KR100962541B1 - Method of calibration of particle counter - Google Patents
Method of calibration of particle counter Download PDFInfo
- Publication number
- KR100962541B1 KR100962541B1 KR1020100036594A KR20100036594A KR100962541B1 KR 100962541 B1 KR100962541 B1 KR 100962541B1 KR 1020100036594 A KR1020100036594 A KR 1020100036594A KR 20100036594 A KR20100036594 A KR 20100036594A KR 100962541 B1 KR100962541 B1 KR 100962541B1
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- KR
- South Korea
- Prior art keywords
- standard
- measuring
- particle
- reference voltage
- calibration
- Prior art date
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Classifications
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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
- G01N15/10—Investigating individual particles
- G01N15/14—Electro-optical investigation, e.g. flow cytometers
-
- 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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/15—Preventing contamination of the components of the optical system or obstruction of the light path
-
- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/27—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands using photo-electric detection ; circuits for computing concentration
-
- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/27—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands using photo-electric detection ; circuits for computing concentration
- G01N21/272—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands using photo-electric detection ; circuits for computing concentration for following a reaction, e.g. for determining photometrically a reaction rate (photometric cinetic analysis)
-
- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/47—Scattering, i.e. diffuse reflection
- G01N21/49—Scattering, i.e. diffuse reflection within a body or fluid
- G01N21/53—Scattering, i.e. diffuse reflection within a body or fluid within a flowing fluid, e.g. smoke
Abstract
Description
The present invention relates to a method for calibrating in-water fine particles, and more particularly, to a method for calibrating in-water fine particles, which can increase the homogeneity and reliability of the device.
In the semiconductor manufacturing process, many processes such as washing a silicon wafer or performing various processes such as deposition and etching on a silicon wafer are repeated. Such a semiconductor manufacturing process requires a large amount of ultrapure water for cleaning or chemical liquids used in the semiconductor process.
Ultrapure water or chemical liquids used in semiconductor manufacturing processes are highly likely to cause defects in semiconductor chips if they contain foreign substances therein. Therefore, the number of foreign matter contained in ultrapure water or chemical liquid should be adjusted to below a certain value. In order to control the number of foreign matter contained in the ultrapure water or the chemical liquid, it is necessary to accurately detect the fine particles contained in the liquid.
To detect the number of foreign matter contained in the ultrapure water or chemical liquid, ultrapure water or chemical liquid is passed through the transparent measuring cell, and irradiated with light using a light source such as a laser or a light emitting device (LED), Alternatively, there is a method of calculating the size or number of foreign matters by measuring light scattered by foreign matters in ultrapure water or chemical liquid.
The particulate matter detector in water generally includes a transparent measuring cell, a light irradiation part and a light detection part. Such a microparticle measuring device is a very precise device, the error may occur with use. For example, the optical axis between the light irradiation unit or the light detection unit and the measurement cell is changed, or a variation occurs in the output of the light irradiation unit, so that a measurement error may be generated in the liquid fine particle measuring instrument. Therefore, the submerged particulate measuring device needs to be checked regularly or irregularly, and the measuring device needs to be replaced or calibrated according to the inspection result.
In general, the method of checking the submerged particle measuring device is to inject a liquid containing standard particles into the measuring cell, and connect the standard device in series with the submerged particle measuring device to compare the value measured by the standard measuring device with the submerged particle measuring device. By doing so, it is possible to determine whether or not there is an abnormality in the liquid particle measuring instrument.
However, the conventional inspection method using only the standard machine can detect only the presence or absence of the roughness of the fine particle measuring device in the liquid, and there is a problem that some of the internal modules of the fine particle measuring device need to be replaced.
Accordingly, there is a need for a method for more precisely detecting the presence or absence of an abnormality in the liquid particulate measuring instrument and a method capable of precisely calibrating the liquid particulate measuring instrument in accordance with the abnormality.
The technical problem to be achieved by the present invention is to provide a calibration method of the particulate matter measuring instrument that can accurately calibrate the particulate matter measuring instrument, which can increase the homogeneity and reliability of the device.
Technical problems of the present invention are not limited to the technical problems mentioned above, and other technical problems not mentioned will be clearly understood by those skilled in the art from the following description.
