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JP4514785B2 - Total reflection X-ray fluorescence analyzer - Google Patents

Total reflection X-ray fluorescence analyzer Download PDF

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JP4514785B2
JP4514785B2 JP2007308387A JP2007308387A JP4514785B2 JP 4514785 B2 JP4514785 B2 JP 4514785B2 JP 2007308387 A JP2007308387 A JP 2007308387A JP 2007308387 A JP2007308387 A JP 2007308387A JP 4514785 B2 JP4514785 B2 JP 4514785B2
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JP2009133658A (en
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康裕 清水
浩 河野
昭弘 池下
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Rigaku Corp
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Description

本発明は、円板状の試料における縁近傍の周辺部を測定する全反射蛍光X線分析装置に関する。   The present invention relates to a total reflection X-ray fluorescence analyzer that measures a peripheral portion in the vicinity of an edge of a disk-shaped sample.

全反射蛍光X線分析装置は半導体製造プロセスの品質管理分析において、ウェーハ、ガラス基板などの分析に用いられている。ウェーハの縁近傍の周辺部は半導体製造プロセスにおいて汚染し易いために、チップの製造には使用されていなかったが、ウェーハが大径化する一方で、超小型のマイクロチップが製造されており、ウェーハの縁近傍の周辺部が利用できれば、その領域だけで数千個のマイクロチップを製造することができる。そのため、ウェーハの縁近傍の周辺部をできるだけ有効に利用するために、ウェーハの縁の数ミリ手前までの領域を測定してウェーハの縁近傍の周辺部の汚染を調べることができる全反射蛍光X線分析装置がある(参照、特許文献1)。   The total reflection X-ray fluorescence analyzer is used for analyzing wafers, glass substrates and the like in quality control analysis of semiconductor manufacturing processes. Since the peripheral part near the edge of the wafer is easily contaminated in the semiconductor manufacturing process, it was not used for manufacturing the chip, but the wafer was enlarged in diameter, while an ultra-small microchip was manufactured. If the peripheral portion in the vicinity of the edge of the wafer is available, thousands of microchips can be manufactured only in that region. Therefore, in order to use the peripheral part near the edge of the wafer as effectively as possible, the total reflection fluorescent X that can measure the area up to several millimeters before the edge of the wafer and check the contamination near the edge of the wafer. There is a line analyzer (see Patent Document 1).

また、ウェーハの大径化にともなってウェーハを水平にして台に載置した場合、台からはみ出す縁近傍の周辺部はわずかに下方にたれ下がるようにたわむ、そのため、ウェーハの表面への1次X線の入射角度をウェーハの測定位置によって補正する全反射蛍光X線分析装置がある(参照、特許文献2)。この装置では、補正にあたり、各測定位置での蛍光X線の測定強度を用いており(中心強度補正と呼ばれる)、測定位置がウェーハの縁近傍の周辺部にあるときは、縁近傍の周辺部での測定強度が必要となる。
特開2002−5858号公報 特開2006−214868号公報
Also, when the wafer is placed on a table with the wafer diameter increasing, the peripheral part near the edge protruding from the table is bent slightly downward, so that the primary to the surface of the wafer There is a total reflection fluorescent X-ray analyzer that corrects the incident angle of X-rays according to the measurement position of the wafer (see Patent Document 2). In this apparatus, the measurement intensity of fluorescent X-rays at each measurement position is used for correction (referred to as center intensity correction), and when the measurement position is in the vicinity near the edge of the wafer, the periphery near the edge Measurement strength at is required.
Japanese Patent Laid-Open No. 2002-5858 JP 2006-214868 A

しかし、これらの従来の技術では、ウェーハなどの円板状の試料の縁近傍の周辺部における任意の測定部位について正確な分析ができない。ステージで試料の縁を検出器の視野内に移動させると、図4Bに示すように、検出器の視野Fの一部分しか試料Sが占めず、斜線で示された測定部位52からの蛍光X線しか測定することができず、図4Aに示すような検出器の全視野Fを占める測定部位についての測定強度と整合しなくなるからである。   However, these conventional techniques cannot accurately analyze an arbitrary measurement site in the vicinity of the edge of a disk-shaped sample such as a wafer. When the edge of the sample is moved into the field of view of the detector on the stage, as shown in FIG. 4B, the sample S occupies only a part of the field of view F of the detector. This is because it can only be measured and does not match the measurement intensity for the measurement site occupying the entire field of view F of the detector as shown in FIG. 4A.

本発明は前記従来の問題に鑑みてなされたもので、ウェーハなどの円板状の試料の縁近傍の周辺部における任意の測定部位について正確な分析ができる全反射蛍光X線分析装置を提供することを目的とする。   The present invention has been made in view of the above-described conventional problems, and provides a total reflection X-ray fluorescence analyzer capable of performing an accurate analysis on an arbitrary measurement site in the peripheral portion near the edge of a disk-shaped sample such as a wafer. For the purpose.

