CN111650100A - Particle size measuring equipment based on Mie's scattering theory - Google Patents

Particle size measuring equipment based on Mie's scattering theory Download PDF

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CN111650100A
CN111650100A CN202010548966.4A CN202010548966A CN111650100A CN 111650100 A CN111650100 A CN 111650100A CN 202010548966 A CN202010548966 A CN 202010548966A CN 111650100 A CN111650100 A CN 111650100A
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杨亮
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Eastern Liaoning University
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    • G01N15/0205—Investigating particle size or size distribution by optical means
    • G01N15/0211—Investigating a scatter or diffraction pattern
    • G—PHYSICS
    • G01—MEASURING; TESTING
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    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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    • G—PHYSICS
    • G01—MEASURING; TESTING
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    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
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    • G01N21/49—Scattering, i.e. diffuse reflection within a body or fluid
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/02—Investigating particle size or size distribution
    • G01N15/0205—Investigating particle size or size distribution by optical means
    • G01N15/0211—Investigating a scatter or diffraction pattern
    • G01N2015/0222—Investigating a scatter or diffraction pattern from dynamic light scattering, e.g. photon correlation spectroscopy
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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Abstract

The invention discloses a particle size measuring device based on Mie scattering theory, and particularly relates to the field of particle size measuring methods, wherein the particle size measuring device comprises a parallel light generating module, a sample dispersing module, a light scattering collecting module, an electric control two-dimensional guide table and a data processing module; the parallel light generating module, the sample dispersing module and the light scattering collecting module are distributed in a straight line shape from left to right. The invention adopts an area array CCD as a receiving device to obtain an Airy-patch image, extracts position information of the Airy-patch image, realizes image guide centering, obtains centering correction parameters, improves the accuracy of a measurement result, controls the position of the area array CCD by designing a two-dimensional guide table, shoots a plurality of images at different positions, collects a large-angle light scattering energy diagram by using an image splicing technology, dynamically divides a scattering angle by using an image processing method, improves the resolution of granularity measurement, improves the traditional inversion algorithm by using a neural network principle, and improves the accuracy, speed and reliability of the algorithm.

Description

Particle size measuring equipment based on Mie's scattering theory
Technical Field
The embodiment of the invention relates to the field of particle size measurement methods, in particular to particle size measurement equipment based on Mie scattering theory.
Background
Particles are particles with a specific geometry ranging from millimeters to nanometers, such as the powdery substances often found in life, air droplets and air bubbles in water, which can be called granules. In general, we define the size of a particle as the particle size of the particle. The percentage of particles of different sizes in the total particle population is defined as the particle size distribution of the particles.
In the materials industry, many solid products exist in the powder state. The size and distribution of the particle size are important parameters for determining the properties of the powder. For example, the setting time and final strength of cement are greatly related to the granularity of cement; the catalytic effect of the catalyst is closely related to the particle size of the catalyst; the finishing effect and surface gloss of the coating are affected by the particle size of the coating; the absorption rate and the curative effect of the medicine are related to the granularity of the medicine; the quality and properties of mineral filler products are likewise influenced by their particle size, etc. It can be seen that particle size measurement of particles occupies a very important position in various fields, and therefore, how to effectively measure and control the particle size of particles has a very profound significance.
The methods for measuring particle size at home and abroad include microscopy, sieving, resistance, sedimentation, gravimetric, ultrasonic, turbidity, light scattering and the like. The light scattering method has the advantages of non-contact measurement, no interference on the state of a measured object, short measurement time, real-time measurement and the like, and is the most commonly applied measurement method at present.
The foreign laser granularity testing technology is developed earlier and faster, and a plurality of related products are developed and produced. Representative companies are: coulter in the united states, SYMIPATEC GmbH in germany, marwen in the united kingdom, etc. In recent years, researchers want to widen the measurement range of the particle size by various methods, and the main method adopted by the researchers is to select a plurality of detectors based on the mie theory and the fraunhofer diffraction theory, and receive scattered light information at different angles, so as to achieve the purpose of extending the test range. Among them, there are products of several companies which have a large influence.
1. The particle analyzer developed and produced by Coulter corporation in the united states is based on fraunhofer and Mie scattering theories, takes a solid semiconductor laser as a light source, and adopts a double-lens technology, so that the lower limit of measurement is reduced. There are 132 detectors inside, can receive the light signal from all directions accurately.
