WO2023140245A1 - 希釈機構、粒子径分布測定システム、粒子径分布測定方法、及び粒子径分布測定用プログラム - Google Patents

希釈機構、粒子径分布測定システム、粒子径分布測定方法、及び粒子径分布測定用プログラム Download PDF

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Publication number
WO2023140245A1
WO2023140245A1 PCT/JP2023/001142 JP2023001142W WO2023140245A1 WO 2023140245 A1 WO2023140245 A1 WO 2023140245A1 JP 2023001142 W JP2023001142 W JP 2023001142W WO 2023140245 A1 WO2023140245 A1 WO 2023140245A1
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WO
WIPO (PCT)
Prior art keywords
sample
particle size
size distribution
conductivity
concentration
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Ceased
Application number
PCT/JP2023/001142
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English (en)
French (fr)
Japanese (ja)
Inventor
啓二郎 櫻本
哲也 森
一徳 土生
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Horiba Ltd
Horiba Advanced Techno Co Ltd
Original Assignee
Horiba Ltd
Horiba Advanced Techno Co Ltd
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.)
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Priority to KR1020247022747A priority Critical patent/KR20240135756A/ko
Priority to JP2023575251A priority patent/JPWO2023140245A1/ja
Priority to US18/728,729 priority patent/US20250137902A1/en
Priority to CN202380017081.3A priority patent/CN118647850A/zh
Publication of WO2023140245A1 publication Critical patent/WO2023140245A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/06—Investigating concentration of particle suspensions
    • G01N15/0656—Investigating concentration of particle suspensions using electric, e.g. electrostatic methods or magnetic methods
    • 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
    • G01N1/38—Diluting, dispersing or mixing samples
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/02—Investigating particle size or size distribution
    • G01N15/0205—Investigating particle size or size distribution by optical means
    • G01N15/0211—Investigating a scatter or diffraction pattern
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/10—Investigating individual particles
    • G01N15/14—Optical investigation techniques, e.g. flow cytometry
    • G01N15/1425—Optical investigation techniques, e.g. flow cytometry using an analyser being characterised by its control arrangement
    • 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
    • G01N1/38—Diluting, dispersing or mixing samples
    • G01N2001/386—Other diluting or mixing processes
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N2015/0038—Investigating nanoparticles
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N2015/0042—Investigating dispersion of solids
    • G01N2015/0053—Investigating dispersion of solids in liquids, e.g. trouble
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/02—Investigating particle size or size distribution
    • G01N15/0205—Investigating particle size or size distribution by optical means
    • G01N15/0211—Investigating a scatter or diffraction pattern
    • G01N2015/0222—Investigating a scatter or diffraction pattern from dynamic light scattering, e.g. photon correlation spectroscopy
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/10—Investigating individual particles
    • G01N15/14—Optical investigation techniques, e.g. flow cytometry
    • G01N2015/1493—Particle size

