CN113433041A - System and method for detecting particle size concentration of nanoparticles - Google Patents
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- CN113433041A CN113433041A CN202110709229.2A CN202110709229A CN113433041A CN 113433041 A CN113433041 A CN 113433041A CN 202110709229 A CN202110709229 A CN 202110709229A CN 113433041 A CN113433041 A CN 113433041A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
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Abstract
The invention provides a system for detecting the particle size concentration of nanoparticles, which comprises a sample collecting and cleaning system, a detection chip and a laser, wherein the sample collecting and cleaning system is connected with the detection chip and controls the flow of a sample and a cleaning solution in the detection chip. The detection system can deduce the particle size and concentration of the nanoparticles by observing the motion trail and the number of the nanoparticles in a solution state, can ensure that the nanoparticles are in an original state, and has accurate and reliable results. The system can be used as a module to be combined with a nanoparticle synthesis system, so that the artificial interference caused by separate experiments is reduced. The system of the invention has the characteristics of simple and convenient operation and high flux.
Description
Technical Field
The invention belongs to the field of nanotechnology, and particularly relates to a system and a method for detecting particle size concentration of nanoparticles.
Background
The nano particles are widely applied to the fields of electronic information, biomedicine, chemical industry, aerospace and the like, and the characteristics of the micro structures such as the particle size, the shape and the like of the nano particles have important relations with the characteristics of the micro structures, so that the representation of the micro structures of the nano materials is important for promoting the development and the importance of the nano materials, and the measurement of the size and the concentration of the nano particles is a key technology.
Currently, methods for measuring the size of nanoparticles include Dynamic Light Scattering (DLS), Nanoparticle Tracking Analysis (NTA), Atomic Force Microscope (AFM), Transmission Electron Microscope (TEM), and the like. Wherein, NTA collects the scattered light signal of the nanometer particle through the optical microscope, observes the particle and does the image of the Brownian motion in the solution in a period of time, and tracks and analyzes each particle, and then calculates the fluid mechanics size and concentration of the nanometer particle through the Einstein equation. Compared with other technologies, the NTA technology has simpler sample processing, can better ensure the original state of the nanoparticles, and has higher detection speed.
In the prior art, the size information of the nanoparticles is obtained by performing partial differential equation filtering processing, particle individual segmentation, local region fitting and other steps on an image. The equipment cost is high, and professional operation is required. The method needs to process the sample, and can damage the biological sample and influence the observation result. In the prior art, an atomic force microscope is used for sampling and scanning a sample attached with nanoparticles at a plurality of positions, and particle size and concentration results are obtained by calculating the number of particles and the scanning area. However, this method requires high equipment cost and requires mastering of AFM operation techniques. The method is not suitable for high-throughput detection, and the samples are not uniformly distributed, so that the obtained concentration information cannot be ensured to be accurate.
Disclosure of Invention
Therefore, the present invention is directed to overcome the drawbacks of the prior art, and to provide a system and a method for detecting the particle size concentration of nanoparticles.
In order to achieve the above object, a first aspect of the present invention provides a system for detecting a concentration of a nanoparticle diameter, the system for detecting a concentration of a nanoparticle diameter includes a sample collection and cleaning system, a detection chip, and a laser, wherein the sample collection and cleaning system is connected to the detection chip and controls the flow of a sample and a cleaning solution in the detection chip.
According to the first aspect of the present invention, the system for detecting the particle size concentration of nanoparticles comprises a sample collection tube, a sample detection sensor, a sample collection tube, a sample collection mechanical arm movement module, a peristaltic pump, a multi-channel valve and a waste liquid collection tube.
The nanoparticle size concentration detection system according to the first aspect of the present invention, wherein the sample collection tube is mounted on the sample detection sensor; and/or
The sample collection tube is moved by the sample collection mechanical arm motion module.
According to the nanoparticle size concentration detection system of the first aspect of the invention, an inlet of the peristaltic pump is connected with the sample collection pipe through a conduit, an outlet of the peristaltic pump is connected with the multi-channel valve, and the multi-channel valve is respectively connected with the detection chip and the cleaning solution.
According to the nanoparticle size concentration detection system of the first aspect of the present invention, the detection chip includes a temperature control system and a cavity.
According to the nanoparticle size concentration detection system of the first aspect of the present invention, the temperature control system includes a temperature control heat sink, a thermal insulation layer, a semiconductor temperature control sheet, a heat conducting sheet, a thermal insulation layer, a temperature sensor mounting hole, and a sensor.