2. The particle analyzer developed by Cilas (Cilas) of france adopts a semiconductor laser and a fiber laser as light sources. Can be connected with a CCD image controller, and can carry out real-time observation.
3. The particle size analyzer developed by the German New Bartaic (Sympatec) is based on the Fraunhofer principle, 31 sensors are arranged in the particle size analyzer, a helium light source is used as a light source, the dry test is a unique technology, the sample consumption is small, and the repeatability of the particle size analyzer is good.
In the late 20 th century and 80 s, China began to research and develop laser particle size analyzer. Early granulators were mainly of the sedimentation type, and the principle thereof was that dust particles could be classified during sedimentation, and these granulators had many defects, so commercial granulators were mainly imported. Along with the progress of scientific technology in recent years, the development of laser particle size testing technology in China is rapid, the performance of a particle size analyzer is continuously improved, the dynamic range is wider and wider, and the representative main points are as follows: products such as ' Oumecke ' of the Zhuhai, ' Baite ' of the Dandong, ' micro-nano ' of the Jinnan ' and ' Jingxin ' of the Sichuan Chengdu.
The market of the laser particle analyzer in China develops rapidly, and the prospect is very optimistic. The method has stable market demand, large demand and vitality, and provides good power for the development of a domestic particle analyzer. However, compared with the foreign particle analyzer products, the domestic particle analyzer has some gaps, which mainly show the aspects of test range, measurement precision, measurement repeatability, resolution and reliability of the instrument, and the like.
Disclosure of Invention
Therefore, the embodiment of the invention provides particle size measuring equipment based on the Mie scattering theory, and aims to solve the problems of weak testing range, measuring precision, measuring repeatability, instrument resolution and reliability of a domestic particle size analyzer in the prior art.
In order to achieve the above object, the embodiments of the present invention provide the following technical solutions: a particle size measuring device based on Mie's scattering theory comprises a parallel light generating module, a sample dispersing module, a light scattering collecting module, an electric control two-dimensional guide table and a data processing module;
the parallel light generating module is used for emitting monochromatic parallel light beams, and the light beams pass through a sample pool in the sample dispersing module and are focused on the light scattering collecting module to form a scattered light energy image;
the output end of the light scattering acquisition module is connected with the input end of the data processing module, the light scattering acquisition module is used for acquiring the image and sending the image to the data processing module, and the data processing module is used for converting the acquired image information into digital signals and calculating to obtain the results of particle size and distribution;
the light scattering acquisition module is arranged on the electric control two-dimensional guide table and is adjusted and fixed through the electric control two-dimensional guide table.
Further, the parallel light produces the module and includes from left to right is a style of calligraphy laser instrument, spatial filter, collimating lens and the diaphragm that distributes in proper order, spatial filter comprises beam expanding lens, support and pinhole, beam expanding lens and pinhole set up side by side between laser instrument and collimating lens, and the beam expanding lens is close to the laser instrument side and sets up, beam expanding lens and pinhole are installed on the support.
Further, the sample dispersion module includes sample cell, agitator, ultrasonic wave deconcentrator and discharging equipment, the agitator is installed in the sample cell top, the ultrasonic wave deconcentrator is installed in the sample cell bottom, discharging equipment sets up in sample cell bottom one side, discharging equipment specifically is the discharge valve.
Further, the sample cell is made of quartz glass material, and a surfactant is added into the sample cell.
Furthermore, the sample dispersing module further comprises a cleaning system, the cleaning system is composed of a water pump and a water tank, the sample tank and the water tank are communicated through a cleaning pipeline, and the water pump is installed on the cleaning pipeline and used for pumping clean water in the water tank into the sample tank to clean the sample tank.
Further, the light scattering acquisition module comprises a Fourier lens, an area array CCD and a photocell, the Fourier lens is arranged between the sample cell and the area array CCD and is concentrically arranged with the diaphragm, the photocell is arranged on the outer side of the area array CCD, and the area array CCD and the photocell are both connected with the data processing module.
Further, the electronic control two-dimensional guide table comprises a two-dimensional guide table and a main control chip, the two-dimensional guide table comprises a transverse screw rod, a longitudinal screw rod and two sliders which are respectively installed outside the transverse screw rod and the longitudinal screw rod in a threaded mode, the longitudinal screw rod is installed on the sliders outside the transverse screw rod, the longitudinal screw rod is perpendicular to the transverse screw rod, and the area array CCD is installed on the sliders outside the transverse screw rod.
