Dilution device and particle size measurement system using same

The dilution device with multiple stages and automated control addresses the challenge of achieving high accuracy and reproducibility in particle size measurements by enabling precise, high-ratio dilution, particularly for semiconductor polishing slurries.

WO2026094893A1PCT designated stage Publication Date: 2026-05-07NISHIMURA CHEMITECH CO LTD
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Patent Information

Authority / Receiving Office
WO · WO
Patent Type
Applications
Current Assignee / Owner
NISHIMURA CHEMITECH CO LTD
Filing Date
2025-10-28
Publication Date
2026-05-07

AI Technical Summary

Technical Problem

Existing particle size measurement systems face challenges in achieving high accuracy and reproducibility, particularly for highly viscous liquids and polishing slurries used in semiconductor production, requiring extremely high dilution ratios that are difficult to achieve with existing dilution devices.

Method used

A dilution device with multiple stages of dilution, utilizing syringe pumps and in-line mixing, and equipped with ultrasonic or thermal flow meters, allowing precise control and automation of dilution processes to achieve extremely high dilution ratios with minimal manual effort.

Benefits of technology

Enables reproducible dilution at extremely high ratios, reducing the need for large volumes of diluent and minimizing user effort, while maintaining precision in particle size measurements, especially for semiconductor polishing slurries.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention provides a dilution device capable of simply diluting a measurement sample at an extremely high magnification. A dilution device (100) according to the present invention is provided with: a first container (11) configured so as to be capable of receiving liquids from a stock solution supply source (20) and a first supply source (31) of a dilution medium to obtain a first diluted solution and transporting the first diluted solution; and a second container (12) capable of receiving the first diluted solution from the first container (11) and a liquid from a second supply source (32) of a dilution medium to obtain a second diluted solution. The stock solution supply source (20) is configured so as to be capable of quantitatively supplying a raw material in the range of 1 ml to 100 ml.
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Description

Dilution device and particle size measurement system using the same

[0001] The present invention relates to a dilution device and a particle size measurement system using the same, particularly a dilution device for diluting a sample to a measurable state for measuring the particle size in a liquid and a particle size measurement system using the same.

[0002] Generally, when confirming the properties, quality, etc. of a powder product, particularly a slurry product in which powder is dispersed in a liquid, during the development or production of the powder product, physical quantities related to sample particles such as the particle size distribution of the powder, particularly the slurry, are measured. For example, in the measurement of particle size distribution, a laser scattering / diffraction method or the like is used.

[0003] In the laser scattering / diffraction method, parallel light such as laser light is irradiated onto sample particles, and the particle size distribution is calculated by measuring and analyzing the pattern of the light diffracted and scattered by the sample particles.

[0004] In such a particle size measurement device of this type, it is common to dilute the dispersion containing sample particles for measurement.

[0005] Patent Document 1 discloses a particle size measurement system including such a dilution device.

[0006] Japanese Patent Application Laid-Open No. 2018-004537

[0007] In recent years, the miniaturization of semiconductors has advanced to an extreme level, and there is a need to control the quality of polishing slurries for semiconductors containing abrasive particles with extremely high precision. Specifically, it is necessary to manage even the number of abrasive particles at the nanolevel contained in the polishing slurry. This is extremely important particularly for the quality control of the slurry during the production of the polishing slurry.

[0008] Therefore, an extremely high level is also required for the accuracy of particle size measurement, and it is necessary to perform the dilution of the polishing slurry at an extremely high dilution ratio with high reproducibility.

[0009] Furthermore, when the liquid containing particles has a very high viscosity, or when performing particle size measurement using the Single Particle Optical Sensing (SPOS) method or the laser scattering / diffraction method, it is necessary to dilute the liquid to an extremely high dilution ratio before performing particle size measurement.

[0010] Therefore, the present invention aims to provide a dilution device that can easily and reproducibly dilute a measurement sample at an extremely high dilution ratio, and a particle size measurement system using the same.

[0011] The inventors have found that the above problems can be solved by the present invention, which includes the following embodiments.

