CN102494975A - Single beam cross-correlation high concentration nanoparticle measuring apparatus and method thereof - Google Patents
Single beam cross-correlation high concentration nanoparticle measuring apparatus and method thereof Download PDFInfo
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Abstract
The present invention relates to a single beam cross-correlation high concentration nanoparticle measuring apparatus and a method thereof. According to the present invention, a beam emitted by a laser sequentially passes through a polarizer and a lens, and is focused in a sample cell; scattered light emitted from the sample cell passes through a first pinhole diaphragm, and then passes through a symmetrical two-branch luminous power distributor to separate into two light paths, wherein the scattered light emitted from the sample cell forms an angel of 90 DEG with the incident light path; the two light paths respectively pass through a second pinhole diaphragm and a third pinhole diaphragm, and then pass through a filter; two photoelectric detectors respectively collect and receive the two lights of the two light paths, and transmit the two lights to a digital correlator to carry out processing. With the present invention, the influence due to the stray light can be effectively removed, the system coherence can be improved, the system signal-to-noise ratio can be reduced, the measuring precision is high, the measuring speed is rapid, the on-line measurement can be performed, the apparatus cost is low, the apparatus is easy to maintain, and the replacement parts can be convenient to buy.
Description
Technical field
The present invention relates to a kind of measurement mechanism, particularly a kind of single beam simple crosscorrelation highly concentrated nano particle measurer and method.
Background technology
Nano particle is meant the ultra-fine grain of granularity between 1-100nm, because character such as its distinctive light, magnetic, electricity, heat and catalysis make it at aspects such as catalysis, optical filtering, light absorption, medicine, magnetic medium and new materials wide application prospect arranged.The granularity of nano particle directly affects its various character, so the measuring technique of nano particle is the necessary condition that nanosecond science and technology are able to develop.DLS (Dynamic Light Scattering; Dynamic light scattering) during nano particle is measured; Photon correlation spectroscopy method (Photon Correlation Spectroscopy; PCS) be one of present nano particle standard method of measuring; Owing to have advantages such as measuring speed is fast, scope wide (0.003 μ m-2 μ m), good reproducibility, contactless property, be widely used in the ultra-fine grain in fields such as medicine, space flight, bad border, chemical industry or the measurement of nano particle in recent years, and become the important means that nano particle characterizes in the lean solution scope.But traditional P CS method all requires tested sample is diluted before measuring, to avoid multiple scattering.This has just caused sample to form and has been easy to change, and signal to noise ratio (S/N ratio) reduces, and is subject to the interference problems such as (like dusts, light) of external environment factor, thereby can't be being applied aspect the online in real time measurement.
To this problem, relatively have the method for research potential to have following several kinds at present:
1. simple crosscorrelation dynamic light scattering method.The ultimate principle of simple crosscorrelation dynamic light scattering method is: because multiple scattering light and single scattering light exist wave vector poor; When two beam spreadings are penetrated signal and are carried out simple crosscorrelation; The degree of correlation of multiple scattering and single scattering or multiple scattering and multiple scattering signal is all far below the auto-correlation of single scattering and single scattering signal.Equate that as long as therefore satisfy the scattering wave vector reflection of the cross correlation function of scattered light intensity decay live width is the information of single scattering light so, thereby has eliminated the influence of multiple scattering light.The cross correlation measurement method can well be eliminated the multiple scattering effect in theory; But since its to require two photomultiplier positions to satisfy the scattering wave vector identical; Therefore in practical application, exist device to install and regulate and require a too high difficult problem, the system signal noise ratio of this method is low in addition also is another limitations.
2. (Diffusing Wave Spectroscopy, DWS), this method is proposed in 1988 by D. J. Pine etc. the dilatation wave spectrometry the earliest.Its basic theories be through measure incident light between granular system repeatedly the light intensity after the scattering change, obtain the autocorrelation function of system, and then obtain the method for particle grain size information, therefore be applicable to the measurement under the high concentration.But because it requires not comprise in the scattered signal single scattering light; So restricted application (surfactant solution and the grain graininess in the gel rheology like very high concentrations are measured); And the theoretical system of this method is perfect not enough, and correlation technique still is in conceptual phase.
