CN211122430U - Device for measuring micro-nano particles - Google Patents
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- CN211122430U CN211122430U CN201922061900.8U CN201922061900U CN211122430U CN 211122430 U CN211122430 U CN 211122430U CN 201922061900 U CN201922061900 U CN 201922061900U CN 211122430 U CN211122430 U CN 211122430U
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Abstract
The utility model discloses a device for measuring receive granule a little, wherein, the device includes: the microporous membrane is serially arranged in the cavity to divide the cavity into a plurality of chambers, micropores are formed in the microporous membrane, two adjacent chambers are communicated through the micropores, and each chamber is provided with an electrode. The technical scheme of the utility model can realize receiving the measurement of the three-dimensional form attribute of nano-particle under the solution state.
Description
Technical Field
The utility model relates to a receive the particle measurement technical field a little particularly, relate to a device for measuring receive the particle a little.
Background
Particulate materials are widely used in the fields of medicine, chemical industry, materials, and the like based on their specific properties, and in the application of particulate materials, it is important to measure properties such as the three-dimensional morphology of particulate materials (hereinafter, referred to as particles).
At present, common particle measurement equipment comprises an optical microscope, a scanning electron microscope and a transmission electron microscope, but because the resolution of the optical microscope is low, particles with the size smaller than 300 nanometers are difficult to observe by using the optical microscope, and the common particle measurement equipment is not suitable for measuring micro-nano particles. The scanning electron microscope and the transmission electron microscope can obtain the three-dimensional morphology of the particles by tilting the particle sample at different angles under vacuum, but the real morphology information cannot be obtained for the biological particle sample or the particle sample needing to be measured in a solution state.
Therefore, the problem that the three-dimensional morphology of the micro-nano particles in the solution cannot be measured still exists in the prior art.
Disclosure of Invention
In order to solve the technical problem, the utility model provides a device for measuring receive granule a little for three-dimensional form attribute of receiving the granule a little under the liquid state detects.
Wherein, the utility model discloses the technical scheme who adopts does:
the device for measuring the micro-nano particles comprises a cavity and at least two microporous membranes, wherein the microporous membranes are serially arranged in the cavity and divide the cavity into a plurality of chambers, micropores are formed in the microporous membranes, two adjacent chambers are communicated through the micropores, and each chamber is provided with an electrode.
In another exemplary embodiment, in the measuring state, the electrode at one end of the cavity is grounded, and voltages with different magnitudes are loaded on the other electrodes, and the magnitude sequence of the voltages corresponds to the distance between the electrode and the grounded electrode.
In another exemplary embodiment, in a measuring state, each chamber is filled with an electrolyte, and micro-nano particles to be measured continuously pass through the micropores along with the electrolyte.
In another exemplary embodiment, the micropores of each of the microporous membranes have the same shape, and the centers of the micropores are located on the same line.
In another exemplary embodiment, the inner diameter of the micro-pores is 1 nm to 10 μm.
In another exemplary embodiment, the microporous membrane has a thickness of 1 nanometer to 10 micrometers.
In another exemplary embodiment, the microporous membrane is integrally formed with the cavity, or the microporous membrane is disposed in a membrane stack within the cavity with a separation distance between each microporous membrane.
In another exemplary embodiment, the microporous membrane is an inorganic membrane, and the material of the inorganic membrane includes any one of low stress silicon nitride, silicon oxide, and silicon wafer.
In another exemplary embodiment, the device further comprises a liquid driver adjacent the chamber at one end of the cavity for driving liquid flow within the device.
In another exemplary embodiment, the driving manner of the liquid driver includes any one of electric force driving, hydraulic driving, and magnetic force driving.
In the technical scheme, a cavity of the device for measuring the micro-nano particles is divided into a plurality of chambers by the serially arranged microporous films, two adjacent chambers are communicated through micropores in the microporous films, and each chamber is provided with an electrode. In a measuring state, electrolyte is filled in each chamber, the electrolyte contains micro-nano particles to be measured, the micro-nano particles sequentially pass through each micropore along with the flowing of the electrolyte, and the three-dimensional morphological attributes of the micro-nano particles to be measured in the electrolyte can be obtained by analyzing electric signal data between two electrodes adjacent to the micropore in the process, so that the three-dimensional morphological attributes of the micro-nano particles in a solution state can be measured.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the invention as claimed.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and together with the description, serve to explain the principles of the invention.