[0012] In one embodiment, the dilution apparatus of the present invention comprises a first container capable of receiving liquid from a stock solution supply source and a first supply source of dilution medium to obtain a first dilution and being capable of transporting the first dilution, and a second container capable of receiving the first dilution from the first container and liquid from a second supply source of dilution medium to obtain a second dilution, wherein the stock solution supply source is configured to supply raw materials in a fixed amount in the range of 1 ml to 100 ml.

[0013] According to the dilution apparatus of the present invention, since it is configured to supply raw materials in a quantitative manner, the dilution of the measurement sample can be easily performed at an extremely high dilution ratio with good reproducibility.

[0014] In one embodiment, the dilution apparatus of the present invention is configured such that the stock solution supply source transports the stock solution by a syringe pump.

[0015] In the dilution apparatus of the present invention, transporting the stock solution using a syringe pump makes it possible to accurately measure and use minute amounts of the stock solution, which is extremely advantageous because it allows for quantitative transport of the stock solution with high reproducibility.

[0016] In one embodiment, the dilution apparatus of the present invention has the first and second sources of the dilution medium connected to the same source.

[0017] In the dilution apparatus of the present invention, supplying the dilution medium from the same source is advantageous because it allows for a simpler configuration of the apparatus.

[0018] In one embodiment, the dilution apparatus of the present invention is configured to allow in-line mixing of the first diluent and the dilution medium from the second supply source.

[0019] When the dilution apparatus of the present invention is configured in this manner, it is preferable because dilution with the dilution medium becomes very easy.

[0020] In one embodiment, the dilution apparatus of the present invention is equipped with an ultrasonic flow meter or a thermal flow meter between the first container and the second container.

[0021] This configuration of the dilution apparatus of the present invention is preferable because it allows for the measurement of extremely small amounts without the need for a syringe pump.

[0022] In one embodiment, the dilution apparatus of the present invention is configured such that the first container and the second container can be washed with the dilution medium.

[0023] When the dilution apparatus of the present invention is configured in this way, it becomes possible to clean the dilution apparatus fully automatically, which is preferable because it significantly reduces the effort required for the user.

[0024] In one embodiment, the dilution apparatus of the present invention further comprises a third container, wherein the second container is configured to transport the second diluent and to receive the second diluent from the second container and the liquid from a third source of dilution medium.

[0025] According to the dilution apparatus of this embodiment, the stock solution can be diluted in at least three stages, making it possible to reproducibly dilute the stock solution at extremely high ratios, such as 1 million times. Furthermore, when diluting polishing slurries for semiconductors, it is necessary to use ultrapure water costing several hundred yen per liter as the diluent, and even diluting 1 ml of polishing slurry 100,000 to 1 million times incurs high costs. However, with such a multi-stage dilution apparatus, even when diluting 1 ml of polishing slurry 1 million times, only about 1 liter of diluent is required, which is extremely advantageous.

[0026] In one embodiment, the dilution apparatus of the present invention has a first supply source, a second supply source, and a third supply source of the dilution medium connected to the same supply source.

[0027] In the dilution apparatus of the present invention, supplying the dilution medium from the same source is advantageous because it allows for a simpler configuration of the apparatus.

[0028] In one embodiment, the dilution apparatus of the present invention is configured such that the third container is capable of receiving the first dilution from the first container.

[0029] When the dilution apparatus of the present invention is configured in this way, it is advantageous because, when diluting at a dilution ratio of about 10,000 times, dilution can be performed without using the second container.

[0030] In one embodiment, the dilution apparatus of the present invention is configured to allow in-line mixing of the second diluent and the dilution medium from the third supply source.

[0031] When the dilution apparatus of the present invention is configured in this manner, it is preferable because dilution with the dilution medium becomes very easy.

[0032] In one embodiment, the dilution apparatus of the present invention is equipped with an ultrasonic flow meter or a thermal flow meter between the second container and the third container.

[0033] This configuration of the dilution apparatus of the present invention is preferable because it allows for the measurement of extremely small amounts without the need for a syringe pump.

[0034] In one embodiment, the dilution apparatus of the present invention is configured such that the third container can be washed with the dilution medium.

[0035] When the dilution apparatus of the present invention is configured in this way, it becomes possible to clean the dilution apparatus fully automatically, which is preferable because it significantly reduces the effort required for the user.