According to the system for detecting the particle size concentration of the nanoparticles, the cavity of the detection chip comprises an upper cover plate, a lower bottom plate and a channel layer;
preferably, the upper cover plate, the channel layer and the lower cover plate are sealed through sealing glue and/or a rubber gasket.
According to the nanoparticle size concentration detection system of the first aspect of the present invention, a chip outlet and a chip inlet are disposed on the upper cover plate; and/or
The lower bottom plate is made of a transparent material; preferably, the lower base plate material is selected from one or more of the following: glass, quartz, sapphire, and plexiglass.
The nanoparticle size concentration detection system according to the first aspect of the present invention, wherein the channel layer includes a channel structure for storing a detection liquid;
preferably, the side material of the channel layer is a transparent material, so that laser can irradiate;
more preferably, the side material of the channel layer is selected from one or more of the following: glass, quartz, sapphire, and plexiglass.
The second aspect of the present invention provides a method for detecting the concentration of the nanoparticle size, which uses the system for detecting the concentration of the nanoparticle size according to the first aspect.
The invention aims to provide a nanoparticle analysis and detection instrument based on a microfluidic chip technology, which can be provided with a modular microfluidic chip, integrates particle size detection and spectral analysis functions, and can realize real-time analysis of nanoparticles, thereby improving the research and development iteration speed of the nanoparticles and accelerating the research and development process.
The system for detecting the particle size concentration of the nano particles has high system and low requirement on the skill of operation. The test in the solution state enables the nano particles to be measured in a state closer to the original state, and the authenticity and the validity of the measured data are ensured. The distribution of nanoparticles in the solution is more uniform than in a solid phase (AFM) sample and therefore the concentration measurement is more accurate.
The invention is suitable for detecting and analyzing the particle size and concentration of the nano particles in the fluid sample. The method can quickly and accurately obtain the particle size and concentration information of the nanoparticles, is simple and convenient to operate, has low cost and has the characteristic of high flux. Therefore, the method can be used not only in the basic and clinical research of biomedicine, but also in the production, quality inspection and other links of biological and medical products.
The system of the present invention may have, but is not limited to, the following beneficial effects:
the invention calculates the size of the nano particles by tracking the moving path of the nano particles and displacement, and calculates the concentration of the nano particles by counting the number of particles in a visual field, the size of the visual field and the depth.
1. The particle size and concentration of the nanoparticles are deduced by observing the motion trail and the number of the nanoparticles in a solution state, so that the nanoparticles can be ensured to be in an original state, and the result is accurate and reliable.
2. The system can be used as a module to be combined with a nanoparticle synthesis system, so that the artificial interference caused by separate experiments is reduced.
3. Simple operation and high flux.
Drawings
Embodiments of the invention are described in detail below with reference to the attached drawing figures, wherein:
FIG. 1 shows the structure of the nanoparticle detection system of the present invention.
FIG. 2 shows a structure of the detection chip of the present invention.
Fig. 3 shows the detection result of the detection system of the present invention, wherein fig. 3(a) shows a block diagram of a particle size derivation procedure. Fig. 3(B) shows image filtering noise reduction and gaussian blur processing. Fig. 3(C) shows an example of particle trajectory tracking. Fig. 3(D) shows the results of particle size measurement of particles 40nm in diameter.
FIG. 4 shows a particle size analysis detection light path diagram of the detection system of the present invention.
Description of reference numerals:
1. a sample collection robotic arm; 1', a sample collection tube; 2. a sample detection sensor 1; 3. a waste liquid collecting pipe; 4. a sample detection sensor 2; 5. a sample collection tube; 6. a mechanical arm motion module; 7. an inlet; 8. an outlet; 9. a laser; 10. a chip outlet; 11. a chip inlet; 12. detecting a chip; 13. a multi-channel valve; 14. a peristaltic pump; 15. a temperature control radiating fin; 16. a thermal insulation layer; 17. a semiconductor temperature control sheet; 18. a heat conductive sheet; 19. a thermal insulation layer; 20. an upper cover plate; 21. a channel layer; 22. a fixed mount; 23. a lower base plate; 24. a temperature sensor mounting hole; 25. a sample chamber; 26. an objective lens.
Detailed Description
The invention is further illustrated by the following specific examples, which, however, are to be construed as merely illustrative, and not limitative of the remainder of the disclosure in any way whatsoever.
This section generally describes the materials used in the testing of the present invention, as well as the testing methods. Although many materials and methods of operation are known in the art for the purpose of carrying out the invention, the invention is nevertheless described herein in as detail as possible. It will be apparent to those skilled in the art that the materials and methods of operation used in the present invention are well within the skill of the art, provided that they are not specifically illustrated.
