CN118111873A - Optical particle size measurement system, method, device and storage medium - Google Patents
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Abstract
The present disclosure relates to an optical particle size measurement system, method, apparatus, and storage medium. By emitting laser light toward a target sample; collecting scattered light of a plurality of angles formed by scattering the laser by the first particles, and screening scattered light of a preset angle from the scattered light of the plurality of angles for imaging; acquiring the intensity of the scattered light of the screened preset angle according to the imaging result, and calculating the particle size of the first particles according to the intensity of the scattered light of the screened preset angle; the optical particle size measurement system can analyze the particle sizes of various particles in a sample one by one, avoids the difficulty in mathematical treatment and errors caused by the difficulty in mathematical treatment caused by the analysis of all scattered light together, solves the problem that signals of large particles are easy to submerge signals of small particles, improves the accuracy of measuring the particle size distribution, does not need to track the particles, can quickly obtain measurement results, and saves the measurement time.
Description
Technical Field
The present disclosure relates to the field of optics, and in particular, to an optical particle size measurement system, method, apparatus, and storage medium.
Background
Currently, there are three main types of techniques for analyzing the particle size distribution of nano-to micron-sized samples using optical methods, namely, particle size analysis techniques based on static light scattering (STATIC LIGHT SCATTERING, SLS), particle size analysis techniques based on dynamic light scattering (DYNAMIC LIGHT SCATTERING, DLS), and particle size analysis techniques based on particle tracking (Nanoparticle TRACKING ANALYSIS, NTA). The SLS-based particle size analysis technique and the DLS-based particle size analysis technique have the following problems: 1. after mixing different particle sizes, light scattering signals are overlapped, and the overlapped signals are difficult to decompose by mathematical means, so that the accuracy is low and the interference is easy to occur; 2. large particle size particles generally scatter light strongly, small particle size particles scatter light weakly, and for smaller particles (particles in the rayleigh scattering range), the scattered light intensity is proportional to the sixth power of the particle size, so the scattered light signal of a large particle is easily submerged in the scattered light signal of a small particle, resulting in the small particle being ignored. NTA-based particle size analysis techniques require tracking of each particle, which must take a period of time, and if statistically significant needs to be achieved, a large number of particles, resulting in a long total measurement time.
Disclosure of Invention
In view of this, the present disclosure proposes an optical particle size analysis system, method, apparatus, and storage medium.
According to an aspect of the present disclosure, there is provided an optical particle diameter measurement system including: a laser transmitter, an optical path device and a data processing device; wherein,
The laser transmitter is used for transmitting laser to a target sample, and the target sample comprises a plurality of particles;
The light path device is used for collecting scattered light of a plurality of angles formed by scattering the laser by the first particles, and screening scattered light of a preset angle from the scattered light of the plurality of angles for imaging; the first microparticle is any microparticle of the plurality of microparticles; the number of the preset angles is a plurality of;
the data processing device is used for obtaining the intensity of the scattered light of the screened preset angle according to the imaging result, and calculating the particle size of the first particles according to the intensity of the scattered light of the screened preset angle.
In one possible implementation, the light path device includes an imaging light path, a plurality of diaphragms, and an imaging sensor; wherein,
The imaging light path is used for collecting scattered light of a plurality of angles formed by scattering the laser light by the first particles;
the plurality of diaphragms are arranged on the focal plane of the imaging light path, wherein each diaphragm enables scattered light of a preset angle corresponding to the diaphragm to pass through in the scattered light of the plurality of angles, and the preset angles corresponding to different diaphragms are different;
The imaging sensor is arranged in an out-of-focus manner relative to the imaging light path and is used for receiving scattered light passing through the diaphragms and imaging, wherein the positions of the scattered light imaging through different diaphragms are different.
In a possible implementation manner, the data processing apparatus is further configured to:
Calculating the intensity of the scattered light of the screened preset angle according to the imaging result;
determining the light intensity distribution of the scattered light with different preset angles in the screened scattered light with the preset angles according to the intensity of the screened scattered light with the preset angles;
comparing the light intensity distribution of the scattered light with different preset angles in the screened scattered light with the standard light intensity distribution of the rice scattering, and determining the particle size of the first particles; wherein the standard light intensity distribution of the Mie scattering represents the light intensity distribution of scattered light of various angles formed by scattering the laser light by spherical particles with different particle diameters.
In one possible implementation manner, the standard light intensity distribution of rice scattering includes intensity ratios of scattered light of different preset angles formed by scattering the laser light by spherical particles with preset particle sizes, wherein the number of the preset particle sizes is a plurality;
the data processing apparatus is further configured to:
Determining the intensity ratio of the scattered light with different preset angles in the screened scattered light with the preset angles by comparing the intensity of the screened scattered light with the preset angles;
And determining the particle size of the first particles according to the intensity ratio of the scattered light with different preset angles in the screened scattered light with the preset angles and the intensity ratio of the scattered light with different preset angles formed by scattering the laser by spherical particles with preset particle sizes.
In a possible implementation, the data processing device is further configured to determine a particle size distribution of the sample according to particle sizes of the plurality of particles.
According to another aspect of the present disclosure, there is provided an optical particle diameter measurement method applied to the above-mentioned optical particle diameter measurement system; the method comprises the following steps:
emitting laser light toward a target sample, the target sample comprising a plurality of microparticles;
Collecting scattered light of a plurality of angles formed by scattering the laser by the first particles, and screening scattered light of a preset angle from the scattered light of the plurality of angles for imaging; the first microparticle is any microparticle of the plurality of microparticles; the number of the preset angles is a plurality of;
and acquiring the intensity of the scattered light of the screened preset angle according to the imaging result, and calculating the particle size of the first particles according to the intensity of the scattered light of the screened preset angle.