Furthermore, the transverse screw rod and the longitudinal screw rod are driven by servo motors, and the servo motors are controlled by a control circuit in the main control chip.
Furthermore, the data processing module comprises a data acquisition circuit and a computer, wherein the data acquisition circuit is used for converting image information acquired by the area array CCD into digital signals and transmitting the digital signals to the computer, and converting analog electric signals output by the photocell into digital signals and transmitting the digital signals to the computer.
Further, the computer gives image centering information by using an image processing technology and guides centering; the computer splices a plurality of scattered light energy images at different positions by using a splicing technology to give large-angle scattered light energy information; the computer adopts an inversion algorithm to calculate, and scattered light energy information obtained by the area array CCD and the photocell is converted into the result of the particle size and the distribution of the particles to be measured.
The embodiment of the invention has the following advantages:
1. the invention adopts an area array CCD as a receiving device to obtain an Airy spot image, extracts the position information of the Airy spot image, realizes image-guided centering, and calculates centering correction parameters to improve the accuracy of a measuring result;
2. the invention controls the position of the area array CCD by designing a two-dimensional guide table, and shoots a plurality of images at different positions;
3. the invention collects a large-angle light scattering energy diagram by using an image splicing technology;
4. the invention utilizes an image processing method to dynamically divide scattering angles and improve the resolution of granularity measurement;
5. the invention utilizes the neural network principle, improves the traditional inversion algorithm and improves the accuracy, speed and reliability of the algorithm.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It should be apparent that the drawings in the following description are merely exemplary, and that other embodiments can be derived from the drawings provided by those of ordinary skill in the art without inventive effort.
The structures, ratios, sizes, and the like shown in the present specification are only used for matching with the contents disclosed in the specification, so as to be understood and read by those skilled in the art, and are not used to limit the conditions that the present invention can be implemented, so that the present invention has no technical significance, and any structural modifications, changes in the ratio relationship, or adjustments of the sizes, without affecting the effects and the achievable by the present invention, should still fall within the range that the technical contents disclosed in the present invention can cover.
FIG. 1 is a block diagram of an overall system provided by the present invention;
FIG. 2 is a schematic structural diagram of a sample distribution module according to the present invention;
FIG. 3 is a schematic diagram of a two-dimensional guide table structure according to the present invention;
FIG. 4 is a scattering diagram of light-irradiated particles provided by the present invention;
in the figure: the device comprises a 1 parallel light generating module, a 11 laser, a 12 spatial filter, a 13 collimating lens, a 14 diaphragm, a 2 sample dispersing module, a 21 sample pool, a 22 stirrer, a 23 ultrasonic disperser, a 24 discharge device, a 25 water pump, a 26 water pool, a 3 light scattering acquisition module, a 31 Fourier lens, a 32 area array CCD, a 33 photocell, a 4 electric control two-dimensional guide table, a 41 two-dimensional guide table, a 42 main control chip, a 5 data processing module, a 51 data acquisition circuit, a 52 computer, a 6 transverse screw rod, a 7 longitudinal screw rod and an 8 sliding block.
Detailed Description
The present invention is described in terms of particular embodiments, other advantages and features of the invention will become apparent to those skilled in the art from the following disclosure, and it is to be understood that the described embodiments are merely exemplary of the invention and that it is not intended to limit the invention to the particular embodiments disclosed. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Mie scattering theory considers that the scattering, absorption, and spatial angular distribution of scattered light by a particle depends on the properties of the particular particle itself. The method provides an equation set when the plane electromagnetic wave is incident on a uniform medium sphere with any particle size and an analytic solution of the equation set under the boundary condition. In fact, the theory includes the theory of fraunhofer and fischer diffraction and geometric optics, in which the particle size is small compared to the wavelength, and the particle size is larger than the wavelength.
According to the Mie scattering theory, the scattering light intensity distribution of spherical particles with any particle size can be calculated, and the light intensity distribution is closely related to the particle size and the distribution of the particles, which is the basis for measuring the particle size by a light scattering method. Therefore, the particle size distribution of the particles can be calculated by grasping the relationship between the particle size and the scattered light and measuring the scattered light intensity distribution.
