CN102213669A - Device and method for measuring granularity of dynamic light scattering nano particles of image - Google Patents
Device and method for measuring granularity of dynamic light scattering nano particles of image Download PDFInfo
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Abstract
The invention discloses a device and method for measuring granularity of dynamic light scattering nano particles of an image. The device comprises a laser source, a sample pool, a lens and a surface array photosensitive device which are coaxially arranged from left to right. The method comprises the steps: incident laser of a laser beam irradiates particles in the sample pool, the particles making a Brownian movement in the sample pool generate dynamic light scattering under the irradiation of the incident laser, dynamic light scattering signals of the particles are shot by a surface array digital camera configured on the focus surface of the lens after passing through the lens, and the exposure time of the camera is controlled so that scattering spots of the particles form a tracking line on a shot image, and granularity and distribution of the particles are obtained after data processing is carried out. The invention has the advantages that the scattering light dynamic signals of the particles are simultaneously measured by using the surface array digital camera and are processed to obtain the granularity and the distribution of the particles, the measurement time is short and the particles with a granularity range from nanometer to micrometer can be simultaneously measured.
Description
Technical field
The present invention relates to a kind of grain graininess measuring method, thereby particularly a kind of employing face battle array digital camera single frames single exposure image taking particle Brownian movement track obtains nanometer, sub-micron based on the dynamic light scattering principle
A kind of image dynamic light scattering nano particles measurement mechanism and method with micron particles granularity and distribution.
Background technology
The main method of particle sizing has the laser particle analyzer based on light scattering theory, is the static scattered light of measuring particle in laser particle analyzer.Its ultimate principle is when laser incides tested particle; particle meeting scattering incident laser; the space distribution of its scattering luminous energy is relevant with the size of particle, measures the space distribution of its scattering luminous energy, uses the size-grade distribution that light scattering theory and inversion algorithm can obtain tested particle then.In this measuring method and laser particle analyzer,, measure so be called the static light scattering method because only consider the scattered light intensity of particle and the relation of grain size based on this method development.This method is applicable to the granulometry of submicron particles to micron particles, is subjected to the restriction of static light scattering principle, not the granularity of energy measurement nano particle.
The multiple dynamic light scattering nano particles measuring method that the granulometry of nano particle mainly contains electron microscope and develops based on the dynamic light scattering theory, photon correlation spectroscopy method most importantly wherein, Photon correlation spectroscopy is called for short PCS.
The ultimate principle of PCS nano particles measuring method is when beam of laser incides tested nano particle sample, because the Brownian movement of nano particle in liquid, its scattered light can be pulsed, and the height of its ripple frequency is relevant with the coefficient of diffusion of particle, and coefficient of diffusion
D t Relevant with the granule size of particle, the diffusion of particle and the relation of granularity can be described with the Stocks-Einstein formula:
In the formula
K B Be the graceful constant of bohr thatch,
TBe absolute temperature,
ηBe viscosity,
RIt is the radius of particle to be measured.
PCS nano particles method based on the classics of above-mentioned theory is measured its scattered light pulse in incident light 90 degree directions with photomultiplier or avalanche diode, adopts the correlator deal with data, obtains the coefficient of diffusion of particle
D t , obtain the size-grade distribution of nano particle then according to above-mentioned theory.This kind measuring method is existing historical for many years, is the main method that present nano particle is measured, but still comes with some shortcomings, as being to obtain enough particle informations, the sampling time requires very long, the apparatus structure complexity, require tested granule density extremely low, cause specimen preparation difficulty etc.
Patent WO2010/149887 has improved this measuring method, adopts the rear orientation light of back to 180 degree angular measurement nano particles, and uses optical fiber input instead and receive measuring light, can measure the nano particle of high concentration.