前記目的を達成するために、本発明の全反射蛍光X線分析装置は、円板状の試料の表面に微小な入射角度で1次X線を入射させ、発生する蛍光X線の強度を検出器で測定する全反射蛍光X線分析装置であって、前記検出器に対する試料の初期位置を検知する初期位置検知手段と、前記初期位置から試料を移動させることにより、試料の表面における任意の測定部位を前記検出器の視野内に移動させるステージと、前記初期位置検知手段で検知した初期位置ならびに前記ステージによる移動の方向および量に基づいて、前記検出器に対する試料の移動後の位置を算出し、その算出した検出器に対する試料の移動後の位置、試料の所定寸法形状および試料表面の高さにおける前記検出器の視野の所定寸法形状に基づいて、前記検出器の視野内における試料表面の面積である前記測定部位の面積を算出し、その算出した測定部位の面積および前記検出器で測定した測定強度に基づいて、単位面積あたりの測定強度を算出する算出手段とを備えている。 In order to achieve the above object, the total reflection X-ray fluorescence analyzer of the present invention detects the intensity of generated X-rays by making primary X-rays incident on the surface of a disk-shaped sample at a minute incident angle. A total reflection X-ray fluorescence analyzer for measuring with a measuring instrument, wherein an initial position detecting means for detecting an initial position of the sample with respect to the detector, and an arbitrary measurement on the surface of the sample by moving the sample from the initial position Based on the stage for moving the part within the visual field of the detector, the initial position detected by the initial position detecting means, and the direction and amount of movement by the stage , the position after movement of the sample with respect to the detector is calculated. , the position after the movement of the sample to the calculated detector, based on a predetermined size and shape of the field of view of the detector in height of a predetermined geometry and the sample surface of the sample, you within the field of view of the detector Calculating the area of the measurement site is the area of that surface of the sample, and a calculation means based on the measurement strength measured by the area and the detector of the measurement site was the calculated, to calculate the measured intensity per unit area ing.

本発明の全反射蛍光X線分析装置によれば、検出器の視野内における測定部位の面積を算出し、その算出した測定部位の面積および検出器で測定した測定強度に基づいて、単位面積あたりの測定強度を算出するので、ウェーハなどの円板状の試料の縁近傍の周辺部における任意の測定部位について正確な分析ができる。   According to the total reflection X-ray fluorescence spectrometer of the present invention, the area of the measurement site in the field of view of the detector is calculated, and based on the calculated area of the measurement site and the measured intensity measured by the detector, per unit area Therefore, it is possible to accurately analyze an arbitrary measurement site in the vicinity of the edge of a disk-shaped sample such as a wafer.

本発明の全反射蛍光X線分析装置においては、前記ステージが、試料の傾きを変化させることにより前記入射角度を変化させる入射角度調整手段を有し、試料表面から均一に発生する基準X線について、試料の表面における基準となる基準部位での測定強度に任意の測定部位での測定強度が合致するように、前記入射角度調整手段に前記任意の測定部位での入射角度を変化させる制御手段を備え、その制御手段が、前記合致させる両測定強度として、前記算出手段が算出した単位面積あたりの測定強度を用いることが好ましい。   In the total reflection X-ray fluorescence analyzer of the present invention, the stage has an incident angle adjusting means for changing the incident angle by changing the inclination of the sample, and the reference X-rays generated uniformly from the sample surface The control means for changing the incident angle at the arbitrary measurement site in the incident angle adjusting unit so that the measurement intensity at the arbitrary measurement site matches the measurement intensity at the reference site serving as a reference on the surface of the sample. Preferably, the control means uses the measured intensity per unit area calculated by the calculating means as the two measured intensities to be matched.

この好ましい構成によれば、試料の縁近傍の周辺部における任意の測定部位について、正確な測定強度を得て、1次X線の入射角度を適切に補正できる。   According to this preferable configuration, an accurate measurement intensity can be obtained for an arbitrary measurement site in the peripheral portion near the edge of the sample, and the incident angle of the primary X-ray can be appropriately corrected.

以下、本発明の実施形態である全反射蛍光X線分析装置について説明する。図1に示すように、この全反射蛍光X線分析装置1は、シリコンウェーハなどの円板状の試料の表面Saに、X線管11からのX線12を分光素子13で単色化して1次X線14として微小な入射角度θ、例えば0.05°で照射するX線源6と、載置された試料Sを回転、移動させるXYθステージ22および試料Sの傾きを調整するスイベルステージ23を備えるステージ21と、試料Sから発生する蛍光X線15の強度を測定するSSDなどの検出器16と、検出器16に対する試料Sの初期位置を検知する初期位置検知手段20を構成するビームセンサ24と、初期位置検知手段20で検知した初期位置ならびにステージ21による移動の方向および量に基づいて、検出器16の視野内における測定部位の面積を算出し、その算出した測定部位の面積および検出器16で測定した測定強度に基づいて、単位面積あたりの測定強度を算出する算出手段31を有し、入射角度調整手段であるスイベルステージ23を制御する制御手段30とを備える。   Hereinafter, a total reflection X-ray fluorescence analyzer which is an embodiment of the present invention will be described. As shown in FIG. 1, the total reflection X-ray fluorescence spectrometer 1 uses a spectroscopic element 13 to monochromatize X-rays 12 from an X-ray tube 11 on a surface Sa of a disk-like sample such as a silicon wafer. The X-ray source 6 that irradiates the next X-ray 14 at a minute incident angle θ, for example, 0.05 °, the XYθ stage 22 that rotates and moves the placed sample S, and the swivel stage 23 that adjusts the inclination of the sample S. , A detector 16 such as an SSD for measuring the intensity of the fluorescent X-ray 15 generated from the sample S, and a beam sensor constituting an initial position detecting means 20 for detecting the initial position of the sample S relative to the detector 16. 24, based on the initial position detected by the initial position detecting means 20 and the direction and amount of movement by the stage 21, the area of the measurement site in the field of view of the detector 16 is calculated and calculated. Based on the area of the fixed part and the measured intensity measured by the detector 16, the calculating means 31 for calculating the measured intensity per unit area and the control means 30 for controlling the swivel stage 23 as the incident angle adjusting means are provided. Prepare.

