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CN102297823A - Method and apparatus for measuring dynamic light scattering nano-particles based on bandpass filtering - Google Patents

Method and apparatus for measuring dynamic light scattering nano-particles based on bandpass filtering Download PDF

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CN102297823A
CN102297823A CN2011101270517A CN201110127051A CN102297823A CN 102297823 A CN102297823 A CN 102297823A CN 2011101270517 A CN2011101270517 A CN 2011101270517A CN 201110127051 A CN201110127051 A CN 201110127051A CN 102297823 A CN102297823 A CN 102297823A
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laser
particles
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particle
photoelectric detector
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CN102297823B (en
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沈建琪
王华睿
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University of Shanghai for Science and Technology
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Abstract

The invention discloses a method and an apparatus for measuring dynamic light scattering nano-particles based on bandpass filtering. According to the invention, lasers are radiated on nano-particles performing Brownian motions in a solution. The scattered lights of the particles are directly detected; or the scattered lights of the particles are interfered with part of the original lights, and are detected; or the scattered lights are fed-back into a laser-tube cavity, self mixing is occurred, and self mixing signals are detected. Signals output by a photoelectric detector are pre-amplified, and are simultaneously delivered into a circuit formed by components of an M route buffer, bandpass filters with different central frequencies, and an RMS root-mean-square processor, which are connected in series, such that signal root-mean-square values at different frequencies with a number of M are obtained. The values are sampled by an A/D collecting card, such that power spectrum density functions at different frequencies with a number of M are obtained. With the method and the apparatus provided by the invention, a problem in prior arts of poor robustness of inverse calculations caused by seriously ill-conditioned coefficient matrix is solved. With the method and the apparatus provided by the invention, requirements on data collecting speed, data collecting amount, storage amount and processing amount are reduced; data processing time is reduced; and rapid measuring of nano-particle sizes can be realized.

Description

Dynamic light scattering nano-particle measuring method and device based on band-pass filtering
Technical Field
The invention relates to a method and a device for measuring nanoparticles, in particular to a method and a device for measuring dynamic light scattering nanoparticles based on band-pass filtering, and belongs to the technical field of measurement. Can be used in a plurality of fields relating to the production and the process control of nano particles, such as scientific research, biological medicine, chemical energy, environmental protection, and the like.
Background
In the dynamic light scattering nanoparticle measurement technology, a digital correlator is generally used to obtain an autocorrelation function of a scattered light signal or a power spectrum density function of the scattered light signal is obtained by a power spectrum estimation method, so that a particle size distribution parameter of a nanoparticle is obtained by matrix inversion.
Laser emitted by the laser is converged by one or a plurality of lenses and then irradiates nanoparticles in the solution for scattering, and the scattered light signal contains particle size information of the particles.
There are generally three ways to detect the scattered light signal: directly detecting scattered light signals or detecting the scattered light signals after converging through a lens; secondly, detecting the scattered light signal after interfering with part of laser emitted by the light source; and thirdly, the scattered light is fed back into the laser cavity, self-mixing modulation laser output is generated between the scattered light and the laser in the laser cavity, and the self-mixing modulation laser output is detected by a photoelectric detector arranged at the rear end of the laser.