Because the scattered light intensity of nano particle is very weak,, must adopt more powerful laser instrument for obtaining the signal of sufficient intensity.Japan Shimadzu company has proposed a kind of new nano particle measuring method and instrument IG-1000 Particle Size Analyzer.In this method, light-sensitive detector spare is not a scattered light of measuring nano particle, but the electric field that produces with comb electrode earlier forms grating with tested nano particle, and beam of laser is incided this grating, measures its diffraction light.Remove electric field then, particle can spread, and measure the change procedure of diffraction light this moment again, will obtain the size-grade distribution of particle after the Measurement and Data Processing.
Patent GB2318889(NanoSight) a kind of method of measuring each nano particles according to nano particle Brownian movement track following has been proposed.In the method, one hemibase of sample cell plates metal level as thin as a wafer, second half bottom surface, transparent sample pond is plated film not, converge laser beam inciding from the side between sample cell plated film district and border that plated film does not go from sample cell, tested particle is produced than strong scattering light by diffraction effect and plasma resonant vibration effect meeting under laser radiation, is received with microcobjective at the incident light an angle of 90 degrees.Because particle is done Brownian movement, the scattered light meeting random drift that produces when particle is done Brownian movement under the laser radiation, write down the random drift movement locus of each particle with the digital micro-analysis object lens that have the CCD camera, be the Brownian movement track of tested nano particle, just can obtain the granularity of each particle according to Stocks-Einstein formula (1).
Summary of the invention
The objective of the invention is to develop a kind of dynamic light scattering nano particle that can measure a plurality of particles simultaneously
A kind of image dynamic light scattering nano particles measurement mechanism and the method for granularity.
Ultimate principle of the present invention: when nano particle suspends, be subjected to a large amount of unordered bumps of fluid molecule of periphery in liquid, can produce motion at random, this motion of particle is called Brownian movement.When laser incided tested nano particle sample, light scattering all can take place in all particles that shine, and adopted lens to receive the scattered light of particle, and the scattered light of particle can form luminous point on the focal plane of lens.Because the Brownian movement of tested nano particle, these scattering luminous points are not static on focal plane, but random motion.According to theory of Brownian motion, particle is more little, and its random motion is fierce more, and movement velocity is fast more, and particle is big more, and random motion is slow more, and movement velocity is also low more, in the expectation value of the relative origin displacement of moment particle square is:
Therefore, if can record nano particle in process
Displacement after time just can obtain coefficient of diffusion
D t ,Use formula (1) to obtain the radius of tested particle then
R
According to theory of Brownian motion and Stocks-Einstein formula, the displacement that can take the scattering luminous point of record particle with the face battle array digital camera that is arranged on the lens focal plane.Accurate time shutter of control CCD and CMOS camera, can be so that each scattering luminous point of nano particle form 1 trajectory on image, rather than 1 luminous point, shown in Fig. 1.The corresponding nano particle of the length of this trajectory is in the camera exposure displacement that Brownian movement causes in the time.Measure the length of this trajectory, just can obtain the Brownian movement displacement of tested particle, and then obtain the granularity of particle.Owing to write down the light scattering point of many particles on 1 two field picture simultaneously, all the light scattering points on this two field picture are carried out data processing, according to the difference of the course length of each particle, just can obtain the size-grade distribution of particle.
Based on above-mentioned inventive principle, technical scheme of the present invention is: a kind of image dynamic light scattering nano particles measurement mechanism, be characterized in, this measurement mechanism is from left to right by lasing light emitter, sample cell, lens, face battle array photosensitive device coaxial arrangement constitutes, the particle of the laser beam incident laser radiation that lasing light emitter sends in the sample cell, the particle of doing Brownian movement in the sample cell produces dynamic light scattering under the incident laser irradiation, the dynamic light scattering signal of these particles is through behind the lens, the face battle array digital camera that is disposed on the lens focal plane is taken, the time shutter of control camera, make the scattering luminous point of particle on the image of taking, form trajectory.These trajectories are carried out data processing, obtain the granularity and the distribution of particle.
