CN101699265A - Device and method for measuring scattering particles by using dynamic polarized light - Google Patents
Device and method for measuring scattering particles by using dynamic polarized light Download PDFInfo
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- CN101699265A CN101699265A CN200910197776A CN200910197776A CN101699265A CN 101699265 A CN101699265 A CN 101699265A CN 200910197776 A CN200910197776 A CN 200910197776A CN 200910197776 A CN200910197776 A CN 200910197776A CN 101699265 A CN101699265 A CN 101699265A
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Abstract
The invention relates to a device and a method for measuring scattering particles by using dynamic polarized light. The laser light emitted by a laser enters a polarizer, a half-wave plate and an incident light path consisting of lenses in turn; light output by lenses focus radiates on a particle sample in a sample cell; the scattered light, which is generated by sample particles irradiated by laser beams and is vertical to the direction of incident laser light, enters an aperture stop, an analyzer and a receiving light path consisting of the aperture stop in turn and finally enters a photomultiplier to convert optical signals into electric signals which are output and enter a digital correlator to perform counting, and finally, data is sent into a microcomputer for processing. The device and the method improve the concentration of a measurable sample, and a measuring system has a simple structure, strong applicability, convenient later maintenance and a low cost.
Description
Technical field
The present invention relates to a kind of nano particle diameter measurement mechanism, particularly a kind of device and method of under middle and high concentration, directly measuring nano particle diameter.
Background technology
Dynamic light scattering (Dynamic Light Scattering, DLS) technology is to survey the important means of particle movement character, it is mainly used is the translation coefficient of diffusion that can measure in the solution big molecule or particle rapidly and accurately, thereby learns its size or hydrodynamic radius.The DLS technology has been widely used in the nano particles measurement in fields such as medicine, space flight, environment, chemical industry at present, and becomes the standard approach that ultra-fine grain characterizes in the lean solution.
But because the restriction of design concept, present DLS method only is applicable to the measurement in the lean solution scope, depends on the sampling dilution when measuring the middle and high concentration particle, to avoid multiple scattering effect between particle more.But this also may cause sample to form and change, and signal to noise ratio (S/N ratio) reduces, and is subject to the interference problems such as (as dusts, light) of external environment factor, has limited it further applying aspect the online in real time measurement.Thereby the research in this field in recent years mainly concentrates on: how to solve the difficult problem that the dynamic light scattering technology can't directly be measured grain diameter under the middle and high concentration, the most representative in the present method have simple crosscorrelation spectroscopic methodology and a dilatation wave spectrometry.But the former can only use it owing to too high to the accuracy requirement of device under laboratory condition; And the latter's algorithm is also too complicated, and only is applicable to the grain graininess measurement of ultrahigh concentration solution, therefore still is in the experimental study stage.In addition, also have additive method as: the scattering spot is analyzed, delustring pulsation method, ultrasonic attenuation method, and low-coherence measuring method etc., but also has indivedual technological difficulties on specific implementation, and cost is relatively also higher.
Summary of the invention
The present invention be directed to the existing problem that the middle and high concentration particle has difficulties of measuring, a kind of scattering particles by using dynamic polarized light measurement mechanism and measuring method have been proposed, being used to solve the measurement volumes percent concentration is 0.1%～10%, and particle diameter is the technical matters of the grain diameter between 10～1000nm.
Technical scheme of the present invention is: a kind of scattering particles by using dynamic polarized light measurement mechanism, comprise that sample cell also comprises laser instrument, the polarizer, / 2nd wave plates, lens, aperture diaphragm, analyzer, photomultiplier, digital correlator, microcomputer, the laser that laser instrument is launched enters the polarizer successively, / 2nd wave plates, the input path that lens are formed, on the particulate samples of rayed in sample cell by lens focus output, the scattered light perpendicular to incident laser direction that is produced by the sample particle of laser beam irradiation enters aperture diaphragm successively, analyzer, aperture diaphragm is formed receiving light path, enter photomultiplier at last and convert light signal to electric signal output and enter digital correlator and count, final data is sent in the microcomputer and is handled.
