CN115569675B - Micro-droplet generation method and generation device thereof - Google Patents

Micro-droplet generation method and generation device thereof Download PDF

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CN115569675B
CN115569675B CN202211162402.2A CN202211162402A CN115569675B CN 115569675 B CN115569675 B CN 115569675B CN 202211162402 A CN202211162402 A CN 202211162402A CN 115569675 B CN115569675 B CN 115569675B
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micro
droplets
optical fiber
sample liquid
liquid
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CN115569675A (en
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汤晓云
黄智亮
张郑
于津健
张亚勋
刘志海
张羽
郭春雨
苑立波
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Harbin Engineering University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/50Containers for the purpose of retaining a material to be analysed, e.g. test tubes
    • B01L3/502Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
    • B01L3/5027Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/02Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/50Containers for the purpose of retaining a material to be analysed, e.g. test tubes
    • B01L3/502Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
    • B01L3/5027Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
    • B01L3/50273Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip characterised by the means or forces applied to move the fluids
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/50Containers for the purpose of retaining a material to be analysed, e.g. test tubes
    • B01L3/502Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
    • B01L3/5027Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
    • B01L3/502769Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip characterised by multiphase flow arrangements
    • B01L3/502784Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip characterised by multiphase flow arrangements specially adapted for droplet or plug flow, e.g. digital microfluidics
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00Additional constructional details
    • B01L2300/08Geometry, shape and general structure
    • B01L2300/0861Configuration of multiple channels and/or chambers in a single devices
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2400/00Moving or stopping fluids
    • B01L2400/04Moving fluids with specific forces or mechanical means
    • B01L2400/0403Moving fluids with specific forces or mechanical means specific forces
    • B01L2400/0406Moving fluids with specific forces or mechanical means specific forces capillary forces

Abstract

The invention discloses a method for generating micro liquid drops, which comprises the following steps: according to the quantity and the size of the prepared micro-droplets and the distance from the liquid level to the liquid surface, the output power of a laser is adjusted, the laser is connected with one end of an optical fiber, an optical fiber probe connected with the other end of the optical fiber is inserted into the sample liquid, light emitted by the laser is transmitted to the sample liquid through the optical fiber probe, a photo-thermal effect occurs, cold air flow and hot steam flow are blown to two sides of the top surface of the sample liquid respectively until a light source heating area is formed, the temperature of the sample liquid is gradually increased, the sample liquid is subjected to liquid-gas phase transition to form steam, and the steam is condensed when meeting the temperature lower than the saturation temperature to form micro-droplets. The method for generating the micro-droplets realizes the generation of the micro-droplets which are suspended and can regulate the size, the number and the positions of the micro-droplets above the liquid level of the sample, and has the advantages of simple structure, small requirements on environment, easy implementation, strong anti-interference capability, convenient preparation and the like.

