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WO2017163456A1 - Procédé et dispositif de mesure de la concentration d'oxydant et dispositif de nettoyage de matériel électronique - Google Patents

Procédé et dispositif de mesure de la concentration d'oxydant et dispositif de nettoyage de matériel électronique Download PDF

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Publication number
WO2017163456A1
WO2017163456A1 PCT/JP2016/076829 JP2016076829W WO2017163456A1 WO 2017163456 A1 WO2017163456 A1 WO 2017163456A1 JP 2016076829 W JP2016076829 W JP 2016076829W WO 2017163456 A1 WO2017163456 A1 WO 2017163456A1
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Prior art keywords
cleaning
sulfuric acid
oxidant concentration
oxidant
measuring
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PCT/JP2016/076829
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English (en)
Japanese (ja)
Inventor
小川　祐一
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Kurita Water Industries Ltd
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Kurita Water Industries Ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods

Definitions

  • the present invention relates to a method and apparatus for measuring an oxidant concentration in a sulfuric acid solution containing a metal and an oxidant.
  • the present invention also relates to an electronic material cleaning apparatus using this apparatus.
  • sulfuric acid-based oxidant solutions such as SPM (mixed solution of sulfuric acid and hydrogen peroxide solution), SOM (ozone blowing sulfuric acid), and electrolytic sulfuric acid are used for resist removal, metal etching, and the like.
  • SPM mixed solution of sulfuric acid and hydrogen peroxide solution
  • SOM ozone blowing sulfuric acid
  • electrolytic sulfuric acid is used for resist removal, metal etching, and the like.
  • resist removal and metal etching using a sulfuric acid-based oxidant solution the effect of the concentration of the oxidant in the sulfuric acid-based oxidant solution on the processing effect is large. For this reason, measurement and management of the oxidant concentration of the sulfuric acid-based oxidant solution are important requirements.
  • a method for measuring the oxidant concentration in SPM or electrolytic sulfuric acid there are the following methods.
  • the present invention can measure the oxidant concentration in a sulfuric acid solution containing a metal and an oxidant accurately and efficiently without being affected by impurities such as metal, and the oxidant concentration can be easily brought online. It is an object of the present invention to provide a measuring method, a measuring apparatus, and an electronic material cleaning apparatus using the measuring method and measuring apparatus.
  • the present inventor can measure the absorbance after adding a potassium iodide solution to a sulfuric acid solution, and easily and accurately adjust the oxidant concentration in the sulfuric acid solution without being affected by impurities such as mixed metals. It was confirmed that it could be measured.
  • the gist of the present invention is as follows.
  • a method for measuring the oxidant concentration of a sulfuric acid solution containing a metal and an oxidant wherein a mixing step of mixing the sulfuric acid solution and a potassium iodide solution, and any of wavelengths of 200 to 600 nm of the obtained mixed solution
  • a method for measuring an oxidant concentration comprising: an absorbance measurement step for measuring the absorbance, and a quantitative step for quantifying the oxidant concentration of the sulfuric acid solution based on the measurement result of the absorbance.
  • the sulfuric acid solution is a semiconductor wafer cleaning liquid or a cleaning waste liquid used for cleaning the semiconductor wafer, and the cleaning liquid is supplied to the semiconductor wafer cleaning process.
  • a part of the cleaning liquid or the cleaning waste liquid is separated from the feeding system or the cleaning drainage system for discharging the cleaning drainage from the semiconductor wafer cleaning process, and the oxidant concentration is measured online. Measuring method of oxidant concentration.
  • An apparatus for measuring the oxidant concentration of a sulfuric acid solution containing a metal and an oxidant the mixing means for mixing the sulfuric acid solution and the potassium iodide solution, and any of wavelengths of 200 to 600 nm of the obtained mixed liquid
  • An oxidant concentration measuring device comprising: an absorbance measuring unit that measures the absorbance; and a quantifying unit that quantifies the oxidant concentration of the sulfuric acid solution based on the measurement result of the absorbance.
  • the sulfuric acid solution is a semiconductor wafer cleaning liquid or a cleaning waste liquid used for cleaning the semiconductor wafer, and the cleaning liquid is supplied to the semiconductor wafer cleaning process.
  • An electronic material cleaning apparatus comprising: the oxidant concentration measuring unit according to any one of [4] to [6].
