CN109030298B - Measurement method realized by utilizing back scattering nano-particle granularity measurement device - Google Patents
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Abstract
A measuring method realized by utilizing a back scattering nano-particle granularity measuring device belongs to the technical field of particle granularity detection. The method is characterized in that: a lens (5), a laser (8) and a GRIN lens (9) are sequentially arranged on the rear side of the sample cell (1), the output end of the GRIN lens (9) is connected with the input end of a photomultiplier (10), and the output end of the photomultiplier (10) is connected with the input end of a photon correlator (11); the device is also provided with a lens adjusting device used for adjusting the distance between the lens (5) and the sample cell (1), and the lens (5) is arranged in the lens adjusting device. According to the measurement method realized by the back scattering nanoparticle size measurement device, the incident light and the scattered light are both positioned at the rear side of the sample cell, so that the scattered light does not need to completely pass through a test sample in the sample cell, the scattering optical path is reduced, the multiple light scattering effect is reduced, and the size measurement of a high-concentration test sample is realized.
Description
Technical Field
A measuring method realized by utilizing a back scattering nano-particle granularity measuring device belongs to the technical field of particle granularity detection.
Background
The particle size and the distribution of the nano particles are important parameters for representing the performance of the nano particles, and the dynamic light scattering technology is an effective method for measuring the particle size of the nano particles. Photon correlation spectroscopy is a commonly used method in prior art dynamic light scattering particle measurement techniques. Photon correlation spectroscopy is the method of measuring the fluctuation of scattered light at a fixed spatial location to obtain particle size information. Because the photon correlation spectroscopy theoretical model is established on the basis that only single scattering occurs to incident light, for a sample with high concentration, because the particle distance is small, a large amount of multiple scattering light is contained in the scattering light, and just because of the influence of the multiple scattering light, the photon correlation spectroscopy cannot be directly used for measuring the particle size of particles in the sample with high concentration. Therefore, in order to avoid multiple scattering of incident light, the concentration of a test sample is required to be extremely low, so that the traditional photon correlation spectroscopy cannot be directly used for measuring samples with large concentration and opaque systems such as suspension, and the application of the dynamic light scattering technology in high-concentration samples such as food, paint coating, gel and the like is limited.
When incident light is irradiated to a high concentration sample, there are two approaches to solving the problem of multiple scattering: the first approach is an improved detection method using cross-correlation spectroscopy and low-coherence dynamic light scattering techniques. The former uses two photodetectors to measure scattered light at different angles simultaneously, and then calculates the cross-correlation function of the two sets of scattered signals. The effect of multiple scattering can be attenuated by calculating the cross-correlation function, since the correlation between multiple scattered light and single scattered light is lost. However, this method requires that the error of the two scattered wave vectors must be smaller than 1/10, which is difficult to achieve in practice, and it is difficult to measure samples with concentrations over 5% by cross-correlation spectroscopy to ensure sufficient single scattered light. The latter adopts a phase modulation technology, utilizes the characteristic of a low-coherence light source to effectively inhibit multiple scattered light, and establishes a detection method aiming at the particle size distribution and the dynamic characteristic of particles in a high-concentration suspended sample on the basis of a single scattering theory. However, this method requires the use of a piezoelectric ceramic-based micro-motion stage to adjust the optical path of the reference light, making the optical path and control system very complicated.
The second approach is to develop a theory that can deal with multiply scattered light, so that information about the properties of the particle system can be extracted from the changes of multiply scattered light, and diffusion spectroscopy is the theory developed based on this idea. Maret and Wolf firstly put forward the concept of diffusion spectroscopy in 1987, and the diffusion spectroscopy theory obtains a light intensity autocorrelation function by detecting the change of multiple scattered light along with time by using a high-speed photon correlator, and calculates the characteristic attenuation time of the autocorrelation function by using a fitting algorithm so as to obtain the average particle size of particles and the kinetic information of the particles. Since diffusion spectroscopy requires that the scattered light received is only multiply scattered light, it is only applicable to very high concentrations of particulate samples without single scattering. In addition, since the diffusion spectroscopy obtains information on the particle size of the particles by sufficiently diffusing photons in the particle system, only the average particle size of the particle system can be measured, and information on the distribution of the particle size cannot be obtained.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the method overcomes the defects of the prior art, and provides the measuring method which is realized by utilizing the back scattering nanoparticle granularity measuring device and realizes the granularity measurement of the high-concentration test sample.