From the mie theory, when a beam has a wavelength of λ, the light intensity is I0When a single spherical particle is irradiated by the monochromatic plane wave, the light intensity distribution of the scattered light is as follows:
Figure RE-GDA0002615417410000051
phi is the angle between the vibration surface of the incident light and the scattering surface, and gamma is the distance between the observation point and the scattering body. Intensity function i1、i2Comprises the following steps:
Figure 1
Figure 2
wherein, an、bnIs the Mie's coefficient, which is a parameter of the relative refractive index m and no dimension of the particle
Figure RE-GDA0002615417410000063
The function of (2) can be represented by a half-integer-order Bessel function and a second-class Hankel function. τ n, π n are related to the scattering angle θ, and can be expressed in terms of the legendre and first order associative legendre functions of cos θ.
Under the irradiation of parallel light beams, the particles generate scattered light, and the scattering direction and the incident direction form an included angle related to the particle size of the particles. The relationship is that the smaller the particle size, the larger the angle at which light is scattered; the larger the particle, the smaller the angle at which the light is scattered. The number of particles determines the intensity of scattered light, the more particles, the greater the intensity of scattered light, and by measuring the intensity of scattered light at different angles, the particle size distribution of the particle sample to be measured can be obtained.
The scattered light is imaged by the fourier lens 31 in its focal plane to form concentric rings of different sizes, the energy of the scattered light being the light scattered by the particles over the respective annular area, the integral of its light energy. After the parallel light beam passes through the particles, the unscattered light is converged at the focal point of the fourier lens 31 to form an airy disk. As shown in fig. 4.
The position of the maximum value of scattered light energy is obtained by Mie's theory as follows:
Figure RE-GDA0002615417410000064
where rm is the maximum halo radius of energy, λ is the wavelength of incident light, f is the focal length of the lens, DmIs the particle size.
The size of the light receiving ring of the detector determines the upper limit and the lower limit of the measuring range. The calculation formula of the diameter of the Airy spot formed on the focal plane of the parallel light beam after passing through the Fourier transform lens is
Figure RE-GDA0002615417410000071
Where f is the focal length of the Fourier lens 31, DlIs the diameter of the diaphragm 14. The focal length f of the fourier lens 31 used in the present invention is 75mm, the wavelength λ of the laser 11 is 0.671 μm, and Dl40mm, so the diameter d of the airy diskaIs 3 μm.
And calculating parameters such as the width of each ring band of the scattered light energy ring, the inner diameter and the outer diameter of each ring and the like according to the Mie's theory. The photocell 33 for small particle measurement is designed for size and position.
The area array CCD32 and the photocell 33 transmit the received light ring information to the computer 52 through the data acquisition circuit 51, and the computer 52 processes the data and adopts an inversion algorithm to obtain the particle size and the distribution condition thereof.
The current inversion algorithms are mainly classified into two types, one is a non-independent mode algorithm, and the other is an independent mode algorithm. The dependent mode algorithm generally knows that the particle size distribution of the particle system satisfies a certain functional relation expression in advance, and then solves the particle size distribution on the basis of the mathematical model. This method is very limited in practical use.
Therefore, the present invention will employ a standalone mode algorithm. The algorithm can obtain the particle size distribution of any particle system, but is sensitive to noise and easy to distort the particle size result. Therefore, the invention introduces the neural network theory to improve on the basis of the traditional independent mode algorithm, and improves the measurement precision, the measurement speed and the reliability. The method comprises the following specific steps:
referring to the attached drawing 1 of the specification, the particle size measuring device based on the Mie scattering theory of the embodiment comprises a parallel light generating module 1, a sample dispersing module 2, a light scattering collecting module 3, an electric control two-dimensional guide table 4 and a data processing module 5;
the parallel light generating module 1, the sample dispersing module 2 and the light scattering acquisition module 3 are distributed in a straight line shape from left to right, the parallel light generating module 1 is used for emitting monochromatic parallel light beams, and the light beams pass through a sample cell 21 in the sample dispersing module 2 and are focused on the light scattering acquisition module 3 to form a scattered light energy image;
the output end of the light scattering acquisition module 3 is connected with the input end of the data processing module 5, the light scattering acquisition module 3 is used for acquiring the image and sending the image to the data processing module 5, and the data processing module 5 is used for converting the acquired image information into a digital signal and calculating to obtain the result of the particle size and the distribution;
the light scattering acquisition module 3 is arranged on the electric control two-dimensional guide table 4, and the light scattering acquisition module 3 is adjusted and fixed through the electric control two-dimensional guide table 4.