Fig. 1 is a sectional view illustrating an apparatus for measuring micro-nano particles according to an exemplary embodiment;
FIG. 2 is a schematic of a set of sequential electrical signal data obtained by collecting electrical signal data between two electrodes adjacent to each microwell during sequential passage of a standard spherical particle through each microwell of the apparatus of FIG. 1;
FIG. 3 is a schematic representation of a set of sequential electrical signal data obtained by collecting electrical signal data between two electrodes adjacent to each microwell during sequential passage of a standard cube of particles through each microwell of the apparatus of FIG. 1;
FIG. 4 is a schematic diagram illustrating signal cell division for electrical signal data in accordance with an exemplary embodiment;
FIG. 5 is a schematic representation of electrical signal data collected during the continuous passage of a 200 nanometer diameter styrene microsphere through a plurality of micropores.
Description of reference numerals: 100. a device for measuring micro-nano particles; 101. a cavity; 102. a microporous membrane; 103. micropores; 104. a liquid driving device.
While certain embodiments of the present invention have been illustrated by the accompanying drawings and described in detail below, the drawings and the description are not intended to limit the scope of the inventive concepts in any way, but rather to explain the inventive concepts to those skilled in the art by reference to particular embodiments.
Detailed Description
Reference will now be made in detail to the exemplary embodiments, examples of which are illustrated in the accompanying drawings. When the following description refers to the accompanying drawings, like numbers in different drawings represent the same or similar elements unless otherwise indicated. The embodiments described in the following exemplary embodiments do not represent all embodiments consistent with the present invention. Rather, they are merely examples of apparatus and methods consistent with certain aspects of the invention, as detailed in the appended claims.
It should be noted that the micro-nano particles described in this embodiment refer to physical particles with sizes of micro-and nano-scale, and generally include organic particles, inorganic particles, magnetic particles, silica particles, agarose gel particles, styrene particles, metal particles, colloidal particles, particles conjugated with molecules, particles conjugated with biomolecules, particles conjugated with immunoglobulins, particles conjugated with nucleic acids, biological particles, biological cells, blood cells, sperm, egg cells, microbial cells, bacterial cells, fungal cells, viruses, subcellular organelles, mitochondria, nuclei, chloroplasts, lysosomes, ribosomes, atomic particles, ionic particles, molecular particles, polymeric particles, nucleic acids and chemical variants thereof, deoxyribonucleic acids and chemical variants thereof, nucleic acids and chemical variants thereof, proteins and chemical variants thereof. The inorganic particles typically include particulate materials such as silicon dioxide, titanium dioxide, aluminum oxide, calcium carbonate, and aluminum nitride.
The micro-nano particles have unique electrical, optical, magnetic and other properties, and physical properties such as particle size, potential and the like of the micro-nano particles have great influence on the properties of the micro-nano particles, so that the physical properties of the micro-nano particles are very necessary to be measured. For example, biological macromolecules include 4 types of substances such as nucleic acids, proteins, saccharides and lipids, and these biological macromolecules exist in the form of micro-nano particles in the living body, and by measuring the physical properties of these biological macromolecules, the research on the life behaviors will be of great significance.
Referring to fig. 1, fig. 1 is a cross-sectional view of an apparatus for measuring micro-nano particles according to an exemplary embodiment, which may be used to measure three-dimensional morphological properties of micro-nano particles, such as electrical mobility, sphericity, and particle size.
As shown in fig. 1, in an exemplary embodiment, an apparatus 100 for measuring micro-nano particles includes a cavity 101 and at least two microporous membranes 102 (3 are shown in fig. 1), wherein each microporous membrane 102 is serially connected in the cavity 101 to divide the cavity 101 into a plurality of chambers, the microporous membranes 102 are provided with micropores 103, such that two adjacent chambers are connected through the micropores 103, and each chamber has an electrode therein.