[0036] In one embodiment, the particle size measurement system of the present invention comprises the above-described dilution device and particle size measurement device, and is configured to be able to transport a second dilution from the second container to the particle size measurement device, or to be able to transport a third dilution from the third container to the particle size measurement device.

[0037] In one embodiment, the particle size measurement system of the present invention is such that the particle size measurement device is a SPOS type or a laser scattering / diffraction type particle size measurement device.

[0038] Particle size measurement systems are highly advantageous when used in combination with dilution devices as described above. In particular, SPOS or laser scattering / diffraction type particle size measurement devices are especially advantageous when used in combination with such dilution devices, as it is important to measure at the same concentration for comparison with other measurement results.

[0039] In one embodiment, the method for producing a slurry of the present invention includes diluting the slurry using the dilution device and measuring the particle size using the particle size measuring device.

[0040] In one embodiment, the method for polishing a substrate according to the present invention includes sampling a polishing slurry used in a polishing apparatus, diluting the polishing slurry using the dilution apparatus, and measuring the particle size using the particle size measuring apparatus.

[0041] According to the present invention, it is possible to provide a dilution device that can easily dilute a measurement sample at an extremely high dilution ratio, and a particle size measurement system using the same.

[0042] FIG. 1 schematically shows the particle size measurement system device according to the first embodiment of the present invention. FIG. 2 schematically shows the particle size measurement system device according to the second embodiment of the present invention. FIG. 3 schematically shows the particle size measurement system device according to the third embodiment of the present invention.

[0043] The present invention will be specifically described below by taking the following embodiments as examples, but the present invention is not limited thereto. When there is no particularly detailed reference to each device, mechanism, means, etc. in this specification, those skilled in the art can use well-known mechanical devices, mechanisms, means, etc. for these. Each embodiment can be combined based on the ordinary knowledge of those skilled in the art, and for the configurations not specifically described in each embodiment, they can have the same configuration as other embodiments or a configuration suitable for that embodiment. In addition, the configurations not particularly mentioned in the drawings can be understood by those skilled in the art based on ordinary knowledge.

[0044] FIG. 1 schematically shows the particle size measurement system according to the first embodiment of the present invention.

[0045] The particle size measurement system of the present invention consists of a dilution device 100 and a particle size measurement device 200. Various devices, valves, pumps, regulators, flow meters, etc. are connected to a control device (PLC) so that the dilution device 100 can be fully automatically controlled.

[0046] This dilution device 100 has an upstream source 20 of the stock solution (Chemical) and a source 30 of deionized water (DIW) as the dilution medium, and also has a gas source 60 of air or nitrogen. Further, this dilution device 100 has a waste liquid line 70 downstream.

[0047] This dilution device 100 can receive the liquid from the stock solution supply source 20 (first supply line 41a) and the first supply line 31 of the dilution medium to obtain a first diluted solution so as to be able to perform dilution in three stages, and has a first container 11 to which a first transport line 41b for the first diluted solution is connected. It can receive the liquid from the transport line 41b (second supply line 42a) for the first diluted solution and the second supply line 32 of the dilution medium to obtain a second diluted solution, and has a second container 12 to which a second transport line 42b for the second diluted solution is connected. And it has a third container 13 configured to be able to receive the liquid from the second transport line 42b (third supply line 43a) for the second diluted solution and the third supply line 33 of the dilution medium.

[0048] This dilution device 100 can dilute, for example, a stock solution by 10 times, 50 times, 100 times, 1000 times, 10,000 times, 100,000 times, or 500,000 times or more in terms of volume ratio, and may be diluted to 5,000,000 times or less, 3,000,000 times or less, 1,000,000 times or less, 500,000 times or less, or 100,000 times or less.

[0049] The capacity of each of the first container 11 to the third container 13 may be, for example, 10 liters or less, 5 liters or less, 3 liters or less, or 2 liters or less. These containers can be equipped with stirrers, measuring instruments, etc. respectively.

[0050] By using a syringe pump as the first supply means 51, the stock solution supply source 20 can supply the stock solution to the first container 11 through the first supply line 41a. By using a syringe pump, the stock solution can be supplied to the first container 11 in the range of 1 ml to 50 ml, particularly in the range of 1 ml to 10 ml. Since the stock solution is sent in such a very small amount, the first supply line 41a can be in the form of a small-diameter tube, and by connecting a gas supply source 60, the stock solution can be pressure-fed with gas.

