TW202018273A - The particles identification counting method and analysis device - Google Patents

Abstract

The present invention relates the particles identification counting method and analysis device. The optical difference between switching back-light source and front-light source to illuminate the test specimen can strengthen the counting and identification between the glassy and non-glassy particles, even black particles in non-glassy particles. Microscopic imaging unit is placed right above the test specimen to record the observed results. When the test specimen is illuminated by the upward back-light source, each of particles is observed as image with a grain profile. The observed number of imaging particles is the total number of all particles. When the test specimen is illuminated by the multi-angle front-light source, different kinds of particles presented different observed results under monochromatic background. The glassy particles almost disappeared because of their diaphaneity. The non-glassy particles excluding the black particles brightened when reflecting the light, but the black particles remained black because of their non-reflection. The observed number of bright particles is the total number of non-glassy particles excluding black particles, and the observed number of black ones on a non-black background is the total number of black particles. The sum of these two is the total number of non-glassy particles. The total number of all particles minus the total number of non-glassy particles is equal to the total number of glassy particles.

Description

Particle identification counting method and analysis device

The technical content of the present invention relates to a method and a device for particle identification, in particular to a method for identifying and counting vitreous particles and non-glassy particles and an analysis device. The test object is appropriately sampled to prepare a sample test piece with uniformly dispersed particles and placed On the stage, the counting particles are identified by microscopic observation.

The current more advanced particle identification and counting method is to observe and identify with a microscope camera and supplement with image analysis software to perform counting. Generally, a polarizing microscope is often used to identify particles. If necessary, filter light or rotate the sample test piece to observe the optical changes outside the particles, such as color change, extinction change, etc., in order to accurately distinguish its glassy, crystalline or Other impurities.

The current device uses a single light source to illuminate the sample test piece, and the observed image is only the result of a single light. Under no comparison, the original image is difficult to identify, even if it is supplemented by powerful image analysis software. Analysis, there is still a certain degree of identification error. If you need to rotate the sample test piece for observation, because the apparent optical changes of individual particles are not synchronized, when the number of observations is large, the operation is even more troublesome and not conducive to counting.

In order to improve the shortcomings of the current methods and devices, we have worked hard to develop a particle identification counting method and analysis device, which is particularly suitable for the identification and counting of glassy particles and non-glassy particles. Non-glassy particles can also be identified if they contain all black particles Counting, the characteristic is to use the backlight and the positive light source to illuminate the optical difference of the sample test piece, and compare the images taken by the two light source directions to illuminate the sample test piece to strengthen the particle identification and facilitate the analysis and calculation. The operation is convenient and easy And more efficient.

After proper sampling, the test object can be made into a sample test piece in any suitable way. The particle size in the test piece should not be too large and should be evenly dispersed, for identification and counting analysis. Place the prepared sample test piece in the center of the stage, and adjust the microscopic device to adjust the optimal brightness, focal length and magnification for observation.

When illuminating with a backlight, turn off the positive light source, turn on the backlight below the stage, and illuminate the sample test piece upwards. Observed from the microscopic camera directly above the sample test piece, all particles will produce images with particle contours. Calculate the number of imaging particles is the total number of all particles Nt . When illuminating with a positive light source, turn off the backlight, turn on the positive light source above the stage, irradiate the sample test piece with a multi-angle depression angle and match with a monochrome background plate, observe from the microscopic camera directly above the sample test piece. Transparent can transmit light and almost disappear, while non-glass particles excluding all black particles will reflect light and shine, and all black particles will appear black because they do not reflect light. Calculating the number of shiny particles is the reason for excluding all black particles The total number of glassy particles Ns , the number of black particles observed on a non-black background is the total number of black particles Nb , the sum of the two is equal to the total number of non-glassy particles Nng . The total number of all particles Nt minus the total number of non-glassy particles Nng is the total number of glassy particles Ng .