In one possible implementation manner, the collecting the scattered light of multiple angles formed by scattering the laser light by the first particles, and screening out the scattered light of preset angles from the scattered light of multiple angles for imaging includes:
Collecting scattered light of a plurality of angles formed by scattering the laser light by the first particles through an imaging light path;
Screening scattered light with a preset angle from the scattered light with a plurality of angles through a plurality of diaphragms; the plurality of diaphragms are arranged on a focal plane of the imaging light path, each diaphragm enables scattered light of a preset angle corresponding to the diaphragm to pass through in the scattered light of a plurality of angles, and preset angles corresponding to different diaphragms are different;
Receiving scattered light passing through the plurality of diaphragms by an imaging sensor and imaging; the imaging sensor is arranged in an out-of-focus mode relative to the imaging light path, and the imaging positions of scattered light passing through different diaphragms are different.
In one possible implementation manner, the obtaining the intensity of the scattered light at the screened preset angle according to the imaging result, and calculating the particle size of the first particles according to the intensity of the scattered light at the screened preset angle includes:
Calculating the intensity of the scattered light of the screened preset angle according to the imaging result;
determining the light intensity distribution of the scattered light with different preset angles in the screened scattered light with the preset angles according to the intensity of the screened scattered light with the preset angles;
comparing the light intensity distribution of the scattered light with different preset angles in the screened scattered light with the standard light intensity distribution of the rice scattering, and determining the particle size of the first particles; wherein the standard light intensity distribution of the Mie scattering represents the light intensity distribution of scattered light of various angles formed by scattering the laser light by spherical particles with different particle diameters.
In one possible implementation manner, the standard light intensity distribution of rice scattering includes intensity ratios of scattered light of different preset angles formed by scattering the laser light by spherical particles with preset particle sizes, wherein the number of the preset particle sizes is a plurality;
comparing the light intensity distribution of the scattered light with different preset angles in the screened scattered light with the standard light intensity distribution of the rice scattering, and determining the particle size of the first particles, wherein the method comprises the following steps:
Determining the intensity ratio of the scattered light with different preset angles in the screened scattered light with the preset angles by comparing the intensity of the screened scattered light with the preset angles;
And determining the particle size of the first particles according to the intensity ratio of the scattered light with different preset angles in the screened scattered light with the preset angles and the intensity ratio of the scattered light with different preset angles formed by scattering the laser by spherical particles with preset particle sizes.
In one possible implementation, the method further includes: determining a particle size distribution of the sample based on the particle sizes of the plurality of microparticles.
According to another aspect of the present disclosure, there is provided an optical particle diameter measuring apparatus including: a processor; a memory for storing processor-executable instructions; wherein the processor is configured to implement the above-described method when executing the instructions stored by the memory.
According to another aspect of the present disclosure, there is provided a non-transitory computer readable storage medium having stored thereon computer program instructions, wherein the computer program instructions, when executed by a processor, implement the above-described method.
According to another aspect of the present disclosure, there is provided a computer program product comprising a computer readable code, or a non-transitory computer readable storage medium carrying computer readable code, which when run in a processor of an electronic device, performs the above method.
Embodiments of the present disclosure provide for the generation of a laser beam by emitting a laser beam toward a target sample; collecting scattered light of a plurality of angles formed by scattering the laser by the first particles, and screening scattered light of a preset angle from the scattered light of the plurality of angles for imaging; acquiring the intensity of the scattered light of the screened preset angle according to the imaging result, and calculating the particle size of the first particles according to the intensity of the scattered light of the screened preset angle; the optical particle size measurement system can analyze the particle sizes of various particles in a sample one by one, so that mathematical processing difficulty caused by combining all scattered light together for analysis and errors caused by the mathematical processing difficulty are avoided; in addition, as each particle is analyzed one by one, the signals of the large particles cannot submerge the signals of the small particles, the obtained particle size distribution is more accurate and reliable, and the accuracy of measuring the particle size distribution is improved; meanwhile, the optical particle size measurement system disclosed by the disclosure does not need to track particles, can quickly obtain a measurement result, improves the measurement speed and saves the measurement time.
Other features and aspects of the present disclosure will become apparent from the following detailed description of exemplary embodiments, which proceeds with reference to the accompanying drawings.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate exemplary embodiments, features and aspects of the present disclosure and together with the description, serve to explain the principles of the disclosure.
Fig. 1 shows a schematic view of a static light scattering device.
Fig. 2 shows a schematic diagram of the trajectory of the brownian motion of three particles.
Fig. 3 shows a schematic diagram of the dynamic light scattering principle.
Fig. 4 shows a second order correlation function for particles of different sizes.
Fig. 5 shows a schematic diagram of the principle of the particle tracking technique.
Fig. 6 shows a block diagram of an optical particle size measurement system according to an embodiment of the disclosure.
Fig. 7 shows a block diagram of an optical particle size measurement optical path according to an embodiment of the present disclosure.
Fig. 8 shows a schematic view of two particles illuminating an area array image sensor with scattered light emitted at three different angles.
Fig. 9 shows a flow chart of an optical particle size measurement method according to an embodiment of the disclosure.
Fig. 10 shows a block diagram of an electronic device according to an exemplary embodiment of the present disclosure.
Detailed Description
Various exemplary embodiments, features and aspects of the disclosure will be described in detail below with reference to the drawings. In the drawings, like reference numbers indicate identical or functionally similar elements. Although various aspects of the embodiments are illustrated in the accompanying drawings, the drawings are not necessarily drawn to scale unless specifically indicated.
The word "exemplary" is used herein to mean "serving as an example, embodiment, or illustration. Any embodiment described herein as "exemplary" is not necessarily to be construed as preferred or advantageous over other embodiments.
In addition, numerous specific details are set forth in the following detailed description in order to provide a better understanding of the present disclosure. It will be understood by those skilled in the art that the present disclosure may be practiced without some of these specific details. In some instances, methods, means, elements, and circuits well known to those skilled in the art have not been described in detail in order not to obscure the present disclosure.
