CN110857909A - System for measuring particle size of particles - Google Patents

System for measuring particle size of particles Download PDF

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CN110857909A
CN110857909A CN201810973274.7A CN201810973274A CN110857909A CN 110857909 A CN110857909 A CN 110857909A CN 201810973274 A CN201810973274 A CN 201810973274A CN 110857909 A CN110857909 A CN 110857909A
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pulse signals
time
time period
correlation
particle size
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CN110857909B (en
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张达
王继军
江学舟
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Beijing Century Chaoyang Technology Development Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
    • G01N15/02Investigating particle size or size distribution
    • G01N15/0205Investigating particle size or size distribution by optical means, e.g. by light scattering, diffraction, holography or imaging
    • G01N15/0211Investigating a scatter or diffraction pattern

Abstract

The present disclosure relates to a system for measuring particle size of a microparticle. The system comprises: the sensor and the identification amplifying circuit are used for receiving the scattered light of the particles to be detected and generating a plurality of pulse signals; an electronic circuit for determining the reception timings of a plurality of pulse signals; a computer configured to: in the measurement time period, respectively determining the number of pulse signals in each sampling time period according to the receiving moments of the pulse signals and the sampling time periods in at least one relevant time; respectively calculating a correlation function value of each correlation time according to the number of pulse signals in a plurality of sampling time periods; and obtaining the diameter or radius value of the particle to be measured according to the correlation function value of at least one correlation time. The method for measuring the particle size of the particles can reduce the complexity of a hardware circuit, can cope with the high counting condition, and can set different sampling time for different related time so as to reduce random errors and system errors and improve the speed and the precision of particle size measurement.