  • the oxidant concentration in a sulfuric acid solution containing a metal and an oxidant such as a sulfuric acid-based oxidant solution mixed with a metal used in the cleaning process of the electronic material can be measured easily and stably with high accuracy without being affected by impurities such as metals. Also, continuous online monitoring can be performed easily.
  • the sulfuric acid-based oxidizer solution such as SPM or electrolytic sulfuric acid and a metal or resist resulting from wafer cleaning is mixed, the sulfuric acid-based oxidizer solution is not affected by impurities such as metal.
  • concentration of the oxidizing agent can be accurately measured.
  • this measurement technique is used when cleaning waste liquid from a sulfuric acid-based oxidant solution is recovered and the oxidant in the sulfuric acid-based oxidant solution is regenerated and reused for cleaning.
  • the oxidant concentration in the cleaning liquid can be accurately monitored, and efficient cleaning can be performed with the cleaning liquid having a predetermined oxidant concentration.
  • a potassium iodide (KI) solution is added to a sulfuric acid solution containing a metal and an oxidizing agent, and an oxidizing agent (oxidizing substance) such as peroxodisulfuric acid in the sulfuric acid solution is selected as KI in the following reaction formula. Reaction to produce yellow color with free iodine (I 2 ).
  • oxidizing substance such as peroxodisulfuric acid in the sulfuric acid solution
  • concentration contains a metal and an oxidizing agent, and there is no restriction
  • the present invention is used for cleaning a semiconductor wafer in which metal is exposed on at least a part of the surface, thereby measuring the oxidant concentration of a sulfuric acid oxidant solution such as electrolytic sulfuric acid, SPM, or SOM containing metal as an impurity. Useful.
  • the present invention provides a cleaning process in the case of cleaning a semiconductor wafer using such a sulfuric acid-based oxidant solution as a cleaning liquid, recovering the cleaning waste liquid, regenerating the oxidant, and reusing it as a cleaning liquid. This is effective when the oxidant concentration in the cleaning liquid supplied to the cleaning liquid or the cleaning waste liquid discharged from the cleaning process is measured online to control the concentration.
  • Examples of the potassium iodide solution include an aqueous potassium iodide solution of about 10 to 200 g / L from the viewpoint of handleability.
  • the amount of potassium iodide solution added to the sulfuric acid solution to be measured is appropriately determined depending on the oxidant concentration in the sulfuric acid solution.
  • the potassium iodide solution is added so that the amount of KI added is about 5 to 20 times (volume ratio) with respect to oxidizing substances such as peroxysulfuric acid, hydrogen peroxide, and ozone in the sulfuric acid solution to be measured. It is preferable.
  • a sulfuric acid solution containing a metal and an oxidizing agent is diluted as necessary, and after adding and mixing a potassium iodide solution, the absorbance at a wavelength of 200 to 600 nm is measured.
  • the measurement wavelength is preferably 200 to 500 nm, more preferably 250 to 400 nm.
  • the absorbance can be measured using a commercially available absorptiometer.
  • the measurement target liquid of the present invention has an oxidant concentration of about 0.001 to 1 mol / L as a measurement concentration. This measured concentration is the oxidant concentration of the sulfuric acid solution containing the metal and oxidant before dilution for measuring the oxidant concentration.
  • Oxidant concentration 0.001-1 mol / L
  • Oxidant concentration 0.01 to 10 mol / L
  • Oxidant concentration 0.001-1 mol / L
  • the measurement of the oxidant concentration according to the present invention can be performed by a batch method in which the dilution of the sulfuric acid solution to be measured and the potassium iodide solution are mixed in the mixing tank, and then the absorbance of the mixed solution is measured.
  • a flow-type absorptiometer By using a flow-type absorptiometer, online mixing is facilitated by mixing these lines.
  • pure water for dilution is introduced into the sample liquid introduction pipe 11 to the flow type absorptiometer 1 having the pump P 1 .
  • the pipe 11 a sulfuric acid solution containing a metal and an oxidizing agent such as oxidizing agent containing sulfuric acid based cleaning fluid from the cleaning process of the semiconductor wafer are injected from the pipe 12 having a pump P 2, the oxidizing agent containing sulfuric acid based cleaning solution with pure water Diluted.
  • Pipe 13 having a pump P 3 for injecting a potassium iodide solution is connected downstream of the injection point of the oxidizing agent containing sulfuric acid based cleaning solution.
  • a potassium iodide solution is injected into the diluted oxidant-containing sulfuric acid-based cleaning solution from the pipe 13.