The scattered light signal of the particle to be detected is processed by a correlator to obtain an autocorrelation function:
Figure 2011101270517100002DEST_PATH_IMAGE002
(1)
the corresponding power spectral density function is:
Figure 2011101270517100002DEST_PATH_IMAGE004
(2)
wherein, jis the grade number of the particle diameter
Figure 2011101270517100002DEST_PATH_IMAGE006
Corresponding to different particle size grades,
Figure 2011101270517100002DEST_PATH_IMAGE008
the total grading number of the particle size;x j is the firstjAverage particle size of the particles;
Figure 2011101270517100002DEST_PATH_IMAGE010
is the firstjThe step width of the step particle size; with respect to the power spectral density function,iis the frequency channel number
Figure 2011101270517100002DEST_PATH_IMAGE012
The frequency of the signal corresponding to the different frequencies,is the total number of channels; with respect to the auto-correlation function,iis the relative time stepping serial number
Figure 279072DEST_PATH_IMAGE012
The correlation time is, for different correlation times,is the total number of relevant times; when the detection mode is adopted, the method comprises
Figure 2011101270517100002DEST_PATH_IMAGE016
(ii) a When the detection mode is two or three, there areqIs the scattering vector;D j is the firstjParticle diffusion coefficient of particle size range, including nanoparticle sizex j The information of (a);ω i is as followsiAngular frequency on the channel related to brownian motion;
Figure DEST_PATH_IMAGE020
is the firstjParticle distribution function of particle size. Equations (1) and (2) can be written in matrix form, respectively:
(3)
Figure DEST_PATH_IMAGE024
(4)
whereinRIs the column vector of the distribution of the autocorrelation function,Sis a power spectral density distribution column vector,Tis a matrix of coefficients of the distribution of the autocorrelation function,Kis a matrix of coefficients of the power spectral density distribution,His the particle size distribution array vector.
In existing methods, the particle size distribution is obtained either from inversion of autocorrelation signals or from inversion of power spectrum signals. When inverting, the matrixTOr
Figure DEST_PATH_IMAGE026
Vector is obtained by theoretical calculation according to the definition in the formula (1) or (2)ROr
Figure DEST_PATH_IMAGE028
Selecting proper inversion method for measuring quantity to obtain vector
Figure DEST_PATH_IMAGE030
The specific numerical value of (1). However, whether based on inversion of autocorrelation signals or power spectrum signals, the coefficient matrix is severely ill-conditioned, and as shown in fig. 5, a small error in the measured signal will result in a large deviation in the particle size distribution, and even a wrong particle size distribution. This limits the confidence in the particle size of the particles. Secondly, the processing of the autocorrelation signals requires expensive digital correlators, the estimation of the power spectrum of the dynamic scattered light requires a high sampling rate of a data acquisition card (a/D card), large computer storage resources and a certain CPU processing time, which is disadvantageous for cost control and real-time measurement.
Disclosure of Invention
The invention aims to improve the original theory and the signal processing mode by means of an analog band-pass filtering technology on the basis of the traditional dynamic light scattering nano-particle measuring principle. The difficulty that the coefficient matrix of the original theoretical model is seriously ill is solved, and the robustness of inversion calculation is improved. The use of a digital correlator is avoided, the requirement on a data acquisition card is reduced, the signal processing time is saved, and the economical and rapid measurement of the particle size is realized.
The technical scheme of the invention is as follows: a dynamic light scattering nanoparticle measurement method based on a band-pass filtering technology is characterized by comprising the following steps:
1. laser emitted by a laser irradiates on nano particles in a solution, scattered light of the particles is directly detected by a photoelectric detector, or is detected by the photoelectric detector after being interfered with partial light of original laser, or is fed back into a laser cavity to generate self-mixing frequency modulation laser output with laser in the cavity, and is detected by the photoelectric detector arranged at the rear end of the laser;