Definitions

  • the present invention relates to a dilution mechanism, a particle size distribution measuring system, a particle size distribution measuring method, and a particle size distribution measuring program.
  • particles such as slurry are sometimes used for polishing semiconductors, and if these particles contain too large particles, they may damage the semiconductor.
  • the transmitted light intensity when detecting the transmitted light intensity, it is necessary to increase the concentration of the sample, which tends to cause the above-mentioned multiple scattering. Therefore, it is not suitable for combination with the particle size distribution of the dynamic light scattering method. If the particles are minute (for example, nanoscale), the transmitted light intensity is high and the rate of change is small, making it difficult to accurately control the concentration.
  • the scattered light intensity depends on the particle size distribution, and if the scattered light at a certain scattering angle is detected, the concentration can only be obtained when the particle size distribution is fixed. Therefore, when the particle size distribution fluctuates, it is difficult to control the concentration with high accuracy.
  • the present invention was made to solve the above-mentioned problems at once, and in order to ensure measurement accuracy in particle size distribution measurement using the dynamic light scattering method, the main problem is to be able to accurately control the concentration of particles contained in a sample even when the particle size distribution of the particles contained in the sample fluctuates.
  • the dilution mechanism according to the present invention is a dilution mechanism that is used with a particle size distribution measuring device that measures a particle size distribution by a dynamic light scattering method, and includes a sample line that guides a sample containing particles to the particle size distribution measuring device, a dilution line that joins the sample line and through which a diluent flows, concentration adjusting means for adjusting the concentration of particles contained in the sample after dilution, conductivity measuring means for measuring the conductivity of the sample after dilution, and the conductivity measured by the conductivity measuring means or a value calculated from the conductivity. and a control unit for controlling the concentration adjusting means so that a certain conductivity-related value becomes a predetermined target value.
  • the concentration control means is controlled so that the conductivity of the sample or a conductivity-related value calculated from the conductivity becomes a predetermined target value. Therefore, unlike the case where the concentration is controlled using the transmitted light intensity or the scattered light intensity, even if the particle size distribution of the particles contained in the sample fluctuates, the concentration of the particles contained in the sample can be controlled with high accuracy.
  • concentration calculation unit that calculates the concentration of particles contained in the sample after dilution as the conductivity-related value from the conductivity measured by the conductivity measurement unit, and the control unit controls the concentration adjustment unit so that the concentration calculated by the concentration calculation unit becomes the target value.
  • a correlation data storage unit that stores correlation data indicating the correlation between the conductivity of the sample after dilution and the concentration of particles contained in the sample, and the concentration calculation unit calculates the concentration of particles contained in the sample after dilution using the correlation data.
  • the concentration adjusting means may include a fluid control valve provided in at least one of the sample line and the dilution line. With this, the density can be controlled with a low cost and simple configuration.
  • the sample line takes the sample from a manufacturing system used in a given manufacturing process.
  • the particle size distribution of the particles used in the manufacturing system can be measured on-line.
  • An embodiment in which the above-described dilution mechanism exerts the action and effect more remarkably includes an embodiment in which the sample has a chemical component that causes a correlation between the concentration of particles contained in the sample and the conductivity of the sample.
  • a particle size distribution measuring system is characterized by comprising the above-described dilution mechanism and a particle size distribution measuring device that measures the particle size distribution of particles contained in the sample diluted by the dilution mechanism by a dynamic light scattering method.
  • the particle size distribution measuring method is a particle size distribution measuring method for measuring a particle size distribution by a dynamic light scattering method, comprising the steps of: introducing a sample containing particles to a particle size distribution measuring device through a sample line; joining a diluent into the sample line; adjusting the concentration of particles contained in the diluted sample using a concentration adjusting means; measuring the conductivity of the diluted sample using a conductivity measuring means; and controlling the concentration adjusting means such that the conductivity-related value, which is the value to be measured, is a predetermined target value.
  • a program for measuring particle size distribution is a program used in a particle size distribution measuring system comprising: a particle size distribution measuring device that measures a particle size distribution by a dynamic light scattering method; a sample line that guides a sample containing particles to the particle size distribution measuring device; a dilution line that merges with the sample line and through which a diluent flows; a concentration adjusting means that adjusts the concentration of particles contained in the sample after dilution;