1 ‧‧‧Backlight

1a ‧‧‧light from back light

2 ‧‧‧Positive light source

2a ‧‧‧light from backlight

3 ‧‧‧ sample test piece

3a ‧‧‧ cover slip

3b ‧‧‧ slides

4 ‧‧‧ Microscopic observation objective lens

5 ‧‧‧ stage

5a ‧‧‧ Round hole of stage

6 ‧‧‧Monochromatic background board

6a ‧‧‧Red background board

6b ‧‧‧ Black background board

7 ‧‧‧Black shading

8 ‧‧‧ Microscopic observation screen illuminated by backlight

8a ‧‧‧ glassy particles (still with outline)

8b ‧‧‧Exclude all non-glass particles of black particles

8c ‧‧‧All black particles

9 ‧‧‧ Microscopic observation screen illuminated by positive light source and red background

9a ‧‧‧Glass particles (almost disappear due to transmission)

9b ‧‧‧Exclude all black particles of non-glass particles (reflective shiny)

9c ‧‧‧All black particles (black without reflection)

10 ‧‧‧ Microscopic observation screen illuminated by positive light source and black background

10a ‧‧‧ glassy particles (almost disappear due to transmission)

10b ‧‧‧Exclude all black particles of non-glass particles (reflective shiny)

10c ‧‧‧ All black particles (almost disappeared due to the same background black)

Figure 1 is a schematic diagram of the components of the device of the present invention.

Figure 2 is a schematic diagram of the device of the present invention using a rotating mechanism to remove or replace a monochrome background plate.

FIG. 3 is a schematic diagram of the device of the present invention with the monochrome background plate removed and the backlight illumination turned on.

Fig. 4 is a schematic diagram of the microscopic observation screen of the present invention with the monochrome background plate removed and illuminated by the backlight.

Figure 5 is a schematic diagram of the device of the present invention using a red background plate and turning on the positive light source.

FIG. 6 is a schematic diagram of a microscopic observation screen of the present invention illuminated with a positive light source using a red background plate.

Fig. 7 is a schematic diagram of the device of the present invention using a black background plate and illuminating with a positive light source.

Fig. 8 is a schematic diagram of a microscopic observation screen of the present invention illuminated with a positive light source using a black background plate.

FIG. 9 is a schematic internal cross-sectional view of the positive light source of the present invention having a hemispherical ring structure.

FIG. 10 is a schematic top view of the appearance of the positive light source of the present invention having a hemispherical ring structure.

The present invention is to observe the sample of the particle mixture by optical microscopy, and the particle size range suitable for observation falls between 0.5 and 500 microns. According to the present invention, the preferred related schematic diagrams, as shown in Figures 1 to 10, the actual device can be appropriately changed in design, not limited to the pattern in this case.

Referring to FIG. 1, the particle identification and analysis device of the present invention includes components: a microscopic observation unit, which observes particle imaging with a microscopic observation objective lens 4 ; a stage 5 with a transparent hole 5a in the center and a sample test piece 3 Placed above the round hole 5a of the stage; backlight 1 is located below the stage 5 ; positive light source 2 is located above the stage 5 ; monochrome background plate 6 can be replaced with different color plates, removed without covering Or it can be positioned to cover the round hole 5a of the stage; the camera analysis unit can capture the microscopic imaging image and analyze the particle count. When performing the analysis, the device is adjusted for optimal brightness, focal length, and magnification for observation.

Sample test piece 3 can be made in any suitable way. The larger the test piece area, the more points can be observed. The key point is that the particle size in the test piece should not be too large and should be evenly dispersed. For the purpose of identification and counting analysis. The preferred method is to prepare a sample test piece 3 in which particles are uniformly dispersed and sandwiched between the cover glass 3a and the slide glass 3b . In order to make the particle size in the test piece not too different, the particle mixture sample should have a specific particle size range, the maximum and minimum particle size should not exceed 5 times, preferably not exceed 2 times, according to the test plan or requirements, from the test object It is obtained by sieve analysis and sampling. In order to disperse the particles in the test piece uniformly, you can select the appropriate dispersant or refracting oil according to the properties of the sample particles, and drip into the test piece to mix with the particles to help them evenly disperse. Care should be taken to avoid bubbles during operation.

