JP2004184134A - Particle size distribution measuring instrument - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To relatively simply find a refractive index required for particle size distribution measurement, with high reliability. <P>SOLUTION: A particle size distribution is measured in advance as to sample particles of a kind same to measuring objective particles, using an instrument for measuring the particle size distribution without finding the refractive index as in a SEM, an optical microscope or the like, scattered light generated by irradiating the sample particles with a fixed wavelength of light is measured also, measured result information obtained directly or indirectly from a measured result therein is compared with a corresponding calculated result information calculated based on temporarily set tentative refractive index information, and the true refractive index of the measuring objective particles is found from the tentative refractive index information based on a degree of consistency. <P>COPYRIGHT: (C)2004,JPO&NCIPI

Description

[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to a particle size distribution measuring device that measures a particle size distribution from scattered light generated by irradiating light to a measurement target particle in a sample with at least a refractive index of the measurement target particle as a parameter.
[Prior art]
This type of device can easily measure the particle size in near real-time compared to a device that requires relatively large labor and time to measure the particle size distribution, such as an SEM or an optical microscope. It is suitably used for applications in which the particle size of a product is inspected and quality control is continuously performed.
[0002]
By the way, in this type of apparatus, in order to measure the particle size distribution, the refractive index of the particle to be measured is required as a parameter. However, the refractive indices of all substances for light are not actually obtained, and there are many unknown particles to be measured whose refractive indices have not yet been measured. Therefore, in such a case, various methods for obtaining the refractive index for measuring the particle size distribution have been conventionally considered.
[0003]
For example, as shown in Patent Literature 1, a method of selecting a refractive index at which the median diameter of a particle size distribution calculated using this apparatus is the largest, or a method of calculating a backscatter from a measured scattering pattern and a calculated particle distribution. A method of selecting a refractive index having the best matching degree with a pattern has been proposed. Of course, besides, for example, a liquid having various known refractive indices is prepared, and the refractive index approximate to the refractive index of the liquid which becomes the most transparent liquid by dispersing the particles to be measured therein, There is also a method of estimating the refractive index of the light.
[Patent Document 1]
JP-A-06-07492
[Problems to be solved by the invention]
However, although the former method can be easily realized in this type of measuring device, it may not be applicable depending on the shape of the distribution and the like.
[0004]
In the latter method, when inaccurate information due to noise or the like is included in the scattering pattern, there is a possibility that the non-optimal refractive index may show the optimum degree of coincidence. May be required.
[0005]
Further, when directly calculating the refractive index as in the last method, it is extremely troublesome, and moreover, it can be generally applied to them, including the method described above, but the obtained refractive index is inaccurate or It is not reliable because it is different.
[0006]
Therefore, the present invention uses a device such as an SEM or an optical microscope that can measure the particle size distribution without obtaining the refractive index, and measures the particle size distribution of sample particles of the same kind as the particles to be measured in advance. The scattered light generated by irradiating the sample particles with light of a certain wavelength is measured, and the measurement result information obtained directly or indirectly from the measurement results is calculated based on the temporarily set temporary refractive index information. By making it possible to compare with the corresponding calculated result information, the true refractive index of the measurement target particle can be obtained from the provisional refractive index information by the degree of coincidence, and this kind of particle diameter distribution The main object of the measurement apparatus is to make it possible to obtain the refractive index required for measuring the particle size distribution with high reliability and relatively easily.
[0007]
[Means for Solving the Problems]
That is, the particle size distribution measuring device according to the present invention is scattered light information that is information on scattered light generated by irradiating light to the measurement target particles in the sample, and information on the refractive index of the measurement target particles with respect to the light. A temporary refractive index information receiving unit that calculates particle diameter distribution information that is information about the particle diameter distribution using the refractive index information, and receives temporary refractive index information that is information about a temporarily set refractive index. A measured scattered light information receiving unit that receives measured scattered light information obtained by irradiating measurement target particles having known particle size distribution information with light, and virtual based on the temporary refractive index information and the measured scattered light information. A virtual particle size distribution information calculating unit for calculating virtual particle size distribution information, which is information on a typical particle size distribution, and comparing the virtual particle size distribution information with known particle size distribution information of the measurement target particles. Output to, characterized in that it comprises a refractive index setting support unit for supporting the setting of the refractive index of the measured particles.
[0008]
In such a case, even when the particle refractive index is unknown, the appropriate refractive index information is relatively easily obtained by using the particle size distribution information obtained in advance using an SEM, an optical microscope, or the like. be able to. The refractive index information has extremely high reliability verified by comparison with a known particle size distribution. In addition, since the particle size distribution of other particles of the same type can be more accurately obtained based on the obtained refractive index information, for example, in applications where the particle size distribution is inspected and quality control is continuously performed. It becomes very suitable.
[0009]
Here, the term “information about” includes not only information indicating the target directly but also information indicating the target indirectly, for example, information on the way of the calculation. "Comparable output" means output in a similar manner so that it can be printed or displayed on the screen. More specifically, for example, it is displayed or printed as a graph in an overlaid or arranged state, or printed. To do. “Accept” means receiving input information, receiving information via communication means, or acquiring internally stored or generated information.
