WO2021112079A1 - 蛍光ｘ線分析装置 - Google Patents

蛍光ｘ線分析装置 Download PDF

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Publication number
WO2021112079A1
WO2021112079A1 PCT/JP2020/044667 JP2020044667W WO2021112079A1 WO 2021112079 A1 WO2021112079 A1 WO 2021112079A1 JP 2020044667 W JP2020044667 W JP 2020044667W WO 2021112079 A1 WO2021112079 A1 WO 2021112079A1
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ray
fluorescent
rays
liquid sample
axis
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PCT/JP2020/044667
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English (en)
French (fr)
Japanese (ja)
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肇 二位
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株式会社堀場アドバンスドテクノ
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Publication of WO2021112079A1 publication Critical patent/WO2021112079A1/ja

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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
    • G01N23/22—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

Definitions

  • the present invention relates to a fluorescent X-ray analyzer capable of measuring the concentration of an element contained in a liquid sample.
  • the silicon concentration in phosphoric acid has been measured by, for example, the ion-selective electrode method (see Patent Document 1).
  • the ion-selective electrode method see Patent Document 1.
  • this measurement method since it is necessary to cool the phosphoric acid to a predetermined temperature, it is difficult to measure the silicon concentration in the phosphoric acid circulating at a high temperature in the etching control device in-line.
  • this measurement method since this measurement method has a problem that running is high, a measurement method that is easier to use is required.
  • the present invention has been made in view of the above-mentioned problems, and the influence of scattered X-rays is less likely to appear on the output of the detector, and fluorescence X generated by exciting a light element such as silicon (Si) is generated. It is an object of the present invention to provide a fluorescent X-ray analyzer capable of lowering the lower limit of detection of a line and accurately measuring its concentration.
  • the fluorescent X-ray analyzer is a fluorescent X-ray analyzer that analyzes a liquid sample containing a first element to be measured and a second element having a larger atomic number than the first element.
  • the X-ray source that emits the first X-ray and the second X-ray that is excited by the first X-ray to generate the second X-ray are provided so that the second X-ray is incident on the liquid sample.
  • the concentration of the first element in the liquid sample is calculated based on the next target, a detector that detects fluorescent X-rays generated in the liquid sample excited by the second X-ray, and the output of the detector.
  • the irradiation center which is the intersection of the second X-ray irradiation optical axis with respect to the sample surface of the liquid sample, and the visual field center, which is the intersection of the detection optical axis of the detector with respect to the sample surface.
  • it is characterized in that it is configured to be separated in the sample plane.
  • the detector since the detector has the field of view centered at a portion deviated from the irradiation center on the sample surface, the intensity of the scattered X-rays of the second X-ray generated at the irradiation center is large. The component in the scattering direction can be made difficult to enter the field of view of the detector.
  • the fluorescent X-rays generated at the irradiation center are uniformly emitted in all directions, the amount of fluorescent X-rays incident in the field of view of the detector is scattered X-rays even if the irradiation center and the field center are shifted. Does not decrease compared to.
  • an X-ray permeable film that comes into contact with the liquid sample and forms a sample surface is further provided, and the second X-ray passes through the X-ray permeable film. Anything may be used as long as it is configured to irradiate the liquid sample.
  • the X-ray tube, the secondary target, and the detector and the measurement system can be arranged under the liquid sample to perform fluorescent X-ray analysis. Even if the liquid sample evaporates, the vapor does not affect the measurement system. Therefore, the configuration is particularly suitable when the liquid sample has a risk of deterioration of the measurement system due to vapor such as phosphoric acid.
  • the measurement system when the measurement system is arranged above the liquid sample and a film or the like is provided to prevent the steam of the liquid sample, bubbles are generated between the liquid sample and the film, which hinders fluorescent X-ray analysis. There is a possibility that extra scattering may occur, but if the liquid sample is analyzed from below via the X-ray transmission film, such a problem can be prevented from occurring in the first place.
  • the line-transmitting membrane may be formed of polyimide, aromatic polyetherketone, polyphenylene sulfide, aramid, graphene, or diamond dry carbon.
  • the scattered X-rays of the second X-ray generated in the liquid sample are less likely to be incident on the detector, and each device is densely packed, and the optical path length of the fluorescent X-rays generated in the liquid sample to reach the detector.
  • the irradiation optical axis of the first X-ray is orthogonal to the Z-axis and the Z-axis at the light source point of the X-ray source.
