisfying the Bragg equation, and the Bragg equation is established as follows.
【００３２】ｎλ＝２ｄ・ｓｉｎθ ここで、λはＸ線の波長，ｄは格子面間隔，θはＸ線の
回折角度である。ｎは回折の次数で、一般に１として扱
われる。即ち、Ｂｒａｇｇの式を満たすＸ線の入射角度
に対して強い回折があり、回折Ｘ線６の強度が大きくな
る。Nλ = 2d · sin θ where λ is the wavelength of X-rays, d is the lattice spacing, and θ is the diffraction angle of X-rays. n is the order of diffraction and is generally treated as 1. That is, there is strong diffraction with respect to the incident angle of the X-ray that satisfies the Bragg equation, and the intensity of the diffracted X-ray 6 becomes large.
【００３３】格子面間隔ｄは個々の材料が有する物性値
で、Ｘ線の波長が分かれば、Ｂｒａｇｇの式に、Ｘ線の
回折強度が得られる回折角度θを代入することで求めら
れる。これは、材料を決めれば、Ｘ線の回折角度θが決
定されることを意味している。The lattice spacing d is a physical property value of each material, and if the X-ray wavelength is known, it can be obtained by substituting the diffraction angle θ for obtaining the X-ray diffraction intensity into the Bragg equation. This means that if the material is determined, the diffraction angle θ of the X-ray is determined.
【００３４】従って、皮膜３，基板２の材料を特定すれ
ば、Ｘ線の回折角度θが決定され、材料を特定したＸ線
の入射角度αに対して、強い回折があり、回折Ｘ線６の
強度が大きくなることを意味している。しかも、Ｘ線強
度検出器５が、基板２からの回折Ｘ線６のみを検出する
位置に固定されているので、Ｘ線強度検出器５により、
基板２からの回折Ｘ線６は検出されるが、皮膜３からの
回折Ｘ線６は検出されない。Therefore, if the material of the film 3 and the substrate 2 is specified, the diffraction angle θ of the X-ray is determined, there is strong diffraction with respect to the incident angle α of the X-ray specifying the material, and the diffracted X-ray 6 It means that the strength of is increased. Moreover, since the X-ray intensity detector 5 is fixed at a position for detecting only the diffracted X-rays 6 from the substrate 2, the X-ray intensity detector 5
The diffracted X-rays 6 from the substrate 2 are detected, but the diffracted X-rays 6 from the film 3 are not detected.
【００３５】従って、上述のようにＸ線の入射角度αを
０度（皮膜の表面と平行な方向）から増加させると、入
射角度α（ｋ１）までは、Ｘ線は皮膜３のみに入り、基
板２には到達せず、基板２によるＸ線の回折は起こらな
い。皮膜３で回折された回折Ｘ線はＸ線強度検出器５に
より検出されない。入射角度α（ｋ１）になると、Ｘ線
は基板２で回折されて回折Ｘ線６が生じる。Ｘ線の入射
角度がさらに増加されると、Ｘ線が基板２の内部に深く
入り、基板２による回折Ｘ線６の回折量が多くなること
から、Ｘ線強度検出器５により検出される回折Ｘ線６の
強度が増加する。Therefore, when the incident angle α of X-rays is increased from 0 degree (direction parallel to the surface of the film) as described above, the X-rays enter only the film 3 until the incident angle α (k1). The substrate 2 is not reached, and the X-ray diffraction by the substrate 2 does not occur. The diffracted X-rays diffracted by the film 3 are not detected by the X-ray intensity detector 5. At the incident angle α (k1), the X-rays are diffracted by the substrate 2 to generate diffracted X-rays 6. When the incident angle of X-rays is further increased, the X-rays penetrate deep inside the substrate 2 and the amount of diffraction of the diffracted X-rays 6 by the substrate 2 increases, so that the diffraction detected by the X-ray intensity detector 5 is increased. The intensity of the X-ray 6 increases.