In the calibration method of the submerged particle measuring apparatus according to an embodiment of the present invention for achieving the above technical problem, a measuring cell that passes through the sample liquid therein and transmits at least a part of the light, the light irradiation unit for irradiating light to the measuring cell And preparing a fine particle measuring device including a light detector detecting the light, and cleaning the inside of the measuring cell.
Connecting a standard group capable of detecting particulates in the liquid in series with the particulate matter meter, and performing a first efficiency test comparing the measured values of the standard and the particulate matter analyzer with each other, and a plurality of first standard particles in the measurement cell Injecting a sample solution containing a, measuring each voltage value representing the shape and size of each of the first standard particles through the light detection unit, the cumulative value of the number of each of the first standard particles having each voltage value And calculating a reference point for setting a voltage value corresponding to the maximum value among the accumulated values as a reference voltage.
The calibration method of the submerged particle detector according to the present invention has the following effects in detecting and correcting the abnormality of the submerged particle detector.
First, it is possible to pinpoint the cause of the error that occurs in the liquid particle detector.
Second, depending on the situation, even if the module itself of the submerged particle detector can be corrected more precisely, it is possible to calibrate the submerged particle meter while minimizing time and cost.
1 is a schematic block diagram of an apparatus for measuring particulate matter in liquid.
2 is a flow chart for explaining a calibration method of the particulate matter measuring instrument according to an embodiment of the present invention.
3 to 5 are device configuration diagrams for explaining a calibration method of the liquid particulate matter measuring apparatus according to an embodiment of the present invention.
Figure 6 is a graph of the cumulative number with respect to the voltage value of the standard particles measured in the step of setting the calibration reference point in the method for measuring the fine particles in the liquid according to an embodiment of the present invention.
7 is a graph in which the graph of FIG. 6 is corrected.
Advantages and features of the present invention and methods for achieving them will be apparent with reference to the embodiments described below in detail with the accompanying drawings. However, the present invention is not limited to the embodiments disclosed below, but can be implemented in various different forms, and only the embodiments make the disclosure of the present invention complete, and the general knowledge in the art to which the present invention belongs. It is provided to fully inform the person having the scope of the invention, which is defined only by the scope of the claims. Like reference numerals refer to like elements throughout.
Hereinafter, with reference to Figure 1 will be described in detail with respect to the particulate matter measuring instrument.
The submerged
The submerged
The
The
The
The
The
Hereinafter, a method of calibrating a submerged particle detector according to an embodiment of the present invention will be described in detail with reference to FIGS. 2 to 5. 2 is a flow chart for explaining a calibration method of the particulate matter measuring instrument according to an embodiment of the present invention, Figures 3 to 5 is a device configuration for explaining a calibration method of the particulate matter measuring instrument according to an embodiment of the present invention It is degrees.
First, referring to FIGS. 2 and 3, the inside of the liquid particle detector is washed (S100). Residues of various chemical liquids remain in the
In order to clean the submerged
In this case, the cleaning liquid may be a liquid that can remove the harmful substances inside the
On the other hand, the
The washing liquid that has passed through the
Next, referring to FIGS. 2 and 4, the standard is connected in series to the liquid particulate measuring device and the measured values are compared (S200). A standard device 400 is installed in the inlet pipe P1 between the pressurizer 200 and the
Standard 400 is a device that can measure the size or number of particles in the liquid, it is possible to compare the performance of the liquid
Standard 400 can measure the size and number of particulates in a liquid in substantially the same manner as particulate in
The efficiency comparison using the standard 400 will be described in detail. The ultrapure water is filled in the
When the measured value of the standard device 400 for the ultrapure water is 100 or less, standard particles are injected into the ultrapure water. At this time, the size of the standard particle is injected a size slightly larger than the set value of the standard 400. For example, when the set value of the standard group 400 is 0.1 μm, the standard particles may use 0.294 μm, and when the set value of the standard group 400 is 0.2 μm, the standard particles may use 0.506 μm.
Standard particles are injected into the
At this time, by using the
When the concentration of the dilution liquid is measured by the standard 400 based on 0.2 μm, the dilution concentration is set to be in the range of 5000 to 12000 pieces.