  • the computer functions as a control unit for controlling the concentration adjusting means so that the calculated conductivity or a conductivity-related value, which is a value calculated from the conductivity, becomes a predetermined target value.
  • the present invention configured in this way, in particle size distribution measurement using the dynamic light scattering method, even if the particle size distribution of the particles contained in the sample fluctuates, it is possible to accurately control the concentration of the particles contained in the sample in order to ensure measurement accuracy.
  • FIG. 1 is a schematic diagram showing the configuration of a particle size distribution measuring system according to one embodiment;
  • FIG. The schematic diagram which shows the structure of the particle size distribution measuring apparatus of the same embodiment.
  • the schematic diagram which shows the structure of the dilution mechanism of the same embodiment.
  • the functional block diagram which shows the function of the control apparatus of the same embodiment.
  • the flowchart figure which shows the operation
  • the particle size distribution measuring system 100 of the present embodiment is used together with a manufacturing system 200 used in a predetermined manufacturing process, such as a semiconductor manufacturing system, and measures the particle size distribution of particles used in the manufacturing system 200 online.
  • the particle size distribution measuring system 100 includes a dilution mechanism 10 that collects and dilutes a sample containing particles from the manufacturing system 200, and a particle size distribution measuring device 20 that measures the particle size distribution of the particles contained in the diluted sample.
  • the sample to be measured has a chemical component that causes a correlation between the concentration of particles contained in the sample and the conductivity of the sample.
  • An example of this is polishing slurry such as CMP slurry.
  • the particle size distribution measuring system 100 of the present embodiment is characterized by the dilution mechanism 10, the particle size distribution measuring device 20 will be briefly described first, and then the details of the dilution mechanism 10 will be described.
  • the particle size distribution measuring device 20 measures the particle size distribution by the dynamic light scattering method (DLS), and here, for example, can measure the particle size distribution in a range including the nanoscale particle size range.
  • DLS dynamic light scattering method
  • the particle size distribution measuring apparatus 20 includes a laser light source 21 that emits a laser beam to a flow cell C containing a sample, one or more photodetectors 22 arranged around the flow cell C, and a computer that is a computing unit 23 that calculates an autocorrelation function based on the time variation of the scattered light intensity, which is an actual measurement of the scattered light detected by the photodetector 22, and calculates the particle size distribution from the autocorrelation function.
  • the dilution mechanism 10 includes a sample line L1 for collecting a sample containing particles from the manufacturing system 200 described above, a dilution line L2 through which a diluent for diluting the collected sample flows, a concentration adjusting means 11 for adjusting the concentration of particles contained in the diluted sample (hereinafter also referred to as the diluted sample), a conductivity measuring means 12 for measuring the conductivity of the diluted sample, and a control device 13 for controlling the concentration adjusting means 11 using the measured value of the conductivity measuring means 12. It has
  • the sample line L1 has an upstream end connected to a pipe that constitutes the manufacturing system 200 and a downstream end connected to the particle size distribution measuring device 20, and collects a sample flowing through the pipe and guides it to the particle size distribution measuring device 20.
  • the dilution line L2 merges with the sample line L1, and its downstream end is connected to a predetermined confluence point X set in the sample line L1.
  • the diluent flowing through the dilution line L2 is a liquid that does not contain particles to be measured, and is water here.
  • a mixer M such as a static mixer is provided downstream of the junction X of the sample line L1 to improve the mixing performance of the particles contained in the sample and the diluent.
  • the concentration adjustment means 11 adjusts the ratio of the sample collected via the sample line L1 and the diluent mixed with the sample, thereby adjusting the concentration of particles contained in the diluted sample.
  • this concentration adjusting means 11 is a fluid control valve provided in at least one of the sample line L1 and the dilution line L2, as shown in FIG.
  • These fluid control valves control the flow rate or pressure of the sample or diluent, and the opening of the valves is controlled by the control device 13, which will be described later.
  • the conductivity measuring means 12 is provided downstream of the confluence point X in the sample line L1, and measures the conductivity of the diluted sample by the principle of, for example, the AC two-electrode method or the electromagnetic induction method.
  • the conductivity measuring means 12 of the present embodiment is provided downstream of the mixer M described above, and is configured to sequentially transmit a measurement signal indicating the magnitude of the measured conductivity in real time to the control device 13, which will be described later, via, for example, a wireless or wired connection.
