JP2019219310A - Device and method for evaluating coating film - Google Patents

Abstract

To provide a technique for evaluating the distribution of the particle size of not only a sample particle in the surface of a coating film of an evaluation target object but also a sample particle in the inside of the coating film.SOLUTION: The method for evaluating a coating film is for evaluating the distribution of the particle size of particles of a sample, and includes: an irradiation step of irradiating an evaluation target object in which the sample is formed with an irradiation light from an arbitrary direction; a scattering light imaging step of imaging a scattering light from a sample particle in the surface and in the inside of the evaluation target object irradiated with the irradiation light; an analysis step of performing binarization of the taken image of the detected scattering light and analyzing the particle region from the binarized image; and an evaluation value generation step of generating an evaluation value for evaluating the distribution of the particle size of the sample on the basis of the analyzed particle region.SELECTED DRAWING: Figure 1

Description

  The present invention relates to a coating film evaluation device and a coating film evaluation method.

  When the shape of the battery is cylindrical, the lithium-ion battery cell is sandwiched between a positive electrode and a negative electrode by a porous insulating film called a separator that allows lithium ions to move, and the positive and negative electrodes are similar to Baumkuchen. The insulating film is wound into a container so as to overlap several layers and placed in a container.

  The separator is formed of an electrolyte film containing lithium ions, and the film is filled with silica particles for adsorbing the electrolyte. Ideally, silica particles include small particles including particles having a size of, for example, 1 μm or less, but they are aggregated due to mixing or the like.

  If the silica particles are smaller than the thickness of the coating film of the separator, the positive electrode and the negative electrode do not short-circuit. However, if the silica particles are larger than the thickness of the coating film, the short-circuit occurs. Therefore, a technique for evaluating whether or not there is a particle larger than the thickness of the coating film is required.

  Patent Literature 1 discloses that an external wall material having a granular pattern on its surface poses a problem in external design when an external wall material having a variation in appearance quality is constructed adjacently. It discloses a quality measuring means for stabilizing quality.

  Patent Document 1 states that “a granular pattern measuring device of the present invention is a device that measures the distribution of a granular pattern applied to the surface of a plate material, and an imaging unit that captures an image of the surface of the plate material; Extraction means for extracting pattern particles on the surface by binarizing the image information, and counting means for counting the number of pixels included in the pattern particles extracted by the extraction means. A configuration including a particle size distribution measuring means for classifying the pattern particles into numerical regions divided according to the number of pixels according to the number of pixels, and measuring the particle size distribution of the pattern particles by accumulating for each numerical region. Yes. "

JP-A-2000-206029

  The method described in Patent Literature 1 is to image the appearance of a granular pattern of an outer wall material manufactured by spraying paint particles of a color different from that of a base on the surface of a plate material, and perform binarized image processing. Then, the particle size distribution of the granular pattern on the surface of the plate material is evaluated.

  An object of the present invention is to make it possible to evaluate the particle size distribution of not only sample particles present on the surface of a coating film of an evaluation object but also sample particles present in the coating film.

  A preferred example of the coating film evaluation method of the present invention is a method for evaluating the particle size distribution of particles of a sample, and irradiating the evaluation object on which the sample is formed with irradiation light from any direction. A scattered light imaging step of imaging scattered light from the sample particles on the surface and inside of the evaluation object irradiated with the irradiation light, and a binarization process of the captured scattered light detection image, It is configured to include an analysis step of analyzing a particle region from a digitized image, and an evaluation value generation step of generating an evaluation value for evaluating the particle size distribution of the sample based on the analyzed particle region.

  As another feature of the present invention, in the method for evaluating a coating film, the irradiating step is a step of irradiating the evaluation object with irradiation light from a plurality of different directions, and the scattered light imaging step is performed. Capturing the scattered light from the sample particles inside and outside the surface of the evaluation object irradiated with the irradiating light from a plurality of different directions, respectively, into different images, wherein the analyzing step is performed by capturing the different images. Each scattered light detection image is binarized, and the particle region is analyzed from the binarized image.Each of the analyzed particle regions is a single particle region or an overlapping region of a plurality of particle regions. Identifying, and dividing the overlap region and the identified particle region into single particle regions by comparing corresponding particle regions analyzed from the different scattered light detection images. Ri, the evaluation value generating step, based on a single particle region, a step of generating an evaluation value for evaluating the particle size distribution of the sample.

  Further, as still another feature of the present invention, in the method for evaluating a coating film, the irradiating step is a step of irradiating the evaluation object with irradiation light from a plurality of different directions. Is a step of capturing scattered light from the sample particles on the surface and inside of the evaluation object irradiated with the irradiating light from a plurality of different directions, respectively in different images, and a plurality of scattered lights captured in the different images. The image processing apparatus further includes a combining step of generating a combined image from the light detection image, and the analyzing step is a step of performing a binarization process on the combined image and analyzing a particle region from the binary image.

  In a preferred example of the coating film evaluation apparatus of the present invention, an illumination unit that irradiates irradiation light from an arbitrary direction to an evaluation target on which a sample is formed, and the evaluation target that is irradiated with the irradiation light A scattered light detector that captures scattered light from sample particles on the surface and inside of the object, and a sample particle analyzer that binarizes the captured scattered light detection image and analyzes the particle area from the binary image And an evaluation value generation unit that generates an evaluation value for evaluating the particle size distribution of the sample based on the analyzed particle region.

  According to the present invention, it is possible to evaluate the particle size distribution of not only the sample particles present on the surface of the coating film of the evaluation target but also the sample particles present in the coating film.

