WO2023037564A1 - Procédé de récupération de liquide d'analyse - Google Patents

Procédé de récupération de liquide d'analyse Download PDF

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Publication number
WO2023037564A1
WO2023037564A1 PCT/JP2021/037835 JP2021037835W WO2023037564A1 WO 2023037564 A1 WO2023037564 A1 WO 2023037564A1 JP 2021037835 W JP2021037835 W JP 2021037835W WO 2023037564 A1 WO2023037564 A1 WO 2023037564A1
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WO
WIPO (PCT)
Prior art keywords
analysis
substrate
analysis liquid
nozzle
outer tube
Prior art date
Application number
PCT/JP2021/037835
Other languages
English (en)
Japanese (ja)
Inventor
克彦 川端
イー・ソンジェ
Original Assignee
株式会社 イアス
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 株式会社 イアス filed Critical 株式会社 イアス
Publication of WO2023037564A1 publication Critical patent/WO2023037564A1/fr

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/10—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices

Definitions

  • the present invention relates to a method for recovering an analysis liquid when analyzing an analysis target such as trace metals contained in a substrate or anions present on the substrate surface using a substrate analysis nozzle.
  • impurities such as trace metals and organic substances mixed in the substrate during the manufacturing process and anions present on the substrate surface are recovered and analyzed using a trace amount of analysis liquid.
  • a minute amount of analysis liquid is discharged onto the surface of a substrate such as a silicon wafer, the substrate surface is swept with the discharged analysis liquid to recover impurities, and the recovered analysis liquid is analyzed by an inductively coupled plasma mass spectrometer (ICP-MS). MS), ion chromatography, or the like.
  • ICP-MS inductively coupled plasma mass spectrometer
  • MS ion chromatography
  • a substrate analysis nozzle is used that ejects an analysis liquid from its tip onto a substrate, sweeps the surface of the substrate with the ejected analysis liquid, and then sucks the analysis liquid.
  • the substrate analysis nozzle discharges the analysis liquid from the tip onto the substrate, sweeps the substrate surface with the discharged analysis liquid, and then sucks the analysis liquid.
  • an outer tube arranged on the outer periphery of the nozzle body so as to surround the sweeping analysis liquid for example, Patent Document 1.
  • the double-tube structure substrate analysis nozzle disclosed in Patent Document 1 is capable of sweeping the substrate surface in a short period of time, and has the characteristic that the analysis liquid is less likely to fall off during the sweep.
  • the substrate analysis nozzle 1 is composed of a double tube consisting of a nozzle body 10 and an outer tube 20.
  • the nozzle body 10 is connected to a syringe pump 30 by a tube. It is possible to discharge from.
  • the outer tube 20 is provided with a suction means 21 connected to a pump (not shown) so that the space between the nozzle body 10 and the outer tube 20 becomes a reduced pressure atmosphere.
  • the analysis liquid D held at the tip of the nozzle body 10 sweeps the surface of the substrate to be analyzed. During the sweep, the atmosphere between the nozzle body 10 and the outer tube 20 is reduced to prevent the analysis liquid held at the tip of the nozzle body 10 from falling off.
  • the present invention provides a method for recovering an analysis liquid that can recover an analysis liquid at a high recovery rate when analyzing a substrate having a highly hydrophilic surface using a substrate analysis nozzle with a double-tube structure. intended to provide
  • the present invention provides a nozzle body capable of discharging and sucking an analysis liquid, and an outer tube arranged around the nozzle body so as to surround the analysis liquid held at the tip of the nozzle body and sweeping the substrate.
  • a method for recovering an analytical liquid comprising: using a substrate analyzing nozzle equipped with a suction means for creating a reduced pressure atmosphere between a nozzle body and an outer tube; When sweeping the substrate surface with the liquid, the height position of the tip of the nozzle body and the outer tube is the same. It is characterized by recovering the analytical solution.
  • the analysis solution was swept and collected according to the following procedure.
  • the tip of the substrate analysis nozzle (the tip of the nozzle body and the tip of the outer tube are at the same height position) is moved to the vicinity of the substrate surface.
  • the analysis liquid is discharged from the tip of the nozzle body.
  • the space between the nozzle main body and the outer tube is in a reduced pressure atmosphere, the analysis liquid is held at the tip side of the substrate analysis nozzle without leaking from the outer tube.
  • the substrate surface is swept with the analysis liquid.
  • the analysis liquid is collected by sucking it from the tip of the nozzle body.