【００３６】従って、横軸にＸ線の入射角度を取り、縦
軸に回折Ｘ線６の強度を取った関係図を作れば、Ｘ線の
入射角度が所定の角度の範囲までは基板２からの回折Ｘ
線６の強度は零で、Ｘ線の入射角度が入射角度α（ｋ
１）より大きくなると、基板２からの回折Ｘ線６の強度
が増加することになる。そして、図２に示す関係図から
立上り点Ｗ（Ｘ線の入射角度）を横軸上で読むことによ
り、入射角度α（ｋ１）が求められ、入射角度α（ｋ
１）がＸ線の入射深さに換算され、Ｘ線の入射深さが皮
膜３の膜厚となる。Therefore, by making a relational diagram in which the horizontal axis represents the incident angle of X-rays and the vertical axis represents the intensity of the diffracted X-rays 6, it is possible to measure the incident angle of X-rays from the substrate 2 up to a predetermined angle range. Diffraction X
The intensity of the line 6 is zero, and the incident angle of the X-ray is the incident angle α (k
If it is larger than 1), the intensity of the diffracted X-ray 6 from the substrate 2 will increase. Then, by reading the rising point W (incident angle of X-ray) on the horizontal axis from the relationship diagram shown in FIG. 2, the incident angle α (k1) is obtained, and the incident angle α (k
1) is converted into the X-ray incident depth, and the X-ray incident depth becomes the film thickness of the film 3.
【００３７】次に、本実施例の実験例を説明する。基板
２としてＳＵＳ３０４ステンレス鋼が用いられ、この基
板２上に物理蒸着法により皮膜３として窒化チタンを蒸
着した試料１が準備される。Next, an experimental example of this embodiment will be described. SUS304 stainless steel is used as the substrate 2, and a sample 1 in which titanium nitride is vapor-deposited as the film 3 on the substrate 2 by the physical vapor deposition method is prepared.
【００３８】Ｘ線照射装置４の管電流を１００ｍＡ、管
電圧を４０ｋＶとし、Ｘ線の入射角度は０ないし５度の
範囲で変化される。Ｘ線強度検出器５の設定角度は５
０．８８３度（皮膜の表面に対して）である。これは、
基板２の材料であるＳＵＳ３０４ステンレス鋼（γ−Ｆ
ｅ）の（００２）面の面間隔１．７９４オングストロー
ム、Ｘ線の波長は１．５４オングストロームとしてＢｒ
ａｇｇの式より求めたものである。The tube current of the X-ray irradiator 4 is 100 mA, the tube voltage is 40 kV, and the X-ray incident angle is changed in the range of 0 to 5 degrees. The setting angle of the X-ray intensity detector 5 is 5
0.883 degrees (relative to the surface of the coating). this is,
SUS304 stainless steel (γ-F
In (e), the spacing of the (002) plane is 1.794 angstroms, and the X-ray wavelength is 1.54 angstroms.
It is obtained from the agg equation.
【００３９】図２に示すように、立上り点Ｗを生じさせ
る入射角度α（ｋ１）を求めると２．０度となり、入射
角度２．０度を入射深さに換算して皮膜３の膜厚２．０
μｍが求められる。この膜厚２．０μｍは走査型電子顕
微鏡による測定で確認されている。そして、図３に示す
ように、０．１μｍのレベルで膜厚が測定され、測定点
をプロットすると、直線Ｚが得られ、本実施例に係わる
Ｘ線回折を利用した膜厚測定方法による測定結果と、走
査型電子顕微鏡による測定結果が一致していることが示
されており、本実施例に係わるＸ線回折を利用した膜厚
測定方法による測定精度が高いことが実証されている。As shown in FIG. 2, the incident angle α (k1) that causes the rising point W is calculated to be 2.0 degrees, and the incident angle of 2.0 degrees is converted into the incident depth to obtain the film thickness of the film 3. 2.0
μm is required. This film thickness of 2.0 μm has been confirmed by measurement with a scanning electron microscope. Then, as shown in FIG. 3, the film thickness was measured at a level of 0.1 μm, and when the measurement points were plotted, a straight line Z was obtained, which was measured by the film thickness measuring method using X-ray diffraction according to this example. It is shown that the result and the measurement result by the scanning electron microscope are in agreement, and it is proved that the measurement accuracy by the film thickness measuring method using X-ray diffraction according to the present embodiment is high.