The counting efficiency of the submerged
Counting efficiency = (measured value of measuring instrument / measured value of standard instrument)
If the counting efficiency is in the range of 70 to 110%, the particulate
Next, the laser output and the voltage of the
In order to verify the reliability of the
First, the initial input voltage and output voltage of the
Subsequently, a calibration reference point is set with reference to FIGS. 2, 5, and 6 (S400). Figure 6 is a graph of the cumulative number with respect to the voltage value of the standard particles measured in the step of setting the calibration reference point in the method for measuring the fine particles in the liquid according to an embodiment of the present invention.
The calibration reference point refers to first setting the reference voltage for the reference particle to set the reference voltage for each particle. Here, the calibration particles may be particles having a smallest diameter, but are not limited thereto.
On the other hand, the calibration reference point may be set after verifying the light source of the
For accurate calibration, first clean the inside of the submerged
When the inside of the liquid
When the
After precisely adjusting the flow rate, the concentration of the sample liquid containing the first standard particles is adjusted by diluting the concentration so that 10000 to 12000 can be included in the sample liquid flowing for 1 minute.
The
The
The
The
Referring to FIG. 6, the
If the submerged
On the other hand, as shown in Figure 6, if the cumulative value of the first standard particle for each channel is a complex graph to calculate the maximum value of the cumulative value for each channel is not easy to cut- It is possible to precisely determine a small section by setting the cut off section. For example, in the graph of FIG. 6, an arbitrary maximum peak point P1 is set, and the cumulative number of first standard particles for an arbitrary maximum peak point P1 is obtained, and having a value of 50% of the cumulative number. Set the channel to valid interval. Thereafter, the maximum peak point P1 in the effective section can be precisely found.
Also, the calibration reference point may be set by converting the graph of FIG. 6 into a graph in which a reference voltage can be easily set. For example, as in the graph of FIG. 7, the graph of FIG. 6 may be corrected and converted into a smooth graph connecting each peak point.
Thereafter, the calibration reference point can be precisely set by setting an effective section based on the points C1 and C2 corresponding to 50% of the maximum peak point P2.
In this way, the calibration reference point can be set. At this time, if the measured reference voltage falls within the range shown in Table 1 below, setting of the calibration reference point is completed.
Table 1 below shows the range of recommended reference voltage for each standard particle size.
1100 ± 50
Next, the noise of the particulate matter measuring instrument in liquid is measured (S500).
After setting the reference value for each particle of the submerged
In the cleaning method, as described above, the ultrafine water is injected into the
After the inside of the fine
If an abnormality is found in the measuring
If the measured value is within the range of the reference value, the calibration for each particle diameter is performed (S600).
The calibration reference point is set using a sample liquid containing first standard particles having a predetermined size, and when the calibration reference point is set, a calibration reference point using a sample liquid containing second standard particles having a different size from the first standard particles. The calibration value for the second standard particle can be set based on this. The calibration method may be performed substantially the same as the calibration reference point setting method.
This process may be repeated a plurality of times using standard particles having a different size from the first standard particles.
2 and 4, after the calibration for each particle diameter, the standard is connected in series to the particulate matter measuring instrument in series and the measured values are compared (S700). This efficiency comparison step may be performed in substantially the same manner as the above-described efficiency comparison step. That is, when finally compared to the efficiency range within the desired range, the calibration of the
Although embodiments of the present invention have been described above with reference to the accompanying drawings, those skilled in the art to which the present invention pertains may implement the present invention in other specific forms without changing the technical spirit or essential features thereof. I can understand that. It is therefore to be understood that the above-described embodiments are illustrative in all aspects and not restrictive.
100: liquid particle measuring instrument 110: measuring cell
120: light irradiation unit 130: light detection unit
200: pressurizer 300: flow meter
400: standard 500: mass meter
600: analysis device 610: crest analyzer
620: oscilloscope
Claims (12)
Cleaning the inside of the measurement cell;
Connecting a standard group capable of detecting particulates in liquid in series with the particulate matter meter, and performing a first efficiency test comparing the measured values of the standard and the particulate matter analyzer with each other; And
Injecting a sample solution containing a plurality of first standard particles in the measuring cell,
Measuring each voltage value representing the shape and size of each of the first standard particles through the photodetector;
The cumulative value of the number of each said 1st standard particle which has each said voltage value is calculated | required,
And setting a calibration reference point for setting a voltage value corresponding to a maximum value among the cumulative values as a reference voltage.