[0010]
As another aspect having the same operation and effect as the above invention, a provisional refractive index information receiving unit that receives provisional refractive index information that is information about a provisionally set refractive index, and a particle to be measured whose particle size distribution information is known A measured scattered light information receiving unit that receives measured scattered light information obtained by irradiating light, and virtual scattered light that is information on virtual scattered light based on the temporary refractive index information and the known particle size distribution information. A virtual scattered light information calculation unit for calculating information, and a refractive index setting support unit that outputs the virtual scattered light information so as to be able to be compared with the actually measured scattered light information and supports setting of a refractive index of the measurement target particle. Can be mentioned.
[0011]
As a preferred specific mode for efficiently determining the refractive index, the temporary refractive index information receiving unit receives a plurality of temporary refractive index information, and the virtual particle diameter distribution information calculating unit calculates each of the temporary refractive index information. The virtual particle size distribution information is calculated based on the above, and in the refractive index setting support unit, the respective virtual particle size distribution information can be compared with the known particle size distribution information of the measurement target particles. What is output, and while calculating the virtual scattered light information information based on the respective provisional refractive index information in the virtual scattered light information calculation unit, the refractive index setting support unit, An example in which virtual scattered light information is output so as to be comparable with the actually measured scattered light information can be given.
[0012]
In order to contribute by setting the refractive index, a coincidence calculating unit that compares the virtual particle diameter distribution information with the known particle diameter distribution information of the measurement target particles and calculates the coincidence according to a predetermined calculation formula. And the refractive index setting support unit preferably further outputs the coincidence calculated by the coincidence calculation unit.
[0013]
Without manually inputting a plurality of temporary refractive indices, in order to automatically bring the temporary refractive index closer to the true refractive index and to obtain a desired refractive index more easily, the provisional refractive index A temporary refractive index information receiving unit that receives temporary refractive index information that is information, and a measured scattered light information receiving unit that receives measured scattered light information obtained by irradiating light to the measurement target particles whose particle size distribution information is known. Based on the provisional refractive index information and the measured scattered light information, a virtual particle diameter distribution information calculation unit that calculates virtual particle diameter distribution information that is information about a virtual particle diameter distribution, and the virtual particle diameter distribution information A coincidence calculating unit that compares the degree of coincidence with a known particle diameter distribution information of the particles to be measured and calculates the degree of coincidence according to a predetermined calculation formula, and in order to bring the degree of coincidence closer to a target value, calculate the degree of coincidence. Based on the provisional refractive index information Those and a provisional refractive index information changing unit for changing the desirable.
[0014]
As a device having the same function and effect, a provisional refractive index information receiving unit that receives provisional refractive index information that is information about a provisionally set refractive index, and irradiating light to measurement target particles whose particle size distribution information is known. A measured scattered light information receiving unit that receives the measured scattered light information obtained as described above, and calculates virtual scattered light information that is information on virtual scattered light based on the provisional refractive index information and the known particle size distribution information. A virtual scattered light information calculation unit, and a coincidence calculation unit that compares the virtual scattered light information with the measured scattered light information cloth information and calculates the coincidence according to a predetermined calculation formula, and sets the coincidence to a target value. In order to approach, a temporary refractive index information changing unit that changes the temporary refractive index information based on the calculated degree of coincidence can be cited.
[0015]
As a specific example in which the effect of the present invention is remarkable, the scattered light information indicates an angular distribution of the intensity of scattered light generated when the particles are irradiated with light.
[0016]
BEST MODE FOR CARRYING OUT THE INVENTION
Hereinafter, embodiments of the present invention will be described with reference to the drawings. In addition, the same code | symbol shall be attached | subjected to the member corresponding in each embodiment.
<First embodiment>
[0017]
The particle size distribution measuring apparatus 1 according to the present embodiment utilizes that a scattering pattern of scattering light (angular distribution of scattered light intensity) generated when the particles are irradiated with light is determined by the particle size from Mie scattering theory, The particle size distribution is measured by detecting the scattering pattern. Specifically, as schematically shown in FIG. 1, a cell 2 containing a sample in which particles to be measured are dispersed in a solvent, and a light source (for example, a light source that irradiates the cell 2 with coherent light L) He-Ne laser) 7 and scattered light and / or diffracted light (hereinafter referred to as scattered light) LS, which are arranged around the cell 2 and are irradiated with the laser light L, are received. A plurality of detectors 3 that output scattered light intensity signals as signals, and an information processing device 4 that receives the scattered light intensity signals output from each of the detectors 3 and calculates a particle size distribution in a sample are provided. ing. In the figure, reference numeral 5 denotes a beam expander for expanding the diameter of light emitted from the light source, and reference numeral 6 denotes a convex lens for collecting scattered light on the light receiving surface of the detector 3.
[0018]
The information processing device 4 is physically separated into a general-purpose computer such as a personal computer and a dedicated processing computer from the viewpoint of, for example, processing speed, usability, and maintenance (of course, it may be integrated). As shown in FIG. 2, a basic device configuration as a whole includes a CPU 101, a main body 42 including an input / output interface 102, a storage device 104 (internal memory 1041 and external memory 1042), a preamplifier 411, and a multiplexer. 412, an AD converter 413, and the like, in addition to a signal converter 41 interposed between each of the detectors 3 and the main body 42, a display 43, an input means 44, a printer 45, and the like.