  • the secondary target is the said. It is sufficient that the target surface on which the first X-ray is incident is provided, and the target surface is inclined with respect to the XZ plane and also with respect to the YZ plane.
  • Examples thereof include those whose surfaces are inclined with respect to the XZ plane and the YZ plane.
  • the detector includes a detection surface for detecting fluorescent X-rays, and the detection surface is an XZ plane. It suffices that the detection surface faces the X-ray source side while being inclined with respect to the X-ray source.
  • the secondary targets are required to generate second X-rays separately. It may consist of a plurality of target elements arranged in.
  • two target elements are used. , Those arranged so as to sandwich the detector.
  • the fluorescence analyzer of the present invention can reduce the running cost as compared with the ion-selective electrode method. Moreover, the concentration of silicon (Si) can be accurately measured. In addition, the concentration of silicon (Si) can be measured in-line.
  • the distance between the irradiation center and the visual field center is 3 mm or more and 10 mm or less.
  • the fluorescent X-ray analyzer of the present invention since the irradiation center and the detection center are displaced on the sample surface, the intensity of the scattered X-rays generated on the sample surface is high.
  • the direction in which the high component is contained makes it easy to deviate from the solid angle that can be detected by the detector, and the intensity of the fluorescent X-ray to be measured can be relatively increased. Therefore, since the background value at the output of the detector can be lowered, the lower limit of detection of fluorescent X-rays can also be lowered. Therefore, even fluorescent X-rays of light elements such as silicon (Si) can be sufficiently detected, and quantitative analysis can be performed.
  • FIG. 6 is a schematic view of the fluorescent X-ray analyzer according to the same embodiment when viewed along the Z-axis direction.
  • FIG. 6 is a schematic view of the fluorescent X-ray analyzer according to the same embodiment when viewed along the Y-axis direction. Schematic graph showing the peaks and absorption edges of fluorescent X-rays of phosphorus (P) and silicon (Si).
  • P phosphorus
  • Si silicon
  • the fluorescent X-ray analyzer 100 measures, for example, the concentration of silicon (Si), which is an element contained in a high-temperature phosphoric acid solution used for wet etching of a nitride film in a semiconductor manufacturing process.
  • Si silicon
  • phosphoric acid is in a high temperature state of 100 ° C. to 300 ° C., and in this embodiment, it is a liquid sample LS having a temperature of about 160 ° C. or 160 ° C.
  • silicon (Si) contained in phosphoric acid is a trace element present at a concentration of about 1/1000 to 1/10000 with respect to phosphorus (P).
  • the fluorescent X-ray analyzer 100 of the present embodiment performs fluorescent X-ray analysis on a liquid sample containing a large amount of the second element having an atomic number larger than that of the first element by one.
  • a part of phosphoric acid circulating in the etching apparatus is sampled, and fluorescent X-ray analysis is performed in a liquid state without cooling to obtain a silicon (Si) concentration. Is used to measure.
  • the fluorescent X-ray analyzer 100 only silicon (Si) is excited to derive fluorescent X-rays, and fluorescent X-rays are not excited from phosphorus (P), or silicon (Si) and phosphorus (P) are excited. ) Are both excited, but the amount of fluorescent X-rays generated from phosphorus (P) is small enough to have little effect on calculating the concentration of silicon (Si).
  • the fluorescent X-ray analyzer 100 is in contact with the X-ray source 1, the primary collimator 2, the secondary target 3, the secondary collimator 4, and the liquid sample LS. It is provided with at least a permeable film 5, a detector 6, and a concentration calculator.
  • the Cartesian coordinates of the right-handed system are set with the Z-axis as the emission direction of the first X-ray emitted from the X-ray source 1 and the light source point of the X-ray source 1 as a reference, and are used in the description.
  • the axis that is perpendicular to the Z-axis through the light source point and forms a surface parallel to the sample surface SP of the liquid sample LS formed by the X-ray transmission film 5 is the X-axis, and the X-axis passes through the light source point.
  • the axis orthogonal to the Z axis and the Z axis is set as the Y axis.
  • the sample plane SP and the XZ plane are horizontal planes, and the Y axis coincides with the vertical direction.
  • the X-ray source 1 emits the first X-ray, and emits X-rays having an energy different from the energy irradiated to the liquid sample LS.
  • the fluorescent X-ray generated by irradiating the secondary target 3 with the first X-ray is used as the second X-ray to irradiate the liquid sample LS.
  • the X-ray source 1 is, for example, a vacuum vessel 11 in which the inside is kept in a vacuum and a beryllium (Be) window is formed as an X-ray transmission window 12, and an electron beam source (not shown) provided in the vacuum vessel 11.
  • a primary target 13 in which electrons emitted from an electron beam source are incident and a first X-ray is generated.
  • the primary collimeter 2 limits the range of irradiation of the first X-ray to a predetermined range. That is, the primary collimator 2 limits the first X-ray emitted from the beryllium window into a cylinder having a predetermined radius extending along the Z axis.
  • the main energy of the second X-ray emitted from the secondary target 3 excites silicon (Si), which is the first element contained in the liquid sample LS, to generate the corresponding fluorescent X-ray, and the liquid.