図2に示すように、ビームセンサ24は、帯状のラインビームLを照射する照射部24aと、照射部24aに対向する位置に配置されてラインビームLを線状に受光する受光部24bとで構成され、試料Sの縁近傍の周辺部がラインビームLの一部を遮光するような位置に配置されている。図示したビームセンサ24は照射部24aと受光部24bとが一体として示されているが、別体であってもよい。ステージ21は、既に知られた位置決め装置(参照、特開平8−161049号公報)を用いており、XYθステージ22は試料Sを載置する試料台22aと試料台22aを駆動する駆動部22bで構成されている。   As shown in FIG. 2, the beam sensor 24 includes an irradiation unit 24a that irradiates a band-shaped line beam L, and a light receiving unit 24b that is arranged at a position facing the irradiation unit 24a and receives the line beam L in a linear shape. The peripheral portion in the vicinity of the edge of the sample S is arranged at a position where a part of the line beam L is shielded. In the illustrated beam sensor 24, the irradiating unit 24a and the light receiving unit 24b are shown as one body, but may be separate. The stage 21 uses a known positioning device (refer to Japanese Patent Laid-Open No. 8-161049), and the XYθ stage 22 includes a sample stage 22a on which the sample S is placed and a drive unit 22b that drives the sample stage 22a. It is configured.

図3に示すように、検出器16の視野Fは試料の表面Saの高さにおいて円形で所定の視野面積を有し、ステージ21の初期状態において、検出器16の視野Fの中心25と試料台22aの中心とは合致している。試料台22aは検出器16の視野Fの中心25を原点(0、0)として空間に固定されたXY座標において、試料Sの方位を変化させずにXY方向に移動でき、自身の中心(回転軸)まわりにφ方向に回転できる。試料Sは、初期状態の試料台22aの中心に試料Sの中心51が合致するように、かつ、初期状態の試料台22aの所定方向、例えばY方向に試料SのノッチN方向(試料Sの中心51からノッチNへの方向)が合致するように、ロボットハンド(図示なし)により試料台22aに載置される。しかし、通常、これらは完全には合致せず、わずかながらずれる。このようにずれて載置される試料Sについて、検出器16に対する初期位置が、ビームセンサ24を用いて以下のように検知される。   As shown in FIG. 3, the field of view F of the detector 16 is circular at the height of the surface Sa of the sample and has a predetermined field of view. In the initial state of the stage 21, the center 25 of the field of view F of the detector 16 and the sample It coincides with the center of the table 22a. The sample stage 22a can move in the XY directions without changing the orientation of the sample S in the XY coordinates fixed in the space with the center 25 of the field of view F of the detector 16 as the origin (0, 0), and the center (rotation) of itself. (Axis) can be rotated in the φ direction. The sample S is arranged so that the center 51 of the sample S coincides with the center of the sample stage 22a in the initial state, and in a predetermined direction of the sample stage 22a in the initial state, for example, the notch N direction of the sample S (the direction of the sample S). The sample is placed on the sample stage 22a by a robot hand (not shown) so that the direction from the center 51 to the notch N matches. However, they usually do not match perfectly and are slightly off. The initial position with respect to the detector 16 is detected using the beam sensor 24 for the sample S placed in such a manner as follows.

制御手段30によりステージ21を制御して、試料Sを載置した試料台22aを360度回転させると、回転角に応じて、つまり試料台22aの中心と試料Sの中心51とのずれおよびノッチNの切欠きに応じて、ビームセンサ24の受光量(Lb(図2)の長さ)が変化する。試料Sの寸法形状は既知であるので、この回転角に応じた受光量変化から、初期状態の試料台22aの中心つまり検出器16の視野の中心25に対する試料Sの中心51およびノッチNの位置が、制御手段30により求められる。これが、検出器16に対する試料Sの初期位置であり、ビームセンサ24、ステージ21および制御手段30が初期位置検知手段20を構成する。   When the stage 21 is controlled by the control means 30 and the sample stage 22a on which the sample S is placed is rotated 360 degrees, according to the rotation angle, that is, the deviation between the center of the sample stage 22a and the center 51 of the sample S and the notch The amount of light received by the beam sensor 24 (the length of Lb (FIG. 2)) changes according to the notch of N. Since the dimensional shape of the sample S is known, the position of the center 51 of the sample S and the position of the notch N with respect to the center of the sample stage 22a in the initial state, that is, the center 25 of the visual field of the detector 16 from the change in the amount of received light according to the rotation angle. Is obtained by the control means 30. This is the initial position of the sample S with respect to the detector 16, and the beam sensor 24, the stage 21 and the control means 30 constitute the initial position detection means 20.

