WO2017154505A1 - 多元素同時型蛍光x線分析装置および多元素同時蛍光x線分析方法 - Google Patents
多元素同時型蛍光x線分析装置および多元素同時蛍光x線分析方法 Download PDFInfo
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- WO2017154505A1 WO2017154505A1 PCT/JP2017/005678 JP2017005678W WO2017154505A1 WO 2017154505 A1 WO2017154505 A1 WO 2017154505A1 JP 2017005678 W JP2017005678 W JP 2017005678W WO 2017154505 A1 WO2017154505 A1 WO 2017154505A1
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/207—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
- G01N2223/076—X-ray fluorescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/30—Accessories, mechanical or electrical features
- G01N2223/33—Accessories, mechanical or electrical features scanning, i.e. relative motion for measurement of successive object-parts
- G01N2223/3307—Accessories, mechanical or electrical features scanning, i.e. relative motion for measurement of successive object-parts source and detector fixed; object moves
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/60—Specific applications or type of materials
- G01N2223/611—Specific applications or type of materials patterned objects; electronic devices
- G01N2223/6116—Specific applications or type of materials patterned objects; electronic devices semiconductor wafer
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- the present invention relates to a multi-element simultaneous X-ray fluorescence analyzer and a multi-element simultaneous X-ray fluorescence analysis method for correcting the background of a sample which is a semiconductor wafer.
- an X-ray source for irradiating a sample with primary X-rays is provided, and a spectroscopic element and a detection device are provided.
- a multi-element simultaneous X-ray fluorescence analyzer equipped with a fixed goniometer for each wavelength to be measured, which has a detector and measures the intensity of fluorescent X-rays generated from a sample.
- a scanning X-ray fluorescence spectrometer that links a spectroscopic element and a detector with a goniometer
- the background intensity is measured before and after the wavelength of the fluorescent X-ray to be measured, and the background intensity at the wavelength of the fluorescent X-ray is estimated.
- the correction can be made by subtracting from the measured intensity of fluorescent X-rays.
- a multi-element simultaneous X-ray fluorescence spectrometer as described in Patent Document 1, if a fixed goniometer is added to measure the background intensity, the configuration of the apparatus becomes complicated and the cost increases. Therefore, in a multi-element simultaneous X-ray fluorescence analyzer, it is desired to correct the background without adding a background fixed goniometer.
- the thickness of the semiconductor wafer decreases and the thickness of the thin film formed on the semiconductor wafer also decreases (for example, several nm).
- the intensity of the X-ray fluorescence generated from the ultra-thin film is weak. It is necessary to measure by integrating. When measurement is performed by integrating for a long time, the measured intensity of the background also increases, and high-precision analysis cannot be performed unless this increased background is corrected.
- the present invention has been made in view of the above-mentioned conventional problems, and even if a notch is formed on the sample stage, the background is accurately corrected without adding a background fixed goniometer, and a semiconductor wafer is obtained. It is an object of the present invention to provide a multi-element simultaneous fluorescent X-ray analysis apparatus and a multi-element simultaneous fluorescent X-ray analysis method that can be analyzed with high accuracy.
- a multi-element simultaneous X-ray fluorescence spectrometer of the present invention performs a sample stage on which a sample which is a semiconductor wafer is placed, and places and removes the sample on the sample stage. It has a transfer arm, a stage for moving the sample stage, and an X-ray source for irradiating the sample with primary X-rays, and has a spectroscopic element and a detector to measure the intensity of fluorescent X-rays generated from the sample.
- a fixed goniometer for each wavelength to be measured, and controls the transfer arm, the stage, the X-ray source, and the fixed goniometer to measure the intensity of fluorescent X-rays at a plurality of measurement points on the sample surface;
- a multi-element simultaneous X-ray fluorescence analyzer equipped with a control means for obtaining the distribution of the measured intensity in the sample table, wherein the sample stage is formed with a notch for allowing the transfer arm to pass in the vertical direction
- the control means has a background correction means, and the background correction means determines the measurement intensity at the measurement point for each measurement point on the blank wafer.
- the intensity obtained by subtracting the measurement intensity of the reference measurement point on the notch is stored in advance as the background intensity of the measurement point, and for each measurement point in the sample to be analyzed, the measurement point is determined from the measurement intensity of the measurement point. Is corrected by subtracting the background intensity.
- the intensity obtained by subtracting the measurement intensity of the reference measurement point on the notch from the measurement intensity of the measurement point As the background intensity of the measurement point, each measurement point in the sample to be analyzed is corrected by subtracting the background intensity of the measurement point from the measurement intensity of the measurement point, so that a notch is formed in the sample stage.
- the semiconductor wafer can be analyzed with high accuracy by accurately correcting the background without adding a fixed goniometer for the background.