  • the second element phosphorus (P) contained in the sample LS is selected so as not to be excited and to generate fluorescent X-rays. That is, the energy of the absorption edge of silicon (Si), which is the first element, is E1, the energy of the absorption edge of phosphorus (P), which is the second element, is E2, and the energy of the second X-ray generated by the first X-ray on the target surface 31.
  • the energy peak is EP
  • the secondary target 3 is configured so as to satisfy E1 ⁇ EP ⁇ E2.
  • the secondary target 3 is formed of phosphorus (P) which is not a measurement target.
  • the energy EP of the K ⁇ ray which is a fluorescent X-ray generated by the incident of the first X-ray on phosphorus (P)
  • the energy E2 at the absorption edge of phosphorus (P) is smaller than the energy E2 at the absorption edge of phosphorus (P).
  • the secondary collimator 4 limits the irradiation range and irradiation direction of the second X-ray generated by the secondary target 3 with respect to the sample surface SP. That is, the secondary collimator 4 defines the irradiation optical axis LA of the second X-ray in a predetermined direction.
  • the X-ray transmission film 5 is a film extending along a horizontal plane, and forms a sample surface SP in contact with the liquid sample LS on the upper surface thereof.
  • the X-ray transmission film 5 is, for example, a resin film having a film thickness of ⁇ m, and is configured to suppress the attenuation of incident second X-rays and fluorescent X-rays generated in the liquid sample LS as much as possible.
  • the X-ray transmission film 5 is formed of polyimide or aromatic polyetherketone.
  • the second X-ray generated by the secondary target 3 penetrates through the X-ray transmission film 5 and penetrates into the liquid sample LS to a predetermined depth.
  • the predetermined depth is about several tens of ⁇ m to several hundreds of ⁇ m.
  • the second X-ray incident on the liquid sample LS generates fluorescent X-rays for silicon (Si) contained in the liquid sample LS and also generates scattered X-rays at the same time.
  • the X-ray permeable membrane 5 may be formed of polyphenylene sulfide, aramid, graphene, or diamond-like carbon.
  • the detector 6 detects fluorescent X-rays generated in the liquid sample LS, and the detection surface 61 is arranged so as to be parallel to the sample surface SP. That is, the detection optical axis DA of the detector 6 is provided so as to be perpendicular to the sample surface SP, and as shown in FIGS. 3 and 4, the detection center which is the intersection of the sample surface SP and the detection optical axis DA. Is placed directly above the detector 6. Further, the detector 6 is arranged so that the area directly below the irradiation center is the outer peripheral portion of the detection surface 61.
  • the irradiation center which is the intersection of the irradiation optical axis LA of the second X-ray generated by the secondary target 3 and the sample surface SP, and the detection center are a predetermined distance on the sample surface SP. It is configured to shift.
  • the irradiation center is separated from the detection center by a predetermined distance with respect to the X-axis direction according to the tilting direction of the target surface 31 of the secondary target 3, and the separation distance is, for example, 3 mm or more and 10 mm. It is set as follows. In particular, as shown in FIG.
  • the detection optical axis LA of the second X-ray and the detection optical axis DA of the detector 6 are arranged so as to be offset, the detection is detected by the detector 6 for the following reasons.
  • the ratio of fluorescent X-rays to X-rays can be increased.
  • the scattered X-rays generated at the irradiation center are dependent on the scattering angle, and a high-intensity component is generated centering on the direction perpendicular to the sample surface SP (Y-axis direction).
  • the detection center is separated from the irradiation center, and the area directly below the irradiation center is located on the outer edge of the detection surface 61.
  • the intensity of the scattered X-rays in the solid angle of the field of view of the detector 6 It is possible to prevent the high directional component from being included so that the component with a weak scattering angle and a shallow scattering angle is mainly detected.
  • fluorescent X-rays are not angle-dependent and are emitted uniformly in all directions. Therefore, even if the irradiation center and the detection center are deviated, the fluorescent X-rays incident on the solid angle of the field of view of the detector 6 The amount does not decrease as much as the scattered X-rays mentioned above.
  • the background value due to the influence of scattered X-rays on the sample surface SP of the second X-ray can be reduced in the output of the detector 6, and the lower limit of detection of fluorescent X-rays mainly of silicon (Si) can be lowered. ..
  • the function of the concentration calculator 7 is realized by, for example, a CPU, a memory, an A / D converter, a D / A converter, and a so-called computer having various input / output means.
  • the program stored in the memory is executed by the CPU, and various devices cooperate to determine the concentration of silicon (Si) contained in the liquid sample LS based on the output of the detector 6. calculate.
  • a specific calculation formula for example, a known one is used.
  • silicon which is a trace element contained in the liquid sample LS in the liquid state without cooling or evaporating the liquid sample LS.
  • the (Si) concentration can be measured based on fluorescent X-rays.