[0019]
In the present embodiment, the CPU 101 and its peripheral devices are operated according to a predetermined program stored in the storage device 104, so that the information processing device 4 temporarily stores the refraction, as shown in FIG. Temporary refractive index information receiving unit F1 for receiving temporary refractive index information, which is information on refractive index, and measured scattered light information for receiving measured scattered light information obtained by irradiating light to measurement target particles whose particle size distribution information is known A receiving unit F2, a virtual particle size distribution information calculating unit F3 that calculates virtual particle size distribution information that is information relating to a virtual particle size distribution based on the provisional refractive index information and the actually measured scattered light information, A refractive index setting support unit F4 that outputs the diameter distribution information in a manner that can be compared with the known particle diameter distribution information of the measurement target particles, and supports setting of the refractive index of the measurement target particles. It said and let a function of the virtual particle size distribution information as the matching degree calculating unit F6 like calculated according to the known a is compared with the particle size distribution information that matches the degree a predetermined calculation formula of the measurement target particles.
[0020]
Hereinafter, with reference to FIG. 3 and FIG. 4, a detailed description of these units will be made while also explaining the operation of the present apparatus 1.
[0021]
First, the particle diameter distribution of the measurement target particle whose unknown refractive index is unknown is determined in advance by using an apparatus capable of measuring the particle diameter distribution without determining the refractive index, such as an SEM or an optical microscope, and is determined as a known particle. deep. Then, the known particle size distribution information stored in the stationary or temporary storage area in the storage device 104 is associated with the information on the known particle size distribution and the type identifier for identifying the type of the measurement target particle. It is stored in the unit D1 in advance.
[0022]
Next, after filling the cell 2 with a sample in which the particles to be measured are dispersed in a solvent such as water, the sample is irradiated with laser light L. The laser light L is scattered by the measurement target particles in the sample to become scattered light LS, and the scattered light LS is detected by each of the detectors 3 and output as a scattered light intensity signal.
[0023]
The scattered light intensity signal output from each of the detectors 3 is transmitted to the input / output interface 102 via the signal converter 41, and an actually measured scattered light information receiving unit configured using the input / output interface 102 F2 receives these scattered light intensity signals as measured scattered light information indicating the angular distribution of the scattered light intensity (step ST01). The measured scattered light information receiving unit F2 stores the received measured scattered light information in the measured scattered light information storage unit D2 set in a stationary or temporary storage area of the storage device 104, and stores the type identifier and Store them in association.
[0024]
On the other hand, a screen prompting the operator to input a temporary refractive index is displayed on the display 43. Specifically, the refractive index n is represented by a complex number of n '+ ik, so that n' and k can be input. When the temporary refractive index is set on the screen by an arbitrary or selective input by the operator, the temporary refractive index information receiving unit F1 receives the temporary refractive index information as temporary refractive index information (step ST02). The temporary refractive index information is stored in a temporary or temporary storage area in association with the type identifier in a temporary refractive index information storage unit D3.
[0025]
Next, the virtual particle size distribution information calculation unit F3 acquires the provisional refractive index information and the actually measured scattered light information, and calculates virtual particle size distribution information, which is information relating to a virtual particle size distribution, based on these information ( Step ST03). The virtual particle size distribution information is stored in a virtual particle size distribution information storage unit (not shown).
[0026]
Thereafter, the coincidence calculating unit F6 acquires the virtual particle diameter distribution information and the known particle diameter distribution information, and calculates the degree of coincidence of those distributions (step ST04). The degree of coincidence may be, for example, a parameter having a difference value, a ratio, an absolute value of the difference, a value obtained by squaring the difference, or the like.
[0027]
On the other hand, the refractive index setting support unit F4 obtains the virtual particle size distribution information and the particle size distribution information, and, for example, obtains the information so that the operator can visually and intuitively determine the difference between the two distribution shapes. Are displayed simultaneously on the screen (step ST05), and the degree of coincidence is also displayed (step ST06).
[0028]
Therefore, in such a case, if the operator determines, for example, that the set provisional refractive index is inappropriate from the overwritten distribution graph and the degree of coincidence, the operator inputs the provisional refractive index again, By repeating this multiple times, an appropriate refractive index can be easily set. In addition, the finally set refractive index has extremely high reliability verified by comparison with a known particle size distribution. And since it is possible to more accurately determine the particle size distribution of other particles of the same type based on the obtained refractive index, for example, for applications such as inspecting the particle size distribution and performing continuous quality control, It will be very suitable.
[0029]
As shown in steps ST11 to ST16 in FIG. 5, the temporary refractive index information receiving unit F1 is configured to be able to receive a plurality of pieces of temporary refractive index information in parallel or to automatically generate a plurality of pieces of temporary refractive index information. The diameter distribution information calculation unit F3 calculates virtual particle diameter distribution information based on the respective provisional refractive index information, and the refractive index setting support unit F4 converts the virtual particle diameter distribution information to the known particle diameter distribution information. You may make it output so that comparison is possible.