ステージ21は、制御手段30から指令を受け、載置した試料Sを初期位置から試料Sの方位を変化させずにXY方向に移動させることにより、試料Sの表面における任意の測定部位を検出器16の視野F内に移動させる。制御手段30が有する算出手段31は、前記初期位置検知手段20で検知した試料Sの初期位置ならびに前記ステージ21による試料Sの移動の方向および量に基づいて、検出器16に対する試料Sの移動後の位置を算出する。そして、その算出した検出器16に対する試料Sの移動後の位置、前記試料Sの所定寸法形状および前記試料表面の高さにおける検出器16の視野Fの所定寸法形状に基づいて、検出器16の視野F内における試料表面の面積つまり測定部位の面積を算出する。測定部位が例えば試料Sの中心部で検出器16の視野Fのすべてを占める場合には、視野面積と測定部位の面積は等しいが、測定部位が試料Sの縁近傍の周辺部で検出器16の視野Fの一部しか占めない場合には、視野面積よりも測定部位の面積は小さい。算出手段31は、さらに、算出した測定部位の面積および検出器16で測定した測定強度に基づいて、単位面積あたりの測定強度を算出する。ここで、単位面積は、視野面積でもよいし、視野面積とは無関係の値、例えば1cmでもよい。 The stage 21 receives a command from the control means 30, and moves the placed sample S from the initial position in the XY direction without changing the orientation of the sample S, thereby detecting an arbitrary measurement site on the surface of the sample S. Move into 16 fields of view F. The calculation means 31 included in the control means 30 is based on the initial position of the sample S detected by the initial position detection means 20 and the direction and amount of movement of the sample S by the stage 21 after the movement of the sample S relative to the detector 16. The position of is calculated. Based on the calculated position of the sample S relative to the detector 16, the predetermined dimension shape of the sample S, and the predetermined dimension shape of the field of view F of the detector 16 at the height of the sample surface, The area of the sample surface in the field of view F, that is, the area of the measurement site is calculated. For example, when the measurement site occupies the entire field of view F of the detector 16 at the center of the sample S, the area of the field of view is equal to the area of the measurement site, but the measurement site is the peripheral portion near the edge of the sample S. In the case where only a part of the visual field F is occupied, the area of the measurement site is smaller than the visual field area. The calculation means 31 further calculates a measurement intensity per unit area based on the calculated area of the measurement site and the measurement intensity measured by the detector 16. Here, the unit area may be a visual field area or a value irrelevant to the visual field area, for example, 1 cm 2 .

また、ステージ21は、入射角度調整手段としてスイベルステージ23を有し、試料の傾きを変化させることにより前記入射角度θを変化させる。そして、制御手段30は、前述の中心強度補正を行うべく、試料表面から均一に発生する基準X線について、試料の表面における基準となる基準部位での測定強度に任意の測定部位での測定強度が合致するように、入射角度調整手段に前記任意の測定部位での入射角度を変化させる。ここで、制御手段30は、前記合致させる両測定強度として、前記算出手段31が算出した単位面積あたりの基準X線の測定強度を用いる。   The stage 21 has a swivel stage 23 as incident angle adjusting means, and changes the incident angle θ by changing the tilt of the sample. Then, the control means 30 performs the measurement intensity at any measurement site in addition to the measurement intensity at the reference site serving as the reference on the surface of the sample for the reference X-rays generated uniformly from the sample surface in order to perform the above-described center intensity correction. So that the incident angle adjustment means changes the incident angle at the arbitrary measurement site. Here, the control means 30 uses the measurement intensity of the reference X-ray per unit area calculated by the calculation means 31 as the two measurement intensities to be matched.