Microscopic observation unit, adjustable magnification, magnification between 50 and 1000 times, from the top of the sample test piece 3 to observe the particle imaging with the microscopic observation objective 4 , by connecting the camera analysis unit to capture the microscopic imaging image And analyze the particle count.

Backlight 1 , adjustable brightness, located under the stage 5 , its light 1a can be irradiated upward through the stage round hole 5a towards the sample test piece 3 , in order to prevent interference from external light, black shading 7 can also be installed, As shown in Figures 1 and 3. When the backlight 1 is turned on for analysis, the positive light source 2 should be turned off, and the monochrome background plate 6 should be removed so as not to cover the round hole 5a of the stage to allow the backlight light 1a to pass through. Basically, you can get a good particle imaging effect by directly irradiating with appropriate brightness white light, but you can also choose filtering as needed, and convert it to polarized light or specific visible wavelength light, thereby increasing the imaging difference and assisting particle recognition.

The positive light source 2 can adjust the brightness, and is located above the stage 5 , and its light 2a can be irradiated toward the sample test piece 3 at multiple depression angles, with a monochromatic background plate 6 , as shown in Figures 1 , 5 , and 7. When the positive light source 2 is turned on for analysis, the backlight source 1 should be turned off. The monochromatic background plate 6 is positioned to cover the round hole 5a of the stage and form the visual background of the observation particle image. Basically, the best particle imaging effect can be obtained by directly irradiating with appropriate brightness white light without special filtering.

Monochromatic background board 6 , can be removed or replaced by any suitable mechanism design or manual extraction. Basically, the color plate that can be replaced must have a black plate, and at least one non-black plate, such as red, yellow, blue, and green, should not be too dark or too light to facilitate particle recognition. When the positive light source 2 is irradiated and analyzed, the plate should be positioned at an appropriate position under the sample test piece 3 , covering the hole at the upper or middle section or the lower hole of the round hole 5a of the stage and forming the background of the field of view of the observed particle image; backlight 1 During irradiation analysis, the plate should be removed so as not to cover the round hole 5a of the stage to allow the backlight light 1a to pass through. Fig. 2 reveals the design of positioning at the middle of the round hole 5a of the stage to cover the hole and remove or replace the monochrome background plate 6 by the rotating mechanism.

Referring to Figures 3 and 4, the microscopic observation screen 8 illuminated by the backlight shows that all particles will produce an image of the particle contour. Although the glassy particles 8a will transmit light, their side edges will still form an image of the contour due to optical factors. The non-glass particles 8b excluding all black particles will block or refract light to show images of different particle contours. All black particles 8c will completely block light and show images of all black particles. The number of imaging particles is all The total number of particles Nt .

Referring to Figures 5 and 6, the microscopic observation screen 9 illuminated by the positive light source with the red background plate 6a shows that the glassy particles 9a almost disappear due to transparent and transparent light, and the non-glassy particles 9b excluding all black particles will be reflected Light shines, all black particles 9c appear black because they do not reflect light. The number of bright particles is calculated as the total number of non-glass particles excluding all black particles Ns , and the number of black particles is the total number of black particles Nb , both The sum is equal to the total number of non-glass particles Nng . The total number of all particles Nt minus the total number of non-glassy particles Nng is the total number of glassy particles Ng .

Referring to Figures 7 and 8, the microscopic observation screen 10 illuminated by a positive light source with a black background plate 6b shows that the glassy particles 10a almost disappear due to transparent and transparent light, and the non-glassy particles 10b excluding all black particles will be reflected The light shines, and the all-black particles 10c almost disappear because they do not reflect the light and are close to the background black. At this time, the shiny particles will be particularly obvious, which can be used to review the correctness of the number of shiny particles. Calculating the number of shiny particles is the total number of non-glass particles excluding all black particles Ns . Practically, if there is no all black particles in the sample, it is best to directly use a black background plate. At this time, the number of bright particles is the total number of non-glass particles Nng . The total number of all particles Nt minus the total number of non-glassy particles Nng is the total number of glassy particles Ng .