The implementation scenario is specifically as follows: the parallel light generating module 1 generates parallel monochromatic light beams to irradiate a sample cell 21 in a sample dispersing module 2, and when no particles exist in the sample cell 21, the parallel light beams pass through a Fourier lens 31 in a light scattering collecting module 3 and are focused at the center of a receiving surface;
when a particle sample is in the sample cell 21, a part of the converged light beam is scattered by the particles, and a ring-shaped image, namely a scattered light energy image, is formed at the back focal plane, namely a receiving plane, of the Fourier lens 31;
the light scattering acquisition module 3 acquires and sends the image to the data processing module 5, the data processing module 5 processes the image, the analog signal is converted into a digital signal, and the result of the particle size and the distribution is obtained through calculation.
Referring to specification figure 1, parallel light produces module 1 includes from left to right is a style of calligraphy laser 11, spatial filter 12, collimating lens 13 and the diaphragm 14 that distributes in proper order, spatial filter 12 comprises beam expander, support and pinhole, beam expander and pinhole set up side by side between laser 11 and collimating lens 13, and the beam expander is close to the setting of 11 sides of laser, beam expander and pinhole are installed on the support.
The implementation scenario is specifically as follows: the parallel light generating module 1 of the invention has the main function of expanding and collimating the thin light beam emitted by the laser 11 to form a parallel light beam with proper size and uniform light intensity as the incident light of the sample cell 21. The structure of the laser mainly comprises a laser 11, a spatial filter 12, a collimating lens 13, a diaphragm 14 and the like. The spatial filter 12 is composed of a beam expander, a support and a special pinhole, and mainly functions to reduce interference caused by high-order scattered light. The laser thin beam is converged to a back focus by a beam expander, and the back focus of the beam expander is coincided with a front focus of a collimating lens 13. A pinhole is placed at the common focus for filtering, so that high-frequency noise can be eliminated, and then the high-frequency noise is diverged from the focus to form spherical waves. The collimating lens 13 adjusts the spherical wave into a plane wave with a larger diameter, so that the sample cell 21 with a certain size can be conveniently irradiated, and an ideal rice-type scattering model can be obtained;
the invention selects the semiconductor laser 11 with long service life, low power consumption and short preheating time, the wavelength is 671nm, and the power is 5 mw. The laser 11 can work continuously for a long time, and the failure rate of the instrument is reduced to a great extent. The beam expander used in the spatial filter 12 was 40x, the pinhole diameter was 15 μm, and the focal length of the collimator lens 13 was 75 mm.
Referring to the attached fig. 2 of the specification, the sample dispersing module 2 includes a sample cell 21, an agitator 22, an ultrasonic disperser 23, and a discharge device 24, wherein the agitator 22 is installed at the top of the sample cell 21, the ultrasonic disperser 23 is installed at the bottom of the sample cell 21, the discharge device 24 is disposed at one side of the bottom of the sample cell 21, and the discharge device 24 is specifically a discharge valve.
Further, the sample cell 21 is made of quartz glass material, and a surfactant is added in the sample cell 21.
Further, the sample dispersing module 2 further comprises a cleaning system, the cleaning system is composed of a water pump 25 and a water tank 26, the sample tank 21 and the water tank 26 are communicated through a cleaning pipeline, and the water pump 25 is installed on the cleaning pipeline and used for pumping clean water in the water tank 26 into the sample tank 21 to clean the sample tank 21.
The implementation scenario is specifically as follows: in the particle size measurement, the dispersion of the sample is very important, but because the physical and chemical properties, the polarity and the existing state of the sample are gaseous, liquid, solid or colloid, the sample dispersion work is influenced, if the sample cannot be uniformly and well dispersed, the aggregated particles are equivalent to large particles, and thus the measurement accuracy is not guaranteed.