2. signals detected by a photoelectric detector are amplified by a preamplifier and then are sequentially sent to a circuit formed by connecting an M route buffer, band-pass filters with different frequency centers and an RMS root-mean-square processor in series, signal root-mean-square values at M different frequencies are obtained, the signal root-mean-square values are sampled by an A/D acquisition card, and finally power spectral density functions at M different frequencies are obtained, and the theoretical formula can be expressed as follows:
Figure DEST_PATH_IMAGE032
Figure 782877DEST_PATH_IMAGE012
(5)
wherein,iis the frequency channel number
Figure 150404DEST_PATH_IMAGE012
The frequency of the signal corresponding to the different band-pass frequencies,is the total number of channels;jis the grade number of the particle diameter
Figure 667153DEST_PATH_IMAGE006
Figure 248307DEST_PATH_IMAGE008
The total grading number of the particle size;x j is the firstjAverage particle size of the particles;is the firstjThe step width of the step particle size; in the case where the scattered light from the particles reaches the photodetector directly, there areIn the case where the scattered light of the particle interferes with part of the original laser light and reaches the photodetector, or in the case where the scattered light of the particle is fed back into the laser cavity to modulate the laser output, there is a case where the scattered light of the particle is fed back into the laser cavity to modulate the laser output
Figure 328893DEST_PATH_IMAGE018
qIs the value of the scattering vector;D j is the firstjParticle diffusion coefficient of particle size range, including nanoparticle sizex j The information of (a);ωis the angular frequency associated with brownian motion;
Figure DEST_PATH_IMAGE034
is the firstiThe frequency response function of the channel band-pass filter is suitable for passive and active filters of each order;
Figure 826870DEST_PATH_IMAGE020
is the firstjA particle size distribution function for the particle size;
3. converting equation (5) into a matrix form, expressed as
Figure DEST_PATH_IMAGE036
Wherein the power spectral density distribution column vectorSA coefficient matrix of power spectral density distribution obtained by actual measurement of a simulation circuit for a group of measurement quantitiesKAccording to equation (5)
Figure DEST_PATH_IMAGE038
Defining theoretical calculation to obtain, solving matrix equation
Figure 34736DEST_PATH_IMAGE036
Obtaining the column vector of the particle size distribution of the measured particlesH
A device for realizing a dynamic light scattering nano-particle measuring method based on band-pass filtering is characterized by comprising a laser, a measuring area, a photoelectric detector and an analog circuit, wherein the analog circuit comprises a preamplifier, M circuits corresponding to the total number M of frequency channels, a circuit formed by connecting M circuits of buffers, band-pass filters with different frequency centers and an RMS square root processor in series, light beams emitted by the laser irradiate the measuring area, particle scattering light in the measuring area is received by the photoelectric detector, signals output by the photoelectric detector are amplified by the preamplifier and then are parallelly sent to the M circuits formed by connecting M circuits of buffers, band-pass filters with different frequency centers and the RMS square root processor in series, a plurality of signal square root values at different frequencies are obtained, and are sampled by an A/D acquisition card to finally obtain a plurality of power spectral density values.
The invention has the beneficial effects that: the method solves the problem of poor inversion calculation robustness caused by serious morbidity of the coefficient matrix in the original model. The power spectral density is directly acquired by adopting the analog circuit, so that the requirements on the aspects of data acquisition speed, data acquisition quantity, data storage quantity, data processing quantity and the like are reduced, the data processing time is greatly shortened, and the rapid measurement can be realized. Can be used in a plurality of fields relating to the production and process control of nano particles, such as scientific research, biological medicine, chemical energy, environmental protection, and the like.
Drawings
FIG. 1 is an analog signal processing system;
FIG. 2 is a schematic view of an embodiment 1 of the measuring apparatus of the present invention;
FIG. 3 is a schematic view of an embodiment 2 of the measuring apparatus of the present invention;
FIG. 4 is a schematic view of an embodiment 3 of the measuring apparatus of the present invention;
FIG. 5 is a coefficient matrix of the original dynamic light scattering methodKA distribution map of;
FIG. 6 coefficient matrix of the prior art dynamic light scattering methodKDistribution diagram of (c).