In the related art, there are three main types of techniques for analyzing the particle size distribution of nano-to micron-sized samples using an optical method, which are a particle size analysis technique based on static light scattering, a particle size analysis technique based on dynamic light scattering, and a particle size analysis technique based on a particle tracking technique, respectively.
Particle size analysis technology based on static light scattering is a technology for obtaining sample particle size information by measuring the angular distribution of scattered light intensity. Particle size analysis techniques based on static light scattering obtain the particle size of a sample by measuring the intensity of scattered light at more than two scattering angles and comparing it to a standard light intensity distribution of rice scattering (MIE SCATTERING). If information of many angles can be accurately collected, the particle size distribution of the fine particles can be obtained roughly in principle by mathematical inversion. Fig. 1 shows a schematic view of a static light scattering device. As shown in fig. 1, the Laser (Laser) passes through the nip and then through the Lens (Lens) to converge on the center of the Sample (Sample), which is typically located in a cylindrical Sample cell. Scattered light is collected by a collection light path (Collecting Optics), received by detectors (e.g., photomultiplier and single photon Detector sensors), and analyzed by subsequent electronics (Detector electronics). The scattered light signals corresponding to different scattering angles can be collected by rotating the collecting light path around the sample. The light trap (Primary beam stop) may absorb unwanted light passing through the lens. However, inverting the particle size distribution using this method encounters the following difficulties: 1. after different particle sizes are mixed together, light scattering signals are superimposed, the difficulty of decomposing the superimposed signals through a mathematical means is high, the accuracy is low, and the interference is easy to occur; 2. the large particle size particles generally scatter light more strongly, and the small particle size particles scatter light less strongly, and for smaller particles (particles in the Rayleigh scattering range), the scattered light intensity is proportional to the size of the particles to the six-fold, so the scattered light signal of the large particles tends to drown out the scattered light signal of the small particles.
Particle size analysis technology based on dynamic light scattering is a technology for obtaining sample particle size information by measuring the time dependence of scattered light intensity. The principle of the particle size analysis technology based on dynamic light scattering is as follows: particles in air and solution inevitably have random thermal motion (i.e., brownian motion) when the ambient temperature is above absolute zero. Fig. 2 shows a schematic diagram of the trajectory of the brownian motion of three particles. For the typical case of dynamic light scattering measurement, the extent of brownian motion of particles can be measured by the diffusion coefficient (D). According to Fick's second law:
wherein, Representing the density distribution of particles (for a single particle,/>Representing the probability density distribution of the particles), t represents time, x represents position, and D represents diffusion coefficient. The diffusion coefficient is related to factors such as temperature, viscosity coefficient, and particle size of the particles. In low reynolds number solvents, the diffusion coefficient of the particles satisfies Stokes-einstein equation (Stokes-Einstein equation):
Where k B is the boltzmann constant, T is absolute temperature, pi is the circumference ratio, η is the viscosity coefficient, and r is the hydrodynamic radius of the particles. For solutions with large numbers of particles, brownian motion results in the distance between the particles changing over time. These particles are irradiated with a laser beam having good coherence, and scattered light of these particles interferes with each other to form scattered light. The variation in the intensity of the scattered light is related to the brownian motion of the particles and thus indirectly also to the particle size of the particles. Fig. 3 shows a schematic diagram of the dynamic light scattering principle. Particle size information of a sample is obtained by measuring the relation of the scattering light intensity of particles with time based on a particle size analysis technology of dynamic light scattering. The relationship of the scattered light intensity of a particle over time is generally represented by a second order correlation function G2:
G2(τ)＝<Is(t)Is(t+τ)>
Where τ represents the correlation time, I s (t) represents the scattered light intensity at time t, and I s (t+τ) represents the scattered light intensity at time t+τ. Fig. 4 shows a second order correlation function for particles of different sizes. The particle size of the microparticles can be obtained by analysis of the second order correlation function, for example, by an algorithm such as the cumulant method (cumulants method). However, analyzing the particle size distribution based on the dynamic light scattering technique has the following difficulties: 1. because the whole effect of all particles in the measuring area is measured, the method also needs to decompose the total signal of the light scattering of all particles by mathematical means, has great difficulty, low accuracy and is easy to be interfered, like a static light scattering method; 2. as with the static light scattering method, generally, the scattering light of particles of large particle size is strong, the scattering light of particles of small particle size is weak, and for smaller particles (particles in the rayleigh scattering range), the scattering light intensity is proportional to the hexagonal of the particle size, so that for a sample in which large particles and small particles are mixed, the scattering light signal of large particles easily floods the scattering light signal of small particles, resulting in that small particles are ignored.
Particle size analysis methods based on particle tracking techniques are methods for analyzing the particle size of a sample by tracking the change in position of particles due to brownian motion over a period of time. Similar to dynamic light scattering techniques, nanoparticle tracking techniques are also based on brownian motion of the particles (see fig. 2). Particles in air and solution, when the ambient temperature is above absolute zero, cause the particles to be constantly impacted by a large number of ambient molecules, resulting in irregular brownian motion, due to thermal motion of the molecules in the environment. The extent of brownian motion of particles (which can be measured by the diffusion coefficient) is related to factors such as temperature, viscosity coefficient, and particle size of the particles. Unlike particle size analysis techniques based on dynamic light scattering, nanoparticle tracking techniques directly track the motion of each particle, and the particle size of each particle is calculated by analyzing the relative displacement of each particle. The particle size distribution of the particles is obtained by counting the particle sizes of a large number of particles. Fig. 5 shows a schematic diagram of a principle of particle tracking technology, as shown in fig. 5, 1 shows a tracking and data analysis computer, 2 shows a sensitive digital camera, 3 shows optical amplification, 4 shows a sampling amount, 5 shows a sample, 6 shows laser light, 7 shows a scattered sample, and the laser light is incident on the sample, each particle in the sample scatters the laser light to form scattered light, the scattered light is received by an optical path device and imaged on an image sensor, the position of the particle at each moment can be obtained on the image sensor, the diffusion coefficient of the particle can be obtained through mathematical analysis, and then the particle size of each particle can be obtained through stokes-einstein equation. The particle size analysis method based on the particle tracking technique has the disadvantages that: since each particle needs to be tracked, which must take a period of time, for example 10 seconds, if a measurement can track 10 particles, then an average of 1 second is required for one particle, and if statistically significant needs to be reached, a large number of particles (for example 10000 particles) must be tracked, resulting in a long total measurement time.