- the fluorescent X-ray analysis method of the present invention includes a sample stage on which a sample that is a semiconductor wafer is placed, a transfer arm that places and removes the sample on the sample stage, a stage that moves the sample stage, An X-ray source for irradiating the sample with primary X-rays, and a fixed goniometer that has a spectroscopic element and a detector to measure the intensity of fluorescent X-rays generated from the sample for each wavelength to be measured, Control means is provided for controlling the transport arm, the stage, the X-ray source, and the fixed goniometer to measure the intensity of fluorescent X-rays at a plurality of measurement points on the sample surface and obtaining the distribution of the measured intensity in the sample.
- a multi-element simultaneous X-ray fluorescence analysis apparatus in which a notch for allowing the transfer arm to pass in the vertical direction is formed on the sample stage. Then, for each measurement point on the blank wafer, the intensity obtained by subtracting the measurement intensity of the reference measurement point on the notch from the measurement intensity of the measurement point is obtained as the background intensity of the measurement point. For each measurement point, correction is performed by subtracting the background intensity at the measurement point from the measurement intensity at the measurement point.
- the intensity obtained by subtracting the measurement intensity at the reference measurement point on the notch from the measurement intensity at the measurement point The background intensity is corrected by subtracting the background intensity at the measurement point from the measurement intensity at the measurement point for each measurement point in the sample to be analyzed. Even if the notch is formed, the semiconductor wafer can be analyzed with high accuracy by accurately correcting the background without adding a fixed background goniometer.
- FIG. 1 is a schematic diagram of a multi-element simultaneous fluorescent X-ray analyzer according to a first embodiment of the present invention. It is a top view which shows the sample stand with which the apparatus is equipped. It is a figure which shows the measurement point in a sample. It is a conceptual diagram which shows generation
- this multi-element simultaneous fluorescent X-ray analyzer is equipped with a sample stage 2 on which a sample 1 which is a semiconductor wafer is placed, and placing and removing the sample 1 on the sample stage 2.
- 2 includes a transfer arm 22 (FIG. 2) to be performed, a stage 11 for moving the sample stage 2, and an X-ray source 8 for irradiating the sample 1 with the primary X-ray 7, and a spectroscopic element 25 and a detector 26.
- the fixed goniometer 10 for measuring the intensity of the fluorescent X-ray 9 generated from the sample 1 is provided for each wavelength to be measured, and the transport arm 22, the stage 11, the X-ray source 8 and the fixed goniometer 10 are controlled to control the surface of the sample.
- a multi-element simultaneous X-ray fluorescence analyzer comprising a control means 20 for measuring the intensity of fluorescent X-rays 9 at a plurality of measurement points Pn (FIG. 3) and obtaining the distribution of measured intensity in the sample 1, comprising a sample stage 2
- the transfer arm 22 is vertical. Notches 2e to pass in countercurrent (Figure 2) is formed.
- the control unit 20 has a background correction unit 21, and the background correction unit 21 is not connected to anything on the blank wafer 1 b.
- the intensity obtained by subtracting the measurement intensity of the reference measurement point P0 on the notch 2e from the measurement intensity of the measurement point Pn is stored in advance as the background intensity of the measurement point Pn, and the analysis target sample 1a
- correction is performed by subtracting the background intensity of the measurement point Pn from the measurement intensity of the measurement point Pn.
- the measurement point Pn includes the reference measurement point P0.
- the sample stage 2 is made of, for example, ceramic, a disk-shaped sample 1 having a predetermined diameter, for example, a semiconductor having a diameter of 300 mm in which a CoFeB alloy film having a thickness of 2 nm is formed on a silicon wafer surface.
- the wafer 1 is placed in a disc shape, and includes convex portions 3A and 3B on a part of the upper surface 2a of the sample stage 2, and the upper surfaces 3Aa and 3Ba of the convex portions 3A and 3B are on the same surface, A part of the non-analytic surface (lower surface) of the sample 1 is placed in contact with the upper surfaces 3Aa and 3Ba of the convex portions 3A and 3B.
- the sample table 2 is formed with a substantially rectangular cutout portion 2e through which the transfer arm 22 passes in the vertical direction. The notch 2e is formed beyond the center point 2c of the disk-shaped sample base 2.
- the stage 11 includes an XY table 27 that moves the sample stage 2 along a horizontal plane, and a height adjuster 28 that changes the height of the XY table 27.
- the XY table 27 and the height adjuster 28 are control means. 20. Although only one fixed goniometer 10 is shown in FIG. 1, a fixed goniometer 10 is provided for each wavelength to be measured.
- the operation of the multi-element simultaneous X-ray fluorescence spectrometer of the first embodiment will be described.