[0051] In this embodiment, the first supply line 31 of the dilution medium is connected to the first supply line 41a of the stock solution, and the dilution medium is also sent to the first container 11 through the first supply line 41a, but the first supply line 31 of the dilution medium may be directly connected to the first container 11.

[0052] The stock solution and diluent mixed in the first container 11 are sent to the second container 12 as the first diluent via the first transport line 41b for the first diluent. The first diluent is also diluted at a high ratio with the diluent in the second container 12, so the amount of diluent sent via the first transport line 41b is preferably in the range of 1 ml to 50 ml, particularly 1 ml to 10 ml. To transport such a small amount of diluent, this embodiment may include a flow meter as a second supply means 52 for supplying the first diluent to the second container 12. An ultrasonic flow meter or a thermal flow meter can be used for this purpose. These types of flow meters allow for accurate measurement of minute amounts of liquid.

[0053] Furthermore, the first diluent can be pumped from the first container 11 to the first transport line 41b by supplying gas from the gas supply source 60 to the first container 11, thereby increasing the internal pressure of the first container 11.

[0054] In the embodiment shown in Figure 1, the first diluent from the first transport line 41b can be mixed with the diluent medium in the second supply line 32 and the first in-line mixer 52a. The first diluent and the diluent medium are then transported from the first transport line 41b from the first container 11 to the second container 12 via the second supply line 42a. Naturally, the first diluent and the diluent medium can be transported to the second container 11 via separate lines. In this embodiment, the first supply line 31 and the second supply line 32 for the diluent medium are connected to the same supply source 30 and supplied from the same supply source 30, but the diluent medium may be supplied from separate supply sources, and the diluent medium may be a different type of liquid.

[0055] Furthermore, in this embodiment, the first transport line 41b from the first container 11 is connected not only to the second supply line 42a to the second container 12, but also to a bridge supply line 45 for direct supply to the third container 13. This allows the third container 13 to directly receive the first diluent prepared in the first container 11. In addition, in this embodiment, since the bridge supply line 45 is also connected to the second supply line 32 for the diluent medium, the third container 13 is also configured to directly receive the diluent medium from the second supply line 32 for the diluent medium. Moreover, the third container 13 can receive the mixture from the bridge supply line 45 after the first diluent and the second supply line 32 for the diluent medium have been mixed in the first in-line mixer 52a.

[0056] Each component of the second container 12 is the same as each component 11 of the first container 11. That is, the first diluent and diluent medium received from the second supply line 42a can be transported to the third container 13 via the second transport line 42b. Here, in the second transport line 42b, it is preferable to precisely control the flow rate using a flow meter of the third supply means 53 in order to transport a small amount of the second diluent, and an ultrasonic flow meter or a thermal flow meter can be used as the flow meter for this purpose.

[0057] The second diluent can be pumped from the second container 12 to the second transport line 42b by supplying gas from the gas supply source 60 to the second container 12, thereby increasing the internal pressure of the second container 12.

[0058] The second diluent from the second transport line 42b can be mixed with the diluent medium in the second in-line mixer 53a and the third supply line 33 for the diluent medium. The second diluent and the diluent medium are then transported from the second transport line 42b from the second container 12 to the third container 13 via the third supply line 43a. Naturally, the second diluent and the diluent medium can be transported to the third container 13 via separate lines. In this embodiment, the first supply line 31 and the second supply line 32 for the diluent medium and the third supply line 33 are connected to the same supply source 30 and supplied from the same supply source 30, but the diluent medium may be supplied from separate supply sources, and the diluent medium may be a different type of liquid.

[0059] In the third container 13, the third diluent is prepared and ready for transport to the particle size analyzer 200. Here as well, by supplying gas from the gas supply source 60 to the third transport line 43b from the third container 13, the internal pressure of the third container 13 is increased, thereby pressurizing the transport of the third diluent to the third transport line 43b. The particle size analyzer 200 may also have a configuration that draws the third diluent from the third container 13.