3. optical fiber dynamic light scattering method.The optical fiber dynamic light scattering method is to adopt gradient-index lens as fibre-optical probe, and the scattered light of direct detection probe end face particle, thereby has shortened the scattering light path, has realized the direct measurement to enriched sample.The advantage of this system is that advantages of small volume, closure are good, easy to use; But fiber end face can influence measurement result to reflection of incident light; In addition; Coupling efficiency between scattering light source and the exploring block is lower, and the gradient-index lens cost is high, and problem such as easy loss also is that the optical fiber dynamic light scattering method need overcome a difficult problem.
4. low coherence interferometry.Low coherence interferometry is to utilize relatively shorter these characteristics of light path of single scattering light, utilizes coherent technique that single scattering light is picked out.But this method is not suitable for the measurement under the bulky grain high concentration, and the design more complicated of these systems, and the condition in the experimentation is not easy control, under the situation that is merely able to regulate meticulously in the laboratory scattering sample is measured.
In addition, have also comprising of application potential: the analysis of scattering spot, delustring pulse 1 method, ultrasonic attenuation method etc., but the reliability of these methods still remains a large amount of practice tests, on concrete the realization, has indivedual technological difficulties, and cost is relatively also higher.
Because the particle in the suspending liquid receives particle to carry out the continuous bump of the molecule of Brownian motion on every side, its scattered light light intensity to fixed light source can random fluctuation.The speed of this fluctuation is relevant with particle grain size, and particle is more little, and fluctuation is fast more; Particle is big more, and fluctuation is slow more; Analysis through to the scattered light intensity fluctuation just can obtain particle grain size information.The simple crosscorrelation dynamic light scattering method is measured grain diameter through the cross correlation function that calculates scattered light intensity; It is identical that but traditional simple crosscorrelation dynamic light scattering requires two photoelectric probe positions to satisfy the scattering wave vector; Therefore in practical application, exist device to install and regulate and require a too high difficult problem, therefore be not suitable for the concentration condition with higher.
Summary of the invention
The present invention be directed to the problem of nano particle measuring equipment costliness, the high test difficulty of concentration; A kind of single beam simple crosscorrelation highly concentrated nano particle measurer and method have been proposed; Being used for solving measurement concentration is 20～50000ppm, and particle diameter is the technical matters of the grain diameter between 5～1000nm.
Technical scheme of the present invention is: a kind of single beam simple crosscorrelation highly concentrated nano particle measurer; Comprise laser instrument, the polarizer, lens, sample cell, three pinhole diaphragms, symmetrical two branch optical power distributers, optical filter, two photodetectors, digital correlator; The laser instrument emitted light beams arrives sample cell through the polarizer, lens focus successively, forms input path; Sample cell sends becomes 90 degree with input path scattered light through first pinhole diaphragm after through separating into the two-way light path behind symmetrical two branch optical power distributers; The two-way light path through passing through optical filter behind second pinhole diaphragm and the 3rd pinhole diaphragm, is formed receiving light path respectively; Two photodetectors send digital correlator to handle after gathering the two-way light of receiving light path respectively.
A kind of single beam simple crosscorrelation highly concentrated nano particle sizing method comprises single beam simple crosscorrelation highly concentrated nano particle measurer, specifically comprises following measuring process:
1) with laser instrument (1) as light source, input path shines in the sample cell (4) that fills particle;
2) with two CCD of same model or CMOS (10,11) as photo-detector; The scattered light of 90 degree that sample cell (4) sends is through behind the receiving light path; As photo-detector, the scattered light that receiving light path is penetrated carries out continuous coverage with two CCD of same model or CMOS (10,11);
3) two photodetectors (10,11) convert the light signal that records to the track of scattering spot on the continuous sequential image respectively, and the track of this scattering spot reflects the fluctuating signal of Brownian movement;
4) digital correlator (12) calculates cross correlation function according to pulse signal, and its expression formula is:
In the formula,
r 1,
r 2Be respectively CCD or CMOS (10,11) and record scattering point on the scattered light movement locus with respect to the distance of track origin;<>Be the time ensemble average;
R 12 2Be cross correlation function, it and the translation coefficient of diffusion of describing Brownian movement intensity
D T And time-delay
τFollowing relational expression is arranged:
Wherein
k BBe the Boltzman constant; T is an absolute temperature; η is a solution viscosity;
dBe particle diameter, calculate cross correlation function after, call software for calculation again and calculate grain diameter.