[0030]
In this way, compared to inputting a single piece of temporary refractive index information each time, the time and effort for inputting the information can be saved, and the virtual particle diameter distributions calculated from the plurality of pieces of temporary refractive index information can be compared at once. Further, the tendency of the change in the particle size distribution due to the change in the provisional refractive index information can be more clearly grasped, and the desired refractive index can be set more quickly and easily.
<Second embodiment>
[0031]
The particle size distribution measuring apparatus 1 according to the present embodiment differs from the first embodiment only in the functional part of the information processing apparatus 4 and has the same hardware configuration. Will be explained.
[0032]
That is, as shown in FIG. 6, the information processing apparatus 4 according to the second embodiment includes, as a functional configuration, the provisional refractive index information that changes the provisional refractive index information based on the calculated degree of coincidence in addition to the components. A change unit F7 is further provided.
[0033]
Specifically, the function of the provisional refractive index information changing unit F7 and the function of each unit generated by adding the function will be described below with reference to FIGS.
[0034]
As in the first embodiment, first, the particle size distribution of the measurement target particles whose unknown refractive index is unknown is determined in advance, and is set to a known value. The information on the known particle size distribution is stored in advance in the known particle size distribution information storage unit D1 in association with a type identifier for identifying the type of the particle to be measured.
[0035]
Next, the sample is irradiated with laser light L, and the scattered light LS is detected by each of the detectors 3.
[0036]
The scattered light intensity signal output from each of the detectors 3 is transmitted to the input / output interface 102 via the signal converter 41, and the measured scattered light information receiving unit F2 configured using the input / output interface 102 Then, these scattered light intensity signals are received as measured scattered light information indicating the angular distribution of the scattered light intensity (step ST21). The measured scattered light information receiving unit F2 stores the received measured scattered light information in the measured scattered light information storage unit D2 in association with the type identifier.
[0037]
On the other hand, a screen for inputting the initial value of the provisional refractive index is displayed to the operator, and when the initial provisional refractive index is set by an arbitrary input or selection input by the operator on the screen, this is displayed. The information receiving unit F1 receives the information as initial provisional refractive index information (step ST22), and stores the information in the provisional refractive index information storage unit D3 in association with the type identifier.
[0038]
Next, the virtual particle size distribution information calculation unit F3 acquires the provisional refractive index information and the actually measured scattered light information, and calculates virtual particle size distribution information, which is information relating to a virtual particle size distribution, based on these information ( Step ST23).
[0039]
Then, the coincidence calculating unit F6 acquires the virtual particle diameter distribution information and the known particle diameter distribution information, and calculates the coincidence of those distributions (step ST24).
[0040]
Next, the provisional refractive index information changing unit F7 determines whether or not the calculated degree of coincidence is within the allowable range (step ST26). The temporary refractive index information stored in the temporary refractive index information storage section D3 is changed (step ST26). Specifically, the values of n and k are changed using, for example, a nonlinear least squares method. The permissible range may be stored in a permissible range storage unit (not shown) in advance based on, for example, an operator's prior input.
The steps ST24 to ST26 are performed one or more times, and when the degree of coincidence falls within the allowable range, the refractive index setting support unit F4 acquires the virtual particle diameter distribution information and the known particle diameter distribution information at that time, In order to allow the operator to visually and intuitively judge the difference between the two distribution shapes, for example, a distribution graph obtained from the information is simultaneously displayed on the screen (overlaid display), and the matching degree at that time is displayed. Is also displayed (step ST27, step ST28).
[0041]
Therefore, in such a case, the temporary refractive index information is automatically updated without manually inputting the temporary refractive index information many times, so that a desired refractive index can be obtained more easily, and Burden can be reduced.
[0042]
The range for automatically selecting the refractive index, the refractive index condition information indicating whether light is absorbed or not, and the particle condition information such as a particle diameter range in which particles are never present and a monomodal / multimodal property are also set in advance. The information may be stored in a predetermined storage area and referred to when the provisional refractive index information is changed. This can contribute to more reliable and quicker selection of the refractive index.
[0043]
Further, a graph or a degree of coincidence may be displayed by the refractive index setting support unit F4 every time the degree of coincidence is calculated, and the operator may be asked to input whether or not the temporary refractive index information can be automatically changed each time. For example, the degree of coincidence may be numerically good, but the virtual particle size distribution graph may have irregularities and may not match the shape of the known particle diameter distribution graph in some cases. This is because the operator may judge that the refractive index is appropriate even though the graph shape is more consistent, even if it is somewhat lower.
<Third embodiment>
[0044]
The particle size distribution measuring apparatus 1 according to the present embodiment has the same hardware configuration as that of the first embodiment, except for the functional parts of the information processing apparatus 4, and therefore the differences will be mainly described. I do.