Description

System for measuring particle size of particles
Technical Field
The present disclosure relates to the field of measurement technologies, and in particular, to a system for measuring particle diameters.
Background
Particles in air and solutions, when the ambient temperature is above absolute zero, inevitably have random thermal motion (i.e. brownian motion). For the typical case of dynamic light scattering measurements, the degree of brownian motion of a particle can be measured by the diffusion coefficient (D). In a low reynolds number solvent, the diffusion coefficient is dependent on temperature, viscosity coefficient and particle size of the particles, according to the Stokes-Einstein formula. For solutions with a large number of particles, brownian motion causes the distance between the particles to change with time. The particles are irradiated with laser light of good coherence, the scattered light of the particles interferes to form total scattered light, and the change in the intensity of the total scattered light is related to the brownian motion of the particles and thus indirectly also to the particle size of the particles.
Disclosure of Invention
According to an aspect of the present disclosure, there is provided a system for measuring a particle size of a fine particle, the system including:
the sensor and the identification amplifying circuit are used for receiving the scattered light of the particles to be detected and generating a plurality of pulse signals;
an electronic circuit, connected to the sensor and the discrimination amplification circuit, for determining the reception timings of the plurality of pulse signals;
a computer connected to the electronic circuitry, the computer configured to:
respectively determining the number of pulse signals in each sampling time period according to the receiving moments of the pulse signals and a plurality of sampling time periods in at least one correlation time in a measuring time period, wherein the measuring time period comprises the at least one correlation time;
respectively calculating a correlation function value of each correlation time according to the number of pulse signals in a plurality of sampling time periods;
and obtaining the diameter or radius value of the micro-particles to be detected according to at least one correlation function value of the correlation time.
In one possible embodiment, the sensor and the discrimination amplification circuit are further configured to:
and removing noise signals with amplitude smaller than the threshold amplitude and/or width smaller than the threshold width in the pulse signals.
In one possible implementation, the duration of the sampling period is 1/1000-1/3 of the duration of the associated time.
In one possible implementation, the duration of the sampling period is 1/10 times the duration of the associated time.
In one possible embodiment, the correlation function value of the correlation time is calculated by the following formula:
Figure BDA0001776785280000021
wherein G is2(τ) represents a correlation function value corresponding to the correlation time, τ is a ratio of the correlation time to a sampling time period duration, imax is a total ratio of the measurement time period (i.e., a total time period for acquiring the pulse signals) to the sampling time period, and n (i), (i) and n (i + τ) are the number of the pulse signals in the ith sampling time period and the number of the pulse signals in the (i + τ) th sampling time period in the measurement time period, respectively.
In one possible implementation, the computer is further configured to:
determining the number of pulse signals in a plurality of decomposition time periods of the measurement time period according to the receiving moments of the plurality of pulse signals, wherein the decomposition time periods are time periods obtained by dividing the measurement time period;
obtaining the average pulse signal quantity according to the pulse signal quantity in the measurement time period and the number of the decomposition time periods;
acquiring a standard deviation according to the average pulse signal quantity and the pulse signal quantity in the decomposition time periods;
determining an abnormal time period in the plurality of decomposition time periods according to the number of pulse signals in the plurality of decomposition time periods, the average number of pulse signals and the standard deviation;
and removing the abnormal time period and the pulse signals in the abnormal time period.
In one possible embodiment, determining the abnormal time period in the decomposition time periods according to the number of pulse signals in the decomposition time periods and the standard deviation comprises:
and taking a decomposition period in which the number of pulse signals in the plurality of decomposition periods is not within three standard deviation of the average number of pulses as the abnormal period.
In a possible implementation, the electronic circuit includes one or more of a field programmable gate array FPGA, a complex programmable logic device CPLD, and a single chip.
The method for measuring the particle size of the particles can reduce the complexity of a hardware circuit, can cope with the high counting condition, and can set different sampling time for different related time so as to reduce or even eliminate random errors and system errors and improve the speed and the precision of particle size measurement.
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.
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The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate exemplary embodiments, features, and aspects of the disclosure and, together with the description, serve to explain the principles of the disclosure.
FIG. 1 shows a block diagram of a system for measuring particle size of a microparticle according to an embodiment of the present disclosure.
Fig. 2 shows a flow chart of a method of measuring particle size of a microparticle according to an embodiment of the present disclosure.
Fig. 3 shows a flow chart of a method of measuring particle size of a microparticle according to an embodiment of the present disclosure.
FIG. 4 illustrates a block diagram of a system for measuring particle size of a microparticle according to an embodiment of the present disclosure.
Detailed Description
Various exemplary embodiments, features and aspects of the present disclosure will be described in detail below with reference to the accompanying drawings. In the drawings, like reference numbers can indicate functionally identical or similar elements. While the various aspects of the embodiments are presented in drawings, the drawings are not necessarily drawn to scale unless specifically indicated.
The word "exemplary" is used exclusively 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.
Furthermore, in the following detailed description, numerous specific details are set forth 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 that are well known to those skilled in the art have not been described in detail so as not to obscure the present disclosure.
The particle size of the fine particles in the solution or the air is related to the dynamic change of the scattered light of the fine particles, and therefore, the particle size of the fine particles can be obtained by the dynamic light scattering method.
In view of the above, the present disclosure provides a system for measuring particle size based on dynamic light scattering.
Referring to fig. 1, fig. 1 shows a block diagram of a system for measuring particle size of a particle according to an embodiment of the present disclosure.
As shown in fig. 1, the system includes:
the sensor and discrimination amplifier circuit 300 is used for receiving the scattered light of the particles to be detected and generating a plurality of pulse signals.
In one possible embodiment, the sensor and identifying and amplifying circuit 300 can separate the effective pulse signal and the noise signal in the plurality of pulse signals, so as to achieve the purpose of removing the noise.