【００４０】以上の如き構成によれば、Ｘ線回折の原理
を利用することにより皮膜３の膜厚を求めることができ
る。即ち、皮膜３上に照射されるＸ線の入射角度αだけ
を変化させ、Ｘ線の入射角度αに対応する基板２からの
回折Ｘ線６の強度の関係図上で、測定された回折Ｘ線６
の強度の零値から増加傾向に変化する立上り点Ｗを生じ
させるＸ線の入射角度α（ｋ１）の値を読み取ることに
より、皮膜３の膜厚を求めることができる。According to the above-mentioned structure, the film thickness of the film 3 can be obtained by utilizing the principle of X-ray diffraction. That is, only the incident angle α of the X-rays irradiated on the film 3 is changed, and the measured diffraction X-rays are measured on the relationship diagram of the intensity of the diffracted X-rays 6 from the substrate 2 corresponding to the incident angle α of the X-rays. Line 6
The film thickness of the film 3 can be obtained by reading the value of the incident angle α (k1) of the X-ray that causes the rising point W that changes from the zero value of the intensity of 1 to the increasing tendency.
【００４１】従って、通常は結晶構造を解析するため等
に用いられるＸ線回折装置を、膜厚を測定するための装
置として用いることができ、専用機としての蛍光Ｘ線膜
厚装置に代えることができ、しかも、蛍光Ｘ線膜厚装置
による膜厚測定法と同等若しくはそれ以上の精度を確保
でき、また、蛍光Ｘ線膜厚装置による膜厚測定方法にお
ける検量線を必要とせず、操作の簡便性を満足すること
ができる。Therefore, the X-ray diffractometer, which is usually used for analyzing the crystal structure, can be used as a device for measuring the film thickness, and is replaced with a fluorescent X-ray film thickness device as a dedicated machine. In addition, the accuracy equal to or higher than that of the film thickness measuring method using the fluorescent X-ray film thickness device can be ensured, and the calibration curve in the film thickness measuring method using the fluorescent X-ray film thickness device is not required. The simplicity can be satisfied.
【００４２】また、皮膜３の成膜中に回折Ｘ線６の強度
を測定することにより、セッティングの方法，成膜状態
等の条件に左右されずに膜厚を直接測定し、膜厚の測定
データに誤差を含む可能性を少なくし、所要の膜厚の皮
膜を得ることができる。次に、図４，図５により請求項
２記載の発明の実施例に係わるＸ線回折を利用した膜厚
測定方法について説明する。Further, by measuring the intensity of the diffracted X-rays 6 during the film formation of the film 3, the film thickness is directly measured without being influenced by the setting method, the film forming state and the like, and the film thickness is measured. It is possible to obtain a film having a required film thickness by reducing the possibility that the data contains an error. Next, a film thickness measuring method using X-ray diffraction according to the embodiment of the invention described in claim 2 will be described with reference to FIGS.
【００４３】本実施例に係わる膜厚測定方法は、請求項
１記載の発明の実施例に係わるＸ線回折を利用した膜厚
測定方法における基板，皮膜が用いられ、装置として
も、Ｘ線照射装置，Ｘ線強度検出器が用いられ、これら
に同一符号を付してその説明を省略する。図４に示すよ
うに、本実施例におけるＸ線強度検出器７の位置は、請
求項１記載の発明の実施例に係わるＸ線強度検出器５の
位置とは相違し、皮膜３からの回折Ｘ線６のみを検出す
る位置に固定されている。In the film thickness measuring method according to the present embodiment, the substrate and the film in the film thickness measuring method utilizing X-ray diffraction according to the embodiment of the invention of claim 1 are used. An apparatus and an X-ray intensity detector are used, and the same reference numerals are given to them and their description is omitted. As shown in FIG. 4, the position of the X-ray intensity detector 7 in this embodiment is different from the position of the X-ray intensity detector 5 according to the embodiment of the invention described in claim 1, and the diffraction from the film 3 is different. It is fixed at a position where only the X-ray 6 is detected.