Detailed Description
The invention adopts the analog band-pass filtering technology to realize the recording and processing of the power spectral density measured by the dynamic light scattering nano particles, and the specific implementation is described in detail by combining the attached drawings. The method comprises the following implementation steps:
1. laser emitted by a laser 6 irradiates nanoparticles in a solution in a measurement area 7, scattered light of the particles is directly detected by a photoelectric detector 8, see fig. 2, or is detected by the photoelectric detector 8 after interfering with partial light of original laser obtained by beam splitting through a beam splitter 9, see fig. 3, or the scattered light of the particles is fed back into a cavity of the laser 6, generates self-mixing modulation laser output with laser in the cavity, and is detected by the photoelectric detector 8 arranged at the rear end of the laser, see fig. 4;
2. the signal detected by the photoelectric detector 8 is amplified by the preamplifier 2 and then is sequentially sent to a circuit formed by connecting an M routing buffer 3, band-pass filters 4 with different frequency centers and an RMS root-mean-square processor 5 in series, signal root-mean-square values at M different frequencies are obtained, the signal root-mean-square values are sampled by an A/D acquisition card, and finally power spectral density functions at M different frequencies are obtained, which can be expressed by a theoretical formula:
Figure 805562DEST_PATH_IMAGE012
(5)
wherein,iis the frequency channel number
Figure 158046DEST_PATH_IMAGE012
The frequency of the signal corresponding to the different band-pass frequencies,
Figure 38278DEST_PATH_IMAGE014
is the total number of channels;jis the grade number of the particle size
Figure 476212DEST_PATH_IMAGE006
Figure 896829DEST_PATH_IMAGE008
The total grading number of the particle size;x j is the firstjAverage particle sizeMean value;
Figure 307082DEST_PATH_IMAGE010
is the firstjThe step width of the step particle size; in the case where the scattered light from the particles reaches the photodetector directly, there are
Figure 420532DEST_PATH_IMAGE016
In the case where the scattered light of the particle interferes with part of the original laser light and reaches the photodetector, or in the case where the scattered light of the particle is fed back into the laser cavity to modulate the laser output, there is a case where the scattered light of the particle is fed back into the laser cavity to modulate the laser output
Figure 345762DEST_PATH_IMAGE018
qIs the value of the scattering vector;D j is the firstjParticle diffusion coefficient of particle size range, including nanoparticle sizex j The information of (a);ωis the angular frequency associated with brownian motion;
Figure 570070DEST_PATH_IMAGE034
is the firstiThe frequency response function of the channel band-pass filter is suitable for passive and active filters of each order;
Figure 67785DEST_PATH_IMAGE020
is the firstjA particle size distribution function for the particle size;
3. converting equation (5) into a matrix form, expressed as
Figure 352136DEST_PATH_IMAGE036
Wherein the power spectral density distribution column vectorSA coefficient matrix of power spectral density distribution obtained by actual measurement of a group of measurement quantities by the analog circuit 1KAccording to equation (5)
Figure 764663DEST_PATH_IMAGE038
Defining theoretical calculation, as shown in FIG. 6, solving matrix equation
Figure 730345DEST_PATH_IMAGE036
Obtaining the column vector of the particle size distribution of the measured particlesH
A device for realizing a dynamic light scattering nano-particle measuring method based on band-pass filtering is shown in figures 1-4, and is characterized in that the device comprises a laser 6, a measuring area 7, a photoelectric detector 8 and an analog circuit 1, wherein the analog circuit 1 comprises a preamplifier 2, M circuits corresponding to the total number M of frequency channels, a buffer 3, band-pass filters 4 with different frequency centers and an RMS root-mean-square processor 5 which are connected in series, a light beam emitted by the laser 6 irradiates the measuring area 7, particle scattering light in the measuring area 7 is received by the photoelectric detector 8, a signal output by the photoelectric detector 8 is amplified by the preamplifier 2 and then is sent to the M circuits formed by connecting the buffer 3, the band-pass filters 4 with different frequency centers and the RMS root-square processor 5 in series, so as to obtain a plurality of signal root-square values at different frequencies, sampling by an A/D acquisition card, and finally obtaining a power spectral density function.
Example 1 (scattered light of particles is directly detected by photodetector):
shown in fig. 2, it comprises a semiconductor laser 6, a measuring zone 7, a photodetector 8 and an analog circuit 1. The light beam emitted by the laser 6 impinges on the measuring area 7. The scattered light of the particles in the measurement area 7 is received by the photodetector 8 and finally the power spectral density function is obtained by the analog circuit 1.