本実施形態の全反射蛍光X線分析装置1の動作について説明する。まず、1次X線の入射角度の補正について説明する。試料Sを試料台22aに載置すると、前記したように、試料Sの初期位置が前記初期位置検知手段20により求められる。すなわち、図3に示すように、例えば、検出器16の視野Fの中心25をXY座標の原点(0、0)とすると、試料Sの初期位置である試料Sの中心51の座標(x、y)が求められる。この視野Fの中心25を中心とする部位、すなわち初期位置の試料台22aの中心を中心とする試料部位を、試料の表面Saから均一に発生する基準X線5について試料の表面Saにおける基準となる基準部位50とし、この基準部位50に1次X線14の入射角度θが適切になるようにスイベルステージ23によりステージ角度を調整して、試料の表面Saから均一に発生する基準X線5である、例えばSi−Kα線の基準強度Iを測定する。この場合、基準部位50は試料Sの中心51の近傍部位であるので、その測定面積は検出器16の視野Fの面積Mと同じである。この視野面積Mを単位面積とする。ステージ角度の調整は、前記した特開平8−161049号公報によって既に知られている方法によって調整される。 The operation of the total reflection X-ray fluorescence spectrometer 1 of this embodiment will be described. First, correction of the incident angle of the primary X-ray will be described. When the sample S is placed on the sample table 22a, the initial position of the sample S is obtained by the initial position detecting means 20 as described above. That is, as shown in FIG. 3, for example, if the center 25 of the field of view F of the detector 16 is the origin (0, 0) of the XY coordinates, the coordinates (x 0) of the center 51 of the sample S, which is the initial position of the sample S. , Y 0 ). A portion centered on the center 25 of the field of view F, that is, a sample portion centered on the center of the sample stage 22a at the initial position, is a reference on the surface Sa of the sample with respect to the reference X-ray 5 generated uniformly from the surface Sa of the sample. The reference X-ray 5 is uniformly generated from the surface Sa of the sample by adjusting the stage angle by the swivel stage 23 so that the incident angle θ of the primary X-ray 14 is appropriate to the reference site 50. For example, the reference intensity I 0 of the Si-Kα line is measured. In this case, since the reference part 50 is a part near the center 51 of the sample S, the measurement area is the same as the area M 0 of the field of view F of the detector 16. This visual field area M0 is defined as a unit area. The stage angle is adjusted by a method already known from Japanese Patent Laid-Open No. 8-161049.

次に、図4Aに示すように制御手段30からの指令によりステージ21の駆動部23が、試料Sの方位を変化させずに試料台22上の試料SをX方向にx、Y方向にyの距離を移動させて、例えば試料Sの中心近傍部位である所望の測定部位53を検出器16の視野Fに配置する。このとき、移動後の試料Sの中心51はXY座標(x+x、y+y)の位置になる。算出手段31により、この試料Sの中心51の座標(x+x、y+y)、試料の寸法形状、例えばシリコンウェーハの半径および検出器の視野寸法形状、例えば円形視野Fの半径に基づいて試料Sの中心近傍部位である測定部位53の測定面積が算出される。この場合、測定部位53は試料Sの中心近傍であるので、その測定面積は検出器16の視野Fの面積Mと同じである。 Next, the drive unit 23 of the stage 21 by a command from the control means 30 as shown in FIG. 4A, the sample S on the sample stage 22 without changing the orientation of the sample S x 1, Y-direction in the X-direction By moving the distance y 1 , for example, a desired measurement site 53 that is a site near the center of the sample S is arranged in the field of view F of the detector 16. At this time, the center 51 of the sample S after the movement is in the position of the XY coordinates (x 0 + x 1 , y 0 + y 1 ). By the calculation means 31, the coordinates (x 0 + x 1 , y 0 + y 1 ) of the center 51 of the sample S, the sample size and shape, for example, the radius of the silicon wafer and the field size of the detector, for example, the radius of the circular field F are obtained. Based on this, the measurement area of the measurement site 53 that is a site near the center of the sample S is calculated. In this case, since the measurement site 53 is near the center of the sample S, the measurement area is the same as the area M 0 of the field of view F of the detector 16.

試料Sの中心近傍部位である測定部位53に1次X線14を照射して、Si−Kα線の測定強度Iを測定しながらスイベルステージ23に入射角度θを変化させて、測定部位53での単位面積MあたりのSi−Kα線の測定強度Iを、基準部位50で得られた単位面積MあたりのSi−Kα線の測定強度Iに合致させ、そのときのステージ角度θを制御手段30に記憶する。 The measurement site 53, which is near the center of the sample S, is irradiated with the primary X-ray 14, and the incident angle θ is changed to the swivel stage 23 while measuring the measurement intensity I 1 of the Si-Kα ray. units measured intensity I 1 of the area M Si-K [alpha line per 0, is matched to the measured intensity I 0 of the Si-K [alpha line per unit area M 0 obtained in the reference part 50, a stage angle at that time with θ 1 is stored in the control means 30.