Description

Micro-droplet generation method and generation device thereof
Technical Field
The present invention relates to a droplet generation technology, and more particularly, to a method and apparatus for generating droplets.
Background
The micro-droplets are widely existing in the nature and daily life, have a relatively large specific surface area, and the relatively large specific surface area enables the droplets to maintain a stable state, so that the micro-droplets are good micro-carriers, can realize the microminiaturization of chemical reactions and biomedical detection, are beneficial to reducing reaction reagents, shortening reaction time, regulating and controlling local reaction conditions, increasing reaction precision and the like, and show great application potential.
Microdroplets have great potential for their potential application, and a fundamental prerequisite for microdroplets to truly exert their potential mechanism of application is the ability to stably produce uniform, size and structural precision microdroplets. Therefore, the ability to produce stable, controllable micro-droplets at high frequencies and to achieve high throughput production is a key step in achieving its application value.
Methods of generating microdroplets have heretofore been chips, capillaries, piezoelectrics, acoustic fields, electric fields, magnetic fields, light guides, functional interfaces (super hydrophilic), microwell arrays, and the like, such as:
chinese patent (publication No. CN108671970 a) presents a method for generating double-sized micro-droplets based on microfluidic chips. And injecting the disperse phase and the continuous phase into the microfluidic chip, and forming double-size micro-droplets at the shear cut of the microfluidic chip under the combined action of the shearing force and the pressure applied to the disperse phase by the continuous phase. The performance of the generated liquid drops is stable, the influence of the flow velocity is small in a certain channel size, the repeatability is good, and the size of the small liquid drops can be controlled through the volume; however, the droplets generated by the chip are limited in the micro-channel and isolated from the external space, and the application of the micro-droplets is limited and the generated micro-droplets are difficult to control although the droplets are protected.
The generation of oil-in-water droplets in micro-eddies based on restricted thermal capillaries is given in the literature (Optics Letters,2020,45 (7): 1998-2001). A 1064nm laser was coupled into graphene oxide using an open microfluidic chip, such that the photothermal waveguide served as a heater. Based on the continuity of natural convection heat transfer, a temperature gradient is generated during heating, so that a surface tension gradient is generated around the local area of water; and then, under the drive of a surface tension gradient, the micro vortex of the thermal capillary tube is generated, and the photo-thermal waveguide is moved to generate micro liquid drops. The size and shape of the micro-droplets can be precisely controlled, however, the preparation technology is complex, the cost is high, the liquid incompatibility principle is needed to be used, the generated droplets are limited in the microfluidic chip, and the application of the droplets is limited due to the non-free space micro-droplets.
In summary, these methods for generating microdroplets have limitations in the preparation process, difficulty in operation, cost of preparation, and handling, and cannot meet the requirements of microdroplet application.
Disclosure of Invention
The invention aims to provide a method for generating micro-droplets, which realizes the generation of micro-droplets which are suspended and adjustable in size, number and position above the liquid level of a sample, has the advantages of simple structure, small environmental requirements, easy implementation, strong anti-interference capability, convenient preparation and the like, and has important significance in biomedicine, especially in quantitative transportation of certain medicines or humidification of lung support equipment.
In order to achieve the above object, the present invention provides a method for generating micro-droplets, comprising the steps of:
s1, adjusting the output power of a laser according to the number, the size and the distance from the liquid level of prepared micro liquid drops;
s2, connecting a laser with one end of an optical fiber, inserting an optical fiber probe connected with the other end of the optical fiber into the sample liquid, and transmitting light emitted by the laser to the sample liquid through the optical fiber probe to generate a photo-thermal effect;
s3, respectively blowing a cold air flow and a hot vapor flow to two sides of the top surface of the sample liquid;
s4, until the heat of a certain area in the sample liquid cannot be transferred or the transfer speed is lower than the set requirement, gathering a large amount of heat in a small range under the continuous action of light energy, and forming a light source heating area;
s5, the temperature of the sample liquid is gradually increased, the sample liquid is subjected to liquid-gas phase transition to form vapor, the vapor is condensed when meeting the temperature lower than the saturation temperature to form micro-droplets, and at the moment, under the combined action of the lifting force of the air flow, the gravity of the micro-droplets and the cold air flow and the hot vapor flow, the micro-droplets have upper-lower pressure difference, so that the micro-droplets are suspended on the surface of the sample liquid.