  • the potassium iodide solution is prepared by injecting a high-concentration potassium iodide solution from the pipe 14 having the pump P 4 into the pipe 13 into which pure water is introduced, and diluting and adjusting the concentration.
  • the liquid after the potassium iodide solution is injected is further mixed by the line mixer 2, and then the mixed liquid is introduced into the flow type absorptiometer 1 to measure the absorbance. Since the liquid after the measurement contains potassium iodide and cannot be used as a cleaning liquid, it is discharged out of the system.
  • a predetermined amount of potassium iodide is added to a sulfuric acid solution diluted to a predetermined concentration range by adjusting the flow rates of pure water, sulfuric acid solution, and potassium iodide solution in each pipe.
  • the solution can be added and mixed, and the absorbance can be measured with the flow type absorptiometer 1.
  • the flow rate of each pipe is, for example, as follows. Piping 11: 5 to 2000 times the flow rate of the piping 12 at 0.5 to 200 ml / min Piping 12: 0.1 to 50 ml / min Pipe 13: 20 to 1000 ml / min, 200 to 10,000 times the flow rate of pipe 12
  • FIG. 2 shows an example in which the oxidant concentration measuring apparatus of the present invention is applied to a cleaning liquid production system by electrolysis of a sulfuric acid solution.
  • the electrolytic solution is fed from the storage tank 20 to the electrolytic cell 23 through the pipe 22 including the pump 21.
  • the electrolytic treatment liquid is circulated to the storage tank 20 through the pipe 24, the gas-liquid separator 25, and the pipe 26.
  • a sorting pipe 27 for sorting a part of the electrolyte solution is provided on the downstream side of the pump 21 of the pipe 22, a sorting pipe 27 for sorting a part of the electrolyte solution is provided.
  • a part of the electrolytic solution is collected from the pipe 22 and is supplied to the oxidant concentration measuring unit 28 which is the oxidant concentration measuring device of the present invention, and the oxidant concentration is measured.
  • the liquid after the measurement is discharged out of the system through the pipe 29.
  • a cleaning liquid made of electrolytic sulfuric acid having a desired oxidizing agent concentration is manufactured by adjusting the electrolysis conditions of the electrolytic cell 23 based on the measurement result of the oxidizing agent concentration in the oxidizing agent concentration measuring unit 28. .
  • 3 to 5 are system diagrams showing an embodiment of an electronic material cleaning apparatus to which the oxidant concentration measuring apparatus of the present invention is applied.
  • FIG. 3 shows an application of the oxidant concentration measuring device of the present invention to a batch type cleaning machine using SPM as a cleaning liquid.
  • the cleaning liquid in the storage tank 30 is supplied to the cleaning machine 32 through the pipe 31.
  • the washing waste liquid is circulated to the storage tank 30 through a pipe 36 having a pump 34 and a heat exchanger 35.
  • the pipe 31 is branched by a sorting pipe 37 for sorting a part of the cleaning liquid supplied to the cleaning machine 32 as a sample liquid.
  • the cleaning liquid collected by the pipe 37 is supplied to an oxidant concentration measuring unit 38 which is an oxidant concentration measuring device of the present invention, and the oxidant concentration is measured.
  • the measured sample solution is discharged out of the system through the pipe 39.
  • FIG. 4 shows a batch type washing machine using electrolytic sulfuric acid as a washing liquid, and applying the oxidant concentration measuring device of the present invention.
  • the electrolytic sulfuric acid in the storage tank 40 is supplied as a cleaning liquid to a cleaning machine 44 through pipes 42 and 43 having a pump 41.
  • the washing waste liquid is discharged through a pipe 46 having a pump 45.
  • a part of the washing waste liquid is circulated to the washing machine 44 through a pipe 48 having a heater 47.
  • the remaining portion of the cleaning waste liquid is returned to the storage tank 40 through a pipe 50 having a cooler 49.
  • the electrolytic sulfuric acid (sulfuric acid solution) in the storage tank 40 is supplied to the electrolyzer 55 through a pipe 53 including a pump 51 and a cooler 52.
  • the peroxydisulfuric acid is generated by electrolysis in the electrolyzer 55 and the sulfuric acid solution containing peroxodisulfuric acid is returned to the storage tank 40 via the pipe 56.
  • the storage tank 40 is provided with a pure water supply pipe 57 and a concentrated sulfuric acid supply pipe 58.
  • a part of the electrolytic sulfuric acid in the storage tank 40 is taken out from the pipe 59 and sent to the oxidant concentration measurement unit 60 which is the oxidant concentration measurement device of the present invention, and the oxidant concentration is measured.
  • the measured sample solution is discharged out of the system through the pipe 61.