The sample dispersing module 2 comprises a water pump 25, a stirrer 22, an ultrasonic disperser 23, a sample pool 21, a water pool 26, a discharging device 24 and the like, wherein in the working process of the circulating water pump 25, external force is not directly contacted with particles, and the particles to be detected in the sample pool 21 cannot be influenced;
the stirrer 22 is composed of a direct current motor and a special blade and mainly used for keeping sample particles in the water tank 26 in a uniform suspension state and ensuring that a sample circulated to the sample tank 21 is uniformly dispersed in a solution;
the ultrasonic disperser 23 is arranged at the bottom of the water tank 26 and is used for dispersing particles so as to ensure that the sample particles are in a good dispersion state;
the sample cell 21 is made of quartz glass, the glass has good optical characteristics and is relatively wear-resistant and corrosion-resistant, and the sample cell 21 is convenient to mount, dismount and replace;
the discharging device 24 is mainly used for discharging waste sample solution and waste liquid after cleaning the instrument, and is simple and convenient to operate and safe and reliable to use.
In actual testing, some surfactant is usually added appropriately according to the chemical property of the sample to be tested to enhance the dispersion of the sample, but in wet measurement, the use of chemical surfactant for particle separation produces foam, which affects the accuracy of particle size measurement, so the speed should be controlled during the operation to prevent the generation of foam.
The cleaning system is also a key step for ensuring the accuracy of particle size measurement, and the specific operation steps are as follows: first, the measured sample waste liquid is discharged by the discharging device 24, and then, after purified water is circulated several times in the sample cell 21, the cleaning liquid in the circulation system is discharged by the discharging device 24. In another cleaning method, the pipeline and the sample cell 21 are completely cleaned by ultrasonic waves using an ultrasonic oscillation cell for a sample which is difficult to clean.
Referring to the attached drawing 1 of the specification, the light scattering and collecting module 3 is composed of a fourier lens 31, an area array CCD32 and a photocell 33, the fourier lens 31 is arranged between the sample cell 21 and the area array CCD32 and is arranged concentrically with the diaphragm 14, the photocell 33 is arranged outside the area array CCD32, and both the area array CCD32 and the photocell 33 are connected with the data processing module 5.
The implementation scenario is specifically as follows: the main function of the fourier lens 31 is to converge the scattered light of the particles to the back focal plane, i.e. to find the spatial frequency distribution of the incoming beam. The quality of the fourier lens 31 directly affects the accuracy of the measurement result, and the aberration of the lens is strictly controlled. In the particle size measuring system, the fourier lens 31 plays a very important role, and one key parameter of the fourier lens is the focal length, the particle size measuring range and the lens focal length, which are closely related to the optical energy ring parameters received by the area array CCD32 and the photocell 33. According to the measurement range of the particle system and the design of the ring parameters of the receiving device, the focal length f of the fourier lens 31 is 75mm, which can meet the requirement of the invention.
The area array CCD32 is a photoelectric device that generates signal charges by photoelectric conversion using an internal photoelectric effect, and is composed of a plurality of charge-coupled cells. Has wider application and has a plurality of advantages compared with the silicon photocell 33 adopted by the traditional instrument. The geometric accuracy of the pixel size of the image data which can be automatically collected, calculated and recorded is high, the image quality is clear, the residual image is almost not generated, the adaptability to the external environment is stronger, and the error caused by the unstable light intensity of the light source can be overcome.
The area array CCD32 receiver is first located at its initial position, which is calibrated using a fixed calibration laser 11. And acquiring the Airy spot image, extracting the central point of the Airy spot image, guiding light path centering according to the central point coordinate, and solving centering correction parameters.
The invention adopts a Tiger T8810/T8820 camera, the image resolution of an area array CCD32 is 8856 multiplied by 5280, the pixel size is 5.5 mu m, and the image plane size is 48.71 multiplied by 29.04mm 2. The camera has high light sensitivity and can receive scattered light rings with weak light intensity. The image plane size is large, the range of measurable particle granularity is large, and the number of image splicing can be reduced. The area array CCD32 of the present invention has the collection particle size range of 0.3-1000 micron. The inner diameter of the corresponding scattering light ring is 21 μm, and the outer diameter is 72.46 mm. The CCD pixel size is 5.5 μm, and the inner diameter of the scattering light ring can be distinguished. The outer diameter is combined with an electric control two-dimensional guide table 4 to move the CCD at the focal plane position, and the receiving scattering light ring is completed through image splicing.
The scattered light energy ring corresponding to small particles is large in diameter and weak in energy, so that the photocell 33 is used as a receiver, and a plurality of photocells 33 with corresponding sizes are placed at the energy ring of the (0.1-0.3) mu m particles.