Under the measuring state, electrolyte is filled in each chamber, and the electrolyte contains micro-nano particles to be measured so as to provide a solution environment for the measurement of the micro-nano particles. The micro-nano particles sequentially pass through each micro-hole 103 along with the flowing of the electrolyte, the electrode at one end of the cavity 101 is grounded, and voltages with different sizes are respectively loaded on the rest electrodes. Illustratively, the conductivity of the electrolyte in the electrolyte may be at 10-6~10-3S/cm (Siemens per meter).
The electrolyte flows from the chamber at one end of the chamber 101 to the chamber at the other end of the chamber 101, and the flow direction is determined by the driving direction of the liquid driver 104 at one end of the chamber 101. As shown in fig. 1, in an embodiment, the liquid driver 104 is located at the bottom end of the chamber 101 and adjacent to the bottom end chamber, and the driving direction of the liquid driver 104 for the electrolyte may be from the top end chamber to the bottom end chamber, or from the bottom end chamber to the top end chamber, which is not limited herein. The liquid driver 104 may also be located at the top of the chamber body 101, adjacent to the top chamber.
The liquid driver 104 may be driven by electric field force, hydraulic pressure, magnetic field force, fluid, pneumatic pressure, osmotic pressure, brownian motion, capillary force, or temperature difference diffusion, and accordingly, the liquid driver 104 may be a liquid pump, a pneumatic device, or a syringe, which can provide driving force for the flow of the electrolyte. Illustratively, the driving manner of the liquid driver 104 adopts any one of electric force driving, hydraulic driving and magnetic force driving to provide a fixed driving force for the flow of the electrolyte, thereby driving the electrolyte to flow stably.
In addition, the electrode at one end of the chamber 101 is grounded, and voltages with different magnitudes are applied to the remaining electrodes, and the magnitude sequence of the applied voltages corresponds to the distance between the electrode and the grounded electrode. As shown in fig. 1, if the electrode located in the top chamber is grounded, that is, V0 is 0V, and the voltages applied to the other three electrodes are V3 ≧ V2 ≧ V1, so that the strength of the electric field formed between the two adjacent electrodes is sequentially increased, and it is ensured that the micro-nano particles continuously pass through each micro-pore 103 along with the flow of the electrolyte. The electrodes may be made of platinum or silver chloride.
In the process that the micro-nano particles sequentially pass through each micropore 103 along with the flowing of the electrolyte, electric signal data between two electrodes adjacent to the micropore 103 when the micro-nano particles pass through the micropore 103 are respectively measured, and the obtained electric signal data are analyzed to obtain three-dimensional morphological attributes such as electric mobility, sphericity value and particle size of the micro-nano particles, so that the problem that the attributes of the micro-nano particles in a solution state cannot be measured in the prior art is solved.
The microporous membrane 102 may be an organic membrane or an inorganic membrane.
In one embodiment, the microporous membrane 102 is an inorganic membrane, that is, the microporous membrane 102 is made of an inorganic material, and compared with an organic membrane, the inorganic membrane has better extensibility, which is beneficial for micro-nano particles to move through the micropores 103 along with the flow of the electrolyte. Illustratively, the microporous membrane 102 may be made of an inorganic material such as low-stress silicon nitride, or a silicon wafer, and the microporous membrane 102 made of such an inorganic material has a good film forming effect and a more mature manufacturing technology.
The thickness of the microporous membrane 102 may be 1 nm to 10 micrometers, the inner diameter of the micropores 103 may be 1 nm to 10 micrometers, wherein the inner diameter of the micropores 103 is the pore diameter of the micropores 103, which is the distance from the direction in which the micro-nano particles move through the device 100 in the measurement process. The micro-holes 103 may be in the shape of a cylinder, a rectangular parallelepiped, a conical frustum, a trapezoidal frustum, etc., and illustratively, when the micro-holes 103 are in the shape of a cylinder, the inner diameter of the micro-holes 103 is the diameter of the base circle of the cylinder.
The microporous membrane 102 and the cavity 101 may be integrally formed, so that the device 100 has a high form stability. The microporous membrane 102 may also be disposed in the cavity 101 in a membrane-stacked manner with a certain distance between each microporous membrane 102, for example, a plurality of fluid grooves may be disposed on the inner surface of the cavity 101, and adjacent fluid grooves may be spaced apart from each other, and the microporous membrane 102 is fixed in the fluid grooves, thereby achieving a membrane-stacked arrangement of the microporous membrane 102.