  • FIG. 5 shows an example in which the oxidant concentration measuring device of the present invention is applied to a single wafer cleaning machine using electrolytic sulfuric acid as a cleaning liquid.
  • the same members as those shown in FIG. 4 are denoted by the same reference numerals.
  • Reference numeral 70 denotes a decomposition tank for oxidizing and decomposing residual organic substances such as resist contained in the cleaning drainage discharged from the single wafer cleaning machine 80 through the pipe 71 with the oxidizing agent contained in the cleaning drainage. .
  • the electrolytic sulfuric acid in the storage tank 40 is fed from the pipe 42 provided with the pump 41 to the single-wafer cleaning machine 80 through the filter 72 and the heater 73 as in FIG.
  • the cleaning effluent used for cleaning the semiconductor wafer in the single wafer cleaning machine 80 is sent to the decomposition tank 70 via the pipe 71.
  • the cleaning effluent treated in the decomposition tank 70 is returned to the storage tank 40 through a pipe 50 including a pump 45 and a cooler 49.
  • the electrolytic treatment of the electrolytic sulfuric acid in the storage tank 40 and the measurement of the oxidant concentration are performed in the same manner as the treatment in FIG.
  • a part of the cleaning waste liquid is appropriately discharged out of the system through a pipe 74 branched from the pipe 71.
  • the cleaning solution is oxidized.
  • efficient cleaning can be performed with a cleaning liquid having an appropriate oxidant concentration.
  • the measurement method is evaluated as “ ⁇ ”. ".
  • an ultraviolet-visible spectrophotometer manufactured by JASCO Corporation was used as the flow-type absorptiometer.
  • a Ti standard solution (10000 ppm) was used as a Ti source to be added to the sample solution, and a Co standard solution (10000 ppm) was appropriately diluted as a Co source.
  • Electrolytic sulfuric acid (sulfuric acid concentration 92% by weight, charged oxidant concentration 0.01 mol / L) was introduced into a flow-type absorptiometer at 1 L / min, and the absorbance at a wavelength of 253 nm was measured. Was quantified. The oxidizing agent concentration was 0.01 mol / L.
  • Electrolytic sulfuric acid having a sulfuric acid concentration and an oxidizing agent concentration shown in Table 1 was used as a sample solution.
  • the flow equation shown in FIG. 1 was used.
  • the electrolytic sulfuric acid of the sample solution was injected into the ultrapure water flowing through the pipe 12 at 1 mL / min and the pipe 11 at 400 mL / min, mixed and diluted, and then 75 g / L potassium iodide aqueous solution was injected from the pipe 13 at 5 mL / min. And mixed.
  • the mixed solution was introduced into the flow type absorptiometer 1 and the absorbance at a wavelength of 290 nm was measured to quantify the oxidant concentration before addition of the metal.
  • the potassium iodide aqueous solution is obtained by diluting 375 g / L potassium iodide 1 mL / min from the pipe 14 with 4 mL / min ultrapure water from the pipe 13.
  • Example 8 Using SPM 40: 1 as the sample solution, the oxidizing agent concentration before and after the metal addition was determined in the same manner as in Example 3. The results are shown in Table 1.
  • Example 9 The sample liquid was SPM (liquid obtained by mixing 96 wt% sulfuric acid and 30 wt% hydrogen peroxide water at a ratio of 4: 1 (weight ratio)) (hereinafter referred to as “SPM 4: 1”) in the same manner as in Example 3.
  • SPM 4: 1 liquid obtained by mixing 96 wt% sulfuric acid and 30 wt% hydrogen peroxide water at a ratio of 4: 1 (weight ratio)
  • Example 10 The oxidant concentration before and after the metal addition was determined in the same manner as in Example 3 using SOM (a solution obtained by blowing ozone into 92% by weight sulfuric acid) as a sample solution. The results are shown in Table 1.
  • Example 11 The sample solution before and after the metal addition as in Example 3 was measured for the oxidant concentration as the following batch method instead of the flow method. The results are shown in Table 1.
  • Batch type measurement is performed by adding 400 mL of ultrapure water, 1 mL of electrolytic sulfuric acid and 5 mL of 75 g / L potassium iodide solution to a beaker and mixing them with an absorptiometer (UV-Vis spectrophotometer manufactured by JASCO Corporation). The measurement was performed by measuring the absorbance at a wavelength of 290 nm.
  • an absorptiometer UV-Vis spectrophotometer manufactured by JASCO Corporation.
  • the oxidizing agent concentration in sulfuric acid solutions such as electrolytic sulfuric acid, SPM, SOM, etc. having various oxidizing agent concentrations, sulfuric acid concentrations, and metal concentrations can be easily operated by both flow and batch methods. It is possible to measure accurately without being affected by metal.
  • the absorbance at a wavelength of 290 nm was measured, but the same measurement result could be obtained in the measurement of absorbance at a wavelength of 300 nm, 350 nm, and 355 nm.