1 is a block diagram illustrating a configuration example of a coating film evaluation device according to a first embodiment of the present invention. FIG. 2 is a diagram illustrating an example of a movable range of an illumination unit in the coating film evaluation device in FIG. 1. It is sectional drawing which shows the example of a structure of an evaluation object. It is sectional drawing which shows the example of a structure of the evaluation object contained in a container. FIG. 4 is a top view illustrating a configuration example of an evaluation target illustrated in FIG. 3. FIG. 5 is a top view illustrating a configuration example of an evaluation target illustrated in FIG. 4. It is a figure showing an example of the scattered light detection image obtained from the scattered light detected from the evaluation object. 8 is an image obtained by inverting black and white of an image obtained by binarizing the scattered light detection image of FIG. 7 using a threshold. 3 is a flowchart illustrating an example of a first evaluation value generation process performed by the coating film evaluation device in FIG. 1. FIG. 4 is a diagram illustrating an example of an evaluation value of a particle size distribution of sample particles. FIG. 4 is a diagram illustrating an example of a segment data table. FIG. 9 is a diagram illustrating a process of extracting segment data by performing a search process on a binarized image according to a raster scan method. (A) shows an example of a segment that can be considered to be based on scattered light emitted from one sample particle, and (B) shows an example of a segment in which two particles are partially overlapped in the vertical direction in the coating film. It is. (A)-(F) is a figure explaining the process which compares an overlapping particle area with the particle area obtained from two images, and estimates the back particle area from a difference area. FIG. 9 is a block diagram illustrating a configuration example of a coating film evaluation device according to a second embodiment. 16 is a flowchart illustrating an example of a second evaluation value generation process performed by the coating film evaluation device in FIG. 15. FIG. 4 is a diagram illustrating an example of an evaluation value of a particle size distribution of sample particles. FIG. 3 is a block diagram illustrating a configuration example in which an analysis unit of a coating film evaluation device is mounted on a computer.

  Hereinafter, a plurality of embodiments according to the present invention will be described with reference to the drawings. In all the drawings for describing each embodiment, the same members are denoted by the same reference numerals in principle, and the repeated description thereof will be omitted. Also, in the following embodiments, the components (including element steps, etc.) are not necessarily essential unless otherwise specified or considered to be indispensable in principle. Needless to say. In addition, when saying “consisting of A”, “consisting of A”, “having A”, and “including A”, other elements are excluded unless otherwise specified. Needless to say, it is not something to do. Similarly, in the following embodiments, when referring to the shapes, positional relationships, and the like of the components, the shapes are substantially the same unless otherwise specified, and in cases where it is considered that it is clearly not in principle. And the like.

  FIG. 1 is a block diagram illustrating a configuration example of a coating film evaluation apparatus 10 according to a first embodiment of the present invention. In the coordinate system shown in FIG. 1, the horizontal direction of the drawing is the Y axis, the vertical direction of the drawing is the Z axis, and the direction perpendicular to the drawing is the X axis.

  The coating film evaluation apparatus 10 according to the first embodiment of the present invention includes a mounting table 61, illumination units 62A and 62B, irradiation direction setting units 63A and 63B, irradiation amount setting units 64A and 64B, a lens unit 51, a scattered light detection unit 52, And an analysis unit 20.

  The mounting table 61 is installed parallel to the XY plane, and the evaluation target 70 is mounted thereon. The evaluation target 70 will be described in detail with reference to FIGS.

  The illumination units 62A, 62B irradiate the evaluation target 70 mounted on the mounting table 61 with irradiation light. The irradiation direction setting units 63A and 63B include, for example, a motor, a gear, an arm (all not shown), and the like. The irradiation direction setting units 63A and 63B move the illumination units 62A and 62B connected to one end of the arm according to the control from the coating film evaluation processing control unit 31 of the analysis unit 20 to illuminate the evaluation target 70. The irradiation angles of the units 62A and 62B (the elevation angles when the illumination units 62A and 62B are viewed from the evaluation object 70) are set. The irradiation amount setting units 64A and 64B set the irradiation amounts (light amounts) of the illumination units 62A and 62B to the evaluation target 70. By providing the irradiation direction setting units 63A and 63B and the irradiation amount setting units 64A and 64B, the illumination units 62A and 62B can change the irradiation angle and the irradiation amount.

  The illumination units 62A and 62B may be configured to be able to change the wavelength of the irradiation light to be applied. For example, irradiation light having a wavelength that the particles 73 easily reflect may be applied according to the material of the particles 73 (FIG. 3) formed on the evaluation target 70. Irradiation light having a wavelength that easily transmits materials other than particles may be applied. For example, when the material of the particles 73 is silica, the wavelength of the irradiation light emitted by the illumination units 62A and 62B may be set to 480 nm to 560 nm where the silica easily reflects. Further, by using the lens portion 51 having a large depth of focus, not only particles existing on the surface of the coating film but also scattered light of particles existing in the coating film can be captured.

  The lighting units 62A and 62B, the irradiation direction setting units 63A and 63B, and the irradiation amount setting units 64A and 64B are each provided in two sets in FIG. 1, but may be only one set. Alternatively, three or more sets may be provided.

  FIG. 2 is a diagram illustrating an example of a movable range (a setting range of an irradiation angle) of the lighting units 62A and 62B set by the irradiation direction setting units 63A and 63B.

  For the evaluation target 70 mounted on the mounting table 61 set in parallel with the XY plane, the illumination unit 62A sets the irradiation angle to 0 degree on the YZ plane passing through the center of the mounting table 61, for example (see the drawing). Irradiation light can be emitted at an arbitrary angle from left to 180 degrees (right in the drawing). Similarly, the illumination unit 62B can irradiate the irradiation light on the YZ plane at any angle from 0 degree (right side in the drawing) to 180 degrees (left side in the drawing).

  The example of FIG. 2 shows a case where the illumination angle of the illumination unit 62A is set to 45 degrees and the illumination angle of the illumination unit 62B is set to 60 degrees. As in the example of FIG. 2, the illumination angles of the illumination units 62A and 62B may be set to different angles, or the illumination angles of the illumination units 62A and 62B may be set to the same angle. Further, the irradiation amounts of the illumination units 62A and 62B may be the same or may be different.

  Return to FIG. The lens unit 51 focuses the scattered light of the evaluation target 70 on the scattered light detection unit 52. The scattered light detection unit 52 includes a detection element such as a complementary metal oxide semiconductor (CMOS) image sensor, for example, and generates a scattered light detection image from the scattered light of the evaluation target 70 that enters through the lens unit 51. The scattered light detection unit 52 supplies the generated scattered light detection image to the analysis unit 20.

The analysis unit 20 includes a calculation unit 21, a storage unit 22, an input unit 23, an output unit 24, and a communication unit 25.
The calculation unit 21 includes a coating film evaluation processing control unit 31, a grayscale image processing unit 32, a sample particle analysis unit 33, and an evaluation value generation unit 34.
The storage unit 22 includes a control parameter 41, a grayscale image storage unit 42, a segment data table 43, and an evaluation result storage unit 44.