In one possible embodiment, the sensor and differential amplifier circuit 300 may be an integrated circuit or a specially designed circuit that analyzes the plurality of pulse signals to separate the effective signal from the noise signal, thereby removing the noise signal.
In one possible implementation, noise signals in the pulse signal having an amplitude smaller than a threshold amplitude and/or a width smaller than a threshold width may be removed.
In a possible embodiment, the threshold amplitude and the threshold width may be set according to the actual situation.
By denoising the pulse signal, the speed of measuring the particle size of the particles and the measurement precision can be improved.
And an electronic circuit 310 connected to the sensor and discrimination amplifier circuit 300 for determining the receiving time of the plurality of pulse signals.
In one possible embodiment, laser light (optical signal) emitted by the laser emitter is irradiated on a sample (sample may be, for example, a solution with particles to be detected) including the particles to be detected, the sample is excited by the laser light (laser light is scattered by the particles to be detected), scattered light is emitted, and the sensor and identifying and amplifying circuit 300 receives the scattered light of the sample and outputs a pulse signal.
For example, during a measurement period of 10s, a plurality of pulse signals are continuously transmitted from the sensor and identifying and amplifying circuit 300, and the system records the receiving time of each pulse signal, so that the plurality of pulse signals and the receiving time of the plurality of pulse signals can be obtained.
Some prior arts cannot deal with the high counting condition of multi-pulse signals, and when the pulse signals are continuously appeared and the interval time between pulses is less than the relevant time, the prior arts are generally difficult to deal with, and a large measurement error is generated.
According to the method and the device, the receiving moments of the pulse signals are recorded, so that the buffer storage of the pulse signals is realized, and the condition of high counting rate can be met.
A computer 320 coupled to the electronic circuitry 310, the computer 320 being configurable to perform the method as shown in FIG. 2.
Referring to fig. 2, fig. 2 illustrates a method for measuring particle size of particles according to an embodiment of the present disclosure.
As shown in fig. 2, the method includes:
step S110, in a measurement time period, determining the number of pulse signals in each sampling time period according to the receiving time of the plurality of pulse signals and a plurality of sampling time periods in at least one correlation time, respectively, where the measurement time period includes the at least one correlation time.
In one possible embodiment, the sampling periods corresponding to different correlation times are the same or different in duration.
For example, when the measurement period is 10s, the correlation time may be 100us, 120us, 140us, 160us, etc., the correlation time is smaller than the measurement period, and the duration of the sampling period is smaller than the duration of the correlation time.
In one possible implementation, the duration of the sampling period is 1/1000-1/3 of the duration of the associated time.
For example, for a correlation time of 100us, 1/20 whose sampling time is the correlation time, i.e., 5 us; for a correlation time of 120us, 1/20 whose sampling time is the correlation time, i.e., 6us, may be set. On the other hand, the sampling times of the correlation time of 100us and the correlation time of 120us may be set to 5 us.
In the existing full-hardware correlator technology, sampling time cannot be set for different correlation time respectively, but only one or a plurality of fixed sampling time can be used, so that different correlation time is difficult to be considered. For example, if a smaller sampling period is used, then the random error is larger for larger correlation times; with a larger sampling period, the systematic error is larger for small correlation times. It is difficult to reduce both systematic and random errors regardless of the sampling time.
The method can set different sampling times for different relevant times respectively, and can give consideration to the relevant times with different sizes, thereby reducing random errors and system errors and improving the measurement precision.
In one possible embodiment, the duration of the sampling period may be 1/10 times the duration of the correlation time, and when the sampling period of the correlation time is 1/10 times the correlation time, the method for measuring the particle size of the particles according to the present disclosure has higher accuracy.
For example, when the correlation time is 100us, the duration of the corresponding sampling time period may be 10 us.
In one possible embodiment, the pulse signal is recorded as a pulse signal of the current sampling period when the reception time of the pulse signal is within the sampling period of the relevant time.
Step S120, respectively calculating a correlation function value for each correlation time according to the number of pulse signals in a plurality of sampling time periods.
In one possible embodiment, the correlation function value of the correlation time can be calculated by the following formula:
Figure BDA0001776785280000061
wherein G is2(τ) represents a correlation function value corresponding to the correlation time, τ is a ratio of the correlation time to a sampling time period duration (i.e., the correlation time represented by a sampling time period), imax is a ratio of the measurement time period to the sampling time period, and n (i), (i) and n (i + τ) are the number of pulse signals in the ith sampling time period and the number of pulse signals in the (i + τ) th sampling time period in the measurement time period, respectively.
For example, if the measurement time period is 10s, the correlation time is 100us, and the sampling time period is 10us, the imax is 10s/10us — 1000000, that is, the entire measurement time period may be divided into 1000000 sampling time periods; τ is 100us/10 us-10, i.e. the correlation time τ of 100us can be represented by 10 sample times.
Step S130, obtaining a diameter or radius value of the to-be-detected microparticle according to at least one correlation function value of the correlation time.
In one possible embodiment, the particle size of the particles (diameter or radius) may be obtained by performing an inverse calculation of the particle size, for example, by an algorithm such as cumulants method.
When a plurality of correlation function values of the correlation time are obtained, a correlation function curve can be drawn through the plurality of correlation function values, and the particle size of the particles can be obtained according to the drawn correlation function curve.
For example, a dynamic light scattering measurement is performed on a standard polystyrene bead of 92nm in deionized water, each measurement time period is 100ms, the shortest correlation time is 0.1us, the sampling time period is 1/10 of the correlation time, 100 times of experiments are repeated, the 100 times of measurement results are counted, the standard deviation of the correlation function value at 10us is obtained by analysis and is 2.4%, and the standard deviation of the correlation function value obtained by measurement in the prior art is 8.6% (the sampling time is fixed to be 0.1us), so that the method for measuring the particle size of the particles disclosed by the disclosure improves the measurement accuracy.
In one possible embodiment, the computer 320 may be further configured to perform a method of measuring a particle size in a particle as illustrated in fig. 3.
Referring to fig. 3, fig. 3 is a flow chart illustrating a method for measuring particle size according to an embodiment of the present disclosure.
As shown in fig. 3, the method includes:
in the process of measuring the particle size value of the sample, if dust, dirt, and other impurities are present in the sample, these impurities may emit scattered light even under laser irradiation, and the scattered light emitted from the impurities may be mixed into the scattered light emitted from the sample to affect the final result, and the accuracy of measuring the particle size value may be reduced. Therefore, in the measurement, the influence of scattered light from removing impurities is a problem to be solved.
Steps S310 to S314 may be used to remove the influence of impurities.
Step S310, determining the number of pulse signals in a plurality of decomposition time segments of the measurement time segment according to the receiving time of the plurality of pulse signals, where the decomposition time segments are time segments obtained by dividing the measurement time segment.
In a possible embodiment, the measurement time period may be divided into a plurality of decomposition time periods, and the division manner may be determined according to actual situations, for example, the measurement time period may be divided into segments with the maximum correlation time, or other units may be selected for the segmentation.
For example, the measurement time period may be divided into a plurality of decomposition time periods at intervals of 0.1 second, and the number of pulse signals in each decomposition time period is counted, for example, the number of pulse signals from 0 second to 0.1 second is denoted as n0The number of pulses from 0.1 second to 0.2 second is denoted as n1
Step S311, obtaining an average pulse signal quantity according to the pulse signal quantity in the measurement time period and the number of the decomposition time periods.
Calculating the average value n for the number of pulse signals of all the decomposition time segmentsave(the average number of pulse signals), for example, the total number of pulse signals in the measurement period may be divided by the number of pulse signals of the plurality of decomposition periods to obtain an average value nave
Step S312, obtaining a standard deviation according to the average pulse signal number and the pulse signal numbers in the decomposition time periods.
And acquiring a standard deviation sigma according to the average pulse signal number and the pulse signal numbers in the decomposition time periods.
Step S313, determining an abnormal time period in the plurality of decomposition time periods according to the number of pulse signals in the plurality of decomposition time periods, the average number of pulse signals, and the standard deviation.
In a possible embodiment, the number of pulse signals per decomposition period can be compared one by one, if not in the interval nave-3σ,nave+3σ]And (c) an abnormal time period (influenced by impurities such as dust) is considered.
Step S314, removing the abnormal time period and the pulse signal in the abnormal time period. At this time, if there is no decomposition period that needs to be removed, that is, the number of pulse signals of all the decomposition periods is in the interval [ n ]ave-3σ,nave+3σ]The completion of the filtering of the dust signal is explained;
in addition, in order to completely remove the interference of the foreign matter, the average value n may be recalculated using the decomposition period after the removal of the abnormal period is completedaveAnd the standard deviation σ, and the aforementioned removal step is performed again.
The above steps may be performed a plurality of times (e.g., 3 to 5 times) so that the influence of the impurities is completely removed.
After the influence of the impurities is removed, that is, after the abnormal period is removed, the particle diameter of the fine particles can be measured using the filtered measurement period.
Step S320, determining the number of pulse signals in each sampling time period according to the receiving time of the plurality of pulse signals and a plurality of sampling time periods in at least one correlation time, respectively, where the measurement time period includes the at least one correlation time.
In the present embodiment, the measurement time period is a measurement time period after the exception time period is removed.
For example, after removing the influence of the impurity, that is, after removing the abnormal time period, the measurement time period is divided into several sub-measurement time periods, for example, if the measurement time period is 10s, wherein the abnormal time period is 3-5s, the first sub-measurement time period is 0-3s, and the second sub-measurement time period is 5-10s, in this case, the first sub-measurement time period and the second sub-measurement time period are respectively used as the measurement time period, and the number of pulse signals in each sampling time period is determined.
Step S330, respectively calculating a correlation function value for each correlation time according to the number of pulse signals in a plurality of sampling time periods.
Step S340, obtaining a particle size value of the particle to be measured according to at least one correlation function value of the correlation time.
It should be noted that steps S320-S340 are similar to the steps of the foregoing method for measuring particle size, and the detailed description thereof refers to the foregoing description, which is not repeated herein.
The method for measuring the particle size of the particles can reduce the complexity of a hardware circuit, can cope with the high counting condition, and can set different sampling time for different related time so as to reduce random errors and system errors and improve the speed and the precision of particle size measurement.
Referring to fig. 4, fig. 4 is a block diagram illustrating a system for measuring particle size according to an embodiment of the present disclosure.
As shown in fig. 4, the system includes a sensor and identification amplifying circuit 300, an electronic circuit 310, an interface circuit 330, a clock auxiliary circuit 340, and a computer 320.
The electronic circuit 310 is electrically connected to the sensor and discrimination amplifier circuit 300, the clock auxiliary circuit 340 and the interface circuit 330, and the interface circuit 330 is electrically connected to the clock auxiliary circuit 340 and the computer 320.
In one possible implementation, the clock and other ancillary circuitry 340 may include power circuitry, clock circuitry, and the like, the clock circuitry operable to provide a clock signal to the system, and the power circuitry operable to provide power to the system.
In this embodiment, after the scattered light signal is transmitted to the sensor and identifying amplifier circuit 300, the sensor and identifying amplifier circuit 300 removes a noise signal by analyzing the magnitude relation between the amplitude and width of the photoelectric pulse signal output from the sensor and the threshold value, and outputs a useful pulse signal to the electronic circuit 310, the electronic circuit 310 records the receiving time of the pulse signal, and transmits the information such as the receiving time of the pulse signal to the computer 320 through the interface circuit, and the computer 320 executes a method of obtaining the particle size of the particles to obtain the particle size of the particles.
It should be noted that the above system has been described in the foregoing method and system for obtaining the particle size of the fine particles, and the detailed description thereof is omitted here.
Having described embodiments of the present disclosure, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the disclosed embodiments. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. The terminology used herein is chosen in order to best explain the principles of the embodiments, the practical application, or improvements made to the technology in the marketplace, or to enable others of ordinary skill in the art to understand the embodiments disclosed herein.