【００４４】かかるＸ線照射装置４，Ｘ線強度検出器７
の配置の下に、次のように皮膜３の膜厚が求められる。
先ず、Ｘ線照射装置４からＸ線が皮膜３に照射される。
照射されるＸ線の入射角度αが０度から増加されると、
回折現象が生じ、試料１から回折Ｘ線６が回折し、この
回折Ｘ線６の強度はＸ線強度検出器７により測定され
る。回折Ｘ線６の強度はＸ線の入射角度に対応してお
り、図５に示すように、横軸にＸ線の入射角度，縦軸に
皮膜３からの回折Ｘ線６の強度を取った関係図が得られ
る。The X-ray irradiation device 4 and the X-ray intensity detector 7
Under the arrangement of, the film thickness of the film 3 is obtained as follows.
First, the coating 3 is irradiated with X-rays from the X-ray irradiation device 4.
When the incident angle α of the irradiated X-ray is increased from 0 degree,
A diffraction phenomenon occurs and the diffracted X-ray 6 is diffracted from the sample 1, and the intensity of the diffracted X-ray 6 is measured by the X-ray intensity detector 7. The intensity of the diffracted X-ray 6 corresponds to the incident angle of the X-ray. As shown in FIG. 5, the abscissa represents the incident angle of the X-ray and the ordinate represents the intensity of the diffracted X-ray 6 from the film 3. A relationship diagram is obtained.
【００４５】図５に示す関係図において、測定された回
折Ｘ線６の強度は増加傾向から変位点Ｙを境として減少
傾向に変化する。Ｘ線の入射角度αがＸ線の入射角度α
（ｋ２）より小さく、例えば入射角度αがα（３）の時
には回折Ｘ線６の強度は増加傾向となる。Ｘ線の入射角
度αがＸ線の入射角度α（ｋ２）より大きく、例えば入
射角度αがα（４）の時には回折Ｘ線６の強度は減少傾
向となる。In the relationship diagram shown in FIG. 5, the measured intensity of the diffracted X-ray 6 changes from an increasing tendency to a decreasing tendency at the displacement point Y as a boundary. X-ray incident angle α is X-ray incident angle α
When the incident angle α is smaller than (k2) and the incident angle α is α (3), the intensity of the diffracted X-ray 6 tends to increase. When the incident angle α of X-rays is larger than the incident angle α (k2) of X-rays, for example, when the incident angle α is α (4), the intensity of the diffracted X-rays 6 tends to decrease.
【００４６】図５に示す関係図から、変位点Ｙを生じさ
せるＸ線の入射角度α（ｋ２）が求められ、請求項１記
載の発明の実施例と同様にＸ線の入射角度α（ｋ２）の
値を入射深さに換算して皮膜３の膜厚が求められる。即
ち、Ｘ線の入射角度α（ｋ２）に対応して皮膜３の膜厚
が求められる。次に、本実施例の作用を説明する。From the relationship diagram shown in FIG. 5, the incident angle α (k2) of the X-ray that causes the displacement point Y is determined, and the incident angle α (k2 of the X-ray is the same as in the embodiment of the invention described in claim 1. The value of) is converted into the incident depth to obtain the film thickness of the film 3. That is, the film thickness of the film 3 is determined in accordance with the incident angle α (k2) of the X-ray. Next, the operation of the present embodiment will be described.
【００４７】Ｘ線の入射角度αが０度（皮膜３の表面と
平行な方向）から増加される。この変化に伴い、Ｘ線は
徐々は皮膜３より内部に深く入るようになる。 （１）Ｘ線の入射角度が小さいと、Ｘ線は皮膜３のみに
入り、基板２には到達せず、基板２によるＸ線の回折は
起こらない。皮膜３に照射されたＸ線は、皮膜３で回折
して回折Ｘ線が種々の方向に向けて生じる。Ｘ線強度検
出器７と同角度の回折Ｘ線はＸ線強度検出器７により検
出され、増加する。即ち、Ｘ線の入射角度に対応する回
折Ｘ線６の強度の関係図上で、測定された回折Ｘ線６の
強度は増加傾向となる。The incident angle α of X-rays is increased from 0 degree (direction parallel to the surface of the film 3). With this change, X-rays gradually enter deeper inside the film 3. (1) When the incident angle of X-rays is small, the X-rays enter only the film 3, do not reach the substrate 2, and the diffraction of X-rays by the substrate 2 does not occur. The X-rays applied to the film 3 are diffracted by the film 3 to generate diffracted X-rays in various directions. Diffracted X-rays at the same angle as the X-ray intensity detector 7 are detected by the X-ray intensity detector 7 and increase. That is, the measured intensity of the diffracted X-ray 6 tends to increase on the relationship diagram of the intensity of the diffracted X-ray 6 corresponding to the incident angle of the X-ray.