The positive light source 2 is a key component of the device of the present invention, and its appearance and illumination method can be appropriately designed. The key point is that the light 2a should achieve the function of illuminating the sample test piece 3 at a multi-angle depression angle, and the shiny and reflective particles can be clearly identified . Figures 9 and 10 show an implementation of a hemispherical ring light source. By designing multiple light-emitting diodes with a hemispherical ring internal mirror reflection mechanism, the light can be irradiated from the inner surface of the hemisphere at multiple depression angles to the sample test piece Figure 9 is a schematic cross-sectional view of the inside, Figure 10 is a schematic top view of the outside.

The particle identification counting method and analysis device of the present invention can be operated manually by the testing personnel, and can also be designed to be operated in a partially automatic or fully automatic control mode. It is suitable for the composition analysis, purity analysis, quality inspection or microscopic identification of various types of particulate materials. For example, the detection of optical glass, minerals, carbon black, cement and other industrial powder raw materials or products. Three examples are presented below to illustrate the utility of the present invention.

Example 1: Microscopic observation and analysis of a sample of particulate mixture

A sample of a microparticle mixture is made into a sample test piece. With the device of the present invention, after positioning the sample test piece, the optimal brightness, focal length and magnification are adjusted, microscopic observation is performed, and the captured image is illuminated by the backlight as shown in the fourth In the figure, the screen captured with a positive light source and a red background board is shown in Figure 6, and the screen captured with a positive light source and a black background board is shown in Figure 8, and the analysis is as follows:

1. As shown in Figure 4, all particles will produce an image with a particle outline, a total of 20 particles.

2. As shown in Figure 6, 5 glassy particles will almost disappear, and 15 non-glassy particles will produce particle imaging. Among them, 13 shiny particles exclude non-glass particles that are all black particles, and 2 black particles are all black particles.

3. As shown in Figure 8, 5 glassy particles will almost disappear, 2 all black particles will also almost disappear, and 13 shiny particles will exclude non-glassy particles of all black particles.

4. The total number of all particles Nt=20 , the total number of non-glass particles excluding all black particles Ns=13 , the total number of black particles Nb=2 , the total number of non-glass particles Nng=13+2=15 . The total number of glassy particles Ng=20-15=5 .

Example 2: Detection of various industrial powders

The method and device of the present invention can be used to perform the detection of various industrial powders. The imaging characteristics of various common particulate material powders irradiated by the backlight and positive light source of the present invention are shown in Table 1. Using this imaging feature, the purity analysis of the powder can be designed as a quality check. Example 1: For the analysis of crystalline powder mixed with glassy impurities, under the irradiation of a positive light source, the shining particles are crystalline particles, and the disappearance are impurity particles; Example 2: For the analysis of carbon black powder mixed with non-glassy impurities , The positive light source is irradiated and on a black background, the disappearing is carbon black particles, and the shiny ones are impurity particles.

Example 3: Acceptance of optical glass powder purity

A glass powder is the raw material for the manufacture of optical lenses. Its main component is vitreous particles, but there are a few crystalline impurity particles. Acceptance requirements should not exceed 1%. The test design is as follows:

1. After analysing the analyte properly, make three different samples.

2. Each test piece observes 5 different points, and captures 180 to 220 particles in the field of view.

3. The total number of particles can be obtained by analyzing the backlight.

4. Analysis with positive light source and black background board, the obviously bright particles are miscellaneous particles.

Fifth, the test results are summarized, as shown in Table 2.

In summary, we have accumulated many years of detection experience and research analysis to complete the present invention. The proposed particle identification counting method and analysis device, the method concept and device characteristics have not been seen in the prior art, with novelty and improved efficiency, available for Industrial use, hope to obtain invention patents as soon as possible, to feel good.