To this end, embodiments of the present disclosure propose an optical particle size measurement system by emitting laser light to a target sample; collecting scattered light of a plurality of angles formed by scattering the laser by the first particles, and screening scattered light of a preset angle from the scattered light of the plurality of angles for imaging; and acquiring the intensity of the scattered light of the screened preset angle according to the imaging result, and calculating the particle size of the first particles according to the intensity of the scattered light of the screened preset angle. The optical particle size measurement system disclosed by the embodiment of the disclosure can analyze the particle sizes of various particles in a sample one by one, so that mathematical processing difficulty and errors caused by the fact that all scattered light is combined together for analysis are avoided; in addition, as each particle is analyzed one by one, the signals of the large particles cannot submerge the signals of the small particles, the obtained particle size distribution is more accurate and reliable, and the accuracy of measuring the particle size distribution is improved; meanwhile, the optical particle size measurement system disclosed by the embodiment of the disclosure does not need to track particles, can quickly obtain measurement results, improves the measurement speed and saves the measurement time.
Fig. 6 shows a block diagram of an optical particle size measurement system according to an embodiment of the disclosure. As shown in fig. 6, the system includes: a laser emitter 10, an optical path device 20, and a data processing device 30; wherein the laser emitter 10 is configured to emit laser light toward a target sample, the target sample including a plurality of particles; the light path device 20 is configured to collect scattered light of a plurality of angles formed by scattering the laser light by the first particles, and screen scattered light of a preset angle from the scattered light of the plurality of angles for imaging; the first microparticle is any microparticle of the plurality of microparticles; the number of the preset angles is a plurality of; the data processing device 30 is configured to obtain the intensity of the scattered light at the screened preset angle according to the imaging result, and calculate the particle size of the first particles according to the intensity of the scattered light at the screened preset angle.
Illustratively, the target sample may be a dilute solution of the dispersion.
For example, the specific value of the preset angle and the number of preset angles may be preset according to actual needs, which is not limited. The preset angle may be an included angle between a preset direction of scattered light of the first particles irradiated by the laser and a preset direction of the laser, and an incident angle of the laser may be set to be 0 degree of the preset angle. For example, the preset angles may be two, 90 degrees and 135 degrees, respectively.
The general optical path can be divided into two types, one type is an optical path with spatial resolution capability, for example, a camera, and can distinguish the light intensity at different positions, but has no angular resolution capability, i.e. does not know at which angle the light emitted by one point is emitted; the other is an angular resolution, such as the static light scattering path described above, but does not have spatial resolution, i.e. it is not known where the light emitted at this angle originates from the sample. The optical particle size measurement system according to embodiments of the present disclosure has both spatial resolution (i.e., can resolve which particle emits light) and angular resolution (i.e., can resolve the distribution of scattered light over angle) for a particular sample (e.g., a dilute solution of a dispersion).
In one possible implementation, the optical path device 20 includes an imaging optical path for collecting scattered light of a plurality of angles formed by scattering the laser light by the first particles.
In one possible implementation manner, the optical path device 20 further includes a plurality of diaphragms disposed on a focal plane of the imaging optical path, where each diaphragm passes a preset angle of scattered light corresponding to the diaphragm among the plurality of angles of scattered light, and preset angles corresponding to different diaphragms are different.
The imaging beam path may be a microscope objective and the aperture may be a pinhole aperture. For example, the plurality of diaphragms may be placed at the positions of a common aperture diaphragm in an optical path, for example, the imaging optical path is a microscope objective, and the plurality of diaphragms may be placed at the positions of the focal plane of the microscope objective.
In one embodiment, three angles may be preset, and three corresponding diaphragms are disposed according to the preset three angles, where each diaphragm corresponds to one preset angle, and each diaphragm can only pass scattered light from the preset angle corresponding to the diaphragm. In the prior art, the light path can only measure scattered light of one particle at a time, and by arranging a plurality of diaphragms, the scattered light energy of only specific scattered angles can be limited to continue to propagate, so that the scattered light intensity of a plurality of angles of a plurality of particles can be measured. In order to obtain the particle size of the particles, at least two preset angles and corresponding diaphragms are required, and the measurement effect of a plurality of preset angles and a plurality of corresponding diaphragms is better, but the light path is more complicated.
In one embodiment, a mask may be prefabricated, and corresponding small holes are designed in advance on the mask according to a preset angle, and the mask is placed on the focal plane of the imaging light path; each small hole corresponds to a small hole diaphragm, each small hole corresponds to a preset angle, and each small hole can only pass scattered light from the preset angle corresponding to the small hole. By way of example, the preset angle corresponding to the aperture can be determined more accurately by measurement after the mask is placed.
In a possible implementation, the optical path device 20 further includes an imaging sensor, which is disposed out of focus with respect to the imaging optical path, for receiving and imaging the scattered light passing through the plurality of diaphragms, wherein the positions of the scattered light imaging by the different diaphragms are different.
The imaging sensor may be an area array image sensor, for example. The imaging sensor is placed out of focus relative to the imaging light path, so that scattered light with different angles formed by scattering of the same particle can strike different positions on the imaging sensor, and further measurement of particle size of the particle is realized. For example, scattered light from three different angles emitted by the first particles impinges on an imaging sensor positioned out of focus with respect to the imaging light path, and the three different angles of scattered light will be imaged in three adjacent areas of the imaging sensor. It will be appreciated that the scattered light passing through the plurality of diaphragms is received by the imaging sensor and imaged slightly differently from conventional imaging due to the out-of-focus placement of the imaging sensor relative to the imaging light path. The light intensity distribution at the corresponding position can be measured by the out-of-focus placement mode in the embodiment of the application, so that the particle size of the particles is measured. When the imaging sensor is placed at the focal position of the imaging light path, scattered light emitted by each particle at different angles will be converged at a point (i.e., at a pixel) on the imaging sensor, and measurement of the particle size of the particle cannot be achieved.