  • the irradiation center of the second X-ray on the sample surface SP and the detection center of the detector 6 are separated from each other, the directional component having high intensity among the scattered X-rays generated on the sample surface SP Is difficult to detect by the detection surface 61, and the ratio of fluorescent X-rays of silicon (Si) to the X-rays detected by the detector 6 can be increased. As a result, the lower limit of detection of silicon (Si) can be lowered as compared with the conventional case.
  • the energy of the second X-ray generated by the secondary target 3 is a large amount of phosphorus (P) fluorescence contained in the liquid sample LS.
  • P phosphorus
  • the secondary target 3, the liquid sample LS, and the detector 6 are densely arranged.
  • the optical path length of each X-ray is shortened to prevent attenuation.
  • the X-ray transmission film 5 is also set to have a thin film thickness, it is possible to reduce the attenuation when X-rays pass through the X-ray transmission film 5. Therefore, fluorescent X-rays can be detected with the intensity required to measure the concentration of silicon (Si) contained in the liquid sample LS, which is a trace amount of a light element.
  • the fluorescent X-ray analyzer according to the present invention is not limited to measuring the concentration of silicon (Si) contained in the phosphoric acid solution. It can be used to measure the concentration of the first element based on fluorescent X-rays with respect to a liquid sample containing the first element to be measured and the second element having an atomic number larger than that of the first element.
  • the difference between the atomic numbers of the first element and the second element was 1, but the difference between the atomic numbers of the first element and the second element may be 2, and the difference between the atomic numbers is larger than 2. Is also good.
  • a part of the liquid sample is sampled and the fluorescent X-ray analysis is performed as it is without cooling or evaporating.
  • the fluorescent X-ray analysis is performed while the liquid sample is flowing.
  • Real-time in-line density measurement may be realized.
  • a branch flow path formed of an X-ray permeable film is formed in a part of a pipe through which a liquid sample flows, and fluorescent X-ray analysis is performed in that part, or a window made of an X-ray permeable film is formed in a part of the pipe. May be formed and fluorescent X-ray analysis may be performed through the window.
  • each device constituting the fluorescent X-ray analyzer is not limited to the one shown in the above embodiment.
  • the detection optical axis of the detector may be configured to be obliquely incident on the sample surface instead of being vertically incident on the sample surface.
  • the detection surface of the detector may be tilted toward the X-ray source side where the first X-ray is emitted. In this way, the irradiation center and the detection center can be further shifted to make it difficult for the detector to detect the scattered X-rays generated on the detection surface of the liquid sample, and the proportion of the detected fluorescent X-rays can be increased.
  • the direction in which the detector is tilted may be appropriately different depending on the type of the liquid sample and the equipment used.
  • the detector may be tilted so that the detection surface faces the side opposite to the X-ray source.
  • the target surface of the secondary target is not limited to the one that is inclined with respect to both the XZ plane and the YZ plane as in the above embodiment, but only with respect to either the XZ plane or the YZ plane. It may be inclined.
  • the secondary target 3 may be composed of a plurality of target elements 3E, and the second X-ray generated by each target element 3E may be separately irradiated to the sample surface SP.
  • the target element 3E may be arranged in a substantially V shape so as to sandwich the detector 6 in a mirror plane symmetry with respect to the detection optical axis DA.
  • the fluorescent X-rays generated by the first element from the sample surface SP are incident on the detector 6 symmetrically with respect to the detection optical axis DA.
  • the measurement time can be shortened by about half, or the statistical measurement error can be reduced and more accurate measurement results can be obtained in the same measurement time.
  • the element constituting the secondary target is not limited to phosphorus (P), but may be zirconium (Zr) as shown in FIG. If it is L ⁇ ray which is a component of fluorescent X-ray of zirconium, the above-mentioned relationship between energies is satisfied and the same effect can be obtained. Further, the secondary target may be one formed of yttrium (Y). Further, any element can be used as the secondary target as long as it is an element that generates a second X-ray satisfying E1 ⁇ EP ⁇ E2.
  • a fluorescent X-ray analyzer may be used in which the elements constituting the secondary target are selected so as to satisfy E1 ⁇ EP ⁇ E2 in a state where the irradiation center and the detection center are aligned on the sample surface without shifting.
  • fluorescent X-rays of both the first element and the second element may be generated with the irradiation center and the detection center shifted by a predetermined distance.
  • the material constituting the secondary target described in the embodiment may be used as a material for generating primary X-rays, and the sample may be directly irradiated with primary X-rays.
  • a fluorescent X-ray analyzer capable of sufficiently detecting fluorescent X-rays of a light element such as silicon (Si) and performing quantitative analysis.