Beneficial effect of the present invention is: single beam simple crosscorrelation highly concentrated nano particle measurer of the present invention and method, the influence of effectively removing parasitic light, the coherence who improves system, the signal to noise ratio (S/N ratio) of reduction system; Measuring accuracy is high, speed is fast, and can carry out on-line measurement; The cost of device is low; Be easy to safeguard, can buy the parts of replacement easily.
Description of drawings
Fig. 1 is a single beam simple crosscorrelation highly concentrated nano particle measurer fundamental diagram of the present invention.
Embodiment
Single beam simple crosscorrelation highly concentrated nano particle measurer fundamental diagram of the present invention as shown in Figure 1 comprises laser instrument 1, the polarizer 2, lens 3; Sample cell 4, pinhole diaphragm 5,7,8, symmetrical two branch optical power distributers 6; Optical filter 9, photodetector 10,11, digital correlator 12.Form input path by laser instrument 1, the polarizer 2, lens 3, sample cell 4.By sample cell 4, pinhole diaphragm 5,7,8, symmetrical two branch optical power distributers 6, optical filter 9 is formed receiving light path.Collection and the processing unit of forming scattered signal by photodetector 10,11 and digital correlator 12.Photodetector 10,11 all is the CCD or the CMOS of same model; Be installed on the 90 degree scattering light paths; Make scattered light successively through isolating the two-way light path behind pinhole diaphragm 5, symmetrical two branch optical power distributers 6; This two-way scattered light through behind pinhole diaphragm 7,8 and the optical filter 9, gets into photodetector 10,11 respectively respectively.Wherein pinhole diaphragm 5 is used for the parasitic light of filtered signal in transmission course; Symmetry two branch optical power distributers 6 are used for the road scattered light of accepting is isolated the two-way scattered light; Pinhole diaphragm 7,8 is used for the parasitic light of filtered signal in transmission course, and limits the receptor area of photodetector; Optical filter 9 is used for the optical band of filtered signal parasitic light, to guarantee the coherence of system.
Measurement mechanism operation steps of the present invention is: at first open laser instrument 1 preheating, the adjustment polarizer 2 is confirmed the polarisation of light direction, and adjustment lens 3 make incident light focus on the inboard of sample cell 4 antethecas; Aperture diaphragm 5 is placed on the direction of scattered light 90 degree; Adjusting symmetrical two branch optical power distributers 6 makes the scattered light of its reception 90 degree and isolates the two-way scattered light; The two-way scattered light successively through behind aperture diaphragm 7,8 and the optical filter 9, gets into photodetector 10,11 respectively respectively; The sample cell that fills standard model 4 is put into measurement zone; Start data acquisition software and data computation software in the digital correlator 12, calculate cross correlation function, and calculate particle grain size.
Concrete measuring process of the present invention is:
1) with laser instrument 1 as light source, shine in the sample cell 4 that fills particle;
2) with two photomultipliers 10,11 as photo-detector respectively with 90 the degree scattering angle continuous coverage scattered light signal;
3) photodetector 10,11 converts the light signal that records to the track of the scattering spot on the continuous sequential image respectively, and the track of this scattering spot reflects the fluctuating signal of Brownian movement;
4) digital correlator 12 calculates cross correlation function according to pulse signal, and its expression formula is:
In the formula,
r 1,
r 2Be respectively CCD or CMOS (10,11) and record scattering point on the scattered light movement locus with respect to the distance of track origin;<>Be the time ensemble average;
R 12 2Be cross correlation function, it and the translation coefficient of diffusion of describing Brownian movement intensity
D T And time-delay
τFollowing relational expression is arranged:
Wherein
k BBe the Boltzman constant; T is an absolute temperature; η is a solution viscosity;
dBe particle diameter.After calculating cross correlation function, call software for calculation again and calculate grain diameter.
Adopt the cross correlation function curve of the resulting scattering luminous point of digital correlator computing, calculate the translation coefficient of diffusion
D T For: 2.42 * 10
-8Cm
2S
-1
Laboratory temperature is 25 ℃; The viscosity coefficient η of water is 0.00943dynscm-2; According to Stokes-Einstein formula
, obtain grain diameter d=96nm.