The coating film evaluation processing control unit 31 controls the entire coating film evaluation device 10.
The input unit 23 receives, for example, various commands from the user and inputs from the user such as preset values of the irradiation angle.
The output unit 24 outputs the evaluation value and the like generated by the evaluation value generation unit 34 to, for example, another computer or a display.
The communication unit 25 receives the grayscale image captured by the scattered light detection unit 52 via the network 26, and transmits, for example, the generated evaluation value to the external computer 53 or the like.

  The grayscale image processing unit 32 is a scattered light detection image created and transmitted by the scattered light detection unit 52 (for example, a grayscale image of s pixels × t pixels in which the luminance value of scattered light is stored in each pixel). Is received and stored in the grayscale image storage unit 42. A noise removal process, a density histogram creation process, a binarization process, a black-and-white inversion process, and the like for the stored grayscale image are executed.

  The sample particle analysis unit 33 executes a segment extraction process on the binarized scattered light detection image to create a segment data table, and generates a single particle or an image of particles overlapping in the film. The presence or absence of the overlapped particles is identified, and in the case of overlapping particles, a process of individually identifying the overlapped particles is performed by collating a segment data table obtained from a plurality of scattered light detection images.

  The evaluation value generation unit 34 obtains the particle size of the particle based on the segment data representing a single particle in the binarized scattered light detection image extracted by the sample particle analysis unit 33, and An evaluation value is generated by digitizing the particle size distribution of.

  Although the communication of the image data between the scattered light detection unit 52 and the analysis unit 20 is described in FIG. 1 via the network 26 such as a local area network or the Internet, a dedicated transmission line is used. It may be. In FIG. 1, control lines for the coating film evaluation processing control unit 31, the illumination units 62A and 62B, the irradiation direction setting units 63A and 63B, and the irradiation amount setting units 64A and 64B are omitted.

  Next, the evaluation target 70 mounted on the mounting table 61 will be described.

  FIG. 3 is a cross-sectional view illustrating a configuration example of the evaluation target 70. The evaluation object 70 is assumed to be, for example, a coating film applied on a resin film. However, the evaluation target 70 is not limited to the coating film.

The coating film as the evaluation target 70 has a coating film layer 71 in order from the surface to which light is irradiated (upper side in the figure), and is formed by being laminated on a film 72.
The coating film layer 71 is formed by containing particles (corresponding to the sample of the present embodiment) 73 which are substantially targeted for the particle size distribution evaluation.
The coating film layer 71 has a region where the particles 73 exist and a region where the particles 73 do not exist.

FIG. 4 is a cross-sectional view illustrating another example of the configuration of the evaluation target 70. The evaluation object 70 is assumed to be, for example, a coating liquid 74 contained in a coating liquid container 75. However, the evaluation target 70 is not limited to the coating liquid.
The coating liquid 74 is formed by containing particles (corresponding to the sample of the present embodiment) 73 which are the substantial targets of the particle size distribution evaluation.
The coating liquid 74 has a region where the particles 73 exist and a region where the particles 73 do not exist.

  FIG. 5 is a top view of the evaluation target 70 shown in FIG. 3, and FIG. 6 is a top view of the evaluation target 70 shown in FIG.

Next, FIG. 7 illustrates an example of a scattered light detection image obtained from the scattered light 76 detected from the evaluation target 70 in a state where the irradiation light is irradiated. That is, the irradiation light is light having a wavelength that easily transmits through the coating film 71 and is easily reflected by the material of the particles 73, and is an image capturing scattered light emitted from the entire surface of the particles 73. In this image, the particles are bright white.
When the illumination angles of the illumination units 62A and 62B shown in FIG. 2 are radiated from above which are relatively close to 90 degrees, the irradiation light passes through the coating film layer 71, so that the particles existing on the coating film surface and the particles in the coating film The existing particles look the same color. In addition, the upper and lower particles look like 77 as shown in FIG.
On the other hand, if the illumination angles of the illumination units 62A and 62B are small and shallow, only relatively light shines on the surface of the coating film, so that only particles near the surface of the coating film appear to emerge. By changing the irradiation angle of the part, the appearance of the particles on the surface and inside of the coating film is different. ｝ Is a feature of this embodiment.

  Next, the image shown in FIG. 8 is an image obtained by binarizing the scattered light detection image shown in FIG. 7 using a threshold appropriately selected from the density histogram or a threshold set in advance as a control parameter. This is an image in which the particle region is represented by black pixels so that the particle region is clearly distinguishable from the background region by inverting black and white.

  The grayscale image processing unit 32 stores the scattered light detection image (s pixels × t pixels) of the coating film received from the scattered light detection unit 52 in the grayscale image storage unit 42, and performs the above-described binarization processing and black / white inversion processing. Is executed, and the binary image (s pixels × t pixels) shown in FIG.

  The sample particle analysis unit 33 executes a process of extracting each particle region as a segment from the binarized image (s pixels × t pixels) stored in the gray image storage unit 42. In the segment extraction processing, for example, a known image is searched for and extracted by a raster scan method. This will be described with reference to FIG. The extracted segments are recorded in the segment data table 43 shown in FIG.