[0045]
As shown in FIG. 8, the information processing apparatus 4 according to this embodiment operates the CPU 101 and its peripheral devices in accordance with a predetermined program stored in the storage device 104 to obtain information about the temporarily set refractive index. A provisional refractive index information receiving unit F1 for receiving certain provisional refractive index information, and a measured scattered light information receiving unit for receiving measured scattered light information obtained by irradiating the measurement target particles with known particle size distribution information with laser light L F2, a virtual scattered light information calculation unit F5 that calculates virtual scattered light information that is information on virtual scattered light based on the temporary refractive index information and the known particle size distribution information, and the virtual scattered light information. A refractive index setting support unit F4 that outputs the measured scattered light information in a manner that can be compared with the measured scattered light information, and converts the virtual scattered light information into the measured scattered light information. Compared to the degree of coincidence in which a function as match degree calculating section F6, etc. for calculating according to a predetermined calculation formula.
[0046]
A detailed description of each of these units will be given below while also referring to FIGS.
[0047]
As in the first embodiment, first, the particle size distribution of the measurement target particles whose unknown refractive index is unknown is determined in advance, and is set to a known value. Then, information on the known particle size distribution is stored in advance in the known particle size distribution information storage unit D1 in association with a type identifier for identifying the type of the measurement target particle.
[0048]
Next, the sample is irradiated with laser light L, and the scattered light LS is detected by each of the detectors 3.
[0049]
The scattered light intensity signal output from each of the detectors 3 is transmitted to the input / output interface 102 via the signal converter 41. The measured scattered light information receiving unit F2 configured using the input / output interface 102 receives the scattered light intensity signals as measured scattered light information indicating the angular distribution of the scattered light intensity (step ST31). The information is stored in the information storage unit D2 in association with the type identifier.
[0050]
On the other hand, a screen prompting the operator to input a temporary refractive index is displayed on the display 43. Specifically, the refractive index n is represented by a complex number of n '+ ik, so that n' and k can be input. When the temporary refractive index is set on the screen by an arbitrary or selective input by the operator, the temporary refractive index information receiving unit F1 receives the temporary refractive index information as temporary refractive index information (step ST32). The data is stored in the storage unit D3 in association with the type identifier.
[0051]
Next, the virtual scattered light information calculation unit F5 obtains the provisional refractive index information and the known particle size distribution information, and calculates virtual scattered light information that is information on virtual scattered light based on them (step ST33). ).
[0052]
Thereafter, the coincidence calculating unit F6 acquires the measured scattered light information and the virtual scattered light information, and calculates the degree of coincidence of the scattering pattern, that is, the angle distribution of the scattered light intensity (step ST34). The degree of coincidence may be, for example, a parameter having a difference value, a ratio, an absolute value of the difference, a value obtained by squaring the difference, or the like.
[0053]
On the other hand, the refractive index setting support unit F4 also acquires the actually measured scattered light information and the virtual scattered light information, and for example, so that the operator can visually and intuitively determine the difference between the two scattering patterns, Are simultaneously displayed (overlaid display) on the screen, and the degree of coincidence is also displayed (step ST35, step ST36).
[0054]
Therefore, in such a case, if the operator determines, for example, that the set temporary refractive index is inappropriate from the overwritten scattering pattern graph and the degree of coincidence, the operator inputs the temporary refractive index again. By repeating this a plurality of times, an appropriate refractive index can be easily set. In addition, the finally set refractive index has extremely high reliability verified by comparison with a known particle size distribution. And since it is possible to more accurately determine the particle size distribution of other particles of the same type based on the obtained refractive index, for example, for applications such as inspecting the particle size distribution and performing continuous quality control, It will be very suitable.
[0055]
As shown in steps S41 to ST46 in FIG. 10, the temporary refractive index information receiving unit F1 is configured to be able to receive a plurality of temporary refractive index information in parallel, and the virtual scattered light information calculating unit F5 is configured to receive each temporary refractive index information. The virtual scattered light information may be calculated based on the refractive index information, and the virtual scattered light information may be output in the refractive index setting support unit F4 so as to be comparable with the actually measured scattered light information.
[0056]
In this way, compared to inputting a single piece of temporary refractive index information each time, it is possible to save the trouble of inputting and to compare the virtual scattered light information respectively calculated from the plurality of pieces of temporary refractive index information at once. Further, the tendency of the change of the scattered light due to the change of the temporary refractive index information can be more clearly grasped, and the desired refractive index can be set more quickly and easily.
<Fourth embodiment>
[0057]
The particle size distribution measuring apparatus 1 according to the present embodiment has the same hardware configuration as that of the third embodiment except for the functional part of the information processing apparatus 4, and therefore the differences will be mainly described. I do.
[0058]
That is, as shown in FIG. 11, the information processing apparatus 4 according to the fourth embodiment changes the provisional refractive index information based on the calculated degree of coincidence in addition to the components in the fourth embodiment as a functional configuration. And a provisional refractive index information changing unit F7.
[0059]
Specifically, the function of the provisional refractive index information changing unit F7 and the function of each unit generated by adding the function will be described below with reference to FIGS.
[0060]
As in the third embodiment, first, the particle size distribution of the measurement target particles whose unknown refractive index is unknown is determined in advance, and is set to a known value. Then, information on the known particle size distribution is stored in advance in the known particle size distribution information storage unit D1 in association with a type identifier for identifying the type of the measurement target particle.