【００４８】（２）Ｘ線の入射角度が大きくなり、所定
の角度以上になると、Ｘ線は皮膜３と基板２の両方に入
る。Ｘ線は皮膜３，基板２で回折されて回折Ｘ線が生じ
る。Ｘ線の入射角度の増加に伴って、所定の角度以上に
なると、Ｘ線が基板２に入り、基板２からも回折Ｘ線が
生じるが、基板２にＸ線が照射されても、Ｘ線強度検出
器７が特定された位置にあるので、皮膜３からの回折Ｘ
線の強度はＸ線強度検出器７で計測される回折Ｘ線６の
強度から基板２で回折して生じた回折Ｘ線６の強度を差
し引いた値となり、減少傾向となる。(2) When the incident angle of X-rays becomes large and exceeds a predetermined angle, X-rays enter both the film 3 and the substrate 2. The X-rays are diffracted by the film 3 and the substrate 2 to generate diffracted X-rays. As the incident angle of X-rays increases, when the angle becomes a predetermined angle or more, X-rays enter the substrate 2 and diffracted X-rays are also generated from the substrate 2. However, even if the substrate 2 is irradiated with X-rays, Since the intensity detector 7 is at the specified position, the diffraction X from the film 3
The intensity of the line has a value obtained by subtracting the intensity of the diffracted X-ray 6 generated by the substrate 2 from the intensity of the diffracted X-ray 6 measured by the X-ray intensity detector 7, and tends to decrease.
【００４９】即ち、Ｘ線の入射角度に対応する皮膜３か
らの回折Ｘ線６の強度の関係図を作り、関係図上で、測
定された回折Ｘ線６の強度は変位点Ｙを境にして増加傾
向から減少傾向に変化する。この変位点Ｙを生じさせる
入射角度の値が入射深さに換算されて、皮膜３の膜厚が
求められる。That is, a relational diagram of the intensity of the diffracted X-rays 6 from the film 3 corresponding to the incident angle of the X-rays is prepared, and the intensity of the diffracted X-rays 6 measured on the relational diagram demarcates the displacement point Y. Change from increasing to decreasing. The value of the incident angle that causes the displacement point Y is converted into the incident depth, and the film thickness of the film 3 is obtained.
【００５０】なお、本実施例に係わるＸ線回折を利用し
た膜厚測定方法の原理については、請求項１記載の発明
の実施例に係わるＸ線回折を利用した膜厚測定方法の原
理と基本的に同様なので説明を省略する。本実施例によ
れば、請求項１記載の発明の実施例に係わるＸ線回折を
利用した膜厚測定方法と同様の効果を奏する。Regarding the principle of the film thickness measuring method using X-ray diffraction according to the present embodiment, the principle and basics of the film thickness measuring method using X-ray diffraction according to the embodiment of the present invention are described. Since they are the same, the description is omitted. According to this embodiment, the same effect as the film thickness measuring method using X-ray diffraction according to the embodiment of the invention described in claim 1 can be obtained.
【００５１】[0051]
【発明の効果】請求項１記載の発明によれば、Ｘ線回折
の原理を利用することにより皮膜の膜厚を求めることが
できる。即ち、皮膜上に照射されるＸ線の入射角度だけ
を変化させ、Ｘ線の入射角度に対応する基板からの回折
Ｘ線の強度の関係図を作り、関係図上で、測定された回
折Ｘ線の強度の零値から増加傾向に変化する立上り点を
生じさせるＸ線の入射角度の値を読み取ることにより、
皮膜の膜厚を求めることができる。According to the invention described in claim 1, the film thickness of the film can be obtained by utilizing the principle of X-ray diffraction. That is, only the incident angle of X-rays irradiated on the film is changed, a relational diagram of the intensity of the diffracted X-rays from the substrate corresponding to the incident angle of X-rays is created, and the measured diffraction X-rays are plotted on the relational diagram. By reading the value of the incident angle of the X-ray that causes the rising point that changes from the zero value of the line intensity to the increasing tendency,
The film thickness of the film can be obtained.