In the segment extraction processing, the presence / absence of black pixels constituting the particle region is checked in the pixel column of each row in order from the first row at the top of the binarized image (s pixels × t pixels). FIG. 12 is an example showing a part of the binarized image, and shows that no black pixel has been found in the raster scan search processing from the first row to the n-th row. Then, at the time of searching for the pixel column of the (n + 1) th row, a black pixel is found at the position of (n + 1, a), and is recorded as the first segment in the segment data table 43 of FIG. Subsequently, a black pixel is found at the position (n + 1, b) in the search for the pixel column of the (n + 1) th row, and is recorded as the second segment. Subsequently, in the search for the pixel column of the (n + 1) th row, two black pixel columns at the positions of (n + 1, c) and (n + 1, c + 1)) black pixels continuous in the row direction are called black pixel columns. , (Row address of top pixel, column address of top pixel, number of continuous pixels). ｝ Is found and recorded as the third segment. After the search for the pixel column of the (n + 1) th row is completed, the search for the pixel column of the (n + 2) th row is continued, and the (n + 2, a-1, 3) black pixel column is found. Further, it is found that the pixel is connected to the (n + 1, a) black pixel in the column direction, and the pixel is recorded as a constituent pixel column of the first segment. In the present embodiment, the connection relationship between a plurality of pixels forming one segment is defined as connection when there is a relationship of four neighborhoods connected in the row direction or the column direction. ｝
Subsequently, in the search for the pixel column of the (n + 2) th row, the (n + 2, c−1, 4) black pixel column is found and is connected to the (n + 1, c, 2) black pixel column. Since it can be understood, it is recorded as a constituent pixel row of the third segment. Subsequently, the process proceeds to the search for the pixel column of the (n + 3) th row, the judgment is made in the same manner, and the (n + 3, a, 1) black pixel column is recorded as the constituent pixel column of the first segment, and (n + 3, c The black pixel row of (−1, 4) is recorded as a constituent pixel row of the third segment. Subsequently, in the search for the pixel column of the (n + 4) th row, the (n + 4, c, 2) black pixel column is recorded as a constituent pixel column of the third segment.

  In the search for the pixel column of the (n + 5) th row, a black pixel at the position (n + 5, c-1) is found, but it is determined that the pixel is not connected to the (n + 4, c, 2) black pixel column. Therefore, {circle around (1)} in the present embodiment, it is defined that the positional relationship near 8 is not connected. ｝, (N + 5, c−1) black pixels are recorded as the fourth segment.

  As described above, all the pixel columns of the binarized image (s pixels × t pixels) are searched, and the pixel columns constituting all the segments existing in the image are extracted. Record. That is, the scattered light emitted from each particle of the sample captured in one field of view is extracted as a segment and recorded by the scattered light detection unit 52 of the coating film evaluation apparatus 10.

  After the entire search of the binarized image is completed, the total number of pixels in the constituent pixel column column 89 is calculated for each segment recorded in the segment data table 43 and stored in the area (number of pixels) column 82 I do.

Further, the center of gravity of each segment {Each gray-scale image [binarized image (s pixels × t pixels), are defined coordinates X _g -Y _g for calculating the center of gravity, the origin position is the upper left of the image as the corner, X _g axis in the row direction, Y _g-axis is defined in the column direction. The length of one side of the pixel is calculated by, for example,｝ representing p and stored in the barycentric position column 84 of the segment data table 43.

FIG. 13A shows a comparison obtained from a set of black pixels that can be regarded as being based on the scattered light emitted from one sample particle in the segment where the segment number (81) = 100 in the segment data table 43. An example of one segment that is close to a target circle is shown.
Assuming that the sample particles can be regarded as substantially spherical, the outer peripheral shape of the aggregate of black pixels of the binarized image varies in the degree of approximation to a circle depending on the imaging resolution of the scattered light detection unit 52, but is rectangular. A circle is approximated by a set of pixels.

  On the other hand, FIG. 13B shows a segment in which the segment No. (81) = 200 in the segment data table 43, in which two particles in the coating film appear to partially overlap in the vertical direction. Here is an example.

  In this embodiment, the following processing is performed to identify whether each segment recorded in the segment data table 43 represents a single particle or a case where a plurality of particles partially overlap.

The length of one side of one pixel is represented by p. In this embodiment, the vertical and horizontal lengths of the pixel are the same square. ｝. The total number of pixels of each segment is stored in an area (number of pixels) column 82. Assuming that the segment whose total number of pixels is T _p is based on a single sample particle, assuming that the shape of the segment should be approximated to a circle, the virtual diameter D _s is given by It is represented by 1).

ここで、Ｃ_fは予め定めた換算係数である。

Here, C _f is a predetermined conversion coefficient.

The diameter D _s of the calculated virtual records the segment diameter column 88 of the segment data table 43.

Next, in the segment shown in FIG. 13A, the diameter D _lm 91 in the row direction is calculated by counting the number of pixels in the row direction from the pixel in the leftmost column to the pixel in the rightmost column. Set. Here, it is calculated as 10 and recorded in the row direction diameter column 86 of the segment data table 43. Similarly, the column direction diameter D _rm 92 is set by counting the number of pixels in the column direction from the pixel in the uppermost row to the pixel in the lowermost row. Here, it is calculated as 10 and recorded in the column direction diameter column 87 of the segment data table 43.

Similarly, in the segment shown in FIG. 13B, the diameter D _lm 91 in the row direction and the diameter D _rm 92 in the column direction are calculated, and the row diameter column 86 and the column diameter in the segment data table 43 are calculated. Record in column 87.

From the above calculation results, it is determined whether or not each segment satisfies both of the following equations (Equations 2 and 3).
(Equation 2) C _la · D _s ≦ D _lm · p ≦ C _ua · D _s
(Equation 3) C _la · D _s ≦ D _rm · p ≦ C _ua · D _s
Here, C _la indicates a lower limit allowable coefficient, and _Cua indicates an upper limit allowable coefficient.

That is, the row direction of the segment diameters Dlm91, and none of the column diameter Drm92 is, the diameter D _s of the segment in which the segment is estimated from the total number of pixels in the segment assuming that can be approximated to a circle, The segment is based on the scattered light emitted from a single sample particle if it falls within the lower limit (C _la · D _s ) and the upper limit (C _ua · D _s ) of the allowable error range. It is determined that the image is an image. Then, a flag representing “single” is set in the single or overlapping identification flag column 85 of the segment data table 43.
The above-described lower limit allowable coefficient C _la and upper limit allowable coefficient _Cua are set in advance by the user and registered in the control parameters 41.

For the segment shown in FIG. 13 (B), if it is determined whether or not both equations (2) and (3) are satisfied, both the diameter D _lm · p in the row direction and the diameter D _rm · p in the column direction are determined. but it found greater than C _ua · D _s, number 2, does not satisfy both the numerical formula 3. Therefore, the segment shown in FIG. 13B is determined to be an image in which a plurality of sample particles partially overlap. Then, a flag indicating “overlap” is set in the single or overlap identification flag column 85 of the segment data table 43.