The technical scheme adopted by the invention for solving the technical problems is as follows: this backscattering nanoparticle particle size measuring device, including the sample cell, the test sample is located the sample cell, its characterized in that: the rear side of the sample cell is sequentially provided with a lens, a laser and a GRIN lens, incident light emitted by the laser enters the sample cell through the lens, is emitted from the rear end of the sample cell to enter the GRIN lens after being reflected, the output end of the GRIN lens is connected with the input end of a photomultiplier, and the output end of the photomultiplier is connected with the input end of a photon correlator; and the lens adjusting device is used for adjusting the distance between the lens and the sample cell, and the lens is arranged in the lens adjusting device.
Preferably, the lens adjusting device comprises a fixing frame, the lens is fixed in the fixing frame and provided with a screw rod in threaded connection with the fixing frame, and the stepping motor is coaxially fixed with the screw rod.
Preferably, the screw rod penetrates through one side of the fixing frame, and an internal thread matched with the screw rod is arranged in the fixing frame; and guide posts symmetrically arranged with the screw are arranged on the other side of the fixing frame, and the guide posts penetrate through the fixing frame simultaneously.
Preferably, an attenuation sheet is disposed between the lens and the laser.
Preferably, a computer is further provided, and the output end of the photon correlator is connected with the computer.
Preferably, the GRIN lens is placed at a scattering angle of 170 ° behind the sample cell.
A measurement method realized by utilizing a back scattering nano-particle granularity measurement device is characterized by comprising the following steps: the method comprises the following steps:
step a, a laser is started, incident light emitted by the laser is scattered after irradiating a test sample in a sample cell, and the scattered light is emitted from the back edge of the sample cell in a reverse direction; adjusting the position of the lens through a lens adjusting device to enable the position of the scattering body to be located at the rear edge of the sample cell;
step b, the scattered light of the self-sample continuously passes through the GRIN lens, the photomultiplier and the photon correlator, the light intensity autocorrelation function of the scattered light at the current position of the lens is obtained through measurement, the intercept of the light intensity autocorrelation function is obtained through fitting by using an accumulative analysis method, and the intercept is recorded as the reference value of the interceptβ 1；
C, adjusting the position of the lens through a lens adjusting device to enable the position of the scatterer to be positioned at the center of the sample cell;
d, continuously measuring the scattered light of the self-sample by the GRIN lens, the photomultiplier and the photon correlator to obtain a light intensity autocorrelation function of the scattered light at the current position of the lens, fitting by using an accumulative analysis method to obtain an intercept of the light intensity autocorrelation function, and recording the intercept as a calculated value of the interceptβ 2；
Step e, judging whether incident light is scattered for multiple times or not when the lens is positioned at the current position by using an intercept comparison criterion, executing the step f if the incident light is scattered for multiple times, and executing the step g if the incident light is not scattered for multiple times;
f, enabling the position of the scatterer to move from the center position of the sample pool to the rear edge of the sample pool in sequence at fixed intervals through the lens adjusting device, determining a light intensity autocorrelation function at the position once when the scatterer moves, further obtaining a calculated value of intercept, comparing a reference value of the intercept and the calculated values of the intercept at different positions in sequence according to an intercept comparison criterion, and determining the position of the lens when incident light is not scattered for multiple times;
and g, after determining the position where the incident light is not subjected to multiple scattering, measuring the average particle size and the particle size distribution of the sample at the current position.
Preferably, the reference value of the intercept of the light intensity autocorrelation function is compared with the calculated value of the intercept if β2＞0.8·β1It indicates that the incident light from the laser is not scattered multiple times in the sample cell, and if β2＜0.8·β1The result shows that the concentration of the sample in the sample cell is high, and the incident light emitted by the laser is scattered in the sample cell for multiple times.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the device and the method for measuring the particle size of the back scattering nano particles, the incident light and the scattered light are both positioned at the rear side of the sample cell, so that the scattered light does not need to completely penetrate through a test sample in the sample cell, the scattering optical path is reduced, the multiple light scattering effect is reduced, and the particle size measurement of a high-concentration test sample is realized.
2. Through this backscatter nano-particle size measurement device, can obtain more scattering light intensity, also more sensitive. And the scattered light of larger dust particles is concentrated in the forward scattering area, so the influence of dust can be effectively reduced by adopting a backward scattering method.