[0060] The particle size analyzer 200 can be a commercially available liquid particle counter type particle size analyzer, such as a SPOS type, light shielding type, or laser scattering / diffraction type particle size analyzer. This commercially available particle size analyzer may also have a dilution device, and the third container 13 may be the container of the commercially available particle size analyzer. Examples of commercially available SPOS type particle size analyzers include AccuSizer (trademark, Nippon Integris LLC). Since such particle size analyzers may require dilution at extremely high ratios, it is useful to combine them with the dilution device described above.

[0061] Each line is ultimately connected to the waste liquid line 70 as appropriate, as shown in the diagram, and can be washed using a diluent. The liquid measured by the particle size analyzer 200 can be entirely disposed of in the waste liquid line 70.

[0062] Although not shown in the diagram, the dilution device 100 may also be equipped with containers and supply lines for supplying additives such as an antifoaming agent to remove foam generated in the container, or a contrast agent to facilitate particle size measurement with a particle size analyzer. Since such additives are used in very small quantities, they can be supplied by a syringe pump or by pressurized gas after highly controlled flow rate using an ultrasonic flow meter or thermal flow meter.

[0063] Such particle size measurement systems can be used in the production of slurries containing particles and are particularly useful for controlling the quality of slurries with extremely high precision. Examples of such slurries include polishing slurries for semiconductors, inks for inkjet printing, slurries for fuel cells, drinking water, and pharmaceuticals.

[0064] In other words, the present invention may be a method for manufacturing a slurry, and this method includes the steps of preparing a slurry and diluting the slurry using such a dilution device and measuring the particle size using a particle size measuring device such as a SPOS system. The present invention may also be a particle size measuring system for use in the manufacture of a slurry (particularly a polishing slurry for semiconductors), and this particle size measuring system may comprise such a dilution device and a particle size measuring device (particularly a SPOS system particle size measuring device). In this embodiment, the particle size measuring system is not incorporated into a polishing device.

[0065] On the other hand, in other embodiments, such a particle size measuring system may be incorporated into a polishing apparatus. In this case, the particle size measuring system samples the polishing slurry used in the polishing apparatus and dilutes the polishing slurry using such a dilution device. In this case, the polishing slurry diluted in such a dilution device can be of the same concentration as the polishing slurry used in the polishing apparatus. That is, the present invention may also be a method for polishing a substrate, and may include the steps of sampling the polishing slurry used in the polishing apparatus, diluting the sampled polishing slurry using such a dilution device, and measuring the particle size using such a particle size measuring device.

[0066] For example, the present invention may be a polishing system, which may comprise a source of polishing slurry, a polishing apparatus that performs polishing using the slurry supplied from the source, a dilution apparatus as described above for diluting the slurry supplied from the source, and a particle size measuring apparatus (particularly an SPOS type particle size measuring apparatus) for measuring the particle size of the slurry diluted by the dilution apparatus. Here, the polishing slurry used in the polishing apparatus and the polishing slurry diluted in the dilution apparatus are substantially the same concentration.

[0067] Figure 2 schematically shows a particle size measurement system according to a second embodiment of the present invention. Configurations shown in Figure 2 that are not specifically mentioned in Figure 1 can be understood in the same way as in the first embodiment.

[0068] In this embodiment, the gas supply source 60 shown in the first embodiment is not shown, but the internal pressure can be adjusted as needed to pump the liquid.

[0069] In this embodiment as well, the particle size measurement system consists of a dilution device 100 and a particle size measurement device 200. Here too, various devices, valves, pumps, regulators, flow meters, etc., are connected to a control device not shown in the drawings, allowing the particle size measurement system to be controlled automatically.

[0070] This dilution device 100 has a stock solution supply source 20 and a dilution medium supply source 30 upstream. Furthermore, this dilution device 100 has a waste liquid line 70 downstream, and the waste liquid line 70 is directly connected from the bottom of each of the first containers 11 to the third containers 13, so that each container can be easily cleaned with the dilution medium.

[0071] This dilution device 100 also has a first container 11 which is configured to receive liquid from the stock solution supply source 20 (first supply line 41a) and the first supply line 31 of the dilution medium and is connected to the first transport line 41b for the first dilution, a second container 12 which is configured to receive liquid from the transport line 41b for the first dilution (second supply line 42a) and the second supply line 32 of the dilution medium and is connected to the second transport line 42b for the second dilution, and a third container 13 which is configured to receive liquid from the second transport line 42b for the second dilution (third supply line 43a) and the third supply line 33 of the dilution medium.