  • the tip of the substrate analysis nozzle is arranged near the surface of the substrate, that is, the tip of the nozzle body and the tip of the outer tube are at the same height position.
  • the surface tension between the outer tube and the substrate tends to hold the analysis solution in the gap between the tip of the outer tube and the substrate surface. becomes stronger, cracking occurs when the analysis liquid is recovered at the tip of the nozzle body, and the analysis liquid adhering to the outer tube cannot be recovered.
  • the tip of the outer tube is separated from the substrate surface after the sweep is completed.
  • the analysis liquid is efficiently collected by the nozzle main body. Therefore, according to the present invention, the analysis liquid can be recovered at a high recovery rate, and the amount of the analysis liquid remaining on the substrate surface after recovery can be reduced.
  • the structure of the substrate analysis nozzle for keeping the tip of the outer tube away from the substrate surface is not particularly limited.
  • a structure in which the nozzle body and the outer tube are detachable or a structure in which the outer tube can move up and down with respect to the nozzle body can be adopted.
  • the present invention is suitable for highly hydrophilic substrate surfaces, it can also be applied to hydrophobic substrate surfaces.
  • the analysis liquid is not particularly limited, and a mixed liquid of hydrogen fluoride and hydrogen peroxide, aqua regia, ultrapure water, or the like can be used.
  • the present invention is particularly effective when analyzing a highly hydrophilic substrate surface using ultrapure water.
  • the analytical liquid recovery method of the present invention is capable of recovering the analytical liquid at a high recovery rate even on a highly hydrophilic substrate surface, and the analytical liquid remaining on the substrate surface after recovery can be eliminated. can be reduced.
  • FIG. 3 is a cross-sectional view of a conventional double-tube substrate analysis nozzle.
  • FIG. 2 is a cross-sectional view of a double-tube substrate analysis nozzle of the present invention. Sectional drawing of collection
  • FIG. 2 shows a cross-sectional view of the substrate analysis nozzle of this embodiment.
  • the substrate analysis nozzle 1 shown in FIG. 2 is composed of a double tube consisting of a nozzle body 10 and an outer tube 20.
  • the outer tube 20 is detachable from the nozzle body 10, and has a ring shape. It is attached to the nozzle body 10 via a magnet 22 .
  • the nozzle body 10 is connected to the syringe pump 30 by a tube, so that the analysis liquid D can be discharged to the tip side.
  • the outer tube 10 is provided with a suction means 21 connected to a pump (not shown) so that the space between the nozzle body 10 and the outer tube 20 becomes a reduced pressure atmosphere.
  • the nozzle sweeping operation can be arbitrarily performed on the entire surface of the substrate W by, for example, moving the nozzle from the inside to the outside while rotating the substrate (wafer W).
  • the nozzle body 10 and the outer tube 20 are made of stainless steel or fluororesin.
  • a nozzle body 10 with a tip diameter of 0.8 to 2 mm can be used, and an outer tube with a diameter of 5 mm to 40 mm can be used.
  • the diameter of the outer tube is appropriately determined in consideration of the type of analysis liquid.
  • An 8-inch SiC wafer was used as the substrate to be analyzed, and ultrapure water was used as the analysis liquid in order to analyze the anions on the surface of this substrate, and the recovery rate of the analysis liquid was investigated.
  • the diameter of the nozzle body was 1 mm, and the diameter of the outer tube was 20 mm.
  • the recovery rate of the analytical solution was determined according to the following procedure. First, a predetermined amount (1000 ⁇ L) of ultrapure water is aspirated by the nozzle body alone, and then the outer tube is attached to the nozzle body so that the tips of the nozzle body and the outer tube are at the same height position, and the analysis target is The substrate analysis nozzle was lowered from above the substrate so that the tip of the substrate analysis nozzle was positioned 0.5 mm above the substrate surface. By this operation, the tip of the nozzle main body and the tip of the outer tube are positioned at the same height above the substrate surface by 0.5 mm. Thereafter, 1000 ⁇ L of ultrapure water was discharged from the nozzle body onto the substrate surface to sweep the substrate surface.
  • the space between the nozzle main body and the outer tube was made to have a reduced pressure atmosphere by the suction means.
  • all the ultrapure water is discharged onto the substrate surface, and the substrate analysis nozzle is once raised.
  • an analysis liquid can be recovered at a high recovery rate even with a highly hydrophilic substrate.
  • ultrapure water when ultrapure water is used as the analysis liquid, ultrapure water can be recovered at a high recovery rate. It is possible to improve the analysis accuracy of anion analysis.