次に、図4Bに示すように制御手段30からの指令によりステージ21が、試料Sの初期位置から試料Sの方位を変化させずにX方向にx、Y方向にyの距離を移動させて、試料Sの縁近傍の周辺部である所望の測定部位52を検出器16の視野Fに配置する。このとき、検出器の視野Fの一部分しか試料Sが占めず検出器16の視野面積Mより小さいが、算出手段31により試料Sの中心51の座標(x+x、y+y)を用いて前記と同様にして、斜線で示された測定部位52の測定面積Mが算出される。この測定部位52に1次X線14を照射して、Si−Kα線の測定強度Iを測定しながらスイベルステージ23に入射角度θを変化させて、測定部位52での単位面積MあたりのSi−Kα線の測定強度I×(M/M)を、基準部位50で得られた単位面積MあたりのSi−Kα線の測定強度Iに合致させ、そのときのステージ角度θを制御手段30に記憶する。 Next, as shown in FIG. 4B, the stage 21 moves a distance of x 2 in the X direction and y 2 in the Y direction without changing the orientation of the sample S from the initial position of the sample S by a command from the control means 30. Then, a desired measurement site 52 that is a peripheral portion in the vicinity of the edge of the sample S is arranged in the visual field F of the detector 16. At this time, the sample S occupies only a part of the field of view F of the detector and is smaller than the field of view M 0 of the detector 16, but the coordinates (x 0 + x 2 , y 0 + y 2 ) of the center 51 of the sample S are calculated by the calculation means 31. in the same manner as above using a measuring area M 1 of the measurement site 52 shown by oblique lines are calculated. This was irradiated to the measuring site 52 primary X-ray 14, by changing the incident angle θ to the swivel stage 23 while measuring the measured intensity I 2 of the Si-K [alpha line, per unit area M 0 at the measurement site 52 The measured intensity I 2 × (M 0 / M 1 ) of the Si-Kα line is matched with the measured intensity I 0 of the Si-Kα line per unit area M 0 obtained in the reference region 50, and the stage at that time storing an angle theta 2 to the control unit 30.

本実施形態の全反射蛍光X線分析装置1によれば、検出器の視野Fの一部分しか試料Sが占めないような縁近傍の周辺部における測定部位52について、正確な単位面積Mあたりの基準X線5の測定強度I×(M/M)を得ることによって、1次X線の入射角度θを適切に補正することができる。 According to the total reflection X-ray fluorescence analysis apparatus 1 of the present embodiment, the measurement site 52 in the peripheral portion in the vicinity of the edge where only a part of the field of view F of the detector occupies the accurate unit area M 0 . By obtaining the measured intensity I 2 × (M 0 / M 1 ) of the reference X-ray 5, the incident angle θ of the primary X-ray can be appropriately corrected.

次に、円板状の試料Sの分析対象元素を測定する場合について説明する。前記と同様にして、ステージ21で試料Sを移動させて所望の測定部位を検出器16の視野F内に配置する。検出器16の視野Fのすべてを占める測定部位53の場合には、算出手段31により算出される測定面積は検出器16の視野Fの面積Mと同じ面積となる。次に、この測定部位53に1次X線14を照射して、ステージ角度を記憶したステージ角度θに設定して試料Sから発生する蛍光X線15の強度を測定する。測定部位53が検出器16の視野Fのすべてを占めているので、算出手段31により算出される測定面積は検出器16の視野Fの面積Mと同じ面積となり、試料Sより発生する分析対象元素の蛍光X線15の単位面積Mあたりの強度Kを検出器16により測定し、その測定強度Kを用いて定量分析値を求める。 Next, a case where the analysis target element of the disk-shaped sample S is measured will be described. In the same manner as described above, the sample S is moved on the stage 21 to place a desired measurement site in the field of view F of the detector 16. In the case of the measurement site 53 occupying the entire field of view F of the detector 16, the measurement area calculated by the calculation means 31 is the same as the area M 0 of the field of view F of the detector 16. Next, the measurement site 53 is irradiated with the primary X-ray 14, the stage angle is set to the stored stage angle θ 1, and the intensity of the fluorescent X-ray 15 generated from the sample S is measured. Since the measurement site 53 occupies the entire visual field F of the detector 16, the measurement area calculated by the calculation means 31 is the same as the area M 0 of the visual field F of the detector 16, and the analysis target generated from the sample S the intensity K 0 per unit area M 0 of the fluorescent X-ray 15 of the element is measured by the detector 16, obtains a quantitative analysis using the measured intensities K 0.

検出器16の視野Fの一部しか占めない測定部位52の場合には、算出手段31により算出される測定面積は前記Mとなる。次に、検出器16の視野Fの一部しか占めない測定部位52に1次X線を照射して、ステージ角度を記憶したステージ角度θに設定して試料Sから発生する分析対象元素の蛍光X線15の強度Kを測定し、算出手段31で単位面積Mあたりの蛍光X線15の測定強度K×(M/M)を算出する。この単位面積Mあたりの蛍光X線15の測定強度K×(M/M)を用いて定量分析値を求める。 In the case of the detector 16 measuring sites 52 occupies only part of the field of view F of the measurement area is calculated by the calculating means 31 becomes the M 1. Next, the measurement site 52 that occupies only a part of the visual field F of the detector 16 is irradiated with primary X-rays, and the stage angle is set to the stored stage angle θ 2 , and the analysis target element generated from the sample S is detected. The intensity K 1 of the fluorescent X-ray 15 is measured, and the calculation means 31 calculates the measured intensity K 1 × (M 0 / M 1 ) of the fluorescent X-ray 15 per unit area M 0 . A quantitative analysis value is obtained using the measured intensity K 1 × (M 0 / M 1 ) of the fluorescent X-ray 15 per unit area M 0 .