Example 2 (scattered light of a particle is detected by a photodetector after interfering with a portion of the light of the original laser):
as shown in fig. 3, it includes a semiconductor laser 6, a beam splitter 9, a measurement area 7, a photodetector 8, and an analog circuit 1. The beam splitter 9 is disposed between the laser 6 and the measuring field 7, and the beam emitted by the laser 6 is split into two beams by the beam splitter 9. One beam penetrates through the beam splitter and irradiates the measurement area 7; one beam is reflected by the beam splitter as intrinsic light. The scattered light of the particles in the measuring region 7 interferes with the intrinsic light, is detected by the photoelectric detector 8, and finally the power spectral density function is obtained through the analog circuit 1.
Example 3 (particle scattered light back-fed into the laser cavity to self-mix and modulate the laser output and be detected by the photodetector):
as shown in fig. 4, it comprises a semiconductor laser 6, a measuring zone 7, a photodetector 8 and an analog circuit 1. The photoelectric detector 8 is arranged behind the laser 6, the light beam emitted by the laser 6 irradiates the measuring area 7, and the backward scattered light of the particles is fed back into the laser resonant cavity to be mixed with the original laser. The backward output light of the laser is detected by the photoelectric detector 8, and finally the power spectral density function is obtained through the analog circuit 1.

Claims (4)

1. A dynamic light scattering nanoparticle measurement method based on band-pass filtering is characterized by comprising the following steps:
laser emitted by a laser irradiates nanoparticles in a solution, and scattered light of the particles is directly detected by a photoelectric detector, or is detected by the photoelectric detector after being interfered with partial light of original laser, or is detected by the photoelectric detector after being fed back into a laser cavity to generate a self-mixing signal;
signals detected by a photoelectric detector are amplified by a preamplifier and then are sequentially sent to a circuit formed by connecting an M route buffer, band-pass filters with different frequency centers and an RMS root-mean-square processor in series, signal root-mean-square values at M different frequencies are obtained, the signal root-mean-square values are sampled by an A/D acquisition card, and finally power spectral density functions at M different frequencies are obtained, and the theoretical formula can be expressed as follows:
Figure 66900DEST_PATH_IMAGE001
(5)
wherein,iis the frequency channel number
Figure 779553DEST_PATH_IMAGE002
Figure 2011101270517100001DEST_PATH_IMAGE003
Is the total number of channels;jis the grade number of the particle diameter
Figure 2011101270517100001DEST_PATH_IMAGE005
The total grading number of the particle size of the particles;x j is the firstjAverage particle size of the particles;is the firstjThe step width of the step particle size; in the case of particles whose scattered light reaches the photodetector directly
Figure 2011101270517100001DEST_PATH_IMAGE007
In the case where the scattered light of the particle interferes with part of the original laser light and reaches the photodetector, or in the case where the scattered light of the particle is fed back into the laser cavity to generate the self-mixing modulated laser output, there is a case where the self-mixing modulated laser output is generated
Figure 558787DEST_PATH_IMAGE008
qIs the value of the scattering vector;D j is the firstjParticle diffusion coefficient of particle size range, including nanoparticle sizex j The information of (a);ωis the angular frequency associated with brownian motion;
Figure 2011101270517100001DEST_PATH_IMAGE009
is the firstiThe frequency response function of the channel band-pass filter is suitable for passive and active filters of each order;
Figure 820004DEST_PATH_IMAGE010
is the firstjParticle distribution function of particle size;
transforming equation (5) into a matrix form yields:
Figure 2011101270517100001DEST_PATH_IMAGE011
wherein the power spectral density distribution column vectorSA coefficient matrix of power spectral density distribution obtained by actual measurement of a simulation circuit for a group of measurement quantitiesKAccording to equation (5)
Figure 800467DEST_PATH_IMAGE012
Defining theoretical calculation to obtain, solving matrix equation
Figure 793831DEST_PATH_IMAGE011
Obtaining the column vector of the particle size distribution of the measured particlesH
2. A device for realizing the dynamic light scattering nano-particle measuring method based on band-pass filtering is characterized in that, the device comprises a laser, a measuring area, a photoelectric detector and an analog circuit, wherein the analog circuit comprises a preamplifier, an M route buffer corresponding to the total number M of frequency channels, a circuit formed by connecting band-pass filters with different frequency centers and an RMS root-mean-square processor in series, a light beam emitted by the laser irradiates the measuring area, the scattered light of particles in the measuring area is received by the photoelectric detector, a signal output by the photoelectric detector is amplified by the preamplifier, and the signal square root values at a plurality of different frequencies are obtained and sampled by an A/D acquisition card, and finally a power spectral density function is obtained.