In a possible implementation, the data processing device 30 is further configured to:
Calculating the intensity of the scattered light of the screened preset angle according to the imaging result;
determining the light intensity distribution of the scattered light with different preset angles in the screened scattered light with the preset angles according to the intensity of the screened scattered light with the preset angles;
Comparing the light intensity distribution of the scattered light with different preset angles in the screened scattered light with the standard light intensity distribution of the rice scattering (also called a rice scattering formula) to determine the particle size of the first particles; wherein the standard light intensity distribution of the Mie scattering represents the light intensity distribution of scattered light of various angles formed by scattering the laser light by spherical particles with different particle diameters.
By way of example, by measuring the intensity of the scattered light of the first particles at different preset angles received by the imaging sensor, the light intensity distribution of the scattered light of the first particles at different preset angles may be determined. For example, a correlation coefficient between the light intensity distribution of the scattered light of the first particles at different preset angles and the light intensity distribution of the meter scattering standard may be calculated, and a particle size corresponding to the calculated maximum correlation coefficient may be used as the particle size of the first particles.
In one possible implementation, the standard light intensity distribution of rice scattering includes intensity ratios of scattered light of different preset angles formed by scattering the laser light by spherical particles with preset particle sizes, and the number of the preset particle sizes is a plurality.
In one possible implementation manner, the comparing the light intensity distribution of the scattered light with different preset angles in the screened scattered light with the standard light intensity distribution of the rice scattering, to determine the particle size of the first particles includes: determining the intensity ratio of the scattered light with different preset angles in the screened scattered light with the preset angles by comparing the intensity of the screened scattered light with the preset angles; and determining the particle size of the first particles according to the intensity ratio of the scattered light with different preset angles in the screened scattered light with the preset angles and the intensity ratio of the scattered light with different preset angles formed by scattering the laser by spherical particles with preset particle sizes.
By measuring the intensities of the scattered light of the first particles at different preset angles received by the imaging sensor and comparing the intensities of the scattered light, the ratio of the intensities of the scattered light of the first particles at different preset angles can be calculated.
Illustratively, for spherical particles having a refractive index of 1.5 in an aqueous solution, according to the light intensity distribution of the m scattering standard, spherical particles having a radius of 100nm have a ratio of the light intensity of 135 degrees scattered light to the light intensity of 90 degrees scattered light of 0.74; whereas for spherical particles with a radius of 50nm, the ratio of the intensity of 135 degrees scattered light to 90 degrees scattered light is 0.93. If the ratio of the light intensity of the scattered light of the first particles at 135 degrees to the light intensity of the scattered light at 90 degrees is actually measured to be 0.74, it can be determined that the particle size of the first particles is 100nm.
In a possible implementation, the data processing device 30 is further configured to determine a particle size distribution of the sample according to the particle sizes of the plurality of particles.
Illustratively, the particle size distribution of the sample may be determined by measuring the particle sizes of the plurality of particles in the sample one by measuring the particle sizes of the first particles by the above-described optical particle size measurement system.
Thus, by emitting laser light to the target sample; collecting scattered light of a plurality of angles formed by scattering the laser by the first particles, and screening scattered light of a preset angle from the scattered light of the plurality of angles for imaging; acquiring the intensity of the scattered light of the screened preset angle according to the imaging result, and calculating the particle size of the first particles according to the intensity of the scattered light of the screened preset angle; compared with the particle size analysis technology based on static light scattering and the particle size analysis technology based on dynamic light scattering, the optical particle size measurement system disclosed by the embodiment of the disclosure can analyze the particle sizes of various particles in a sample one by one, so that mathematical processing difficulty caused by combining all scattering lights together for analysis and errors caused by the mathematical processing difficulty are avoided; in addition, as each particle is analyzed one by one, the signals of the large particles cannot submerge the signals of the small particles, the obtained particle size distribution is more accurate and reliable, and the accuracy of measuring the particle size distribution is improved; meanwhile, compared with the particle size analysis technology based on the particle tracking technology, the optical particle size measurement system disclosed by the disclosure does not need to track particles, can quickly obtain measurement results, improves the measurement speed and saves the measurement time.
For example, fig. 7 shows a block diagram of an optical particle size measurement optical path according to an embodiment of the present disclosure. As shown in fig. 7, the sample is irradiated with the incident laser light, which is a beam of light, from the upper left side in the drawing. The sample is located near the middle of the left side of the figure, the sample including a plurality of microparticles; for convenience of description, only two particles are shown in fig. 7 as an example (scattered light of different angles formed by scattering the incident laser light by the two particles is shown by a solid line and a dashed line, respectively), and the number of particles contained in the sample is not limited in the embodiment of the present disclosure. The particles in the sample are irradiated by the laser light, and scattered light is emitted in all directions, and for convenience of description, only three directions of scattered light are drawn for each particle in fig. 7 as an example, and the directions of the scattered light are not limited in the embodiment of the present disclosure. Scattered light from the sample is collected and imaged by an imaging light path (e.g., a microscope objective). Unlike a general microscope optical path in which a plurality of diaphragms are disposed at positions of a general aperture diaphragm (positions corresponding to a microscope objective, i.e., focal planes of the objective), it should be noted that three aperture diaphragms are drawn as examples in fig. 7 for convenience of description, and the number of diaphragms is not limited in the embodiments of the present disclosure. By means of the diaphragms, the scattered light energy of only specific scattering angles can be limited to continue to propagate, namely each diaphragm can only pass the scattered light from the preset angle corresponding to the diaphragm; taking fig. 7 as an example, for two particles in the figure, only the scattered light of the scattering angles corresponding to the three directions shown in the figure passes through the aperture, and the scattered light (not shown in the figure) in the other directions is blocked by the aperture. Unlike conventional out-of-focus placement, the scattered light from each particle at a different angle will converge on a point (pixel) on the sensor, in the disclosed embodiment, the area array image sensor is placed slightly out-of-focus relative to the imaging light path so that the scattered light from different angles scattered by the same particle is incident on different locations (pixels) on the sensor. Fig. 8 shows a schematic view of two particles radiating scattered light at three different angles onto an area array image sensor (fig. 8 is a partial enlarged view of fig. 7). As shown in fig. 8, scattered light emitted from the same particle at three different angles will impinge on three adjacent areas of the sensor. By measuring the signal intensities of the sensors at these adjacent locations and comparing these intensities, the ratio of the scattered light intensity signals from the particles at each scattering angle to each other can be known. And then the particle size of the particles can be calculated by comparing the light intensity distribution with the light intensity distribution of the rice scattering standard. Further, the particle size distribution of the sample can be obtained by analyzing the particle sizes of the plurality of particles at different positions in the sample one by one.