3. The distance between the lens and the sample cell can be adjusted by arranging the lens adjusting device, so that the position where the incident light is not scattered for multiple times is obtained by combining an intercept comparison criterion in a testing method, and the particle size measurement is facilitated.
Drawings
Fig. 1 is a schematic structural diagram of a back scattering nanoparticle size measuring device.
Fig. 2 is a flow chart of the back scattering nanoparticle size measurement.
Fig. 3 is a schematic diagram of a backscatter nanoparticle size measuring apparatus test.
Wherein: 1. the device comprises a sample cell 2, a screw 3, a fixing frame 4, a stepping motor 5, a lens 6, an attenuation sheet 7, a guide pillar 8, a laser 9, a GRIN lens 10, a photomultiplier 11, a photon correlator 12 and a computer.
Detailed Description
FIGS. 1 to 3 illustrate preferred embodiments of the present invention, and the present invention will be further described with reference to FIGS. 1 to 3.
As shown in fig. 1, a backscatter nanoparticle particle size measuring apparatus includes a sample cell 1 in which a test sample is placed, a lens 5 is disposed behind the sample cell 1, an attenuation sheet 6 and a laser 8 are sequentially disposed behind the lens 5, and light emitted from the laser 8 passes through the attenuation sheet 6 and the lens 5 and then enters the sample cell 1.
A GRIN lens 9 is arranged behind the lens 5, the GRIN lens 9 is positioned at one side of the laser 8, the optical output end of the GRIN lens 9 is connected with an optical fiber, the optical fiber is connected with the input end of a photomultiplier tube 10, the output end of the photomultiplier tube 10 is connected with a photon correlator 11, and the output end of the photon correlator 11 is connected with a computer 12.
Light emitted from the laser 8 enters the sample cell 1, then irradiates particles of a test sample, is scattered, is emitted in a reverse direction from the rear of the sample cell 1 after being scattered, enters the GRIN lens 9 through the lens 5 after being emitted, and is output to the cathode surface of the photomultiplier 10 through the optical fiber at the output end after being received by the GRIN lens 9. The photomultiplier 10 converts the scattered photon pulse signal into an electric pulse signal, and sends the electric pulse signal to the photon correlator 11, the photon correlator 11 carries out autocorrelation operation on the pulse signal, and then sends the obtained light intensity autocorrelation function to the computer 12 for processing, and the computer 12 calculates the average particle size and the particle size distribution of the test sample. A GRIN lens 9 is arranged behind the sample cell 1 at a scattering angle of 170 deg. to receive scattered light.
The rear part of the sample cell 1 is provided with a lens adjusting structure, the lens 5 is arranged in the lens adjusting mechanism, the distance between the lens 5 and the sample cell 1 is adjusted through the lens adjusting mechanism, and the position of the scattering body in the sample cell 1 is adjusted. The lens adjusting mechanism comprises a fixing frame 3, a lens 5 is fixed in the fixing frame 3, a screw rod 2 and a guide pillar 7 are respectively arranged at two ends of the fixing frame 3, the screw rod 2 and the guide pillar 7 penetrate through the fixing frame 3 simultaneously, and an internal thread matched with the screw rod 2 is arranged at one end, through which the screw rod 2 penetrates.
The rear end of the screw rod 2 is provided with a stepping motor 4, the motor shaft of the stepping motor 4 is coaxially connected with the screw rod 2, so that the stepping motor 4 drives the screw rod 2 to synchronously rotate when rotating, and the fixed frame 3 is in threaded connection with the screw rod 2, so that the screw rod 2 can drive the fixed frame 3 to reciprocate when rotating,
as shown in fig. 2, the testing method implemented by the backscatter nanoparticle size measuring apparatus includes the following steps:
1001, driving a lens adjusting device to enable a scattering body to be located at the rear edge of a sample cell 1;
starting a laser 8, wherein light emitted by the laser 8 is emitted into the sample cell 1 through an attenuation sheet 6 and a lens 5, incident light is scattered after irradiating a test sample in the sample cell 1, and scattered light is emitted reversely from the rear edge of the sample cell 1; and starting the stepping motor 4, driving the fixing frame 3 and the lens 5 in the fixing frame to move through the screw rod 2, and enabling the position of the scattering body to be located at the position of 0.5mm of the inner side of the rear edge of the sample cell 1. The intersection point of the scattered light and the incident light in the sample cell 1 is the position of the corresponding scatterer.
the attenuation sheet 6 is adjusted so that the intensity of scattered light is 500 kcps.