The position, inner diameter and thickness of the micro-pores 103 on each microporous membrane 102 can be completely consistent, so that the centers of the micro-pores 103 are positioned on the same straight line, and the moving path of the micro-nano particles in the device 100 is kept to be a straight line. The spacing between each microporous membrane 102 may be the same or different.
Another exemplary embodiment of the present invention further provides a method for measuring micro-nano particles, which is implemented based on the apparatus for measuring micro-nano particles described in the above embodiments, so as to determine the attribute data of micro-nano particles to be measured.
In the method, firstly, micro-nano particles to be measured continuously pass through a plurality of micropores in the device described in the embodiment along with electrolyte, and then electric signal data between two electrodes adjacent to each micropore in the process that the micro-nano particles pass through each micropore is obtained, so that attribute data of the micro-nano particles are determined according to the obtained electric signal data.
It should be noted that a set of continuous electrical signal data can be obtained by collecting corresponding electrical signal data in the process that the micro-nano particles continuously pass through a plurality of micropores. Based on the analysis of the continuous electrical signal data, the attribute information related to the three-dimensional morphology of the micro-nano particles can be determined.
The method provided by the embodiment is described in detail below by taking the apparatus 100 for measuring micro-nano particles shown in fig. 1 as an example.
In the device 100 shown in fig. 1, three microporous membranes 102 are arranged in a cavity 101, the microporous membranes 102 divide the cavity 101 into four chambers, and micro-nano particles to be measured continuously pass through the three micropores 103 along with the flow of an electrolyte. In the process that the micro-nano particles flow along with the electrolyte, the micro-nano particles are easy to turn, incline and the like, so that the micro-nano particles pass through each micropore 103 in different postures. During the process that the micro-nano particles pass through each micro-pore 103 in different postures, the data of electric signals between two electrodes adjacent to the micro-pore 103 may be different.
Referring to fig. 2 and 3, fig. 2 is a schematic diagram of a set of continuous electrical signal data obtained by collecting electrical signal data between two electrodes adjacent to each micro-pore 103 during continuous passage of a standard spherical particle through each micro-pore 103, and fig. 3 is a schematic diagram of a set of continuous electrical signal data obtained by collecting electrical signal data between two electrodes adjacent to each micro-pore 103 during continuous passage of a standard cubic particle through each micro-pore 103.
It can be seen that, for micro-nano particles with uniform three-dimensional morphology, such as spherical particles illustrated in fig. 2, the electric signal changes on two electrodes adjacent to each micro-pore 103 are not very different during the process of passing through each micro-pore 103. However, for micro-nano particles with non-uniform three-dimensional morphology, such as the cuboid particles shown in fig. 3, the difference of the electric signal changes on two electrodes adjacent to each micro-pore 103 is large in the process of passing through each micro-pore 103.
In one exemplary embodiment, the property data of the micro-nano particles includes electrical mobility of the micro-nano particles. The speed of the micro-nano particles continuously passing through two adjacent micro holes 103 and the potential difference between the two adjacent micro holes 103 can be determined according to the electric signal data, so that the electric mobility of the micro-nano particles continuously passing through the two adjacent micro holes 103 can be determined according to the obtained speed and the obtained potential difference.
The time for the micro-nano particles to continuously pass through the two adjacent micropores 103 can be obtained according to the electrical signal data, and then the ratio of the distance between the two adjacent micropores 103 to the time is calculated, so that the speed for the micro-nano particles to continuously pass through the two adjacent micropores 103 can be determined. The potential difference between two adjacent micro-holes 103 can be determined according to the electric field intensity and the distance between two adjacent micro-holes 103.
Illustratively, if the distance between two adjacent micro holes 103 is 1000 nm, the time interval of the micro-nano particles passing through two micro holes 103 is 1 millisecond, and the induced potential difference is 100 mv, the electric mobility of the micro-nano particles continuously passing through two adjacent micro holes 103 is calculated to be 10-8m2V-1s-1。
The surface potential of the micro-nano particles can be further determined according to the determined electric mobility when the micro-nano particles continuously pass through the two adjacent micropores 103, and the surface potential of the micro-nano particles corresponds to the posture when the micro-nano particles pass through the micropores 103.