【００５２】従って、通常は結晶構造を解析するため等
に用いられるＸ線回折装置を、膜厚を測定するための装
置として用い、専用機としての蛍光Ｘ線膜厚装置に代え
ることができ、しかも、蛍光Ｘ線膜厚装置による膜厚測
定法と同等若しくはそれ以上の精度を確保でき、また、
蛍光Ｘ線膜厚装置による膜厚測定方法における検量線を
必要とせず、操作の簡便性を満足することができる。Therefore, the X-ray diffractometer, which is usually used for analyzing the crystal structure and the like, can be used as a device for measuring the film thickness, and can be replaced by a dedicated fluorescent X-ray film thickness device. Moreover, it is possible to secure the accuracy equal to or higher than that of the film thickness measurement method using the fluorescent X-ray film thickness measurement device.
The calibration curve in the film thickness measuring method using the fluorescent X-ray film thickness device is not required, and the easiness of the operation can be satisfied.
【００５３】また、皮膜の成膜中に回折Ｘ線の強度を測
定することにより、セッティングの方法，成膜状態等の
条件に左右されずに膜厚を直接測定し、膜厚の測定デー
タに誤差を含む可能性を少なくし、所要の膜厚の皮膜を
得ることができる。請求項２記載の発明によれば、請求
項１記載の発明と同様の効果を奏する。By measuring the intensity of the diffracted X-rays during the film formation, the film thickness can be directly measured without being influenced by the setting method, the film forming state and the like, and the measured data of the film thickness can be obtained. It is possible to obtain a film having a required film thickness by reducing the possibility of including an error. According to the invention of claim 2, the same effect as that of the invention of claim 1 can be obtained.
【図１】請求項１記載の発明の実施例に係わるＸ線回折
を利用した膜厚測定方法の原理説明図である。FIG. 1 is a principle explanatory view of a film thickness measuring method using X-ray diffraction according to an embodiment of the invention described in claim 1.
【図２】同膜厚測定方法におけるＸ線の入射角度と回折
Ｘ線の強度の対応を示す関係図である。FIG. 2 is a relationship diagram showing a correspondence between an X-ray incident angle and a diffracted X-ray intensity in the same film thickness measuring method.
【図３】Ｘ線回折による測定結果と走査型電子顕微鏡に
よる測定結果との対応関係を示す説明図である。FIG. 3 is an explanatory diagram showing a correspondence relationship between a measurement result by X-ray diffraction and a measurement result by a scanning electron microscope.
【図４】請求項２記載の発明の実施例に係わるＸ線回折
を利用した膜厚測定方法の原理説明図である。FIG. 4 is a principle explanatory diagram of a film thickness measuring method using X-ray diffraction according to an embodiment of the invention described in claim 2;
【図５】同膜厚測定方法におけるＸ線の入射角度と回折
Ｘ線の強度の対応を示す関係図である。FIG. 5 is a relationship diagram showing a correspondence between an X-ray incident angle and a diffracted X-ray intensity in the same film thickness measuring method.