Based on the same inventive concept, the embodiment of the application provides an optical particle size measurement method.
Fig. 9 shows a flow chart illustrating an optical particle size measurement method according to an embodiment of the present disclosure. As shown in fig. 9, the optical particle diameter measuring method is applied to the optical particle diameter measuring system; the method comprises the following steps:
Step 901, emitting laser to a target sample, wherein the target sample comprises a plurality of particles;
Step 902, collecting scattered light of a plurality of angles formed by scattering the laser by the first particles, and screening out scattered light of a preset angle from the scattered light of the plurality of angles for imaging; the first microparticle is any microparticle of the plurality of microparticles; the number of the preset angles is a plurality of;
And 903, acquiring the intensity of the scattered light of the screened preset angle according to the imaging result, and calculating the particle size of the first particles according to the intensity of the scattered light of the screened preset angle.
In one possible implementation manner, the collecting the scattered light of multiple angles formed by scattering the laser light by the first particles, and screening out the scattered light of preset angles from the scattered light of multiple angles for imaging includes:
Collecting scattered light of a plurality of angles formed by scattering the laser light by the first particles through an imaging light path;
Screening scattered light with a preset angle from the scattered light with a plurality of angles through a plurality of diaphragms; the plurality of diaphragms are arranged on a focal plane of the imaging light path, each diaphragm enables scattered light of a preset angle corresponding to the diaphragm to pass through in the scattered light of a plurality of angles, and preset angles corresponding to different diaphragms are different;
Receiving scattered light passing through the plurality of diaphragms by an imaging sensor and imaging; the imaging sensor is arranged in an out-of-focus mode relative to the imaging light path, and the imaging positions of scattered light passing through different diaphragms are different.
In one possible implementation manner, the obtaining the intensity of the scattered light at the screened preset angle according to the imaging result, and calculating the particle size of the first particles according to the intensity of the scattered light at the screened preset angle includes:
Calculating the intensity of the scattered light of the screened preset angle according to the imaging result;
determining the light intensity distribution of the scattered light with different preset angles in the screened scattered light with the preset angles according to the intensity of the screened scattered light with the preset angles;
comparing the light intensity distribution of the scattered light with different preset angles in the screened scattered light with the standard light intensity distribution of the rice scattering, and determining the particle size of the first particles; wherein the standard light intensity distribution of the Mie scattering represents the light intensity distribution of scattered light of various angles formed by scattering the laser light by spherical particles with different particle diameters.
In one possible implementation manner, the standard light intensity distribution of rice scattering includes intensity ratios of scattered light of different preset angles formed by scattering the laser light by spherical particles with preset particle sizes, wherein the number of the preset particle sizes is a plurality;
comparing the light intensity distribution of the scattered light with different preset angles in the screened scattered light with the standard light intensity distribution of the rice scattering, and determining the particle size of the first particles, wherein the method comprises the following steps:
Determining the intensity ratio of the scattered light with different preset angles in the screened scattered light with the preset angles by comparing the intensity of the screened scattered light with the preset angles;
And determining the particle size of the first particles according to the intensity ratio of the scattered light with different preset angles in the screened scattered light with the preset angles and the intensity ratio of the scattered light with different preset angles formed by scattering the laser by spherical particles with preset particle sizes.
In one possible implementation, the method further includes: determining a particle size distribution of the sample based on the particle sizes of the plurality of microparticles.
Embodiments of the present disclosure provide for the generation of a laser beam by emitting a laser beam toward a target sample; collecting scattered light of a plurality of angles formed by scattering the laser by the first particles, and screening scattered light of a preset angle from the scattered light of the plurality of angles for imaging; and acquiring the intensity of the scattered light of the screened preset angle according to the imaging result, and calculating the particle size of the first particles according to the intensity of the scattered light of the screened preset angle. The optical particle size measuring method can analyze the particle sizes of various particles in the sample one by one, so that mathematical processing difficulty caused by combining all scattered light together for analysis and errors caused by the mathematical processing difficulty are avoided; in addition, as each particle is analyzed one by one, the signals of the large particles cannot submerge the signals of the small particles, the obtained particle size distribution is more accurate and reliable, and the accuracy of measuring the particle size distribution is improved; meanwhile, the optical particle size measurement system disclosed by the disclosure does not need to track particles, can quickly obtain a measurement result, improves the measurement speed and saves the measurement time.
The disclosed embodiments also provide a computer readable storage medium having stored thereon computer program instructions which, when executed by a processor, implement the above-described method. The computer readable storage medium may be a volatile or nonvolatile computer readable storage medium.
The embodiment of the disclosure also provides an electronic device, which comprises: a processor; a memory for storing processor-executable instructions; wherein the processor is configured to implement the above-described method when executing the instructions stored by the memory.