A kind of a kind of image dynamic light scattering nano particles measuring method of utilizing above-mentioned measurement mechanism is characterized in that these method concrete steps are:
1. the laser beam incident that will be sent by lasing light emitter is added with water or particle dispersion liquid to sample cell in the sample cell;
2. with face battle array digital camera shooting bias light signal pattern and record at this moment;
3. in sample cell, add tested particulate samples;
4. Simulated dynamic scattering light signals image and recorded and stored after shooting adds particulate samples measured in the time shutter of control figure camera and record;
5. behind the image of the dynamic light scattering signal that writes down particulate samples, according to the bias light image particle signal image is handled earlier, eliminated the noise of bias light signal;
6. to the dynamic light scattering track of the particle Brownian movement trajectory analysis particle behind the elimination noise, measure the course length of each particle, according to theory of Brownian motion,
Constantly the expectation value of the relative origin displacement of particle square is:
Track by particle is tried to achieve coefficient of diffusion according to formula (2)
D t , use the Stocks-Einstein formula again:
(1)
Obtain the grain graininess of this track correspondence;
7. the granularity of each particle that will obtain gathers and adds up, and obtains the size-grade distribution of particle.
Described sample cell is arranged in the back of receiver lens, the laser beam of being sent by lasing light emitter incides earlier sample cell behind lens, the dynamic scattering light of its particle is disposed in the face battle array digital camera of forward direction again and takes, and obtains stochastic distribution particle scattered light locus of points image.
Described battle array digital camera is arranged in the incoming laser beam side direction of being sent by lasing light emitter, and be arbitrarily angled to 135 degree angles etc. as an angle of 90 degrees position or side forward direction miter angle or rear flank.
Described battle array digital camera is made up of first battle array digital camera and second battle array digital camera, described lens are made up of first lens and second lens, first battle array digital camera and second battle array digital camera are arranged in the forward direction 0 degree position and the lateral position of the incoming laser beam that is sent by lasing light emitter, as other angles such as 90 degree positions or miter angle positions, the dynamic light scattering signal of incoming laser beam after sample cell is by the particle scattering received by first lens and second lens respectively, taken by first battle array digital camera and second battle array digital camera respectively again, measure the forward direction of particle and the trace image of side direction dynamic scattering luminous point simultaneously.
Described battle array digital camera is CCD or CMOS camera.
The invention has the beneficial effects as follows the scattered light Dynamic Signal that utilizes CCD or CMOS face battle array digital camera can measure many particles simultaneously, dynamic scattering optical track mark to all these particles is handled respectively, just can obtain the size-grade distribution of particle, significantly reduced Measuring Time, and can measure the particle of particle size distribution simultaneously than broad, as several nanometers are promptly arranged, hundreds of nanometers are also arranged, even arrive the particle of micron.And photon correlation spectroscopy method (PCS) the nano particles instrument based on the dynamic light scattering principle at present commonly used is that to obtain the Measuring Time that result accurately needs very long, normally tens of second by more than 100 seconds, and when wide size-grade distribution particle sizing, be difficult to obtain result accurately.
Description of drawings
Fig. 1 is the synoptic diagram of light scattering point track in image;
Fig. 2 is the embodiment of the invention 1 synoptic diagram;
Fig. 3 is the embodiment of the invention 2 synoptic diagram;
Fig. 4 is the embodiment of the invention 3 synoptic diagram;
Fig. 5 is the embodiment of the invention 4 synoptic diagram.
Embodiment
A kind of image dynamic light scattering nano particles measurement mechanism, by shown in Figure 2, this measurement mechanism is from left to right by lasing light emitter 1, sample cell 3, lens 2, face battle array photosensitive device 4 coaxial arrangement constitute, the particle of the laser beam incident laser radiation that lasing light emitter 1 sends in the sample cell 3, the particle of doing Brownian movement in the sample cell 3 produces dynamic light scattering under the incident laser irradiation, the dynamic light scattering signal of these particles is through behind the lens 2, be disposed in the face battle array digital camera 4 on the lens focal plane, take as area array CCD or CMOS camera, the time shutter of control camera, as 10 milliseconds, millisecond, 50 milliseconds 100 milliseconds etc., make the scattering luminous point of particle on the image of taking, form trajectory.These trajectories are carried out data processing, obtain the granularity and the distribution of particle.