A kind of scattering particles by using dynamic polarized light measuring method comprises the scattering particles by using dynamic polarized light measurement mechanism, it is characterized in that method comprises the steps:
1) with laser instrument as light source, by the polarizer and 1/2nd wave plates, by lens focus in the sample cell that fills particle;
2) use photomultiplier as the scattering angle continuous coverage scattered light signals of photo-detector with 90 degree;
3) photodetector converts the light signal that records to the TTL pulse voltage signal, the light-intensity variation of the frequency change reflection scattered light of this pulse signal; Digital correlator calculates autocorrelation function according to pulse signal, and its expression formula is: in G (τ)=1+exp (the 2 Г τ) formula, Г is the Rayleigh live width, it and the translation diffusion coefficient D of describing Brownian movement intensity
TAnd Scattering of Vector q has following relational expression:
Г=D
Tq
2 
K wherein
BBe the Boltzman constant; T is an absolute temperature; η is a solution viscosity; D is a particle diameter, calculates autocorrelation function and sends into microcomputer;
4) autocorrelation function that calculates according to step of microcomputer is tried to achieve particle grain size.
Beneficial effect of the present invention is: scattering particles by using dynamic polarized light measurement mechanism of the present invention and measuring method, but the concentration of raising test sample product, and simple in measurement system structure, application is strong, and the convenient later maintenance cost is low.
Description of drawings
Fig. 1 is a scattering particles by using dynamic polarized light measuring principle block diagram of the present invention.
Embodiment
Scattering particles by using dynamic polarized light measuring principle block diagram as shown in Figure 1, middle and high concentration particle measurer based on the dynamic polarization light scattering of the present invention comprises laser instrument 1, the polarizer 2, / 2nd wave plates 3, lens 4, sample cell 5, aperture diaphragm 6,8, analyzer 7, photomultiplier 9, digital correlator 10, microcomputer 11.
The light that laser instrument 1 is launched enters the input path of the polarizer 2,1/2nd wave plates 3, lens 4 compositions successively.Wherein the polarizer 2 is used to improve the degree of polarization of laser, is the altitude line polarized light to guarantee incident light./ 2nd wave plates 3 are used to change the polarization of incident light direction, and the polarization direction here is perpendicular to scattering surface (being surface level).Lens 4 are used for incident laser is focused in sample cell 5 sample solutions a bit.
Formed receiving light path through aperture diaphragm 6, analyzer 7, aperture diaphragm 8 successively by the scattered light that the particle in the sample cell 5 of laser beam irradiation produces perpendicular to incident laser direction.Receiving light path output light signal enters collection and the processing unit that photomultiplier 9, digital correlator 10 and microcomputer 11 are formed scattered signal.Photomultiplier 9 is installed on the light path of 90 degree scattering angle, makes scattered light successively by aperture diaphragm 6, analyzer 7, aperture diaphragm 8, laggardly goes into photoelectricity multiplier tube 9.Wherein aperture diaphragm 6 is used to limit the scatterer volume to improve scattered light intensity and to determine coherent area, and the polarization direction of analyzer 7 is used for filtering multiple scattering light for being parallel to the incident light polarization direction, and the bonding scattered light accounts for leading.Aperture diaphragm 7 is used to limit the photosensitive area of photodetector to guarantee that it is smaller or equal to coherent area.