Embodiments of the present disclosure also provide a computer program product comprising computer readable code, or a non-transitory computer readable storage medium carrying computer readable code, which when run in a processor of an electronic device, performs the above method.
Fig. 10 is a block diagram illustrating an electronic device 1900 according to an example embodiment. For example, the apparatus 1900 may be provided as a server or terminal device. Referring to fig. 10, the apparatus 1900 includes a processing component 1922 that further includes one or more processors and memory resources represented by memory 1932 for storing instructions, such as application programs, that are executable by the processing component 1922. The application programs stored in memory 1932 may include one or more modules each corresponding to a set of instructions. Further, processing component 1922 is configured to execute instructions to perform the methods described above.
The apparatus 1900 may further include a power component 1926 configured to perform power management of the apparatus 1900, a wired or wireless network interface 1950 configured to connect the apparatus 1900 to a network, and an input/output (I/O) interface 1958. The device 1900 may operate based on an operating system stored in memory 1932, such as Windows Server, mac OS XTM, unixTM, linuxTM, freeBSDTM, or the like.
In an exemplary embodiment, a non-transitory computer readable storage medium is also provided, such as memory 1932, including computer program instructions executable by processing component 1922 of apparatus 1900 to perform the above-described methods.
The present disclosure may be a system, method, and/or computer program product. The computer program product may include a computer readable storage medium having computer readable program instructions embodied thereon for causing a processor to implement aspects of the present disclosure.
The computer readable storage medium may be a tangible device that can hold and store instructions for use by an instruction execution device. The computer readable storage medium may be, for example, but not limited to, an electronic storage device, a magnetic storage device, an optical storage device, an electromagnetic storage device, a semiconductor storage device, or any suitable combination of the foregoing. More specific examples (a non-exhaustive list) of the computer-readable storage medium would include the following: portable computer disks, hard disks, random Access Memory (RAM), read-only memory (ROM), erasable programmable read-only memory (EPROM or flash memory), static Random Access Memory (SRAM), portable compact disk read-only memory (CD-ROM), digital Versatile Disks (DVD), memory sticks, floppy disks, mechanical coding devices, punch cards or in-groove structures such as punch cards or grooves having instructions stored thereon, and any suitable combination of the foregoing. Computer-readable storage media, as used herein, are not to be construed as transitory signals per se, such as radio waves or other freely propagating electromagnetic waves, electromagnetic waves propagating through waveguides or other transmission media (e.g., optical pulses through fiber optic cables), or electrical signals transmitted through wires.
The computer readable program instructions described herein may be downloaded from a computer readable storage medium to a respective computing/processing device or to an external computer or external storage device over a network, such as the internet, a local area network, a wide area network, and/or a wireless network. The network may include copper transmission cables, fiber optic transmissions, wireless transmissions, routers, firewalls, switches, gateway computers and/or edge servers. The network interface card or network interface in each computing/processing device receives computer readable program instructions from the network and forwards the computer readable program instructions for storage in a computer readable storage medium in the respective computing/processing device.
The computer program instructions for performing the operations of the present disclosure may be assembly instructions, instruction Set Architecture (ISA) instructions, machine-related instructions, microcode, firmware instructions, state setting data, or source or object code written in any combination of one or more programming languages, including an object oriented programming language such as SMALLTALK, C ++ or the like and conventional procedural programming languages, such as the "C" programming language or similar programming languages. The computer readable program instructions may be executed entirely on the user's computer, partly on the user's computer, as a stand-alone software package, partly on the user's computer and partly on a remote computer or entirely on the remote computer or server. In the case of a remote computer, the remote computer may be connected to the user's computer through any kind of network, including a Local Area Network (LAN) or a Wide Area Network (WAN), or may be connected to an external computer (for example, through the Internet using an Internet service provider). In some embodiments, aspects of the present disclosure are implemented by personalizing electronic circuitry, such as programmable logic circuitry, field Programmable Gate Arrays (FPGAs), or Programmable Logic Arrays (PLAs), with state information of computer readable program instructions, which can execute the computer readable program instructions.
Various aspects of the present disclosure are described herein with reference to flowchart illustrations and/or block diagrams of methods, apparatus (systems) and computer program products according to embodiments of the disclosure. It will be understood that each block of the flowchart illustrations and/or block diagrams, and combinations of blocks in the flowchart illustrations and/or block diagrams, can be implemented by computer-readable program instructions.
These computer readable program instructions may be provided to a processor of a general purpose computer, special purpose computer, or other programmable data processing apparatus to produce a machine, such that the instructions, which execute via the processor of the computer or other programmable data processing apparatus, create means for implementing the functions/acts specified in the flowchart and/or block diagram block or blocks. These computer readable program instructions may also be stored in a computer readable storage medium that can direct a computer, programmable data processing apparatus, and/or other devices to function in a particular manner, such that the computer readable medium having the instructions stored therein includes an article of manufacture including instructions which implement the function/act specified in the flowchart and/or block diagram block or blocks.
The computer readable program instructions may also be loaded onto a computer, other programmable data processing apparatus, or other devices to cause a series of operational steps to be performed on the computer, other programmable apparatus or other devices to produce a computer implemented process such that the instructions which execute on the computer, other programmable apparatus or other devices implement the functions/acts specified in the flowchart and/or block diagram block or blocks.
The flowcharts and block diagrams in the figures illustrate the architecture, functionality, and operation of possible implementations of systems, methods and computer program products according to various embodiments of the present disclosure. In this regard, each block in the flowchart or block diagrams may represent a module, segment, or portion of instructions, which comprises one or more executable instructions for implementing the specified logical function(s). In some alternative implementations, the functions noted in the block may occur out of the order noted in the figures. For example, two blocks shown in succession may, in fact, be executed substantially concurrently, or the blocks may sometimes be executed in the reverse order, depending upon the functionality involved. It will also be noted that each block of the block diagrams and/or flowchart illustration, and combinations of blocks in the block diagrams and/or flowchart illustration, can be implemented by special purpose hardware-based systems which perform the specified functions or acts, or combinations of special purpose hardware and computer instructions.