Claims (2)
1. single beam simple crosscorrelation highly concentrated nano particle measurer; It is characterized in that; Comprise laser instrument (1), the polarizer (2), lens (3), sample cell (4), three pinhole diaphragms (5,7,8), symmetrical two branch optical power distributers (6), optical filter (9), two photodetectors (10,11), digital correlator (12); Laser instrument (1) emitted light beams is passed through the polarizer (2) successively, lens (3) focus on sample cell (4), forms input path; The scattered light that becomes 90 degree with input path that sample cell (4) sends is back through separating into the two-way light path behind symmetrical two branch optical power distributers (6) through first pinhole diaphragm (5); The two-way light path is passed through optical filter (9) through second pinhole diaphragm (7) and the 3rd pinhole diaphragm (8) back respectively, forms receiving light path; Two photodetectors (10,11) send digital correlator (12) to handle after gathering the two-way light of receiving light path respectively.
2. a single beam simple crosscorrelation highly concentrated nano particle sizing method comprises single beam simple crosscorrelation highly concentrated nano particle measurer, it is characterized in that, specifically comprises following measuring process:
As light source, input path shines in the sample cell (4) that fills particle with laser instrument (1);
2) with two CCD of same model or CMOS (10,11) as photo-detector; The scattered light of 90 degree that sample cell (4) sends is through behind the receiving light path; As photo-detector, the scattered light that receiving light path is penetrated carries out continuous coverage with two CCD or CMOS (10,11);
3) two photodetectors (10,11) convert the light signal that records to the track of the scattering spot on the continuous sequential image respectively, and the track of this scattering spot reflects the fluctuating signal of Brownian movement;
4) digital correlator (12) calculates cross correlation function according to fluctuating signal, and its expression formula is:
In the formula,
r 1,
r 2Be respectively CCD or CMOS (10,11) and record scattering point on the scattered light movement locus with respect to the distance of track origin;<>Be the time ensemble average;
R 12 2Be cross correlation function, it and the translation coefficient of diffusion of describing Brownian movement intensity
D T And time-delay
τFollowing relational expression is arranged:
Wherein
k BBe the Boltzman constant; T is an absolute temperature; η is a solution viscosity;
dBe particle diameter, calculate cross correlation function after, call software for calculation again and calculate grain diameter.
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| CN106501137A (en) * | 2015-09-07 | 2017-03-15 | 济南微纳颗粒仪器股份有限公司 | A kind of use laser particle analyzer measures the system and method for granule sphericity |
| CN109870394A (en) * | 2018-12-30 | 2019-06-11 | 江苏苏净集团有限公司 | A kind of dual-beam aerosol particle concentration detection device |
| CN110426326A (en) * | 2019-08-08 | 2019-11-08 | 杭州晶耐科光电技术有限公司 | Detection and the laser polarization device and method for distinguishing smooth surface and sub-surface particle |
| CN110672559A (en) * | 2019-10-25 | 2020-01-10 | 西安交通大学 | Device and method for simultaneously measuring binary system thermal diffusivity and mutual diffusivity |
| CN113984601A (en) * | 2021-12-28 | 2022-01-28 | 中国电子科技集团公司第二十八研究所 | Environmental dust monitoring system |
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| CN110426326A (en) * | 2019-08-08 | 2019-11-08 | 杭州晶耐科光电技术有限公司 | Detection and the laser polarization device and method for distinguishing smooth surface and sub-surface particle |
| CN110426326B (en) * | 2019-08-08 | 2021-08-03 | 杭州晶耐科光电技术有限公司 | Laser polarization device and method for detecting and distinguishing smooth surface particles from sub-surface particles |
| CN110672559A (en) * | 2019-10-25 | 2020-01-10 | 西安交通大学 | Device and method for simultaneously measuring binary system thermal diffusivity and mutual diffusivity |
| CN110672559B (en) * | 2019-10-25 | 2021-01-19 | 西安交通大学 | Device and method for simultaneously measuring binary system thermal diffusivity and mutual diffusivity |
| CN113984601A (en) * | 2021-12-28 | 2022-01-28 | 中国电子科技集团公司第二十八研究所 | Environmental dust monitoring system |
| CN113984601B (en) * | 2021-12-28 | 2022-04-08 | 中国电子科技集团公司第二十八研究所 | Environmental dust monitoring system |
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Application publication date: 20120613 |