  In the coating film evaluation apparatus 10 according to the present embodiment, the irradiation angle of the illumination units 62A and 62B is set to, for example, 70 degrees with respect to the evaluation target 70, and irradiation is performed from above. A first step of imaging both particles present in the coating film and analyzing the sample particles, and irradiating the irradiation portions 62A and 62B with the irradiation angle set to be as shallow as, for example, 20 degrees, and the vicinity of the surface of the coating film And a second step of analyzing the sample particles by imaging only the particles of the sample. The object 70 to be evaluated is imaged twice with the scattered light detection unit 52 fixed in the same field of view via the lens unit 51 and only the irradiation angles (and irradiation amounts) of the illumination units 62A and 62B are changed in two stages. .

  The scattered light detection images captured twice are subjected to binarization processing by the grayscale image processing unit 32, and the sample particle analysis unit 33 creates a segment data table for each binarized image. The purpose of the coating film evaluation process is to comprehensively evaluate all the sample particles contained in the coating film that fall within the visual field of the image. For this purpose, it is necessary to analyze the image capturing the scattered light of all the particles in the coating film by irradiating the illumination from above in the first step and obtaining an image of the scattered light from the particles. it can. However, when a plurality of particles positioned above and below the coating film appear to overlap, the size of each overlapping particle cannot be evaluated.

  Therefore, in the present embodiment, in the second step, the surface of the evaluation object 70 is irradiated with illumination at a relatively shallow irradiation angle, and only particles existing near the surface of the coating film are raised and imaged. When the analysis is performed, a particle image having no overlap can be obtained.

  Therefore, in the analysis of the image captured in the first step, a segment determined to have an overlap is a segment representing particles near the surface of the coating film at a corresponding location obtained by analysis of the image captured in the second step. In comparison with, the particles hidden behind are identified and their particle sizes are estimated.

<First Evaluation Value Generation Processing by Coating Film Evaluation Apparatus 10>
FIG. 9 is a flowchart illustrating an example of the first evaluation value generation process performed by the coating film evaluation apparatus 10 described above. The first evaluation value generation process is for detecting scattered light by setting the irradiation angles of the illumination units 62A and 62B in two stages, and is started, for example, in response to a start command from the user.

  In step S <b> 11, the user places the evaluation target 70 on the mounting table 61.

Next, in step S12, the irradiation direction setting units 63A and 63B set the irradiation angles of the illumination units 62A and 62B based on the control from the coating film evaluation processing control unit 31. Specifically, the coating film evaluation processing control unit 31 reads out the setting value of the irradiation angle stored in the control parameter 41 and notifies the irradiation direction setting units 63A and 63B of the irradiation direction setting units 63A and 63B. The irradiation angles of 62A and 62B are adjusted to the notified set values. In the present embodiment, in the first step, the irradiation angle of both certification units is set to, for example, 70 degrees, and in the second step, the irradiation angle of both certification units is set to, for example, 20 degrees.
However, the irradiation angles of the illumination units 62A and 62B may be set by the user. In this case, the user inputs a setting value of the irradiation angle using the input unit 23, and the coating film evaluation processing control unit 31 notifies the irradiation direction setting units 63A and 63B of the input setting value of the irradiation angle. do it.
Next, the irradiation amount setting units 64A and 64B set the irradiation amounts of the illumination units 62A and 62B based on the control from the coating film evaluation processing control unit 31, and the illumination units 62A and 62B evaluate with the set irradiation amounts. The object 70 is irradiated. Specifically, for example, the coating film evaluation processing control unit 31 reads out the initial value of the irradiation amount stored in the control parameter 41 and notifies the irradiation amount setting units 64A and 64B, and the irradiation amount setting units 64A and 64B The irradiation amounts of the illumination units 62A and 62B are set to initial values. Then, based on the scattered light detection image (so-called through image) obtained from the scattered light detection unit 52 in a state where the irradiation light is being irradiated, the coating film evaluation processing control unit 31 determines and determines the optimum irradiation amount. The optimum dose is notified to the dose setting units 64A and 64B, and the dose setting units 64A and 64B set the dose of the illumination units 62A and 62B to the optimum value.
Note that the user may also set the irradiation amounts of the illumination units 62A and 62B. In this case, the user may input an irradiation amount using the input unit 23, and the coating film evaluation processing control unit 31 may control the irradiation amount setting units 64A and 64B based on the input irradiation amount.

  Next, in step S13, the scattered light detection unit 52 captures an image of the scattered light emitted from the evaluation target 70 incident through the lens unit 51, and generates a scattered light detection image (for example, a size of s pixels × t pixels). Is generated and transmitted to the analysis unit 20.

  In step S <b> 14, in the analysis unit 20 to which the scattered light detection image has been supplied, the grayscale image processing unit 32 stores the scattered light detection image in the grayscale image storage unit 42.格納 Store the scattered light detection image in the first step and the scattered light detection image in the second step in different storage areas. Then, the grayscale image processing section 32 performs a binarization process and a black-and-white inversion process on the scattered light detection image to generate a binarized image in which the area of the sample particles is represented by black pixels.

In step S15, the sample particle analysis unit 33 executes a process of extracting each sample particle region as a segment from the binary image (s pixels × t pixels) stored in the grayscale image storage unit 42. . The result of processing the entire image is stored in the segment data table 43. (4) The segment data table in the first step and the segment data table in the second step are stored in different storage areas. ｝
After storing all the segment data, the area (number of pixels), the barycentric position, the row direction diameter, the column direction diameter, and the segment diameter of each segment are calculated and stored in the segment data table 43.

  In step S16, the sample particle analysis unit 33 determines whether each segment data stored in the segment data table 43 extracted in step S15 is an image based on scattered light emitted from a single sample particle. Or an image in which a plurality of sample particles are partially overlapped, is determined by the above equation (Equation 2 or 3), and the determination result is displayed in the single or overlap identification flag column 85 of the segment data table 43 as “ A flag indicating “single” or “overlap” is set.

  In step S17, the coating film evaluation processing control unit 31 determines whether the first step or the second step is completed in the processing for setting the irradiation angle of the illumination unit to two levels. If the first step has been completed, the process shifts to S12 to execute the second step. If the second step has also been completed, the process proceeds to S18.

  In step S18, the sample particle analysis unit 33 searches the segment data table 43 (hereinafter, referred to as the first segment data table) created in the first step, and sets each of the flags indicating the “overlap”. For the segment data, a process of classifying and identifying particles on the surface side of the coating film and particles partially hidden on the rear side is executed.