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

L'objectif de la présente invention est de fournir un procédé de récupération de liquide d'analyse avec lequel il est possible de collecter un liquide d'analyse avec un taux de récupération élevé, même dans le cas d'un substrat hautement hydrophile. La présente invention concerne un procédé de récupération de liquide d'analyse destiné à utiliser un corps principal de buse pour récupérer un liquide d'analyse qui a balayé une surface de substrat, au moyen d'une buse d'analyse de substrat qui comprend le corps principal de buse, pouvant évacuer et aspirer le liquide d'analyse, et un tube externe disposé à une périphérie externe du corps principal de buse de manière à contenir le liquide d'analyse qui est maintenu à une extrémité de pointe du corps principal de buse et qui balaie le substrat, la buse d'analyse de substrat étant pourvue d'un moyen d'aspiration pour créer une atmosphère à pression réduite entre le corps principal de buse et le tube externe, et le procédé de récupération de liquide d'analyse étant caractérisé en ce que, lorsque la surface du substrat est balayée par le liquide d'analyse, le corps principal de buse et le tube externe sont disposés de telle sorte que les positions en hauteur des extrémités de pointe de ceux-ci sont les mêmes, et après que le balayage soit terminé, le liquide d'analyse est récupéré au moyen du corps principal de buse dans un état dans lequel l'extrémité de pointe du tube externe est séparée de la surface du substrat.
PCT/JP2021/037835 2021-09-10 2021-10-13 Procédé de récupération de liquide d'analyse WO2023037564A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2021-147567 2021-09-10
JP2021147567 2021-09-10

Publications (1)

Publication Number Publication Date
WO2023037564A1 true WO2023037564A1 (fr) 2023-03-16

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05256749A (ja) * 1992-03-12 1993-10-05 Piyuaretsukusu:Kk 分析前処理器具及び該器具を用いた前処理方法
JP2004170222A (ja) * 2002-11-20 2004-06-17 Technos:Kk スキャン・回収兼用ノズル
JP2006190858A (ja) * 2005-01-07 2006-07-20 Nas Giken:Kk 基板処理装置と基板処理方法
JP2013257272A (ja) * 2012-06-14 2013-12-26 Ias Inc 基板分析用ノズル

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05256749A (ja) * 1992-03-12 1993-10-05 Piyuaretsukusu:Kk 分析前処理器具及び該器具を用いた前処理方法
JP2004170222A (ja) * 2002-11-20 2004-06-17 Technos:Kk スキャン・回収兼用ノズル
JP2006190858A (ja) * 2005-01-07 2006-07-20 Nas Giken:Kk 基板処理装置と基板処理方法
JP2013257272A (ja) * 2012-06-14 2013-12-26 Ias Inc 基板分析用ノズル

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