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Abstract

L'invention concerne un procédé de mesure de la concentration d'oxydant qui peut être facilement mis en ligne et qui est capable de mesurer efficacement, avec une excellente précision, la concentration d'oxydant dans une solution d'acide sulfurique contenant un métal et un oxydant, sans être affectée par des impuretés telles que des métaux. Une solution d'acide sulfurique contenant un métal et un oxydant est mélangée avec une solution d'iodure de potassium, l'absorbance des UV à une longueur d'onde quelconque dans la plage de 200 à 600 nm est mesurée, et la concentration d'oxydant de la solution d'acide sulfurique est déterminée en se basant sur le résultat de la mesure. La solution d'iodure de potassium (KI) est ajoutée à la solution d'acide sulfurique contenant le métal et l'oxydant pour faire réagir sélectivement la substance oxydante dans la solution d'acide sulfurique avec le KI et amener la substance oxydante à être colorée en jaune par l'iode libre. Il en résulte que la sensibilité aux UV devient supérieure à celle des impuretés telles que les métaux, l'effet des impuretés telles que les métaux est réduit et l'absorbance des UV peut être mesurée avec une grande précision.
PCT/JP2016/076829 2016-03-25 2016-09-12 Procédé et dispositif de mesure de la concentration d'oxydant et dispositif de nettoyage de matériel électronique Ceased WO2017163456A1 (fr)

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JP2016-061469 2016-03-25
JP2016061469A JP6168184B1 (ja) 2016-03-25 2016-03-25 酸化剤濃度の測定方法及び測定装置、並びに電子材料洗浄装置

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CN113607671A (zh) * 2021-08-26 2021-11-05 西安热工研究院有限公司 一种除去异丙醇中氧化性杂质的装置及方法

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JP6995329B1 (ja) 2021-09-06 2022-01-14 サラヤ株式会社 過カルボン酸濃度測定用指示薬、それを用いた過カルボン酸濃度測定方法

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