  From the segment data table 43 created in the second step (hereinafter, referred to as a second segment data table), the center of gravity of the segment 100 (exemplified in FIG. 14A) in which the flag indicating the “overlap” is set The segment 101 (exemplified in FIG. 14B) having the center of gravity located relatively close to the position is searched. The retrieved segment 101 (exemplified in FIG. 14B) is a segment obtained from a scattered light detection image captured by imaging only particles existing near the surface of the coating film in the second step. This can be considered to be based on particles existing on the surface side of the coating film.

  Accordingly, when the difference of the segment 101 (illustrated in FIG. 14B) is obtained from the segment 100 (illustrated in FIG. 14A), the remaining segment 102 (illustrated in FIG. 14C) is obtained. , It can be regarded as a segment based on sample particles partially hidden behind.

  Next, the position of the center of gravity of the segment 102 is calculated, and the position is plotted and shown as 103 on FIG. 14D. Similarly, the position of the center of gravity of the segment 101 is plotted and shown at the position of 104. A centerline 105 of the overlapping segment 100 passing through the centers of gravity 103 and 104 is drawn. Then, in the area of the segment 102, distance vectors 106 and 107 to the center of the pixel farthest from the center line 105 on both sides of the center line 105 are obtained. In the example of FIG. 14D, the distance vector 106 is longer than the distance vector 107.

  Next, as shown in FIG. 14 (E), from the center position of the pixel 108 which is the outermost in the direction of the center line 105 from the center of gravity 103 among the pixels of the segment 102, the same length as the distance vector 106 is placed on the center line 105. Assuming that the vector 109 is the center of the segment 102, the tip position of the vector 109 is set as the assumed center 110 of the segment 102. Then, from the hypothetical center 110, a hypothetical arc 111 of the hypothetical outer periphery of the segment 102 whose radius is the length of the vector 109 is drawn to the area of the segment 101.

  Next, as shown in FIG. 14 (F), it is assumed that the pixel of the segment 101 that overlaps the assumed circular arc 111 and is included in the circular arc is the pixel of the segment 102 hidden behind the segment 101. By estimating these pixels and the pixels of the segment 102, it is estimated that the segment 112 is based on a particle partially hidden behind. The estimated segment 112 is registered as a new segment in the first segment data table. For example, the estimated segment 112 is registered as a segment having the segment number (81) = 1561 in the segment data table 43 in FIG. Along with セ グ メ ン ト, the data of the segment 100 in which the flag indicating “overlap” is set is replaced with the data of the segment 101 of the second segment data table which is the segment data of the particles on the coating film surface side.

  The above processing is executed for all the segment data in which the flag indicating “overlap” registered in the first segment data table is set.

In step S19, the evaluation value generation unit 34 reads out the segment diameter values 88 for all the segments that can be considered to be based on a single sample particle registered in the first segment data table, and reads the actual particle size. in terms of the value D _p, for example by counting the number of particles per range of particle size value Dp as shown in FIG. 10, and generates and outputs an evaluation value of a first particle size distribution.

Next, FIG. 15 is a block diagram illustrating a configuration example of the coating film evaluation apparatus 120 according to the second embodiment of the present invention.
The coating film evaluation apparatus 120 is different from the coating film evaluation apparatus 10 of the first embodiment (FIG. 1) in that a scattered light detection image synthesizing section 35 is added to the calculation section 21 of the analysis section 20. Components other than the scattered light detection image synthesizing unit 35 are denoted by the same reference numerals, and description thereof is omitted.

  The scattered light detection image synthesizing unit 35 sets the irradiation angles of the illumination units 62A and 62B to a plurality of different states, and synthesizes a plurality of scattered light detection images obtained by imaging scattered light from the evaluation target 70. Generate an image. Here, the composite image is defined as a pixel value obtained by adding pixel values at the same coordinates in a plurality of scattered light detection images, or an average value of pixel values at the same coordinates in a plurality of scattered light detection images. It is assumed that In the present embodiment, only one irradiation angle of the illumination units 62A and 62B is set, and only one scattered light detection image is input. Is also included in this embodiment as an exception.

  FIG. 16 is a flowchart illustrating an example of the second evaluation value generation process performed by the coating film evaluation apparatus 120 described above. The second evaluation value generation process is for detecting the scattered light by setting the irradiation angles of the illumination units 62A and 62B in a plurality of stages, and is started, for example, in response to a start command from the user.

  In step S <b> 20, the user places the evaluation target 70 on the mounting table 61.

Next, in step S21, similarly to S12, the irradiation direction setting units 63A and 63B set the irradiation angles of the illumination units 62A and 62B based on the control from the coating film evaluation processing control unit 31 or the setting by the user.
Next, the irradiation amount setting units 64A and 64B set the irradiation amounts of the illumination units 62A and 62B based on the control from the coating film evaluation processing control unit 31 or the setting by the user, and the illumination units 62A and 62B are set. The evaluation object 70 is irradiated with the irradiation amount.

  Next, in step S22, the scattered light detection unit 52 images the scattered light emitted from the evaluation target 70 that is incident via the lens unit 51, and generates a scattered light detection image (for example, the size of s pixels × t pixels). Is generated and transmitted to the analysis unit 20.

  In step S23, in the analysis unit 20 to which the scattered light detection image is supplied, the grayscale image processing unit 32 stores the scattered light detection image in the grayscale image storage unit 42.

  In step S24, the coating film evaluation processing control unit 31 determines whether there is an irradiation angle of the illumination unit to be set next. That is, if there is data registered in the control parameter 41 or there is irradiation angle data set by the user, the process proceeds to S21. If there is no irradiation angle data, the process proceeds to S25.

  In step S <b> 25, the scattered light detection image synthesizing unit 35 calculates, for the plurality of scattered light detection images stored in the grayscale image storage unit 42, the sum of the pixel values at the same coordinates of each scattered light detection image, into the synthesized image. Is performed to calculate the pixel value of the same coordinate of the scattered light detection image, or to calculate the average value of the pixel value of the same coordinate of the scattered light detection image as the pixel value of the same coordinate in the composite image. The calculated composite image is stored in the grayscale image storage unit 42.