- the measurement points P0 to P8 (FIG. 3) including the reference measurement point P0 are set for the sample 1 in the control means 20, the transfer arm 22, the stage 11, the X-ray source 8 and the fixed goniometer 10 are controlled by the control means 20.
- the blank wafer 1b is placed on the sample stage 2 by the transfer arm 22, the sample stage 2 is moved by the stage 11, and the measurement points P0 to P8 are sequentially measured.
- the background correction means 21 stores in advance the intensity obtained by subtracting the measurement intensity at the reference measurement point P0 from the measurement intensity at each measurement point P0 to P8 as the background intensity at each measurement point P0 to P8. That is, the background intensity at the reference measurement point P0 is stored in the background correction unit 21 as 0 cps.
- the reference measurement point P0 is on the notch 2e in the sample 1 and corresponds to, for example, the center point 2c of the sample stage 2.
- the background correction means 21 stores the background intensity at each of the measurement points P0 to P8, after the blank wafer 1b is removed from the sample stage 2 by the transfer arm 22, the sample 1a to be analyzed is transferred to the sample stage 2 by the transfer arm 22. It is mounted and sequentially measured for each measurement point P0 to P8 in the same manner as the blank wafer 1b, and the background correction means 21 measures each measurement point P0 to P8 for each measurement point P0 to P8 in the analysis target sample 1a. Correction is performed by subtracting the stored background intensity of each of the measurement points P0 to P8 from the intensity.
- the reference measurement point on the notch 2e from the measurement intensity of each measurement point P0 to P8.
- the measurement points P0 to P8 are measured from the measurement intensity of each measurement point P0 to P8. Since the background intensity of P8 is subtracted and corrected, even if the notch 2e is formed in the sample stage 2, the background is accurately corrected without increasing the background fixed goniometer, and the semiconductor wafer is raised. Analyzes with accuracy.
- the control unit 20 does not have the background correction unit 21, but other configurations are the multi-element simultaneous X-ray fluorescence analyzer of the first embodiment. Is the same.
- the measurement points P0 to P8 (FIG. 3) are set for the sample 1 in the control means 20 of the multi-element simultaneous X-ray fluorescence spectrometer, the transfer arm 22, the stage 11, the X-ray source 8 and the fixed goniometer 10 are controlled. Under the control of the means 20, as shown in FIG.
- the blank wafer 1 b is placed on the sample stage 2 by the transfer arm 22, and the sample stage 2 is moved by the stage 11, and the measurement points P 0 to P 8 are sequentially measured. The Then, for each measurement point P0 to P8, the intensity obtained by subtracting the measurement intensity at the reference measurement point P0 from the measurement intensity at each measurement point P0 to P8 is obtained as the background intensity at each measurement point P0 to P8. That is, the background intensity at the reference measurement point P0 is 0 cps.
- each measurement point P0 to P8 is measured in the same manner as the blank wafer 1b. Are measured sequentially. Then, for each measurement point P0 to P8 in the sample 1a to be analyzed, the background intensity of each measurement point P0 to P8 obtained for the blank wafer 1b is subtracted from the measurement intensity of each measurement point P0 to P8.
- the reference measurement point P0 on the notch 2e from the measurement intensity of each measurement point P0 to P8.
- the intensity obtained by subtracting the measurement intensity of each of the measurement points P0 to P8 is used as the background intensity of each measurement point P0 to P8, and the measurement points P0 to P8 are measured from the measurement intensities of the measurement points P0 to P8. Therefore, even if the notch 2e is formed in the sample stage 2 of the multi-element simultaneous X-ray fluorescence spectrometer, the background intensity can be reduced without adding a background fixed goniometer.
- the semiconductor wafer can be analyzed with high accuracy by correcting the above.
- the background intensity at the measurement point P1 of the sample 1 on the non-notch is larger.
- the primary X-ray 7 that has passed through the sample 1 on the non-notched portion is irradiated to the sample stage 2, and scattered rays 12 are generated from the sample stage 2. Is considered to pass through the sample 1 and be detected by the detector to become the background.
- the primary X-ray 7 irradiated to the measurement point P5 of the sample 1 on the notch and passing through the sample 1 passes through the notch 2e, and is scattered or absorbed by the structure of the apparatus, and back. It is considered not to be detected as ground.
- the sample stage 2 includes the convex portions 3A and 3B on the upper surface 2a, and the upper surfaces 3Aa and 3Ba of the convex portions 3A and 3B are in contact with the lower surface of the sample 1.
- the convex portions 3A and 3B have a width of 1 mm and a height of 500 ⁇ m.
- a space surrounded by the lower surface of the sample 1, the side surfaces of the projections 3A and 3B, and the upper surface 2a of the sample table 2 is formed, but this space is considered to have no significant effect on the measured value.
- the portion of the sample stage 2 below this space is also included in the non-notched portion described above.