Therefore, according to the change of the surface potential of the micro-nano particles in the process of continuously passing through two adjacent micropores 103, the posture change condition of the micro-nano particles in the process of continuously passing through the micropores 103 can be determined, and the three-dimensional form of the micro-nano particles can be analyzed.
In another exemplary embodiment, the property data of the micro-nano particle includes a sphericity value of the micro-nano particle. The electrical signal data are divided into a plurality of signal units, and then the signal units are respectively compared with the signal units corresponding to the standard signals to obtain the contrast coefficient between the electrical signal data and the standard signals, so that the sphericity value corresponding to the standard signal with the highest contrast coefficient is the sphericity value of the micro-nano particles.
First, it should be noted that fig. 4 is a schematic diagram of a set of electrical signal data collected during a process in which a micro-nano particle continuously passes through 3 micro-pores 103, where the set of electrical signal data includes 3 independent electrical signal data, each independent electrical signal data corresponds to a process in which the micro-nano particle passes through different micro-pores 103, and the 3 independent electrical signal data are continuous in time.
As shown in fig. 4, for the electrical signal data in a sinusoidal distribution, the electrical signal data may be divided by the electrical signal peak as a dividing point, thereby obtaining 2 signal units. For the electrical signal data distributed in other forms, the electrical signal data may be divided according to a set time interval, or the electrical signal data may be divided according to a gradient change trend of the electrical signal, which is not limited in this respect.
Dividing the electric signal data into a plurality of signal units, calculating a gradient function f (theta, r) of each signal unit, wherein the calculation formula of the gradient function f (theta, r) is as follows:
f(θ,r)=arctan(θ)
where r represents the slope length of a single signal element and theta represents the slope angle of a single signal element.
The standard signal is known information obtained in advance, and is electric signal data acquired in the process that the micro-nano particles determined by the sphericity value move through the micropores 103, so that the standard signal reflects the sphericity value of the micro-nano particles. The standard signal is divided into a plurality of signal units according to the method.
By comparing the gradient function of each signal unit with the gradient function of the signal unit corresponding to the standard signal, a contrast coefficient between each signal unit of the electrical signal data and each signal unit of the standard signal can be obtained, and the contrast coefficient reflects the similarity degree between each signal unit. Therefore, the higher the contrast coefficient between the signal units is, the closer the sphericity values between the micro-nano particles are.
And aiming at each electric signal data, calculating the average value of the contrast coefficients of all the signal units divided by the electric signal data to obtain the contrast coefficient between the electric signal data and the standard signal.
In order to ensure the practicability of the embodiment, a plurality of standard signals of the micro-nano particles with determined sphericity values are provided in advance, and the comparison coefficients between the electric signal data acquired in the measurement process and different standard signals are calculated, so that the sphericity value corresponding to the standard signal with the highest comparison coefficient is determined as the sphericity value of the measured micro-nano particles.
Fig. 5 is a schematic diagram of a set of electrical signal data collected for a process in which a styrene microsphere with a diameter of 200 nm passes through 3 micropores 103 in series under an actual measurement environment. The electric signal data shown in fig. 5 is analyzed based on the above sphericity value acquisition process, and the sphericity value of the styrene microsphere can be obtained to be 0.95.
In general, the sphericity value obtained by the method provided in this example is 0.8 or more for the nearly spherical micro-nano particles, and 0.2 or less for the rod-shaped micro-nano particles.
It should be further noted that the length-diameter ratio of the micro-nano particles and the sphericity value of the micro-nano particles also have a certain corresponding relationship, so that the length-diameter ratio of the micro-nano particles also has a certain influence on the measurement of the sphericity value of the micro-nano particles.
In another exemplary embodiment, the electrical signal data acquired in the measurement process can be input to a machine learning model, so that the machine learning model predicts the three-dimensional morphology of the micro-nano particles according to the input electrical signal data, and the three-dimensional morphology of the micro-nano particles is directly obtained.