the laser 8 is continuously operated for a period of time, the scattered light reflected from the sample cell 1 is continuously transmitted to the photon correlator 11 through the GRIN lens 9 and the photomultiplier 10, the photon correlator 11 calculates the light intensity autocorrelation function of the scattered light at the current position of the lens 5 and sends the light intensity autocorrelation function to the computer 12, and the computer 12 records the light intensity autocorrelation function at the position.
fitting by using an accumulative analysis method to obtain the intercept of the light intensity autocorrelation function, and recording as the reference value of the interceptβ 1。
Step 1005, driving the lens adjusting device to enable the scatterer to be positioned at the center of the sample cell 1;
the stepping motor 4 is started, the screw 2 drives the fixing frame 3 and the lens 5 therein to move, so that the position of the scattering body is located at the center of the sample cell 1, as shown in fig. 3.
the laser 8 is continuously operated for a period of time, the scattered light reflected from the sample cell 1 is continuously transmitted to the photon correlator 11 through the GRIN lens 9 and the photomultiplier 10, the photon correlator 11 calculates the light intensity autocorrelation function of the scattered light at the current position of the lens 5 and sends the light intensity autocorrelation function to the computer 12, the computer 12 records the light intensity autocorrelation function at the current position, and then the calculated value of the intercept is obtained by fitting the light intensity autocorrelation function by using an accumulative analysis methodβ 2。
comparing the reference value and the calculated value of the intercept of the light intensity autocorrelation function ifβ 2＞0.8·β 1If so, the concentration of the sample in the sample cell 1 is low, and the incident light emitted by the laser 8 is not scattered for multiple times in the sample cell 1; if it is notβ 2＜0.8·β 1If so, the concentration of the sample in the sample cell 1 is high, and the incident light emitted by the laser 8 is scattered for multiple times in the sample cell 1;
when the lens 5 is in the current position, determining whether the incident light is scattered for multiple times, if so, executing step 1009, and if not, executing step 1010;
and driving the stepping motor 4 to work, so that the scatterer moves from the center position of the sample cell 1 to the rear edge of the sample cell 1 in sequence at intervals of a certain distance, determining a calculated value of the intercept of the light intensity autocorrelation function at the position every time the scatterer moves, comparing the calculated value of the intercept with a reference value according to the step 1007, and determining the position of the lens 5 when the incident light is not scattered for multiple times.
after determining the position where the incident light is not multiply scattered, the average particle diameter of the sample and the particle size distribution thereof are measured at the current position.
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (7)
1. A measurement method implemented with a backscatter nanoparticle size measurement apparatus comprising a sample cell (1), a test sample being located in the sample cell (1), characterized in that: a lens (5), a laser (8) and a GRIN lens (9) are sequentially arranged on the rear side of the sample cell (1), incident light emitted by the laser (8) enters the sample cell (1) through the lens (5), is emitted from the rear end of the sample cell (1) to enter the GRIN lens (9) after being reflected, the output end of the GRIN lens (9) is connected with the input end of a photomultiplier (10), and the output end of the photomultiplier (10) is connected with the input end of a photon correlator (11); the device is also provided with a lens adjusting device for adjusting the distance between the lens (5) and the sample cell (1), and the lens (5) is arranged in the lens adjusting device;
the measuring method comprises the following steps:
step a, a laser (8) is started, incident light emitted by the laser (8) is scattered after irradiating a test sample in a sample cell (1), and scattered light is emitted from the back edge of the sample cell (1) in a reverse direction; the position of the lens (5) is adjusted through a lens adjusting device, so that the position of the scatterer is positioned at the rear edge of the sample cell (1);
b, continuously measuring the scattered light of the sample through the GRIN lens (9), the photomultiplier (10) and the photon correlator (11) to obtain the light intensity autocorrelation function of the scattered light at the current position of the lens (5)Then, fitting by using an accumulative analysis method to obtain the intercept of the light intensity autocorrelation function, and recording as the reference value of the interceptβ 1；
C, adjusting the position of the lens (5) by starting a lens adjusting device to enable the position of the scatterer to be positioned at the center of the sample cell (1);
d, continuously measuring the scattered light of the sample by the GRIN lens (9), the photomultiplier (10) and the photon correlator (11) to obtain a light intensity autocorrelation function of the scattered light at the current position of the lens (5), and fitting by using an accumulative analysis method to obtain an intercept of the light intensity autocorrelation function, and recording the intercept as a calculated value of the interceptβ 2；
Step e, judging whether incident light is scattered for multiple times or not when the lens (5) is positioned at the current position by using an intercept comparison criterion, executing the step f if the incident light is scattered for multiple times, and executing the step g if the incident light is not scattered for multiple times;
f, enabling the position of the scatterer to move from the center position of the sample pool (1) to the rear edge of the sample pool (1) in sequence at fixed intervals through a lens adjusting device, measuring a light intensity autocorrelation function at the position once when the scatterer moves, further obtaining a calculated value of the intercept, comparing a reference value of the intercept with calculated values of the intercepts at different positions in sequence according to an intercept comparison criterion, and determining the position of the lens (5) when incident light is not scattered for multiple times;
and g, after determining the position where the incident light is not subjected to multiple scattering, measuring the average particle size and the particle size distribution of the sample at the current position.