- the measured sample 1 is a semiconductor wafer 1 having a diameter of 300 mm and a thickness of 775 ⁇ m in which a CoFeB alloy film having a thickness of 2 nm (design value) is formed on the surface of the silicon wafer.
- the sample 1 was placed on the sample stage 2 so that the detector 26 was not affected by the diffraction lines generated from the sample 1.
- the primary X-ray 7 is irradiated from the X-ray source 8 as a beam having a diameter of 40 mm to the measurement point P5 (FIG. 3) on the notch 2e and the measurement point P8 (FIG. 3) on the non-notch.
- the intensity of Co-K ⁇ rays, Fe-K ⁇ rays and B-K ⁇ rays, which are fluorescent X-rays generated from the sample 1 was measured.
- Measurement points P5 and P8 were corrected by subtracting the respective background intensities of Co-K ⁇ and Fe-K ⁇ rays stored in advance from the measured intensities of Co-K ⁇ and Fe-K ⁇ rays. .
- the continuous X-ray having the same wavelength as that of the B-K ⁇ line out of the primary X-rays 7 has a long wavelength and hardly transmits through the semiconductor wafer 1. There wasn't.
- the measurement point P8 on the notch 2e is 1.996 nm, and the measurement point P8 is on the non-notch.
- the measurement points P0 to P8 are set for the sample 1.
- the measurement point Pn may be stored.
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Abstract
Description
1a 分析対象試料
1b ブランクウエハ
2 試料台
2e 切り欠き部
7 1次X線
8 X線源
9 蛍光X線
10 固定ゴニオメータ
11 ステージ
20 制御手段
21 バックグラウンド補正手段
22 搬送アーム
25 分光素子
26 検出器
P0 基準測定点
Pn 測定点
Claims (2)
- 半導体ウエハである試料が載置される試料台と、
その試料台に対して試料の載置および撤去を行う搬送アームと、
前記試料台を移動させるステージと、
試料に1次X線を照射するX線源とを備えるとともに、
分光素子および検出器を有して試料から発生する蛍光X線の強度を測定する固定ゴニオメータを測定すべき波長ごとに備え、
前記搬送アーム、前記ステージ、前記X線源および前記固定ゴニオメータを制御して、試料表面の複数の測定点について蛍光X線の強度を測定し、試料における測定強度の分布を求める制御手段を備える多元素同時型蛍光X線分析装置であって、
前記試料台に、前記搬送アームが鉛直方向に通過するための切り欠き部が形成されており、
前記制御手段がバックグラウンド補正手段を有し、
そのバックグラウンド補正手段が、
ブランクウエハにおける各測定点について、当該測定点の測定強度から前記切り欠き部上にある基準測定点の測定強度を差し引いた強度を、当該測定点のバックグラウンド強度としてあらかじめ記憶し、
分析対象試料における各測定点について、当該測定点の測定強度から当該測定点の前記バックグラウンド強度を差し引いて補正する多元素同時型蛍光X線分析装置。 - 半導体ウエハである試料が載置される試料台と、
その試料台に対して試料の載置および撤去を行う搬送アームと、
前記試料台を移動させるステージと、
試料に1次X線を照射するX線源とを備えるとともに、
分光素子および検出器を有して試料から発生する蛍光X線の強度を測定する固定ゴニオメータを測定すべき波長ごとに備え、
前記搬送アーム、前記ステージ、前記X線源および前記固定ゴニオメータを制御して、試料表面の複数の測定点について蛍光X線の強度を測定し、試料における測定強度の分布を求める制御手段を備えており、前記試料台に、前記搬送アームが鉛直方向に通過するための切り欠き部が形成されている多元素同時型蛍光X線分析装置を用いて、
ブランクウエハにおける各測定点について、当該測定点の測定強度から前記切り欠き部上にある基準測定点の測定強度を差し引いた強度を、当該測定点のバックグラウンド強度として求め、
分析対象試料における各測定点について、当該測定点の測定強度から当該測定点の前記バックグラウンド強度を差し引いて補正する蛍光X線分析方法。
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US16/076,112 US10883945B2 (en) | 2016-03-08 | 2017-02-16 | Simultaneous multi-elements analysis type X-ray fluorescence spectrometer, and simultaneous multi-elements X-ray fluorescence analyzing method |
EP17762848.4A EP3428630B1 (en) | 2016-03-08 | 2017-02-16 | Simultaneous multi-element analysis x-ray fluorescence spectrometer, and simultaneous multi-element x-ray fluorescence analyzing method |
CN201780016018.2A CN108713138B (zh) | 2016-03-08 | 2017-02-16 | 多元素同时型荧光x射线分析装置和多元素同时荧光x射线分析方法 |
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US10883945B2 (en) | 2021-01-05 |
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