  In step S26, the grayscale image processing unit 32 performs a binarization process and a black-and-white inversion process on the composite grayscale image to generate a binary image in which the sample particle area is represented by black pixels.

  In step S27, the sample particle analysis unit 33 executes a process of extracting each sample particle region as a segment from the binarized image (s pixels × t pixels) stored in the grayscale image storage unit 42. . The result of processing the entire image is stored in the segment data table 43.

  In step S28, after storing all the segment data in S27, the sample particle analysis unit 33 calculates the area (number of pixels) and the segment diameter of each segment, and stores them in the segment data table 43.

In step S29, the evaluation value generation unit 34 does not attach all the segment data registered in the segment data table 43 to the segment based on a single particle or a segment based on overlapping particles. to read each segment diameter value 88, in terms of the actual particle size value D _p, for example by counting the number of particles per range of particle size value Dp as shown in FIG. 17, the second evaluation value of the particle size distribution Is generated and output.

  By the way, the analysis unit 20 in the first and second embodiments can be configured by hardware or can be realized by software. When the analysis unit 20 is realized by software, a program constituting the software is installed in a computer. Here, the computer includes a computer incorporated in dedicated hardware, a general-purpose personal computer that can execute various functions by installing various programs, and the like, for example.

  FIG. 18 is a block diagram illustrating a configuration example of hardware of a computer that realizes the analysis unit 20 by a program.

  In this computer 200, a CPU (Central Processing Unit) 201, a ROM (Read Only Memory) 202, and a RAM (Random Access Memory) 203 are mutually connected by a bus 204.

  The bus 204 is further connected to an input / output interface 205. The input unit 23, the output unit 24, the storage unit 22, the communication unit 25, and the drive 206 are connected to the input / output interface 205.

  The input unit 23 includes an input device such as a keyboard and a mouse. The output unit 24 includes a display device such as an LCD (Liquid Crystal Display), an organic EL display, and various output devices. The storage unit 22 includes a hard disk, a non-volatile memory, and the like. The communication unit 25 includes a network interface and the like. The drive 206 drives a removable medium 207 such as a magnetic disk, an optical disk, a magneto-optical disk, or a semiconductor memory.

  In the computer 200 configured as described above, the CPU 201 loads, for example, a program stored in the storage unit 22 into the RAM 203 via the input / output interface 205 and the bus 204 and executes the program. 20 are realized.

  The program executed by the computer 200 (CPU 201) can be provided by being recorded on, for example, the removable medium 207 as a package medium or the like. Further, the program can be provided via a wired or wireless transmission medium such as a local area network, the Internet, or digital satellite broadcasting.

  In the computer 200, the program can be installed in the storage unit 22 via the input / output interface 205 by attaching the removable medium 207 to the drive 206. The program can be received by the communication unit 25 via a wired or wireless transmission medium and installed in the storage unit 22. In addition, the program can be installed in the ROM 202 or the storage unit 22 in advance.

  Note that the program executed by the computer 200 may be a program in which processing is performed in chronological order according to the sequence described in this specification, or may be performed in parallel or at a required timing such as when a call is made. May be a program that performs the processing.

  The effects described in the present specification are merely examples and are not limited, and may have other effects.

  The present invention is not limited to the above embodiments, but includes various modifications. For example, each of the above-described embodiments has been described in detail in order to explain the present invention in an easy-to-understand manner, and the present invention is not necessarily limited to those having all the described components. Further, a part of the configuration of one embodiment can be replaced with the configuration of another embodiment, and the configuration of one embodiment can be added to the configuration of another embodiment. Further, for a part of the configuration of each embodiment, it is possible to add, delete, or replace another configuration.

  Further, each of the above-described configurations, functions, processing units, processing means, and the like may be partially or entirely realized by hardware, for example, by designing an integrated circuit. Each of the above-described configurations, functions, and the like may be implemented by software by a processor interpreting and executing a program that implements each function. Information such as a program, a table, and a file for realizing each function can be stored in a memory, a storage device such as a hard disk or an SSD (Solid State Drive), or a recording medium such as an IC card, an SD card, or a DVD. In addition, control lines and information lines indicate those which are considered necessary for explanation, and do not necessarily indicate all control lines and information lines on a product. In fact, it may be considered that almost all components are interconnected.

  The present invention can be provided not only in a particle size distribution evaluation method and a coating film evaluation apparatus, but also in various modes such as a system including a plurality of apparatuses and a computer-readable program.

DESCRIPTION OF SYMBOLS 10 ... Coating film evaluation apparatus, 20 ... Analysis part, 21 ... Operation part, 22 ... Storage part, 23 ... Input part, 24 ... Output part, 25 ... Communication part , 26 network, 31 coating film evaluation processing control unit, 32 grayscale image processing unit, 33 sample particle analysis unit, 34 evaluation value generation unit, 35 scattering Photodetection image synthesizing unit, 41: control parameter, 42: grayscale image storage unit, 43: segment data table, 44: evaluation result storage unit, 51: lens unit, 52 ... Scattered light detection unit, 53 ... external computer, 61 ... mounting table, 62A, 62B ... illumination unit, 63A, 63B ... irradiation direction setting unit, 64A, 64B ... irradiation amount setting unit,
70 ... evaluation object, 71 ... coating film layer, 72 ... film, 73 ... particles,
74 ... Coating liquid, 75 ... Coating liquid container, 76 ... Detected scattered light, 77 ... Particle area that appears to partially overlap in the coating film, 91 ... Diameter D in the row direction _lm , 92... diameter in column direction D _rm ,
100: a segment for which a flag indicating “overlap” is set, 101: a segment having a center of gravity relatively close to the segment 100, 102: a difference obtained from the segment 100 by the segment 101 , The center line 105, 106, 107 of the overlapping segment 100 passing through the center of gravity 103 and the center of gravity 104 In the area of 102, the distance vector from the center line 105 to the center of the pixel furthest from the center line 105 on both sides of the center line 105, 108... A distance vector 1 from a center position of a certain pixel, 109... 6, the center of the hypothesis of the segment 102, which is the tip position of the vector 109, 111... The radius of the hypothesis of the hypothesis of the segment 102 whose radius is the length of the vector 109 from the hypothesis center 110. Arc, 112 ... a segment based on a particle partially hidden on the estimated rear side,
120: coating film evaluation apparatus of Example 2, 200: computer, 201: CPU, 202: ROM, 203: RAM, 204: bus, 205: input / output interface , 206: Drive, 207: Removable media