3. The device for realizing the dynamic light scattering nanoparticle measurement method based on band-pass filtering as claimed in claim 2, wherein a beam splitter is disposed between the laser and the measurement region, the beam emitted from the laser is split into two beams by the beam splitter, and one beam passes through the beam splitter and irradiates the measurement region; one beam is reflected by the beam splitter and then used as intrinsic light, particle scattered light in the measuring region is interfered with the intrinsic light and detected by the photoelectric detector, and finally, a power spectral density function is obtained through the analog circuit.
4. The device for realizing the dynamic light scattering nanoparticle measurement method based on band-pass filtering as claimed in claim 2, wherein a photodetector is disposed behind the laser, a light beam emitted from the laser irradiates the measurement region, the backward scattered light of the particles is fed back into the laser resonator to be mixed with the original laser light, the backward output light of the laser is detected by the photodetector, and finally the power spectral density function is obtained through the analog circuit.
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CN110987737A (en) * 2019-12-23 2020-04-10 华中科技大学 Aerosol particle spectrum and concentration measurement method based on light scattering response
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CN103499521B (en) * 2013-09-06 2015-10-21 清华大学 The measuring method of the crucial geometric feature of nano particle
CN103499521A (en) * 2013-09-06 2014-01-08 清华大学 Method for measuring key geometrical characteristics of nanometer particles
CN104458514A (en) * 2014-12-04 2015-03-25 江苏师范大学 Rapid measurement method for particle diameter distribution of laser self-mixing-frequency nano particles
CN105092432B (en) * 2015-06-05 2018-06-15 清华大学 The measuring system of metal nanoparticle grain size
CN105092432A (en) * 2015-06-05 2015-11-25 清华大学 Measurement system of particle size of metal nanoparticles
CN106370569A (en) * 2015-07-22 2017-02-01 天津同阳科技发展有限公司 Particulate matter online monitor signal pre-processing circuit based on Mie scattering
CN105092426A (en) * 2015-07-24 2015-11-25 清华大学 Measuring method for nanoparticle 90-degree scattering spectrum
CN108780030A (en) * 2016-03-21 2018-11-09 皇家飞利浦有限公司 Laser sensor for ultra-fine particle sizes detection
US11119021B2 (en) 2016-03-21 2021-09-14 Trumpf Photonic Components Gmbh Laser sensor for ultra-fine particle size detection
CN109154552A (en) * 2016-05-19 2019-01-04 皇家飞利浦有限公司 Optical particulate sensor
US11092531B2 (en) 2016-05-19 2021-08-17 Trumpf Photonic Components Gmbh Optical particle sensor
CN109154552B (en) * 2016-05-19 2022-08-12 通快光电器件有限公司 Optical particle sensor
CN106940301A (en) * 2017-03-10 2017-07-11 华南师范大学 A kind of particle zeta potential measurement methods and device based on asymmetric electric field
CN106940301B (en) * 2017-03-10 2019-10-11 华南师范大学 A kind of particle zeta potential measurement method and device based on asymmetric electric field
CN110987737A (en) * 2019-12-23 2020-04-10 华中科技大学 Aerosol particle spectrum and concentration measurement method based on light scattering response
CN110987737B (en) * 2019-12-23 2021-02-05 华中科技大学 Aerosol particle spectrum and concentration measurement method based on light scattering response
CN113433038A (en) * 2021-05-31 2021-09-24 昆明理工大学 Novel method for selecting mixed nano fluid particle combination

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