[0061]
Next, the sample is irradiated with the laser light L, and the detector 3 detects the scattered light scattered by the particles to be measured.
[0062]
The scattered light intensity signal output from each of the detectors 3 is transmitted to the input / output interface 102 via the signal converter 41. The measured scattered light information receiving unit F2 configured using the input / output interface 102 receives the scattered light intensity signals as measured scattered light information indicating the angular distribution of the scattered light intensity (step ST51). The information is stored in the optical information storage unit D2 in association with the type identifier.
[0063]
On the other hand, a screen for inputting a temporary refractive index which is an initial value is displayed to the operator. When the initial provisional refractive index is set on the screen by an arbitrary input or selection input by the operator, the provisional refractive index information receiving unit F1 receives this (step ST52) and temporarily stores the temporary refractive index information in the temporary refractive index information storage unit D3. It is stored as refractive index information in association with the type identifier.
[0064]
Next, the virtual scattered light information calculation unit F5 obtains the provisional refractive index information and the known particle size distribution information, and calculates virtual scattered light information that is information on virtual scattered light based on them (step ST53). ).
[0065]
After that, the coincidence calculating unit F6 acquires the measured scattered light information and the virtual scattered light information, and calculates the degree of coincidence of their scattering patterns, that is, the angle distribution of the scattered light intensity (step ST54). The degree of coincidence may be, for example, a parameter having a difference value, a ratio, an absolute value of the difference, a value obtained by squaring the difference, or the like.
[0066]
Next, the provisional refractive index information changing unit F7 determines whether or not the calculated degree of coincidence is within the allowable range (step ST55). The temporary refractive index information stored in the temporary refractive index information storage unit D3 is changed. Specifically, the values of n and k are changed using, for example, the nonlinear least squares method (step ST56). Then, the calculation is again performed by the virtual scattered light information calculation unit F5 and the coincidence calculation unit F6, and it is automatically determined whether the calculated coincidence is within the allowable range. The permissible range may be stored in a permissible range storage unit (not shown) in advance from, for example, an operator's input.
[0067]
The operations of steps ST53 to ST56 are repeated one or more times, and when the coincidence falls within the allowable range, the refractive index setting support unit F4 acquires the virtual scattered light information and the actually measured scattered light information at that time, In order to allow the operator to visually and intuitively determine the difference between the two scattering pattern shapes, for example, a scattering pattern graph obtained from the information is simultaneously displayed on the screen (overlaid display), and the matching at that time is performed. The degree is displayed (steps ST57 and ST58).
[0068]
Therefore, in such a case, the temporary refractive index information is automatically updated without manually inputting the temporary refractive index information many times, so that a desired refractive index can be obtained more easily, and Burden can be reduced.
[0069]
As in the second embodiment, a range in which the refractive index is automatically selected, refractive index condition information indicating whether or not light is absorbed, a particle diameter range in which particles are never present, and a monomodal / multimodal property. The particle condition information may be stored in a predetermined storage area in advance, and may be referred to when the provisional refractive index information is changed. This is because it can contribute to reliable and quick selection of the refractive index.
[0070]
Further, a graph or a degree of coincidence may be displayed by the refractive index setting support unit F4 every time the degree of coincidence is calculated, and the operator may be asked to input whether or not the temporary refractive index information can be automatically changed each time. This is because, similarly to the second embodiment, even if the degree of coincidence is lower from the graph shape, the operator may determine that the refractive index is appropriate.
[0071]
In addition, the present invention is not limited to the illustrated example, and various changes can be made without departing from the gist of the present invention.
[0072]
【The invention's effect】
As described in detail above, according to the present invention, even when the particle refractive index is unknown, by using the particle size distribution information obtained in advance using an SEM, an optical microscope, or the like, it is relatively easy and appropriate. Refractive index information can be obtained. The refractive index information has extremely high reliability verified by comparison with a known particle size distribution. In addition, since the particle size distribution of other particles of the same type can be more accurately obtained based on the obtained refractive index information, for example, in applications where the particle size distribution is inspected and quality control is continuously performed. It is very suitable for
[Brief description of the drawings]
FIG. 1 is an overall schematic diagram of a dynamic scattering particle size distribution measuring apparatus according to each embodiment of the present invention.
FIG. 2 is a device configuration diagram of an information processing apparatus according to each embodiment of the present invention.
FIG. 3 is a functional configuration diagram of a main part of the information processing apparatus according to the first embodiment of the present invention.
FIG. 4 is an exemplary flowchart showing the operation of the information processing apparatus according to the embodiment;
FIG. 5 is an exemplary flowchart showing the operation of the information processing apparatus according to a modification of the embodiment.
FIG. 6 is a functional configuration diagram of a main part of an information processing apparatus according to a second embodiment of the present invention.
FIG. 7 is an exemplary flowchart illustrating the operation of the information processing apparatus according to the embodiment.
FIG. 8 is a functional configuration diagram of a main part of an information processing apparatus according to a third embodiment of the present invention.