Preferably, as the laser power is increased in step S1, the number, size, and distance from the liquid surface of the sample liquid are increased.
Preferably, the wavelength of the light emitted by the laser is greater than the average wavelength of the absorption coefficient of the sample liquid.
Preferably, the sample liquid in step S2 is distilled water;
and step S2 specifically includes the following steps:
s21, placing distilled water on a glass slide, and then installing a CCD camera with an objective lens and an illumination light source on the upper side and the lower side of the distilled water;
s22, adjusting the insertion position and the insertion mode of the optical fiber probe through a micro-operation platform, adjusting the focal length of an objective lens, and observing by a computer connected with a CCD camera;
s23, turning on a laser, a CCD camera, an illumination light source and a computer, adjusting the focal length of an objective lens, and observing the generation of micro liquid drops by using the computer communicated with the CCD camera.
Preferably, in step S22, the fiber probe is first inserted into the sample liquid from different horizontal positions by the micro-operation platform, and the change of micro-droplets is observed according to the different horizontal insertion positions of the fiber probe;
and then the optical fiber probe is inserted into distilled water from different vertical direction positions through the micro-operation platform, and the change of micro-droplets is observed along with the different vertical insertion positions of the optical fiber probe.
The generation device based on the micro-droplet generation method comprises a glass slide used for bearing sample liquid, an optical fiber probe used for being inserted into the sample liquid, an optical fiber with one end connected with the optical fiber probe and a laser connected with the other end of the optical fiber.
Preferably, the upper side and the lower side of the glass slide are respectively provided with an illumination light source and a CCD camera, and the CCD camera is communicated with a computer.
Preferably, an objective lens is fixed on one side of the CCD camera facing the glass slide.
Preferably, the optical fiber between the optical fiber probe and the laser is erected on a micro-operation platform and is used for adjusting the insertion position and the insertion mode of the optical fiber probe.
Preferably, the optical fiber probe is a flat end face single-mode probe, and the sample liquid is distilled water.
Compared with the prior art, the invention has very remarkable effects:
1. the micro-droplets generated based on the photo-thermal effect can be modulated by the related parameters of the light source, the formation and the growth of the micro-droplets are controlled, the number and the size of the droplets can be precisely controlled, and the method has important significance in biomedicine, in particular in quantitative transportation of certain medicines or humidification of lung support equipment.
2. The method of the invention realizes that the micro-droplets stably suspend above the liquid level and are separated from the sample solution, so that the method is more flexible to control and research, and enriches the method for researching the micro-droplets.
3. The method can regulate and control the generation position of the micro liquid drops by changing the position of the optical fiber.
4. Compared with the prior art, the method has the advantages of simple structure, easy implementation, controllable generated liquid drops, strong anti-interference capability and convenient preparation.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
FIG. 1 is a schematic diagram of a method for generating micro-droplets according to an embodiment of the present invention;
fig. 2 is a schematic structural diagram of a generating device according to a method for generating micro-droplets according to an embodiment of the invention.
1. An optical fiber probe; 2. a sample liquid; 3. a glass slide; 4. a light source heating zone; 5. a microdroplet; 6. a flow of cold air; 7. a hot vapor stream; 8. an optical fiber; 9. a laser; 10. a micro-operation platform; 11. an objective lens; 12. a CCD camera; 13. an illumination light source; 14. and a computer.
Detailed Description
The present invention will be further described with reference to the accompanying drawings, and it should be noted that, while the present embodiment provides a detailed implementation and a specific operation process on the premise of the present technical solution, the protection scope of the present invention is not limited to the present embodiment.
Fig. 1 is a schematic diagram of a method for generating micro-droplets according to an embodiment of the present invention, as shown in fig. 1, the present invention includes the following steps:
s1, adjusting the output power of a laser 9 according to the number, the size and the distance from the liquid level of the prepared micro-droplets 5;
preferably, as the power of the laser 9 increases in step S1, the number, size and distance from the liquid surface of the sample liquid 2 of the generated micro droplets 5 increase.
Preferably, the wavelength of the light emitted by the laser 9 is greater than the average wavelength of the absorption coefficient of the sample liquid 2. I.e. 1480nm wavelength.