Concrete measuring process of the present invention is:
1) with laser instrument 1 as light source, by the polarizer and 1/2nd wave plates, by convex lens focus in the sample cell that fills particle;
2) use photomultiplier as the scattering angle continuous coverage scattered light signals of photo-detector 9 with 90 degree;
3) photodetector 9 converts the light signal that records to the TTL pulse voltage signal, the light-intensity variation of the frequency change reflection scattered light of this pulse signal; Digital correlator 10 calculates autocorrelation function according to pulse signal, and its expression formula is: in G (τ)=1+exp (the 2 Г τ) formula, Г is the Rayleigh live width, it and the translation diffusion coefficient D of Brownian movement intensity is described
TAnd Scattering of Vector q has following relational expression:
Г＝D
Tq
2
K wherein
BBe the Boltzman constant; T is an absolute temperature; η is a solution viscosity; D is a particle diameter.Calculate autocorrelation function and send into computing machine 15;
4) microcomputer 11 is tried to achieve particle grain size according to the autocorrelation function that is calculated.
Example: adopt the resulting light intensity autocorrelator trace of digital correlator computing, its exponential damping law is: ln[G (τ)]=-1693 τ, pulse signal according to 14 pairs of photomultiplier outputs of digital correlator by expression formula is: G (τ)=1+exp (2 Г τ), the live width that can obtain decaying is: Г=846s
-1
The He-Ne Lasers wavelength that test is adopted is λ
0=632.8nm, the refractive index of water is m=1.33, scattering angle is 180 degree, according to the computing formula of Scattering of Vector q
Can obtain Scattering of Vector q=2.64 * 10
5Cm
-1
Translation diffusion coefficient D according to decay live width Г and description Brownian movement intensity
TAnd the relational expression of Scattering of Vector q: Г=D
Tq
2, can be in the hope of the translation diffusion coefficient D
TFor: 3.2 * 10
-8Cm
2S
-1
Laboratory temperature is 25 ℃, and the viscosity coefficient η of water is 0.00943dynscm
-2, according to the Stokes-Einstein formula
Obtain grain diameter d=145nm.
Claims (2)
1. scattering particles by using dynamic polarized light measurement mechanism, comprise sample cell (5), it is characterized in that, also comprise laser instrument (1), the polarizer (2), / 2nd wave plates (3), lens (4), aperture diaphragm (6,8), analyzer (7), photomultiplier (9), digital correlator (10), microcomputer (11), the laser that laser instrument (1) is launched enters the polarizer (2) successively, / 2nd wave plates (3), the input path that lens 4 are formed, focus on by lens (4) on the particulate samples of rayed in sample cell (5) of output, the scattered light perpendicular to incident laser direction that is produced by the sample particle of laser beam irradiation enters aperture diaphragm (6) successively, analyzer (7), aperture diaphragm (8) is formed receiving light path, enter photomultiplier (9) at last and convert light signal to electric signal output and enter digital correlator (10) and count, final data is sent in the microcomputer (11) and is handled.
2. a scattering particles by using dynamic polarized light measuring method comprises the scattering particles by using dynamic polarized light measurement mechanism, it is characterized in that method comprises the steps:
1) uses laser instrument (1) as light source,, focus in the sample cell (5) that fills particle by lens (4) by the polarizer (2) and 1/2nd wave plates (3);
2) use photomultiplier (9) as the scattering angle continuous coverage scattered light signals of photo-detector with 90 degree;
3) photodetector converts the light signal that records to the TTL pulse voltage signal, the light-intensity variation of the frequency change reflection scattered light of this pulse signal; Digital correlator (10) calculates autocorrelation function according to pulse signal, and its expression formula is: in G (τ)=1+exp (the 2 Γ τ) formula, Γ is the Rayleigh live width, it and the translation diffusion coefficient D of describing Brownian movement intensity
TAnd Scattering of Vector q has following relational expression: Γ=D
Tq
2 K wherein
BBe the Boltzman constant; T is an absolute temperature; η is a solution viscosity; D is a particle diameter, calculates autocorrelation function and sends into microcomputer (11);
4) autocorrelation function that calculated according to step (3) of microcomputer (11) is tried to achieve particle grain size.
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| CN104089855A (en) * | 2014-07-17 | 2014-10-08 | 清华大学深圳研究生院 | Method and device for measuring particles by polarized light scattering |
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