  • the control device 13 is physically a general-purpose or dedicated computer equipped with a CPU, memory, AD converter, and the like.
  • the control device 13 exhibits at least the function of the control unit 133 that controls the concentration adjustment means 11 described above, by cooperating with the CPU and its peripheral devices according to the particle size distribution measurement program stored in the memory.
  • the control unit 133 controls the concentration adjusting means 11 so that the conductivity-related value, which is the conductivity measured by the conductivity measuring means 12 or a value calculated from the conductivity, reaches a predetermined target value.
  • control device 13 of the present embodiment functions as a concentration calculation section 131 and a correlation data storage section 132 in addition to the control section 133 described above.
  • control device 13 will be described with reference to the flowchart of FIG. 5 while also describing each part.
  • a sample flowing through the piping of the manufacturing system 200 is collected in the sample line L1 (S1), diluted with a diluent (S2), and guided to the particle size distribution measuring device 20.
  • the conductivity of the diluted sample is measured by the conductivity measuring means 12, and a measurement signal indicating the magnitude of the conductivity is sequentially transmitted to the control device 13 (S3).
  • the concentration calculation unit 131 uses the conductivity measured by the conductivity measurement means 12 to calculate the concentration of particles contained in the diluted sample (hereinafter referred to as actual concentration) as the conductivity-related value described above (S4).
  • the concentration calculation unit 131 acquires correlation data indicating the correlation between the conductivity of the diluted sample and the actual concentration of the particles contained in the diluted sample from the correlation data storage unit 132, calculates the actual concentration using the correlation data and the measured conductivity, and outputs the calculated actual concentration to the control unit 133.
  • the correlation data may include, for example, a calculation formula for calculating the actual concentration from the electrical conductivity, a lookup table for obtaining the actual concentration from the electrical conductivity, and the like.
  • control unit 133 controls the density control means described above so that the actual density calculated by the density calculation unit 131 becomes a predetermined target value (S5).
  • control unit 133 compares the actual concentration and the target value, calculates a control amount according to the difference between them, and feedback-controls the valve opening degree of the fluid control valve based on the control amount.
  • the control device 13 of the present embodiment is configured to repeat the calculation of the particle concentration in S4 and the control of the concentration adjusting means 11 in S5, and in a state in which these operations are repeated, the particle size distribution measuring device 20 measures the particle size distribution of the particles contained in the introduced diluted sample.
  • the particle size distribution measuring device 20 configured in this manner, the conductivity of the diluted sample is measured, and the concentration control means is controlled so that the actual concentration of the particles in the diluted sample calculated from the conductivity reaches the target value. Therefore, unlike the case where the concentration is controlled using the transmitted light intensity or the scattered light intensity, even if the particle size distribution of the particles contained in the sample fluctuates, the concentration of the particles contained in the sample can be accurately controlled. It becomes possible. Thereby, the particle size distribution measuring device 20 of the present embodiment contributes to online measurement of the particle size distribution of the particles used in the production system 200 .
  • the present invention is not limited to the above embodiments.
  • control unit 133 in the above embodiment controls the concentration control means so that the actual concentration becomes the target value, but the concentration control means may be controlled so that the conductivity measured by the conductivity measurement means 12 becomes the target value.
  • control device 13 may not have the functions of the concentration calculator 131 and the correlation data storage 132 .
  • control unit 133 may control the concentration control means so that a conductivity-related value such as electrical conductivity, electrical conductivity, electrical resistance, electrical resistivity, or impedance calculated from the electrical conductivity becomes a target value.
  • the particle size distribution measuring system 100 may have a function as a display unit that outputs the particle size distribution, which is the measurement result of the particle size distribution measuring device 20, and the conductivity, which is the measurement result of the conductivity measuring means 12, or a conductivity-related value calculated from the conductivity to the same or different displays in a comparable manner.
  • a specific gravity meter may be provided instead of the conductivity measuring means 12, and the control unit 133 may be configured to control the concentration control means so that the specific gravity of the diluted sample measured by this specific gravity meter or the value calculated from this specific gravity becomes the target value.
  • the present invention in particle size distribution measurement using the dynamic light scattering method, even if the particle size distribution of the particles contained in the sample fluctuates, it is possible to accurately control the concentration of the particles contained in the sample in order to ensure measurement accuracy.