Example 1
This example is for explaining the nanoparticle diameter concentration detection system of the present invention.
The system for detecting the particle size concentration of the nano particles mainly comprises a sample collecting and cleaning system and a detection chip.
The sample collecting and cleaning system is formed as shown in figure 1, a sample collecting pipe 1 'is installed on a sample detection sensor, when the sample sensor detects a sample, a sample collecting mechanical arm motion module 6 moves the sample collecting pipe 1' to the position above a sample collecting pipe 2, the sample flows into the sample collecting pipe 2, an inlet of a peristaltic pump 14 is connected with the sample collecting pipe 5 through a conduit, an outlet 8 of the peristaltic pump is connected with a multi-channel valve 13, and the multi-channel valve 13 is respectively connected with a chip inlet 11 of a detection chip 12 and cleaning solution. When the particle size of the nanoparticles is detected, the multichannel valve 13 enables the peristaltic pump 14 to be connected with the inlet 11 of the detection chip, a sample enters the detection chip 12 under the action of the peristaltic pump 14, then the laser 9 irradiates the side surface of the detection chip 12, the scattered light of the particles is observed through the objective lens 26, the motion trail and the number of the nanoparticles are obtained, and therefore the particle size and the concentration of the nanoparticles can be deduced. After the detection is finished, the multi-channel valve 13 connects the chip inlet 11 with the cleaning solution, the cleaning solution flows into the detection chip for cleaning under the action of the peristaltic pump 14, and the waste liquid flows out from the chip outlet 10, so that the detection chip is cleaned. Wherein the wash solution is stored in a wash bottle that is attached to the sample collection wash system.
The structure of the detection chip is shown in fig. 2, and the temperature control system includes a temperature control heat sink 15, a heat insulation layer 16, a semiconductor temperature control sheet 17, a heat conduction sheet 18, a heat insulation layer 19, a temperature sensor mounting hole 24 and a sensor. The temperature of the nanoparticle solution is controlled by the semiconductor temperature control sheet 17, and the sensor is used for detecting the temperature of the temperature controller. The cavity of the detection chip is composed of three parts, an upper cover plate 20 is provided with a chip outlet 10 and a chip inlet 11, a lower base plate 23 is made of transparent materials and used for observing nano particles, a channel layer 21 comprises a channel structure and used for storing detection liquid, and the side face of the channel layer is made of transparent materials so that laser can irradiate. The upper cover plate 20, the channel layer 21 and the lower bottom plate 23 are sealed through sealant and a rubber pad, so that the detection liquid is prevented from flowing out.
The obtained nano-particle image is processed, analyzed and traced to derive the particle diameter.
Wherein R is the particle radius, kBIs the boltzmann constant, T is the temperature, η is the viscosity, x is the movement distance of the particle between the two images in the x direction, and y is the movement distance of the particle between the two images in the y direction.
The concentration is as follows:
wherein C is concentration, n is the number of particles in the field of view, W is the field of view width, L is the field of view length, h is the depth of field, and m is the correction factor.
When the particle concentration is lower, the number of particles in a visual field is smaller, the number of the counted particles is smaller, and the particle size and concentration errors are larger, in order to solve the problem, a flowing particle size analysis method is adopted, and the method specifically comprises the following steps:
the solution in the chip moves along the x direction with the speed v, the image information of the flowing nano particles is collected, only the Brownian motion of the particles in the y direction is analyzed, and the particle diameter can be obtained:
wherein R is the particle radius, kBIs Boltzmann constant, T is temperature, eta is viscosity, and y isThe distance of movement of the particle in the y-direction between the two images.
The concentration of the particles is
Where C is concentration, n is the number of particles being tracked, W is the field width, L is the field length, h is the depth of field, m is the correction factor, v is the flow velocity, and t is the flow time.
The laser irradiating the nano-particles is convergent light, the convergent angle is alpha, and the laser has higher energy density at the position of the waist beam, so that the particle size analysis of the nano-particles can be realized by adopting a low-power laser and a laser with poorer beam quality, and the system cost is reduced.
Test example 1
This example is provided to explain a specific detection method and detection results of the nanoparticle size concentration detection system of example 1, with reference to fig. 3.
In the test example, light scattering signals of nanoparticles are collected through an optical microscope, a section of images of the nanoparticles making brownian motion in a solution are shot, the brownian motion of each particle is tracked and analyzed, the analysis is finished when the number of the particles represents, and finally, the particle size and the distribution of the nanoparticles are calculated.