Referring to the attached drawing 3 of the specification, the electronic control two-dimensional guide table 4 comprises a two-dimensional guide table 41 and a main control chip 42, the two-dimensional guide table 41 comprises a transverse screw rod 6, a longitudinal screw rod 7 and two sliders 8 which are respectively installed outside the transverse screw rod 6 and the longitudinal screw rod 7 in a threaded manner, the longitudinal screw rod 7 is installed on the slider 8 outside the transverse screw rod 6, the longitudinal screw rod 7 and the transverse screw rod 6 are vertically arranged, and the area array CCD32 is installed on the slider 8 outside the transverse screw rod 6.
Further, the transverse screw rod 6 and the longitudinal screw rod 7 are driven by a servo motor, and the servo motor is controlled by a control circuit in the main control chip 42.
The electrically controlled two-dimensional guide 4 serves to fix the camera and to control the position of the camera receiver, i.e. the area array CCD32, in the back focal plane of the fourier lens 31. The two-dimensional guide table 41 is capable of changing the spatial position of the camera in both the vertical and horizontal directions. The two-dimensional guide table 41 is fixed on a sliding table of an optical path guide rail, and the position of the sliding table is adjusted to enable the area array CCD32 on the camera to be overlapped with the back focal plane of the Fourier lens 31, so that the scattered light energy image is received. The position of the camera in the horizontal and vertical directions is controlled by an electric control system of the two-dimensional guide table 41, and a plurality of scattered light energy images at different positions are collected for later stage splicing.
The electric control two-dimensional guide table 4 adopts an ARM STM32 as a main control chip 42, and the positions of the upper sliding blocks 8 of the lead screws of the electric control two-dimensional guide table are respectively controlled by two groups of motors, so that the spatial position control of the camera in the horizontal direction and the vertical direction is realized. The horizontal direction stroke of the electric control two-dimensional guide table 4 is 120mm, and the vertical direction stroke is 120 mm. And the laser calibration mode is adopted to ensure the starting position accuracy of the area array CCD 32. Thereby ensuring the accuracy of the light path centering result.
Referring to the attached fig. 1 of the specification, the data processing module 5 includes a data acquisition circuit 51 and a computer 52, the data acquisition circuit 51 is configured to convert image information acquired by the area array CCD32 into a digital signal and transmit the digital signal to the computer 52, and convert an analog electrical signal output by the photocell 33 into a digital signal and transmit the digital signal to the computer 52.
Further, the computer 52 gives image centering information by using an image processing technology, and guides centering; the computer 52 splices a plurality of scattered light energy images at different positions by using a splicing technology to give large-angle scattered light energy information; the computer 52 adopts an inversion algorithm to calculate, and converts the scattered light energy information obtained by the area array CCD32 and the photocell 33 into the result of the particle size and the distribution of the particles to be measured.
The implementation scenario is specifically as follows: the space position of the two-dimensional direction of the area array CCD32 is changed through the electric control two-dimensional guide table 4, a plurality of images containing large-particle scattered light energy information are collected, the photocell 33 collects small-particle scattered light energy information, the data collection circuit 51 is divided into two parts, one part converts the image information of the area array CCD32 into digital signals and inputs the digital signals to the computer 52, and the other part converts analog signals output by the photocell 33 into digital signals and inputs the digital signals to the computer 52. The computer 52 functions as follows:
1. image centering information is given by using an image processing technology, and centering is guided;
2. and splicing a plurality of scattered light energy images at different positions by utilizing a splicing technology. Giving out large-angle scattered light energy information;
3. and (3) calculating by adopting an inversion algorithm, and converting scattered light energy information obtained by the area array CCD32 and the photocell 33 into the result of the particle size and the distribution of the particles to be detected.
Although the invention has been described in detail above with reference to a general description and specific examples, it will be apparent to one skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.