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  • Chemical & Material Sciences (AREA)
  • Biochemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
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  • Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
  • Length Measuring Devices By Optical Means (AREA)
PCT/JP2023/001142 2022-01-21 2023-01-17 希釈機構、粒子径分布測定システム、粒子径分布測定方法、及び粒子径分布測定用プログラム Ceased WO2023140245A1 (ja)

Priority Applications (4)

Application Number Priority Date Filing Date Title
KR1020247022747A KR20240135756A (ko) 2022-01-21 2023-01-17 희석 기구, 입자 지름 분포 측정 시스템, 입자 지름 분포 측정 방법 및 입자 지름 분포 측정용 프로그램
JP2023575251A JPWO2023140245A1 (https=) 2022-01-21 2023-01-17
US18/728,729 US20250137902A1 (en) 2022-01-21 2023-01-17 Dilution mechanism, particle size distribution measurement system, particle size distribution measurement method, and program for particle size distribution measurement
CN202380017081.3A CN118647850A (zh) 2022-01-21 2023-01-17 稀释机构、粒径分布测量系统、粒径分布测量方法和粒径分布测量用程序

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JP2022-007802 2022-01-21
JP2022007802 2022-01-21

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WO2023140245A1 true WO2023140245A1 (ja) 2023-07-27

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US (1) US20250137902A1 (https=)
JP (1) JPWO2023140245A1 (https=)
KR (1) KR20240135756A (https=)
CN (1) CN118647850A (https=)
TW (1) TW202334633A (https=)
WO (1) WO2023140245A1 (https=)

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CN121187181A (zh) * 2025-09-23 2025-12-23 冠礼控制科技（上海）有限公司 一种研磨液自动稀释混合供应控制方法及控制系统

Citations (8)

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Publication number Priority date Publication date Assignee Title
US6122956A (en) * 1998-09-09 2000-09-26 University Of Florida Method and apparatus for monitoring concentration of a slurry flowing in a pipeline
JP2002022644A (ja) * 2000-07-10 2002-01-23 Horiba Ltd 工程管理用の粒径分布測定システム
JP2002513151A (ja) * 1998-04-29 2002-05-08 パーティクル、メジュアリング、システムズ、インコーポレーテッド 化学機械的平坦化（ｃｍｐ）スラリーの品質管理プロセスおよび粒子サイズ分布測定システム
JP2002527740A (ja) * 1998-10-15 2002-08-27 パーティクル サイジング システムズ インコーポレイテッド 高分解能粒度分析を行うための自動希釈システム
JP2004053431A (ja) * 2002-07-22 2004-02-19 Horiba Ltd 粒径分布測定方法、粒径分布測定装置および粒径分布測定装置の測定プログラム
JP2004537737A (ja) * 2001-08-09 2004-12-16 コモンウェルス　サイエンティフィック　アンド　インダストリアル　リサーチ　オーガニゼーション 流体中の異物の検出方法及び検出装置
JP2005512042A (ja) * 2001-12-03 2005-04-28 ボード・オブ・リージエンツ，ザ・ユニバーシテイ・オブ・テキサス・システム 粒子インピーダンスセンサ
JP2006064623A (ja) * 2004-08-30 2006-03-09 Horiba Ltd 粒子径分布測定装置

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Publication number Priority date Publication date Assignee Title
JP4354361B2 (ja) * 2004-07-26 2009-10-28 株式会社堀場製作所 粒径分布測定装置
JP2014215041A (ja) * 2013-04-22 2014-11-17 株式会社堀場製作所 粒子計数装置およびその製造方法
JP6539023B2 (ja) * 2014-07-18 2019-07-03 株式会社堀場製作所 粒子分析装置

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002513151A (ja) * 1998-04-29 2002-05-08 パーティクル、メジュアリング、システムズ、インコーポレーテッド 化学機械的平坦化（ｃｍｐ）スラリーの品質管理プロセスおよび粒子サイズ分布測定システム
US6122956A (en) * 1998-09-09 2000-09-26 University Of Florida Method and apparatus for monitoring concentration of a slurry flowing in a pipeline
JP2002527740A (ja) * 1998-10-15 2002-08-27 パーティクル サイジング システムズ インコーポレイテッド 高分解能粒度分析を行うための自動希釈システム
JP2002022644A (ja) * 2000-07-10 2002-01-23 Horiba Ltd 工程管理用の粒径分布測定システム
JP2004537737A (ja) * 2001-08-09 2004-12-16 コモンウェルス　サイエンティフィック　アンド　インダストリアル　リサーチ　オーガニゼーション 流体中の異物の検出方法及び検出装置
JP2005512042A (ja) * 2001-12-03 2005-04-28 ボード・オブ・リージエンツ，ザ・ユニバーシテイ・オブ・テキサス・システム 粒子インピーダンスセンサ
JP2004053431A (ja) * 2002-07-22 2004-02-19 Horiba Ltd 粒径分布測定方法、粒径分布測定装置および粒径分布測定装置の測定プログラム
JP2006064623A (ja) * 2004-08-30 2006-03-09 Horiba Ltd 粒子径分布測定装置

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JPWO2023140245A1 (https=) 2023-07-27
CN118647850A (zh) 2024-09-13
US20250137902A1 (en) 2025-05-01
TW202334633A (zh) 2023-09-01

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