FIG. 9 is an exemplary flowchart illustrating the operation of the information processing apparatus according to the embodiment;
FIG. 10 is an exemplary flowchart showing the operation of the information processing apparatus according to a modification of the embodiment.
FIG. 11 is a functional configuration diagram of a main part of an information processing apparatus according to a third embodiment of the present invention.
FIG. 12 is an exemplary flowchart illustrating the operation of the information processing apparatus according to the embodiment.
[Explanation of symbols]
1: Particle size distribution measuring device
F1 ... provisional refractive index information receiving unit
F2: Measured scattered light information receiving unit
F3: virtual particle size distribution information calculation unit
F4: Refractive index setting support unit
F5: virtual scattered light information calculation unit
F6: Matching degree calculation unit

Claims (15)

The scattered light information, which is information on scattered light generated by irradiating the measurement target particles in the sample with light, and the particle size distribution using the refractive index information, which is information on the refractive index of the measurement target particles with respect to the light, are used. In a particle size distribution measuring device that calculates the particle size distribution information that is information,
A provisional refractive index information receiving unit that receives provisional refractive index information that is information about a provisionally set refractive index,
A measured scattered light information receiving unit that receives measured scattered light information obtained by irradiating the measurement target particles with known particle size distribution information with light,
Based on the provisional refractive index information and the measured scattered light information, a virtual particle size distribution information calculation unit that calculates virtual particle size distribution information that is information on a virtual particle size distribution,
The virtual particle size distribution information is output in a manner that can be compared with the known particle size distribution information of the measurement target particles, and a refractive index setting support unit that supports setting of the refractive index of the measurement target particles. Characteristic particle size distribution measuring device. The provisional refractive index information receiving section receives a plurality of pieces of temporary refractive index information, and the virtual particle diameter distribution information calculating section calculates virtual particle diameter distribution information based on the respective pieces of temporary refractive index information. The particle size distribution measuring device according to claim 1, wherein the ratio setting support unit outputs the respective virtual particle size distribution information so as to be comparable with the known particle size distribution information of the measurement target particles. The scattered light information, which is information on scattered light generated by irradiating the measurement target particles in the sample with light, and the particle size distribution using the refractive index information, which is information on the refractive index of the measurement target particles with respect to the light, are used. In a particle size distribution measuring device that calculates the particle size distribution information that is information,
A provisional refractive index information receiving unit that receives provisional refractive index information that is information about a provisionally set refractive index,
A measured scattered light information receiving unit that receives measured scattered light information obtained by irradiating the measurement target particles with known particle size distribution information with light,
Based on the temporary refractive index information and the known particle size distribution information, a virtual scattered light information calculation unit that calculates virtual scattered light information that is information on virtual scattered light,
The virtual scattered light information is output in a manner that can be compared with the actually measured scattered light information, and a refractive index setting support unit that supports setting of a refractive index of the measurement target particles is provided. apparatus. The temporary refractive index information receiving section receives a plurality of temporary refractive index information, and the virtual scattered light information calculating section calculates virtual scattered light information information based on the respective temporary refractive index information, and 4. The particle size distribution measuring device according to claim 3, wherein the setting support unit outputs each of the virtual scattered light information so as to be comparable with the actually measured scattered light information. The virtual particle diameter distribution information further includes a coincidence degree calculation unit that compares the degree of coincidence with the known particle diameter distribution information of the measurement target particle and calculates the degree of coincidence according to a predetermined calculation formula, and the refractive index setting support unit includes: 3. The particle size distribution measuring device according to claim 1, wherein the degree of coincidence calculated by the degree of coincidence calculation unit is further output. The scattered light information, which is information on scattered light generated by irradiating the measurement target particles in the sample with light, and the particle size distribution using the refractive index information, which is information on the refractive index of the measurement target particles with respect to the light, are used. In a particle size distribution measuring device that calculates the particle size distribution information that is information,
A provisional refractive index information receiving unit that receives provisional refractive index information that is information about a provisionally set refractive index,
A measured scattered light information receiving unit that receives measured scattered light information obtained by irradiating the measurement target particles with known particle size distribution information with light,
Based on the provisional refractive index information and the measured scattered light information, a virtual particle diameter distribution information calculation unit that calculates virtual particle diameter distribution information that is information on a virtual particle diameter distribution, and the virtual particle diameter distribution information A coincidence calculating unit that compares the coincidence with a known particle diameter distribution information of the measurement target particle and calculates the coincidence according to a predetermined calculation formula,
A provisional refractive index information changing unit configured to change the provisional refractive index information based on the calculated degree of coincidence so as to bring the degree of coincidence closer to a target value. When the degree of coincidence and the target value approach within a predetermined range, the virtual particle size distribution information is output in a manner that can be compared with the known particle size distribution information, and the setting of the refractive index of the measurement target particle is supported. 7. The particle size distribution measuring device according to claim 6, further comprising a refractive index setting support unit that performs the setting. The scattered light information, which is information on scattered light generated by irradiating the measurement target particles in the sample with light, and the particle size distribution using the refractive index information, which is information on the refractive index of the measurement target particles with respect to the light, are used. In a particle size distribution measuring device that calculates the particle size distribution information that is information,