And injecting ultrapure water into the measurement cell and measuring noise by measuring a detection value of the photodetector.
And checking the measurement cell when the noise value is greater than or equal to the reference value in the step of measuring the noise.
And injecting a sample liquid including second standard particles having a different size from the first standard particles and setting a calibration value for the second standard particles based on the calibration reference point.
And setting a calibration value for the second standard particle, further comprising a second efficiency test step of connecting the standard group in series with the particulate matter meter and comparing the measured values of the standard and the particulate matter meter with each other. How to calibrate the meter.
And measuring the output change rate of the light irradiation part by measuring an initial input voltage and an output voltage of the light irradiation part after the first efficiency checking.
The reference voltage is a calibration method of a submerged particle measuring instrument having a reference voltage of 90 ~ 110mV or 1050 ~ 1115mV when the diameter of the first standard particle is 0.117㎛.
The reference voltage is a calibration method of the submerged particle measuring instrument having a reference voltage of 100 ~ 110mV, when the diameter of the first standard particle is 0.254㎛.
The reference voltage is a calibration method of a submerged particle measuring instrument having a reference voltage of 140 ~ 160mV, when the diameter of the first standard particle is 0.207㎛.
The reference voltage is a calibration method of the submerged particle measuring device having a reference voltage of 290 ~ 310mV, when the diameter of the first standard particle is 0.791㎛.
The reference voltage is a calibration method of the submerged particle measuring device having a reference voltage of 3000 ~ 3200mV, when the diameter of the first standard particle is 0.352㎛.
The reference voltage is a calibration method of the submerged particle measuring instrument having a reference voltage of 90 ~ 110mV, when the diameter of the first standard particle is 0.123㎛.
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KR1020100013051 | 2010-02-11 | ||
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR20200099588A (en) * | 2018-02-27 | 2020-08-24 | 파나소닉 아이피 매니지먼트 가부시키가이샤 | Particle detection sensor |
KR102390910B1 (en) * | 2021-11-11 | 2022-04-26 | 류준호 | Method and apparatus for calibration of light scattering sensor for measuring fine dust concentration |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS56168532A (en) | 1980-05-30 | 1981-12-24 | Rion Co Ltd | Automatic calibration device for light scattering fine grain meter |
KR960018574A (en) * | 1994-11-10 | 1996-06-17 | 요코야마 아키라 | Method and apparatus for measuring the concentration of insoluble substances in oil |
KR20040080607A (en) * | 2003-03-12 | 2004-09-20 | 김병기 | Tubidity measuring device and its measuring method |
-
2010
- 2010-04-20 KR KR1020100036594A patent/KR100962541B1/en active IP Right Grant
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS56168532A (en) | 1980-05-30 | 1981-12-24 | Rion Co Ltd | Automatic calibration device for light scattering fine grain meter |
KR960018574A (en) * | 1994-11-10 | 1996-06-17 | 요코야마 아키라 | Method and apparatus for measuring the concentration of insoluble substances in oil |
KR20040080607A (en) * | 2003-03-12 | 2004-09-20 | 김병기 | Tubidity measuring device and its measuring method |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR20200099588A (en) * | 2018-02-27 | 2020-08-24 | 파나소닉 아이피 매니지먼트 가부시키가이샤 | Particle detection sensor |
KR102321560B1 (en) | 2018-02-27 | 2021-11-03 | 파나소닉 아이피 매니지먼트 가부시키가이샤 | particle detection sensor |
KR102390910B1 (en) * | 2021-11-11 | 2022-04-26 | 류준호 | Method and apparatus for calibration of light scattering sensor for measuring fine dust concentration |
KR102470182B1 (en) * | 2021-11-11 | 2022-11-25 | (주)랩코 | Operation method of air particle detector |
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