A kind of image dynamic light scattering nano particles measuring method is specifically implemented:
At first laser incides in the sample cell that does not contain tested particle, because the defective of sample cell glass etc. can produce some reflected light spots under the irradiation of incoming laser beam, with the space distribution of CCD or CMOS cameras record luminous point at this moment, is called bias light.Then, add tested particle in sample cell, because the Brownian movement of tested particle, the position can occur in time and the scattering luminous point of random variation, the scattering luminous point of these motions is because the Brownian movement of grain causes.The time shutter of control camera is the τ value as 100ms, owing to constantly move, its scattering luminous point can stay mobile track to particle on camera in this time period.According to the quantity of scattering luminous point, can obtain particle at during this period of time displacement in camera pixel
r, then can be in the hope of the coefficient of diffusion of particle by formula (2)
D t , obtain coefficient of diffusion
D t After, more just can be in the hope of the granularity of tested particle by formula (1)
RAnd the luminous point of bias light record is not owing to be that the Brownian movement of particle causes, and can not produce mobilely in the time shutter, and this luminous point can not form 1 track.So these background luminous points are removed in should be with the picture signal that records before handling the scattering luminous point, disregard, and only handle the scattering light spot signal that the particle Brownian movement causes.
Embodiment 1:
By shown in Figure 2; the laser beam incident that lasing light emitter 1 sends is to sample cell 3; put into tested particulate samples in the sample cell 3; particle meeting scattering incident laser; the scattered light of particle is collected the back forms space distribution on the focal plane of lens scattering luminous point by lens 2; the scattering luminous point of this space distribution is because the varying in size and the effect of Brownian movement of particle; the random variation that can occur the position in time; the random variation quilt cover battle array digital camera 4 of this light spot position; take as CCD or CMOS camera; rationally the time shutter of control camera can obtain the movement locus line of scattering luminous point in the time shutter, rather than luminous point.After obtaining the Brownian movement track of particle, just can in time obtain the granularity of particle.
Embodiment 2:
By shown in Figure 3, sample cell 3 is arranged in the back of receiver lens 2 as different from Example 1, the laser beam of being sent by lasing light emitter 1 incides earlier sample cell 3 behind lens 2, the dynamic scattering light of its particle is disposed in the face battle array digital camera 4 of forward direction again, take as CCD or CMOS camera, obtain stochastic distribution particle scattered light locus of points image.
Embodiment 3:
Shown in Fig. 4, in the present embodiment, face battle array digital camera 4 is not the forward direction that is arranged in incoming laser beam 1, but is arranged in side direction an angle of 90 degrees position, can be arranged in side forward direction miter angle or rear flank to other any lateral angles such as 135 degree angles yet.By the Rayleigh scattering theory is 1/2nd of forward scattering light intensity at the scattered light intensity of nano particle yardstick side direction as can be known, and therefore, face battle array digital camera 4 can record the image of the dynamic light scattering locus of points of particle equally in side direction.
Embodiment 4:
By shown in Figure 5, in the present embodiment, with two face battle array digital cameras and two lens, two face battle array digital cameras are made up of first battle array digital camera 4 and second battle array digital camera 5, two lens are made up of first lens 2 and second lens 6, first battle array digital camera 4 and second battle array digital camera 5 are arranged in the forward direction 0 degree position and side direction 90 degree position or other angle positions of the incoming laser beam that is sent by lasing light emitter 1, as 45 degree positions, 135 degree positions etc.The dynamic light scattering signal of incoming laser beam after sample cell 3 is by the particle scattering received by first lens 2 and second lens 6 respectively, taken by first battle array digital camera 4 and second battle array digital camera 5 respectively again, measure the forward direction of particle and the trace image of side direction dynamic scattering luminous point simultaneously.For aspherical particle, sub-micron and micron particles, forward scattering light intensity and lateral scattering light intensity differ greatly, and forward direction and side direction are measured simultaneously, size-grade distribution that can more accurate definite particle.