Claims (14)

A method for evaluating the particle size distribution of particles of a sample,
An irradiation step of irradiating irradiation light from an arbitrary direction on the evaluation target on which the sample is formed,
A scattered light imaging step of imaging scattered light from sample particles on the surface and inside of the evaluation object to which the irradiation light is irradiated,
An analysis step of binarizing the captured scattered light detection image and analyzing a particle region from the binarized image,
An evaluation value generation step of generating an evaluation value for evaluating the particle size distribution of the sample based on the analyzed particle region,
A coating film evaluation method comprising: The coating film evaluation method according to claim 1,
The evaluation value generation step generates an evaluation value for evaluating the particle size distribution of the sample, with a diameter value when an area obtained by counting the number of pixels of the particle region approximated to a circle is set as a particle size. A method for evaluating a coating film, comprising: The coating film evaluation method according to claim 1,
The irradiation step is a step of irradiating the evaluation object with irradiation light from a plurality of different directions,
The scattered light imaging step is a step of imaging scattered light from the sample particles inside and from the surface of the evaluation object irradiated with the irradiation light from a plurality of different directions into different images,
In the analyzing step, each scattered light detection image captured in the different image is subjected to a binarization process, a particle region is analyzed from the binarized image, and the analyzed particle region is a single particle region. Identify the overlap region of a plurality of particle regions, the particle region identified as the overlap region, a single particle region by comparing the corresponding particle regions analyzed from the different scattered light detection images. It is a separating step,
The evaluation value generating step is a step of generating an evaluation value for evaluating a particle size distribution of the sample based on a single particle region. In the coating film evaluation method according to claim 1,
The irradiation step is a step of irradiating the evaluation object with irradiation light from a plurality of different directions,
The scattered light imaging step is a step of imaging scattered light from the sample particles inside and from the surface of the evaluation object irradiated with the irradiation light from a plurality of different directions into different images,
Further comprising a combining step of generating a combined image from the plurality of scattered light detection images captured in the different images,
The analysis step is a step of performing a binarization process on the composite image and analyzing a particle region from the binarized image. In the coating film evaluation method according to claim 4,
The combining step includes, for the plurality of scattered light detection images, generating the combined image by performing an operation of setting an addition value of pixel values of the same coordinates of each scattered light detection image to a pixel value of the same coordinates of the combined image. A coating film evaluation method, characterized in that: In the coating film evaluation method according to claim 4,
Generating the composite image by performing an arithmetic operation on the plurality of scattered light detection images with an average value of pixel values at the same coordinate of each scattered light detection image as a pixel value at the same coordinate of the composite image; A coating film evaluation method, characterized in that: In the coating film evaluation method according to claim 1,
The irradiating step includes irradiating irradiation light from an arbitrary direction to an evaluation target on which the sample is formed, wherein at least one of an irradiation angle, an irradiation direction, an irradiation amount, and a wavelength of the irradiation light is variable. A coating film evaluation method. An illumination unit that irradiates irradiation light from an arbitrary direction on the evaluation target on which the sample is formed,
A scattered light detection unit that images scattered light from the sample particles inside and outside the surface of the evaluation object to which the irradiation light is irradiated,
A sample particle analysis unit that binarizes the captured scattered light detection image and analyzes a particle region from the binarized image,
Based on the analyzed particle region, an evaluation value generation unit that generates an evaluation value for evaluating the particle size distribution of the sample,
A coating film evaluation apparatus comprising: The coating film evaluation apparatus according to claim 8,
The evaluation value generation unit generates an evaluation value for evaluating the particle size distribution of the sample, with the diameter value when the area obtained by counting the number of pixels of the particle region approximated to a circle as the particle size. A coating film evaluation apparatus, characterized in that: The coating film evaluation apparatus according to claim 8,
The illumination unit irradiates the evaluation object with irradiation light from a plurality of different directions,
The scattered light detection unit captures scattered light from the sample particles on the surface and inside of the evaluation object irradiated with the irradiation light from a plurality of different directions in different images.
The grayscale image processing unit binarizes each scattered light detection image captured in the different image,
The sample particle analysis unit analyzes the particle region from the binarized image, identifies each analyzed particle region as a single particle region or an overlapping region of a plurality of particle regions, and determines the overlapping region. The identified particle region is divided into a single particle region by comparing corresponding particle regions analyzed from the different scattered light detection images,
The said evaluation value production | generation part produces | generates the evaluation value which evaluates the particle size distribution of the said sample based on a single particle area | region, The coating film evaluation apparatus characterized by the above-mentioned. The coating film evaluation apparatus according to claim 8,
The illumination unit irradiates the evaluation object with irradiation light from a plurality of different directions,
The scattered light detection unit captures scattered light from the sample particles on the surface and inside of the evaluation object irradiated with the irradiation light from a plurality of different directions in different images.
Further comprising a scattered light detection image synthesis unit that generates a composite image from a plurality of scattered light detection images captured in the different images,
The coating film evaluation apparatus, wherein the sample particle analysis unit performs a binarization process on the composite image and analyzes a particle region from the binarized image. The coating film evaluation apparatus according to claim 11,
The scattered light detection image synthesizing unit calculates, for the plurality of scattered light detection images, an addition value of pixel values of the same coordinates of each scattered light detection image as a pixel value of the same coordinates of the synthesized image, thereby calculating the synthesized image. A coating film evaluation apparatus characterized by generating: The coating film evaluation apparatus according to claim 11,
The scattered light detection image synthesis unit calculates an average value of pixel values at the same coordinates of each of the scattered light detection images for the plurality of scattered light detection images as a pixel value at the same coordinates of the synthesized image. A coating film evaluation apparatus characterized by generating: The coating film evaluation apparatus according to claim 8,
The illumination unit irradiates irradiation light from an arbitrary direction to the evaluation target on which the sample is formed, wherein at least one of an irradiation angle, an irradiation direction, an irradiation amount, and a wavelength of the irradiation light is variable. A coating film evaluation apparatus characterized in that:

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