Claims (8)

1. A system for measuring the particle size of a particulate, the system comprising:
the sensor and the identification amplifying circuit are used for receiving the scattered light of the particles to be detected and generating a plurality of pulse signals;
an electronic circuit, connected to the sensor and the discrimination amplification circuit, for determining the reception timings of the plurality of pulse signals;
a computer connected to the electronic circuitry, the computer configured to:
respectively determining the number of pulse signals in each sampling time period according to the receiving moments of the pulse signals and a plurality of sampling time periods in at least one correlation time in a measuring time period, wherein the measuring time period comprises the at least one correlation time;
respectively calculating a correlation function value of each correlation time according to the number of pulse signals in a plurality of sampling time periods;
and obtaining the diameter or radius value of the micro-particles to be detected according to at least one correlation function value of the correlation time.
2. The system of claim 1, wherein the sensor and the discrimination amplifier circuit are further configured to remove noise signals from the plurality of pulse signals having an amplitude less than a threshold amplitude and/or a width less than a threshold width.
3. The system for measuring particle size of claim 1, wherein the sampling period is 1/1000-1/3 of the associated time.
4. The system for measuring particle size of claim 1, wherein the duration of the sampling period is 1/10 times the duration of the associated time.
5. The system for measuring a particle diameter of claim 1, wherein the correlation function value of the correlation time is calculated by the following formula:
Figure FDA0001776785270000011
wherein G is2(τ) represents a correlation function value corresponding to a correlation time, τ being the correlation time andthe ratio of the sampling time period duration, imax is the ratio of the measurement time period to the sampling time period, and n (i), (i) and n (i + τ) are the number of pulse signals in the ith sampling time period and the number of pulse signals in the (i + τ) th sampling time period in the measurement time period, respectively.
6. The system for measuring particle size of claim 1, wherein the computer is further configured to:
determining the number of pulse signals in a plurality of decomposition time periods of the measurement time period according to the receiving moments of the plurality of pulse signals, wherein the decomposition time periods are time periods obtained by dividing the measurement time period;
obtaining the average pulse signal quantity according to the pulse signal quantity in the measurement time period and the number of the decomposition time periods;
acquiring a standard deviation according to the average pulse signal quantity and the pulse signal quantity in the decomposition time periods;
determining an abnormal time period in the plurality of decomposition time periods according to the number of pulse signals in the plurality of decomposition time periods, the average number of pulse signals and the standard deviation;
and removing the abnormal time period and the pulse signals in the abnormal time period.
7. The system for measuring particle size of claim 6, wherein determining an abnormal time period in the plurality of decomposition time periods based on the number of pulse signals in the plurality of decomposition time periods and the standard deviation comprises:
and taking a decomposition period in which the number of pulse signals in the plurality of decomposition periods is not within three times of a standard deviation range of the average number of pulse signals as the abnormal period.
8. The system for measuring particle size of any one of claims 1-7, wherein the electronic circuit comprises one or more of a Field Programmable Gate Array (FPGA), a Complex Programmable Logic Device (CPLD), and a single chip microcomputer.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114527043A (en) * 2022-01-11 2022-05-24 成都派斯光科技有限公司 Particle concentration measuring method
CN114527043B (en) * 2022-01-11 2024-02-20 成都派斯光科技有限公司 Particle concentration measuring method

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