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PCT/JP2020/044667 2019-12-02 2020-12-01 蛍光ｘ線分析装置 WO2021112079A1 (ja)

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JPH06249804A (ja) * 1993-03-01 1994-09-09 Seiko Instr Inc 蛍光ｘ線分析装置
US6041095A (en) * 1997-03-12 2000-03-21 Jordan Valley Applied Radiation X-ray fluorescence analyzer
JP2005345442A (ja) * 2004-06-07 2005-12-15 Rigaku Industrial Co 蛍光ｘ線分析用液体試料容器
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JP2008039772A (ja) * 2006-07-14 2008-02-21 Japan Science & Technology Agency Ｘ線分析装置及びｘ線分析方法
JP2009222615A (ja) * 2008-03-18 2009-10-01 Rigaku Corp 蛍光ｘ線分析用試料保持具ならびにそれを用いる蛍光ｘ線分析方法および装置
JP2011127954A (ja) * 2009-12-16 2011-06-30 Sumitomo Metal Ind Ltd 蛍光ｘ線液分析計
JP2017083346A (ja) * 2015-10-29 2017-05-18 株式会社堀場製作所 液体試料分析装置

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JPH01126555U (enrdf_load_stackoverflow) * 1988-02-24 1989-08-29
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JP2001235437A (ja) 2000-02-21 2001-08-31 Technos Kenkyusho:Kk 全反射蛍光ｘ線分析装置
JP3726161B2 (ja) 2003-03-28 2005-12-14 理学電機工業株式会社 蛍光ｘ線分析装置
JP5553300B2 (ja) 2009-11-19 2014-07-16 株式会社日立ハイテクサイエンス 蛍光ｘ線検査装置及び蛍光ｘ線検査方法
JP2013108759A (ja) 2011-11-17 2013-06-06 Fuji Electric Co Ltd 半導体ウェハプロセス用ふっ酸溶液の不純物分析方法および該ふっ酸溶液の交換時期の管理方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06249804A (ja) * 1993-03-01 1994-09-09 Seiko Instr Inc 蛍光ｘ線分析装置
US6041095A (en) * 1997-03-12 2000-03-21 Jordan Valley Applied Radiation X-ray fluorescence analyzer
JP2005345442A (ja) * 2004-06-07 2005-12-15 Rigaku Industrial Co 蛍光ｘ線分析用液体試料容器
JP2006030018A (ja) * 2004-07-16 2006-02-02 Nyuurii Kk 蛍光ｘ線分析装置
JP2008039772A (ja) * 2006-07-14 2008-02-21 Japan Science & Technology Agency Ｘ線分析装置及びｘ線分析方法
JP2009222615A (ja) * 2008-03-18 2009-10-01 Rigaku Corp 蛍光ｘ線分析用試料保持具ならびにそれを用いる蛍光ｘ線分析方法および装置
JP2011127954A (ja) * 2009-12-16 2011-06-30 Sumitomo Metal Ind Ltd 蛍光ｘ線液分析計
JP2017083346A (ja) * 2015-10-29 2017-05-18 株式会社堀場製作所 液体試料分析装置

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