1 ‧‧‧Backlight

2 ‧‧‧Positive light source

3 ‧‧‧ sample test piece

3a ‧‧‧ cover slip

3b ‧‧‧ slides

4 ‧‧‧ Microscopic observation objective lens

5 ‧‧‧ stage

5a ‧‧‧ Round hole of stage

6 ‧‧‧Monochromatic background board

7 ‧‧‧Black shading

Claims (9)

A particle identification and counting method, which uses the backlight and the positive light source to illuminate the optical difference of the sample test piece while avoiding the interference of the external ambient light. The microscopic camera is directly adjusted from the sample test piece to adjust the optimal brightness, focal length and magnification Observe the magnification to identify and count glassy particles and non-glassy particles. There may be all black particles in the non-glassy particles. The steps include: sample preparation, appropriate sampling of the test object, and uniform dispersion of particles. Place the sample test specimens on two colorless transparent slides and place them in the center of the stage; backlight illumination analysis, turn off the positive light source, turn on the backlight under the stage, directly with white light or after selective filtering, one-way upwards towards the sample The test piece is irradiated, and the camera screen shows that all particles will produce an image with particle contours. The number of imaged particles is calculated as the total number of all particles Nt ; positive light source irradiation analysis, turn off the backlight, turn on the positive light source above the stage, directly The white light multi-angle depression illuminates the sample test piece, and the camera screen shows that on a monochromatic background, the glassy particles almost disappear due to transparent and light transmission, and the non-glassy particles excluding all black particles will reflect the light and shine, all black The particles are black because they do not reflect light. The number of shiny particles is the total number of non-glass particles excluding all black particles Ns . The number of black particles observed on a non-black background is the total number of black particles Nb . Both The sum is equal to the total number of non-glassy particles Nng ; the total number of all particles Nt minus the total number of non-glassy particles Nng is the total number of glassy particles Ng . As in the method of claim 1, when illuminating the positive light source, analyze the particle imaging on a non-black background, and then on a black background, and check the correctness of the number of bright particles. The method according to claim 1, wherein the backlight source can be converted into polarized light or specific visible light wavelength light after selective filtering, thereby increasing imaging difference and assisting particle recognition. The method according to claim 1, wherein the particulate mixture sample has a specific particle size range, which is obtained by sieve analysis and sampling of the analyte according to the test plan or requirements, and the average particle size falls between 0.5 and 500 microns. As in the method of claim 1, wherein the microscopic observation can be magnified between 50 and 1000 times. A particle identification and analysis device, which uses a backlight and a positive light source to illuminate the optical difference presented by the sample test piece to enhance the identification of glassy particles and non-glassy particles in the sample. The components include: a microscopic observation unit, which can be adjusted and enlarged Magnification, observe the particle imaging from directly above the sample test piece; the stage is equipped with a transparent hole in the center, the sample test piece is placed above the round hole of the stage; white light backlight, adjustable brightness, located on the stage Below, the light can be directly or optionally filtered through the round hole of the stage to illuminate the sample test piece; the white light positive light source, which can adjust the brightness, is located above the stage, and its light can be directly angled toward the sample Test piece irradiation; Monochromatic background board, different color boards can be replaced in an appropriate way. When the backlight is illuminated for analysis, the board does not cover the round hole of the stage to allow the backlight light to pass through. When the analysis is performed with a positive light source , The plate is positioned to cover the round hole of the stage and form the background of the field of view of the observed particle image; the camera analysis unit can capture the microscopic observation imaging screen and perform particle count analysis. The device according to claim 6, which is used to perform the method according to any one of claims 1 to 5, to detect and analyze a particulate mixture sample. The device according to claim 6, wherein the positive light source is a hemispherical ring, and its light can be irradiated toward the sample test piece from the upper surface of the stage with a hemispherical inner surface. As in the device of claim 6, each component can be set to operate in automatic control mode.

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