本実施形態の全反射蛍光X線分析装置1によれば、検出器16の視野F内における測定部位52、53の面積を算出し、その算出した測定部位52、53の面積および検出器16で測定した蛍光X線15の測定強度に基づいて、単位面積Mあたりの蛍光X線15の測定強度を算出するので、シリコンウェーハなどの円板状の試料Sの縁近傍の周辺部における検出器16の視野Fの一部しか占めない任意の測定部位についても正確な分析ができる。円板状の試料Sで汚染が発生しやすい縁近傍の周辺部、例えば円板状の試料Sの縁に沿った数ミリの領域をも測定して、汚染部位の特定をすることができる。 According to the total reflection X-ray fluorescence spectrometer 1 of the present embodiment, the areas of the measurement parts 52 and 53 in the visual field F of the detector 16 are calculated, and the calculated areas of the measurement parts 52 and 53 and the detector 16 are calculated. Since the measured intensity of the fluorescent X-ray 15 per unit area M 0 is calculated based on the measured intensity of the fluorescent X-ray 15, the detector in the vicinity of the edge of the disk-shaped sample S such as a silicon wafer is detected. Accurate analysis can be performed for any measurement site that occupies only a part of the 16 fields of view F. The peripheral part near the edge where the disk-shaped sample S is likely to be contaminated, for example, an area of several millimeters along the edge of the disk-shaped sample S can be measured to identify the contaminated part.

本実施形態では、基準X線5であるSi−Kα線の強度を、基準部位50である初期位置の試料台22aの中心を中心とする試料部位で1次X線14の入射角度θ(図1)が適切になるようにステージ角度を調整して基準強度Iを測定しているが、基準部位は円板状の試料Sのたわみが生じない試料の表面Saの他の位置であってもよい。基準X線5として試料Sであるシリコンウェーハから発生するSi−Kα線を用いたが、試料Sに均一に分布する主成分元素に限らず、試料Sに形成された膜に均一に分布する元素からの蛍光X線を用いてもよい。 In the present embodiment, the intensity of the Si-Kα ray that is the reference X-ray 5 is set to the incident angle θ of the primary X-ray 14 at the sample site centered on the center of the sample stage 22a at the initial position that is the reference site 50 (see FIG. The reference angle I 0 is measured by adjusting the stage angle so that 1) is appropriate, but the reference portion is another position of the surface Sa of the sample where the deflection of the disk-shaped sample S does not occur. Also good. Although the Si-Kα ray generated from the silicon wafer that is the sample S is used as the reference X-ray 5, the element is not limited to the main component that is uniformly distributed in the sample S, but is also uniformly distributed in the film formed in the sample S X-ray fluorescence may be used.

なお、1次X線の入射角度の補正については、以下のように、測定部位の面積を単位面積とすることもできる。視野面積Mを単位面積とした場合と同様にして、基準部位50のSi−Kα線の基準強度Iを測定する。基準部位50の面積は視野面積Mと同じである。 In addition, about correction | amendment of the incident angle of a primary X-ray, the area of a measurement site | part can also be made into a unit area as follows. The reference intensity I 0 of the Si—Kα line of the reference region 50 is measured in the same manner as when the visual field area M 0 is the unit area. Area of the reference site 50 is the same as the field area M 0.

前記と同様にして、図4Aに示す測定部位53について、測定面積Mが算出される。測定部位53のSi−Kα線の測定強度Iを測定しながらスイベルステージ23に入射角度θを変化させて、測定部位53での単位面積MあたりのSi−Kα線の測定強度Iを、基準部位50で得られた単位面積MあたりのSi−Kα線の測定強度Iに合致させる。 In the same manner as described above, the measurement area M 0 is calculated for the measurement site 53 shown in FIG. 4A. While measuring the measurement intensity I 1 of the Si—Kα ray at the measurement site 53, the incident angle θ is changed to the swivel stage 23, and the measurement intensity I 1 of the Si—Kα ray per unit area M 0 at the measurement site 53 is obtained. The measured intensity I 0 of the Si-Kα ray per unit area M 0 obtained at the reference region 50 is matched.

前記と同様にして、図4Bに示す斜線で示された測定部位52の測定面積Mが算出される。算出手段31で基準部位50の単位面積MあたりのSi−Kα線の測定強度I×(M/M)を算出する。測定部位52のSi−Kα線の測定強度Iを測定しながらスイベルステージ23に入射角度θを変化させて、測定部位52での単位面積MあたりのSi−Kα線の測定強度Iを、算出した基準部位50の単位面積MあたりのSi−Kα線の強度I×(M/M)に合致させる。 In the same manner as above, the measurement area M 1 of the measurement site 52 shown by hatching shown in Figure 4B is calculated. The calculation means 31 calculates the measured intensity I 0 × (M 1 / M 0 ) of the Si-Kα line per unit area M 1 of the reference region 50. While measuring the measurement intensity I 2 of the Si—Kα ray at the measurement site 52, the incident angle θ is changed to the swivel stage 23, and the measurement intensity I 2 of the Si—Kα ray per unit area M 1 at the measurement site 52 is obtained. And the calculated intensity I 0 × (M 1 / M 0 ) of the Si-Kα line per unit area M 1 of the reference region 50.