2. The measurement method using the backscattering nanoparticle size measurement device according to claim 1, wherein: the lens adjusting device comprises a fixing frame (3), a lens (5) is fixed in the fixing frame (3), a screw (2) in threaded connection with the fixing frame (3) is arranged, and a stepping motor (4) is coaxially fixed with the screw (2).
3. The measurement method using the backscattering nanoparticle size measurement device according to claim 2, wherein: the screw (2) penetrates through one side of the fixing frame (3), and an internal thread matched with the screw (2) is arranged in the fixing frame (3); the other side of the fixed frame (3) is provided with a guide post (7) which is symmetrical to the screw rod (2), and the guide post (7) penetrates through the fixed frame (3) at the same time.
4. The measurement method using the backscattering nanoparticle size measurement device according to claim 1, wherein: an attenuation sheet (6) is arranged between the lens (5) and the laser (8).
5. The measurement method using the backscattering nanoparticle size measurement device according to claim 1, wherein: and a computer (12) is also arranged, and the output end of the photon correlator (11) is connected with the computer (12).
6. The measurement method using the backscattering nanoparticle size measurement device according to claim 1, wherein: the GRIN lens (9) is arranged at a scattering angle of 170 DEG behind the sample cell (1).
7. The measurement method using the backscattering nanoparticle size measurement device according to claim 1, wherein: the intercept comparison criterion in step f is: comparing the reference value of the intercept of the light intensity autocorrelation function with the calculated value of the intercept, ifβ 2＞0.8·β 1Indicating that the incident light emitted by the laser (8) does not scatter multiple times in the sample cell (1); if it is notβ 2＜0.8·β 1The concentration of the sample in the sample cell (1) is high, and the incident light emitted by the laser (8) is scattered in the sample cell (1) for multiple times.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US5627642A (en) * | 1995-08-11 | 1997-05-06 | The Research Foundation Of State University Of New York | Method and apparatus for submicroscopic particle sizing by measuring degree of coherence |
| CN101122555A (en) * | 2007-09-12 | 2008-02-13 | 上海理工大学 | High concentration super fine granule measuring device and method based on backward photon related spectrum |
| CN104266945A (en) * | 2014-10-18 | 2015-01-07 | 山东理工大学 | Integrated optical fiber probe for measuring dynamic light scattering particles and detection method |
| CN106605138A (en) * | 2014-09-05 | 2017-04-26 | 马尔文仪器有限公司 | Particle characterization method and apparatus |
| CN108627432A (en) * | 2016-03-16 | 2018-10-09 | 马尔文仪器有限公司 | particle characterization |
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| US10365198B2 (en) * | 2016-04-21 | 2019-07-30 | Malvern Panalytical Limited | Particle characterization |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5627642A (en) * | 1995-08-11 | 1997-05-06 | The Research Foundation Of State University Of New York | Method and apparatus for submicroscopic particle sizing by measuring degree of coherence |
| CN101122555A (en) * | 2007-09-12 | 2008-02-13 | 上海理工大学 | High concentration super fine granule measuring device and method based on backward photon related spectrum |
| CN106605138A (en) * | 2014-09-05 | 2017-04-26 | 马尔文仪器有限公司 | Particle characterization method and apparatus |
| CN104266945A (en) * | 2014-10-18 | 2015-01-07 | 山东理工大学 | Integrated optical fiber probe for measuring dynamic light scattering particles and detection method |
| CN108627432A (en) * | 2016-03-16 | 2018-10-09 | 马尔文仪器有限公司 | particle characterization |
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