And (3) detecting the fluorescent microsphere solution, wherein as shown in a figure 3B, after image filtering noise reduction and Gaussian blur treatment, noise points in the background are obviously weakened. Compared with the microspheres with the particle size of 200nm, the brownian motion of the microspheres with the particle size of 40nm is more intense, and the specific motion track is shown in a 3C diagram. The detection chip of the invention is used for analyzing the grain diameter of the 40nm microsphere, and the obtained result is relatively close to the result obtained by a nano-particle tracing analysis technology (NTA) and is relatively accurate.
Although the present invention has been described to a certain extent, it is apparent that appropriate changes in the respective conditions may be made without departing from the spirit and scope of the present invention. It is to be understood that the invention is not limited to the described embodiments, but is to be accorded the scope consistent with the claims, including equivalents of each element described.
Claims (10)
1. The system for detecting the particle size concentration of the nanoparticles is characterized by comprising a sample collecting and cleaning system, a detection chip and a laser, wherein the sample collecting and cleaning system is connected with the detection chip and controls the flow of a sample and a cleaning solution in the detection chip.
2. The nanoparticle size concentration detection system of claim 1, wherein the sample collection and washing system comprises a sample collection tube, a sample detection sensor, a sample collection tube, a sample collection robotic arm motion module, a peristaltic pump, a multi-channel valve, and a waste collection tube.
3. The system for detecting the concentration of nanoparticles in particle size according to claim 2, wherein the sample collection tube is mounted on the sample detection sensor; and/or
The sample collection tube is moved by the sample collection mechanical arm motion module.
4. The system for detecting the particle size concentration of the nanoparticles as claimed in claim 2 or 3, wherein an inlet of the peristaltic pump is connected with the sample collection tube through a conduit, an outlet of the peristaltic pump is connected with a multi-channel valve, and the multi-channel valve is respectively connected with the detection chip and the cleaning solution.
5. The system for detecting the particle size concentration of nanoparticles as claimed in any one of claims 1 to 4, wherein the detection chip comprises a temperature control system and a cavity.
6. The system for detecting the particle size concentration of nanoparticles of claim 5, wherein the temperature control system comprises a temperature control heat sink, a thermal insulation layer, a semiconductor temperature control plate, a heat conducting plate, a thermal insulation layer, a temperature sensor mounting hole and a sensor.
7. The system for detecting the concentration of the particle size of nanoparticles according to claim 5 or 6, wherein the cavity of the detection chip comprises an upper cover plate, a lower bottom plate and a channel layer;
preferably, the upper cover plate, the channel layer and the lower cover plate are sealed through sealing glue and/or a rubber gasket.
8. The system for detecting the particle size concentration of nanoparticles as claimed in claim 7, wherein the upper cover plate is provided with a chip outlet and a chip inlet; and/or
The lower bottom plate is made of a transparent material; preferably, the lower base plate material is selected from one or more of the following: glass, quartz, sapphire, and plexiglass.
9. The system for detecting the concentration of nanoparticles in particle size according to claim 7 or 8, wherein the channel layer comprises a channel structure for storing a detection liquid;
preferably, the side material of the channel layer is a transparent material, so that laser can irradiate;
more preferably, the side material of the channel layer is selected from one or more of the following: glass, quartz, sapphire, and plexiglass.
10. A method for detecting a concentration of a nanoparticle diameter, the method being performed using the system for detecting a concentration of a nanoparticle diameter according to any one of claims 1 to 9.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2023148528A1 (en) * | 2022-02-07 | 2023-08-10 | Malvern Panalytical Limited | Particle analysis |
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| CN107796741A (en) * | 2017-09-27 | 2018-03-13 | 华中科技大学 | A kind of optical fiber dynamic light scattering detection means of high concentration particle group |
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- 2021-06-25 CN CN202110709229.2A patent/CN113433041A/en active Pending
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| US20110085166A1 (en) * | 2008-02-28 | 2011-04-14 | Lehigh University | Opto-fluidic nanoparticle detection apparatus |
| CN102207443A (en) * | 2011-03-17 | 2011-10-05 | 上海理工大学 | Particle-size measuring instrument |
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| CN104568683A (en) * | 2014-12-25 | 2015-04-29 | 上海理工大学 | Nano-particle size measurement device and method |
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| WO2023148528A1 (en) * | 2022-02-07 | 2023-08-10 | Malvern Panalytical Limited | Particle analysis |
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