[0072] In this embodiment as well, the stock solution supply source 20 can supply the stock solution to the first container 11 through the first supply line 41a by using a syringe pump, which is the first supply means 51. The diluent supply source 30 is also connected to the syringe pump that transports the stock solution through the first washing line 30a, thereby allowing the syringe pump to be washed. In addition, in this embodiment, the diluent can be supplied directly to the first container 11 from the first supply line 31 for the diluent.

[0073] The stock solution and diluent mixed in the first container 11 are sent as the first diluent to the second container 12 via the first transport line 41b for the first diluent. The first transport line 41b is connected to the bottom of the first container 11 and can be discharged into the waste liquid line 70. The first transport line 41b for the first diluent can supply a small amount of the diluent to the second supply line 42a to the second container 12 via the second supply means 52, which is a syringe pump. Here again, the supply source 30 for the diluent is also connected to the second supply means 52 (syringe pump) that transports the first diluent via the second washing line 30b, thereby allowing the second supply means 52 (syringe pump) to be washed.

[0074] In this embodiment as well, the first transport line 41b from the first container 11 is connected not only to the second supply line 42a to the second container 12, but also to a bridge supply line 45 for direct supply to the third container 13. This allows the third container 13 to directly receive the first diluent prepared in the first container 11. In this embodiment, a liquid transfer pump, which is a bridge supply means 55, is connected to the bridge supply line 45, thereby enabling the first diluent to be pumped into the third container 13.

[0075] In the second container 12, the first diluent received from the second supply line 42a and the diluent medium from the second supply line 32 are mixed to prepare the second diluent, which can then be transported to the third container 13 via the second transport line 42b. Here again, the second transport line 42b is connected to the bottom of the second container 12, allowing the waste liquid after washing the second container 12 with the diluent medium to be discharged into the waste liquid line 70.

[0076] In this embodiment, a liquid delivery pump, which is a third supply means 53, is connected to the second transport line 42b of the diluent, so that the second diluent can be pressurized and delivered to the third container 13. Alternatively, the diluent may be delivered to the third container from the second transport line 42b using a syringe pump, or the diluent may be pressurized and delivered using an ultrasonic flow meter or a thermal flow meter, pressurized gas, a pump, etc.

[0077] Figure 3 schematically shows a particle size measurement system according to a third embodiment of the present invention. Configurations shown in Figure 3 that are not specifically mentioned in Figures 1 and 2 can be understood in the same way as in the first and second embodiments.

[0078] In this embodiment as well, the gas supply source 60 shown in the first embodiment is not shown, but the internal pressure can be adjusted as needed to pump the liquid. Here too, various devices, valves, pumps, regulators, flow meters, etc. are connected to a control device not shown in the drawings, so that the particle size measurement system can be controlled automatically.

[0079] This dilution device 100 has first containers 11 to fourth containers 14, and is capable of four-stage dilution. This dilution device 100 has a first container 11 which is configured to receive liquid from a stock supply source 20 (and first supply line 41a) and a first supply line 31 of the dilution medium, and to which a first transport line 41b for the first dilution is connected; a second container 12 which is configured to receive liquid from a transport line 41b (and second supply line 42a) for the first dilution and a second supply line 32 of the dilution medium, and to which a second transport line 42b for the second dilution is connected; a third container 13 which is configured to receive liquid from a second transport line 42b (and third supply line 43a) for the second dilution and a third supply line 33 of the dilution medium; and a fourth container 14 which is configured to receive liquid from a third transport line 43b for the third dilution and a fourth supply line 34 of the dilution medium.

[0080] In this embodiment, a syringe pump is used not only as the first supply means 51 for transporting the stock solution, but also as the second supply means 52 for transporting the first diluent from the first container 11 to the second container 12. Furthermore, a syringe pump is also used as the third supply means 53 for transporting the second diluent from the second container 12 to the third container 13.

[0081] Furthermore, this dilution device 100 has a waste liquid line 70 downstream, and each of the first container 11 to the fourth container 14 is directly connected to the waste liquid line 70 from the bottom, so that each container can be easily cleaned with the dilution medium.