Claims (10)

1. A particle size measurement equipment based on Mie's scattering theory is characterized in that: the device comprises a parallel light generating module (1), a sample dispersing module (2), a light scattering and collecting module (3), an electric control two-dimensional guide table (4) and a data processing module (5);
the device comprises a parallel light generating module (1), a sample dispersing module (2) and a light scattering acquisition module (3), wherein the parallel light generating module (1) is distributed in a straight line shape from left to right, the parallel light generating module (1) is used for emitting monochromatic parallel light beams, and the light beams pass through a sample pool (21) in the sample dispersing module (2) and are focused on the light scattering acquisition module (3) to form a scattered light energy image;
the output end of the light scattering acquisition module (3) is connected with the input end of the data processing module (5), the light scattering acquisition module (3) is used for acquiring the image and sending the image to the data processing module (5), and the data processing module (5) is used for converting the acquired image information into a digital signal and calculating to obtain the result of the particle size and the distribution;
the light scattering acquisition module (3) is arranged on the electric control two-dimensional guide table (4), and the light scattering acquisition module (3) is adjusted and fixed through the electric control two-dimensional guide table (4).
2. The particle size measurement device based on Mie scattering theory as claimed in claim 1, wherein: parallel light produces module (1) and includes that it distributes in proper order to be a style of calligraphy from left to right laser instrument (11), spatial filter (12), collimating lens (13) and diaphragm (14), spatial filter (12) comprise beam expander, support and pinhole, beam expander and pinhole set up side by side between laser instrument (11) and collimating lens (13), and the beam expander is close to laser instrument (11) side and sets up, beam expander and pinhole are installed on the support.
3. The particle size measurement device based on Mie scattering theory as claimed in claim 1, wherein: sample dispersion module (2) includes sample cell (21), agitator (22), ultrasonic wave deconcentrator (23) and discharging equipment (24), install in sample cell (21) top agitator (22), ultrasonic wave deconcentrator (23) are installed in sample cell (21) bottom, discharging equipment (24) set up in sample cell (21) bottom one side, discharging equipment (24) specifically are the discharge valve.
4. The particle size measurement device based on Mie's scattering theory as claimed in claim 3, wherein: the sample cell (21) is made of quartz glass material, and a surfactant is added in the sample cell (21).
5. The particle size measurement device based on Mie's scattering theory as claimed in claim 3, wherein: the sample dispersing module (2) further comprises a cleaning system, the cleaning system is composed of a water pump (25) and a water tank (26), the sample tank (21) and the water tank (26) are communicated through a cleaning pipeline, and the water pump (25) is installed on the cleaning pipeline and used for pumping clean water in the water tank (26) into the sample tank (21) to clean the sample tank (21).
6. The particle size measurement device based on Mie scattering theory as claimed in claim 1, wherein: light scattering collection module (3) comprises Fourier lens (31), area array CCD (32) and photocell (33), Fourier lens (31) set up between sample cell (21) and area array CCD (32), and set up with diaphragm (14) is concentric, photocell (33) set up in the area array CCD (32) outside, area array CCD (32) and photocell (33) all are connected with data processing module (5).
7. The particle size measurement device based on Mie scattering theory as claimed in claim 1, wherein: automatically controlled two-dimensional guide table (4) is including two-dimensional guide table (41) and main control chip (42), two-dimensional guide table (41) is including horizontal lead screw (6), vertical lead screw (7) and respectively the screw thread install in two outside slider (8) of horizontal lead screw (6) and vertical lead screw (7), vertical lead screw (7) are installed on slider (8) of horizontal lead screw (6) outside, vertical lead screw (7) set up with horizontal lead screw (6) are perpendicular, area array CCD (32) are installed on slider (8) of horizontal lead screw (6) outside.
8. The particle size measurement device based on Mie scattering theory as claimed in claim 7, wherein: the transverse screw rod (6) and the longitudinal screw rod (7) are driven by a servo motor, and the servo motor is controlled by a control circuit in the main control chip (42).
9. The particle size measurement device based on Mie scattering theory as claimed in claim 1, wherein: the data processing module (5) comprises a data acquisition circuit (51) and a computer (52), wherein the data acquisition circuit (51) is used for converting image information acquired by the area array CCD (32) into digital signals and transmitting the digital signals to the computer (52), and converting analog electric signals output by the photocell (33) into digital signals and transmitting the digital signals to the computer (52).
10. The particle size measurement device based on Mie scattering theory as claimed in claim 9, wherein: the computer (52) gives image centering information by using an image processing technology and guides centering; the computer (52) splices a plurality of scattered light energy images at different positions by using a splicing technology to give large-angle scattered light energy information; the computer (52) adopts an inversion algorithm to calculate, and converts scattered light energy information obtained by the area array CCD (32) and the photocell (33) into the result of the particle size and the distribution of the particles to be detected.
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Application publication date: 20200911