本例によれば、検出器の視野Fの一部分しか試料Sが占めないような縁近傍の周辺部における測定部位52のSi−Kα線の測定強度Iを、算出した基準部位50の単位面積MあたりのSi−Kα線の強度I×(M/M)に合致させるので、1次X線の入射角度θを適切に補正することができる。 According to this example, the measured unit area of the reference portion 50 calculated from the measured intensity I 2 of the Si—Kα ray of the measurement portion 52 in the vicinity of the edge where the sample S occupies only a part of the field of view F of the detector is calculated. Since it matches the intensity I 0 × (M 1 / M 0 ) of the Si-Kα ray per M 1, the incident angle θ of the primary X-ray can be corrected appropriately.

本発明の実施形態である全反射蛍光X線分析装置の概略図である。1 is a schematic view of a total reflection X-ray fluorescence spectrometer that is an embodiment of the present invention. 同装置のビームセンサと試料台上の試料位置との関係を示した配置図である。It is the arrangement | positioning figure which showed the relationship between the beam sensor of the same apparatus, and the sample position on a sample stand. 同装置の試料の初期位置を示す図である。It is a figure which shows the initial position of the sample of the apparatus. 同装置の試料の中心近傍部位の測定面積を示す図である。It is a figure which shows the measurement area of the center vicinity site | part of the sample of the apparatus. 同装置の試料の縁近傍の周辺部の測定部位の測定面積を示す図である。It is a figure which shows the measurement area of the measurement site | part of the peripheral part of the edge vicinity of the sample of the apparatus.

符号の説明Explanation of symbols

1 全反射蛍光X線分析装置
5 基準X線(Si−Kα線)
14 1次X線
15 蛍光X線
16 検出器(SSD)
20 初期位置検知手段
21 ステージ
23 入射角度調整手段(スイベルステージ)
24 ビームセンサ
30 制御手段
31 算出手段
50 基準部位
S 試料
1 Total reflection X-ray fluorescence analyzer 5 Reference X-ray (Si-Kα ray)
14 Primary X-ray 15 Fluorescent X-ray 16 Detector (SSD)
20 Initial position detection means 21 Stage 23 Incident angle adjustment means (swivel stage)
24 Beam sensor 30 Control means 31 Calculation means 50 Reference part S Sample

Claims (2)

円板状の試料の表面に微小な入射角度で1次X線を入射させ、発生する蛍光X線の強度を検出器で測定する全反射蛍光X線分析装置であって、
前記検出器に対する試料の初期位置を検知する初期位置検知手段と、
前記初期位置から試料を移動させることにより、試料の表面における任意の測定部位を前記検出器の視野内に移動させるステージと、
前記初期位置検知手段で検知した初期位置ならびに前記ステージによる移動の方向および量に基づいて、前記検出器に対する試料の移動後の位置を算出し、その算出した検出器に対する試料の移動後の位置、試料の所定寸法形状および試料表面の高さにおける前記検出器の視野の所定寸法形状に基づいて、前記検出器の視野内における試料表面の面積である前記測定部位の面積を算出し、その算出した測定部位の面積および前記検出器で測定した測定強度に基づいて、単位面積あたりの測定強度を算出する算出手段とを備えた全反射蛍光X線分析装置。
A total reflection X-ray fluorescence analyzer that makes primary X-rays incident on a surface of a disk-shaped sample at a minute incident angle and measures the intensity of the generated fluorescent X-rays with a detector,
An initial position detecting means for detecting an initial position of the sample with respect to the detector;
A stage for moving any measurement site on the surface of the sample into the field of view of the detector by moving the sample from the initial position;
Based on the initial position detected by the initial position detector and the direction and amount of movement by the stage , the position after movement of the sample with respect to the detector is calculated, and the position after movement of the sample with respect to the calculated detector, Based on the predetermined size and shape of the sample and the predetermined size and shape of the field of view of the detector at the height of the sample surface, the area of the measurement site, which is the area of the sample surface within the field of view of the detector, was calculated and calculated A total reflection X-ray fluorescence spectrometer comprising: a calculation means for calculating a measurement intensity per unit area based on an area of a measurement site and a measurement intensity measured by the detector.
請求項1において、
前記ステージが、試料の傾きを変化させることにより前記入射角度を変化させる入射角度調整手段を有し、
試料表面から均一に発生する基準X線について、試料の表面における基準となる基準部位での測定強度に任意の測定部位での測定強度が合致するように、前記入射角度調整手段に前記任意の測定部位での入射角度を変化させる制御手段を備え、
その制御手段が、前記合致させる両測定強度として、前記算出手段が算出した単位面積あたりの測定強度を用いる全反射蛍光X線分析装置。






In claim 1,
The stage has incident angle adjusting means for changing the incident angle by changing the tilt of the sample,
With respect to the reference X-rays generated uniformly from the sample surface, the arbitrary measurement is performed on the incident angle adjusting means so that the measurement intensity at the arbitrary measurement site matches the measurement intensity at the reference site serving as the reference on the surface of the sample. Comprising control means for changing the incident angle at the site;
The total reflection fluorescent X-ray analyzer using the measurement intensity per unit area calculated by the calculation means as the measurement intensity to be matched by the control means.






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