２ 基板 ３ 皮膜 ５ Ｘ線強度検出器 ６ 回折Ｘ線 Ｗ 立上り点 Ｙ 変位点 2 substrate 3 film 5 X-ray intensity detector 6 diffracted X-ray W rising point Y displacement point
Claims (2)
るに際し、 皮膜上に照射されたＸ線が回折して生じた回折Ｘ線の強
度を測定するＸ線強度検出器を、基板からの回折Ｘ線の
みを検出する位置に固定し、 照射されるＸ線の入射角度を０度から変化させて、Ｘ線
強度検出器により、Ｘ線の入射角度に対応する基板から
の回折Ｘ線の強度を測定し、 Ｘ線の入射角度に対応する基板からの回折Ｘ線の強度の
関係図を作り、測定された回折Ｘ線の強度の零値から増
加傾向に変化する立上り点を生じさせるＸ線の入射角度
の値を入射深さに換算して皮膜の膜厚を求めることを特
徴とするＸ線回折を利用した膜厚測定方法。1. An X-ray intensity detector for measuring the intensity of diffracted X-rays generated by diffracting X-rays radiated on the film when measuring the film thickness of the film formed on the substrate. The X-ray intensity detector is used to change the incident angle of the irradiated X-rays from 0 degree, and the diffraction X-rays from the substrate corresponding to the X-ray incident angle are fixed. The intensity of the X-ray is measured, and a relational diagram of the intensity of the diffracted X-ray from the substrate corresponding to the incident angle of the X-ray is created, and a rising point where the measured intensity of the diffracted X-ray changes from zero value to an increasing tendency is generated. A film thickness measuring method using X-ray diffraction, wherein the film thickness of the film is obtained by converting the value of the incident angle of X-rays to the incident depth.
るに際し、 皮膜上に照射されたＸ線が回折して生じた回折Ｘ線の強
度を測定するＸ線強度検出器を、皮膜からの回折Ｘ線の
みを検出する位置に固定し、 照射されるＸ線の入射角度を０度から変化させて、Ｘ線
強度検出器により、Ｘ線の入射角度に対応する皮膜から
の回折Ｘ線の強度を測定し、 Ｘ線の入射角度に対応する皮膜からの回折Ｘ線の強度の
関係図を作り、測定された回折Ｘ線の強度の増加傾向か
ら減少傾向に変化する変位点を生じさせるＸ線の入射角
度の値を入射深さに換算して皮膜の膜厚を求めることを
特徴とするＸ線回折を利用した膜厚測定方法。2. An X-ray intensity detector for measuring the intensity of diffracted X-rays generated by diffracting X-rays irradiated on the film when measuring the film thickness of the film formed on the substrate. The X-ray intensity detector is used to fix the X-ray diffracted X-ray from the film, and the incident X-ray angle is changed from 0 degrees. The intensity of the X-ray is measured, and the relationship diagram of the intensity of the diffracted X-ray from the film corresponding to the incident angle of the X-ray is created, and the displacement point that changes from the increasing tendency of the measured diffracted X-ray intensity to the decreasing tendency is generated. A film thickness measuring method using X-ray diffraction, wherein the film thickness of the film is obtained by converting the value of the incident angle of X-rays to the incident depth.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7163325A JP3000892B2 (en) | 1995-06-29 | 1995-06-29 | Film thickness measurement method using X-ray diffraction |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7163325A JP3000892B2 (en) | 1995-06-29 | 1995-06-29 | Film thickness measurement method using X-ray diffraction |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0914946A true JPH0914946A (en) | 1997-01-17 |
| JP3000892B2 JP3000892B2 (en) | 2000-01-17 |
Family
ID=15771709
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7163325A Expired - Lifetime JP3000892B2 (en) | 1995-06-29 | 1995-06-29 | Film thickness measurement method using X-ray diffraction |
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| Country | Link |
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| JP (1) | JP3000892B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6226348B1 (en) | 1998-12-15 | 2001-05-01 | Philips Electronics North America Corporation | X-ray diffractometer method for determining thickness of multiple non-metallic crystalline layers and fourier transform method |
| JP2013205037A (en) * | 2012-03-27 | 2013-10-07 | Sumitomo Metal Mining Co Ltd | Film thickness measuring method |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108709516B (en) * | 2018-05-11 | 2020-05-26 | 首钢集团有限公司 | Method for measuring thickness of iron scale on steel surface |
-
1995
- 1995-06-29 JP JP7163325A patent/JP3000892B2/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6226348B1 (en) | 1998-12-15 | 2001-05-01 | Philips Electronics North America Corporation | X-ray diffractometer method for determining thickness of multiple non-metallic crystalline layers and fourier transform method |
| JP2013205037A (en) * | 2012-03-27 | 2013-10-07 | Sumitomo Metal Mining Co Ltd | Film thickness measuring method |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3000892B2 (en) | 2000-01-17 |
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