[0082] In this embodiment as well, the stock solution and diluent mixed in the first container 11 are sent to the second container 12 as the first diluent via the first transport line 41b for the first diluent. The first transport line 41b for the first diluent can supply a small amount of the diluent to the second supply line 42a to the second container 12 via a syringe pump, which is the second supply means 52. Here again, the supply source 30 for the diluent is also connected to the second supply means 52 that transports the first diluent via the second washing line 30b, thereby allowing the second supply means 52 to be washed.

[0083] Furthermore, the second diluent mixed in the second container 12 is sent to the third container 13 via the second transport line 42b for the second diluent. The second transport line 42b for the second diluent can supply a small amount of the diluent to the third supply line 43a to the third container 13 via the third supply means 53, which is a syringe pump. Here again, the diluent medium supply source 30 is also connected to the third supply means 53 that transports the second diluent via the third washing line 30c, thereby allowing the third supply means 53 to be washed.

[0084] The first container 11 is connected not only to the second supply line 42a to the second container 12, but also to a bridge supply line 45 for direct supply to the final fourth container 14. This allows the fourth container 14 to directly receive the first diluent prepared in the first container 11. In this embodiment, a liquid transfer pump, which is a bridge supply means 55, is connected to the bridge supply line 45, enabling the first diluent to be pumped into the fourth container 14.

[0085] Furthermore, the second container 12 is connected not only to the third supply line 43a to the third container 13, but also to the second bridge supply line 46 for direct supply to the final fourth container 14. This allows the fourth container 14 to directly receive the second diluent prepared in the second container 12. In this embodiment, a liquid transfer pump, which is the second bridge supply means 56, is connected to the second bridge supply line 46, thereby enabling the second diluent to be pumped into the fourth container 14.

[0086] Transport from the third container 13 to the fourth container 14 can be controlled using a flow meter from the bottom of the third container 13 and carried out via the third transport line 43b. Transport from the fourth container 14 to the particle size measuring device 200 can be carried out via the fourth transport line 44b.

[0087] 11...First container 12...Second container 13...Third container 14...Fourth container 20...Concentrate supply source 30...Dilution medium supply source 31...First supply source of dilution medium 32...Second supply source of dilution medium 33...Third supply source of dilution medium 41a...First supply line 41b...First transport line 42a...Second supply line 42b...Second transport line 43a...Third supply line 43b...Third transport line 45...Bridge line 51...First supply means 52...Second supply means 52a...First inline mixer 53...Third supply means 53a...Second inline mixer 60...Gas supply source 70...Waste liquid line 100...Dilution device 200...Particle size measuring device

Claims

1. A dilution apparatus comprising a first container capable of receiving liquid from a stock solution supply source and a first supply source of diluent medium to obtain a first dilution, and being configured to transport the first dilution, and a second container capable of receiving the first dilution from the first container and liquid from a second supply source of diluent medium to obtain a second dilution, wherein the stock solution supply source is configured to supply raw materials in a fixed quantity within the range of 1 ml to 100 ml.

2. The dilution apparatus according to claim 1, wherein the stock solution supply source is configured to transport the stock solution by a syringe pump.

3. The dilution apparatus according to claim 2, wherein the first and second sources of the dilution medium are connected to the same source.

4. The dilution apparatus according to claim 1, wherein the first diluent and the dilution medium from the second supply source are configured to be mixed in line.

5. The dilution apparatus according to claim 1, further comprising an ultrasonic flow meter or a thermal flow meter between the first container and the second container.

6. The dilution apparatus according to claim 1, wherein the first container and the second container are configured to be washable with the dilution medium.

7. The dilution apparatus according to claim 1, further comprising a third container configured to transport the second diluent from the second container and to receive the second diluent from a third source of dilution medium.

8. The dilution apparatus according to claim 7, wherein the third container is configured to receive the first dilution from the first container.

9. The dilution apparatus according to claim 7, wherein the first, second, and third sources of the dilution medium are connected to the same source.

10. A particle size measuring system comprising a dilution device and a particle size measuring device according to any one of claims 1 to 6, wherein the second dilution can be transported from the second container to the particle size measuring device.

11. The particle size measurement system according to claim 8, wherein the particle size measurement device is a laser scattering / diffraction type particle size measurement device.

Citation Information

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