The foregoing description of the embodiments of the present disclosure has been presented for purposes of illustration and description, and is not intended to be exhaustive or limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the various embodiments described. The terminology used herein was chosen in order to best explain the principles of the embodiments, the practical application, or the technical improvements in the marketplace, or to enable others of ordinary skill in the art to understand the embodiments disclosed herein.
Claims (10)
1. An optical particle size measurement system, comprising: a laser transmitter, an optical path device and a data processing device; wherein,
The laser transmitter is used for transmitting laser to a target sample, and the target sample comprises a plurality of particles;
The light path device is used for collecting scattered light of a plurality of angles formed by scattering the laser by the first particles, and screening scattered light of a preset angle from the scattered light of the plurality of angles for imaging; the first microparticle is any microparticle of the plurality of microparticles; the number of the preset angles is a plurality of;
the data processing device is used for obtaining the intensity of the scattered light of the screened preset angle according to the imaging result, and calculating the particle size of the first particles according to the intensity of the scattered light of the screened preset angle.
2. The optical particle size measurement system of claim 1, wherein the light path means comprises an imaging light path, a plurality of diaphragms, and an imaging sensor; wherein,
The imaging light path is used for collecting scattered light of a plurality of angles formed by scattering the laser light by the first particles;
the plurality of diaphragms are arranged on the focal plane of the imaging light path, wherein each diaphragm enables scattered light of a preset angle corresponding to the diaphragm to pass through in the scattered light of the plurality of angles, and the preset angles corresponding to different diaphragms are different;
The imaging sensor is arranged in an out-of-focus manner relative to the imaging light path and is used for receiving scattered light passing through the diaphragms and imaging, wherein the positions of the scattered light imaging through different diaphragms are different.
3. The optical particle size measurement system of claim 1, wherein the data processing device is further configured to:
Calculating the intensity of the scattered light of the screened preset angle according to the imaging result;
determining the light intensity distribution of the scattered light with different preset angles in the screened scattered light with the preset angles according to the intensity of the screened scattered light with the preset angles;
comparing the light intensity distribution of the scattered light with different preset angles in the screened scattered light with the standard light intensity distribution of the rice scattering, and determining the particle size of the first particles; wherein the standard light intensity distribution of the Mie scattering represents the light intensity distribution of scattered light of various angles formed by scattering the laser light by spherical particles with different particle diameters.
4. The optical particle size measurement system of claim 3, wherein the standard light intensity distribution for rice scattering includes intensity ratios of scattered light at different preset angles formed by scattering the laser light by spherical particles of preset particle sizes, the number of preset particle sizes being a plurality;
the data processing apparatus is further configured to:
Determining the intensity ratio of the scattered light with different preset angles in the screened scattered light with the preset angles by comparing the intensity of the screened scattered light with the preset angles;
And determining the particle size of the first particles according to the intensity ratio of the scattered light with different preset angles in the screened scattered light with the preset angles and the intensity ratio of the scattered light with different preset angles formed by scattering the laser by spherical particles with preset particle sizes.
5. The optical particle size measurement system of claim 1, wherein the data processing device is further configured to determine a particle size distribution of the sample based on particle sizes of the plurality of particles.
6. An optical particle diameter measuring method, characterized by being applied to the optical particle diameter measuring system according to any one of claims 1 to 5; the method comprises the following steps:
emitting laser light toward a target sample, the target sample comprising a plurality of microparticles;
Collecting scattered light of a plurality of angles formed by scattering the laser by the first particles, and screening scattered light of a preset angle from the scattered light of the plurality of angles for imaging; the first microparticle is any microparticle of the plurality of microparticles; the number of the preset angles is a plurality of;
and acquiring the intensity of the scattered light of the screened preset angle according to the imaging result, and calculating the particle size of the first particles according to the intensity of the scattered light of the screened preset angle.
7. The method according to claim 6, wherein collecting the scattered light of a plurality of angles formed by scattering the laser light by the first particles, and screening out the scattered light of a predetermined angle from the scattered light of the plurality of angles, and imaging, comprises:
Collecting scattered light of a plurality of angles formed by scattering the laser light by the first particles through an imaging light path;
Screening scattered light with a preset angle from the scattered light with a plurality of angles through a plurality of diaphragms; the plurality of diaphragms are arranged on a focal plane of the imaging light path, each diaphragm enables scattered light of a preset angle corresponding to the diaphragm to pass through in the scattered light of a plurality of angles, and preset angles corresponding to different diaphragms are different;
Receiving scattered light passing through the plurality of diaphragms by an imaging sensor and imaging; the imaging sensor is arranged in an out-of-focus mode relative to the imaging light path, and the imaging positions of scattered light passing through different diaphragms are different.
8. The method according to claim 6, wherein the step of obtaining the intensity of the scattered light at the selected preset angle based on the imaging result and calculating the particle size of the first fine particles based on the intensity of the scattered light at the selected preset angle comprises:
Calculating the intensity of the scattered light of the screened preset angle according to the imaging result;
determining the light intensity distribution of the scattered light with different preset angles in the screened scattered light with the preset angles according to the intensity of the screened scattered light with the preset angles;
comparing the light intensity distribution of the scattered light with different preset angles in the screened scattered light with the standard light intensity distribution of the rice scattering, and determining the particle size of the first particles; wherein the standard light intensity distribution of the Mie scattering represents the light intensity distribution of scattered light of various angles formed by scattering the laser light by spherical particles with different particle diameters.
9. An optical particle diameter measuring apparatus, comprising:
A processor;
a memory for storing processor-executable instructions;
Wherein the processor is configured to implement the method of any one of claims 6 to 8 when executing the instructions stored by the memory.
10. A non-transitory computer readable storage medium having stored thereon computer program instructions, which when executed by a processor, implement the method of any of claims 6 to 8.
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