It should be noted that the machine learning model used in this embodiment is obtained by training in advance the electrical signal data between two electrodes adjacent to the micro-pore 103 when the micro-nano particles with asymmetric morphology pass through the micro-pore 103.
In another exemplary embodiment, the property data of the micro-nano particles further includes a particle size of the micro-nano particles. Calculating the initial particle size of the micro-nano particles according to the conductivity of the electrolyte, the approximate spherical radius of the micro-nano particles and the radius of the micropores 103, if the ratio of the approximate spherical radius of the micro-nano particles to the radius of the micropores 103 is greater than a preset threshold value, determining a correction coefficient according to the ratio, and correcting the initial particle size through the correction coefficient to obtain the particle size of the micro-nano particles.
wherein D represents the approximate spherical radius of the micro-nano particles, D represents the radius of the micropores 103, and rho represents the conductivity of the electrolyte. If the particle size of the micro-nano particles is far smaller than the radius of the micropores 103, for example, the ratio D/D of the approximate spherical radius of the micro-nano particles to the radius of the micropores 103 is smaller than a set threshold, the initial particle size is the particle size of the micro-nano particles.
If the ratio of the approximate spherical radius of the micro-nano particles to the radius of the micropores 103 is larger than a preset threshold value, correcting the initial particle size by using a correction coefficient to obtain the particle size of the micro-nano particlesThe calculation formula is as follows:
the correction coefficient S is determined according to a ratio of an approximate spherical radius of the micro-nano particle to a radius of the micro-hole 103, and for example, the correction coefficient S may be determined according to table 1.
d/D | S | d/D | S |
0.1 | 1.00 | 0.6 | 1.21 |
0.2 | 1.00 | 0.7 | 1.38 |
0.3 | 1.02 | 0.8 | 1.71 |
0.4 | 1.05 | 0.9 | 2.56 |
0.5 | 1.11 | 0.95 | 3.86 |
TABLE 1
In conclusion, according to the utility model provides a device and method can measure the three-dimensional form attributes such as the electro migration rate that obtains the granule a little, sphericity value, particle diameter to can solve among the prior art and can't measure the problem of the attribute of the granule a little under the solution state.
The above description is only for the preferred exemplary embodiment of the present invention and is not intended to limit the embodiments of the present invention, and those skilled in the art can easily make various changes and modifications according to the main concept and spirit of the present invention, so the protection scope of the present invention should be subject to the protection scope claimed in the claims.
Claims (10)
1. The device for measuring the micro-nano particles is characterized by comprising a cavity and at least two microporous films, wherein:
the microporous membrane is serially arranged in the cavity and divides the cavity into a plurality of chambers, micropores are formed in the microporous membrane, two adjacent chambers are communicated through the micropores, and each chamber is provided with an electrode.
2. The device of claim 1, further comprising a liquid driver positioned adjacent the chamber at one end of the chamber for driving liquid flow within the device.
3. The device of claim 2, wherein the liquid driver is driven by any one of an electric force, a hydraulic force and a magnetic force.
4. The device of claim 1, wherein in the measuring state, the electrode at one end of the cavity is grounded, and voltages with different magnitudes are loaded on the other electrodes, and the magnitude sequence of the voltages corresponds to the distance between the electrode and the grounded electrode.
5. The device according to claim 1, wherein in a measuring state, each chamber is filled with electrolyte, and micro-nano particles to be measured continuously pass through the micropores along with the electrolyte.
6. The device of claim 1, wherein the micropores of each of said microporous membranes are identical in shape and have centers located in a common line.
7. The device of claim 1, wherein the inner diameter of the micropores is from 1 nanometer to 10 micrometers.
8. The device of claim 1, wherein the microporous membrane has a thickness of 1 nanometer to 10 micrometers.
9. The device of claim 1, wherein the microporous membrane is integrally formed with the cavity; or the microporous membranes are arranged in the cavity in a membrane lamination mode, and each microporous membrane has a spacing distance.
10. The device of claim 1, wherein the microporous membrane is an inorganic membrane, and the material of the inorganic membrane comprises any one of low stress silicon nitride, silicon oxide, and silicon wafer.
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