A provisional refractive index information receiving unit that receives provisional refractive index information that is information about a provisionally set refractive index,
A measured scattered light information receiving unit that receives measured scattered light information obtained by irradiating the measurement target particles with known particle size distribution information with light,
Based on the temporary refractive index information and the known particle size distribution information, a virtual scattered light information calculation unit that calculates virtual scattered light information that is information on virtual scattered light,
A coincidence calculating unit that compares the virtual scattered light information with the actually measured scattered light information and calculates the coincidence according to a predetermined calculation formula;
A provisional refractive index information changing unit configured to change the provisional refractive index information based on the calculated degree of coincidence so as to bring the degree of coincidence closer to a target value. When the degree of coincidence and the target value approach a predetermined range, the virtual scattered light information is output in a manner that can be compared with the actually measured scattered light information, and a refractive index setting that assists in setting the refractive index of the measurement target particle. The particle size distribution measuring device according to claim 8, further comprising a support unit. The particle size distribution measuring device according to claim 7 or 9, wherein the refractive index setting support unit further outputs the degree of coincidence. The said scattered light information shows the angular distribution of the intensity | strength of the scattered light produced when light is irradiated to a particle, The claim 1, 2, 3, 4, 5, 6, 7, 8, 9, or 10. Particle size distribution measuring device. The scattered light information, which is information on scattered light generated by irradiating the measurement target particles in the sample with light, and the particle size distribution using the refractive index information, which is information on the refractive index of the measurement target particles with respect to the light, are used. In a particle size distribution measuring device that calculates the particle size distribution information that is information,
A provisional refractive index information receiving unit that receives provisional refractive index information that is information about a provisionally set refractive index,
A measured scattered light information receiving unit that receives measured scattered light information obtained by irradiating the measurement target particles with known particle size distribution information with light,
Based on the provisional refractive index information and the measured scattered light information, a virtual particle size distribution information calculation unit that calculates virtual particle size distribution information that is information on a virtual particle size distribution,
The virtual particle size distribution information is output in a manner that can be compared with the known particle size distribution information of the measurement target particles, and has a function as a refractive index setting support unit that supports setting of the refractive index of the measurement target particles. A program for a particle size distribution measuring device, characterized in that: The scattered light information, which is information on scattered light generated by irradiating the measurement target particles in the sample with light, and the particle size distribution using the refractive index information, which is information on the refractive index of the measurement target particles with respect to the light, are used. In a particle size distribution measuring device that calculates the particle size distribution information that is information,
A provisional refractive index information receiving unit that receives provisional refractive index information that is information about a provisionally set refractive index,
A measured scattered light information receiving unit that receives measured scattered light information obtained by irradiating the measurement target particles with known particle size distribution information with light,
Based on the temporary refractive index information and the known particle size distribution information, a virtual scattered light information calculation unit that calculates virtual scattered light information that is information on virtual scattered light,
The virtual scattered light information is output so as to be comparable with the actually measured scattered light information, and a function as a refractive index setting support unit that supports setting of a refractive index of the measurement target particle is provided. Measurement device program. The scattered light information, which is information on scattered light generated by irradiating the measurement target particles in the sample with light, and the particle size distribution using the refractive index information, which is information on the refractive index of the measurement target particles with respect to the light, are used. In a particle size distribution measuring device that calculates the particle size distribution information that is information,
A provisional refractive index information receiving unit that receives provisional refractive index information that is information about a provisionally set refractive index,
A measured scattered light information receiving unit that receives measured scattered light information obtained by irradiating the measurement target particles with known particle size distribution information with light,
Based on the provisional refractive index information and the measured scattered light information, a virtual particle size distribution information calculation unit that calculates virtual particle size distribution information that is information on a virtual particle size distribution,
A coincidence degree calculation unit that compares the virtual particle diameter distribution information with the known particle diameter distribution information of the measurement target particles and calculates the degree of coincidence according to a predetermined calculation formula,
A program for a particle size distribution measuring apparatus, which has a function as a provisional refractive index information changing unit that changes the provisional refractive index information based on the calculated degree of coincidence so as to bring the degree of coincidence close to a target value. . The scattered light information, which is information on scattered light generated by irradiating the measurement target particles in the sample with light, and the particle size distribution using the refractive index information, which is information on the refractive index of the measurement target particles with respect to the light, are used. In a particle size distribution measuring device that calculates the particle size distribution information that is information,
A provisional refractive index information receiving unit that receives provisional refractive index information that is information about a provisionally set refractive index,
A measured scattered light information receiving unit that receives measured scattered light information obtained by irradiating the measurement target particles with known particle size distribution information with light,
Based on the temporary refractive index information and the known particle size distribution information, a virtual scattered light information calculation unit that calculates virtual scattered light information that is information on virtual scattered light,
A coincidence calculating unit that compares the virtual scattered light information with the actually measured scattered light information and calculates the coincidence according to a predetermined calculation formula;
A program for a particle size distribution measuring apparatus, which has a function as a provisional refractive index information changing unit that changes the provisional refractive index information based on the calculated degree of coincidence so as to bring the degree of coincidence close to a target value. .

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