Claims (6)
1. image dynamic light scattering nano particles measurement mechanism, it is characterized in that, this measurement mechanism is from left to right by lasing light emitter, sample cell, lens, face battle array photosensitive device coaxial arrangement constitutes, the particle of the laser beam incident laser radiation that lasing light emitter sends in the sample cell, the particle of doing Brownian movement in the sample cell produces dynamic light scattering under the incident laser irradiation, the dynamic light scattering signal of these particles is through behind the lens, on lens focal plane, form the scattering luminous point, the face battle array digital camera that is disposed on the lens focal plane is taken, the time shutter of control camera, make the scattering luminous point of particle on the image of taking, form trajectory, these trajectories are carried out data processing, obtain the granularity and the distribution of particle.
2. one kind is utilized a kind of image dynamic light scattering nano particles of the described measurement mechanism of claim 1 to measure
Method is characterized in that, these method concrete steps are:
The laser beam incident that will be sent by lasing light emitter is added with water or particle dispersion to sample cell in the sample cell
Liquid;
With face battle array digital camera shooting bias light signal pattern and record at this moment;
In sample cell, add tested particulate samples;
Dynamic the loosing after shooting adds particulate samples measured in the time shutter of control figure camera and record
Penetrate light signal image and recorded and stored;
Behind the image of dynamic light scattering signal of record particulate samples, earlier according to the bias light image to
The grain signal pattern is handled, and eliminates the noise of bias light signal;
To the dynamic light scattering track of the particle Brownian movement trajectory analysis particle behind the elimination noise, measure
The course length of each particle according to theory of Brownian motion, in the expectation value of the relative origin displacement of moment particle square is:
（2）
Track by particle is tried to achieve coefficient of diffusion according to formula (2)
D t , use the Stocks-Einstein formula again:
(1)
Obtain the grain graininess of this track correspondence;
(7) granularity of each particle that will obtain gathers and adds up, and obtains the size-grade distribution of particle.
3. image dynamic light scattering nano particles measurement mechanism according to claim 1, it is characterized in that, described sample cell is arranged in the back of receiver lens, the laser beam of being sent by lasing light emitter incides earlier sample cell behind lens, the dynamic scattering light of its particle is disposed in the face battle array digital camera of forward direction again and takes, and obtains stochastic distribution particle scattered light locus of points image.
4. image dynamic light scattering nano particles measurement mechanism according to claim 1 is characterized in that described battle array digital camera is arranged in the incoming laser beam lateral arrangement of being sent by lasing light emitter.
5. image dynamic light scattering nano particles measurement mechanism according to claim 1, it is characterized in that, described battle array digital camera is made up of first battle array digital camera and second battle array digital camera, described lens are made up of first lens and second lens, first battle array digital camera and second battle array digital camera are arranged in the forward direction 0 degree position and the lateral position of the incoming laser beam that is sent by lasing light emitter, the dynamic light scattering signal of incoming laser beam after sample cell is by the particle scattering received by first lens and second lens respectively, taken by first battle array digital camera and second battle array digital camera respectively again, measure the forward direction of particle and the trace image of side direction dynamic scattering luminous point simultaneously.
6. image dynamic light scattering nano particles measurement mechanism according to claim 1 is characterized in that described battle array digital camera is CCD or CMOS camera.
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| CN104458510A (en) * | 2013-07-22 | 2015-03-25 | 南通大学 | Particle size and shape detection optical system capable of improving detection accuracy |
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Application publication date: 20111012 |