S2, connecting a laser 9 with one end of an optical fiber 8, inserting a probe 1 of the optical fiber 8 connected with the other end of the optical fiber 8 into the sample liquid 2, and transmitting light emitted by the laser 9 to the sample liquid 2 through the probe 1 of the optical fiber 8 to generate a photo-thermal effect;
preferably, the sample liquid 2 in step S2 is distilled water;
and step S2 specifically includes the following steps:
s21, placing distilled water on the glass slide 3, and then installing a CCD camera 12 with an objective lens 11 and an illumination light source 13 on the upper side and the lower side of the distilled water;
s22, regulating the insertion position and the insertion mode of the probe 1 of the optical fiber 8 through the micro-operation platform 10, regulating the focal length of the objective lens 11, and observing by using a computer 14 connected with the CCD camera 12;
s23, turning on the laser 9, the CCD camera 12, the illumination light source 13 and the computer 14, adjusting the focal length of the objective lens 11, and observing the generation of the micro-droplets 5 by using the computer 14 communicated with the CCD camera 12.
Preferably, in step S22, the optical fiber 8 probe 1 is first inserted into the sample liquid 2 from different horizontal positions by the micro-operation platform 10, and the change of the micro-droplet 5 is observed according to the different horizontal insertion positions of the optical fiber 8 probe 1; in this example, it was observed that the position of the droplet 5 was changed according to the insertion position of the probe 1 of the optical fiber 8.
And then the optical fiber 8 probe 1 is inserted into distilled water from different vertical direction positions through the micro-operation platform 10, and the change of the micro-droplet 5 is observed along with the different vertical insertion positions of the optical fiber 8 probe 1. In this example, it was observed that the time for starting to generate the micro-droplet 5 was reduced with the decrease in the depth of insertion (height from the liquid surface) of the probe 1 of the optical fiber 8, and the micro-droplet 5 was obtained more rapidly due to the difficulty in diffusing the heat generated in the laser field and the rapid rise in temperature.
S3, respectively blowing a cold air flow 6 and a hot steam flow 7 to two sides of the top surface of the sample liquid 2;
s4, until the heat of a certain area in the sample liquid 2 cannot be transferred or the transfer speed is lower than the set requirement, collecting a large amount of heat in a small range under the continuous action of light energy, and forming a light source heating area 4;
s5, the temperature of the sample liquid 2 is gradually increased, the sample liquid 2 is subjected to liquid-gas phase change to form vapor, the vapor is condensed when meeting the temperature lower than the saturation temperature to form micro-droplets 5, and at the moment, under the combined action of the lifting force of the air flow, the gravity of the micro-droplets 5 and the cold air flow 6 and the hot vapor flow 7, the micro-droplets 5 have up-down pressure difference, so that the micro-droplets 5 are suspended on the surface of the sample liquid 2.
Fig. 2 is a schematic structural diagram of a generating device based on a generating method of micro-droplets 5 according to an embodiment of the present invention, and as shown in fig. 2, the generating device based on the generating method of micro-droplets 5 includes a glass slide 3 for carrying a sample liquid 2, an optical fiber 8 probe 1 for being inserted into the sample liquid 2, an optical fiber 8 having one end connected to the optical fiber 8 probe 1, and a laser 9 having the other end connected to the optical fiber 8.
Preferably, the upper side and the lower side of the glass slide 3 are respectively provided with an illumination light source 13 and a CCD camera 12, and the CCD camera 12 is communicated with a computer 14. And an objective lens 11 is fixed to the side of the CCD camera 12 facing the slide 3.
Preferably, the optical fiber 8 between the probe 1 of the optical fiber 8 and the laser 9 is erected on the micro-operation platform 10, and is used for adjusting the insertion position and the insertion mode of the probe 1 of the optical fiber 8.
Preferably, the optical fiber 8 probe 1 is a flat end face single-mode probe, and the sample liquid 2 is distilled water.
Therefore, the method for generating the micro-droplets realizes the generation of the micro-droplets which are suspended and have adjustable size, quantity and position above the liquid level of the sample, and has the advantages of simple structure, small requirement on environment, easy implementation, strong anti-interference capability, convenient preparation and the like.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention and not for limiting it, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that: the technical scheme of the invention can be modified or replaced by the same, and the modified technical scheme cannot deviate from the spirit and scope of the technical scheme of the invention.

Claims (3)

1. A method of generating microdroplets, characterized by: the method comprises the following steps:
s1, adjusting the output power of a laser according to the number, the size and the distance from the liquid level of prepared micro liquid drops;
s2, connecting a laser with one end of an optical fiber, inserting an optical fiber probe connected with the other end of the optical fiber into the sample liquid, and transmitting light emitted by the laser to the sample liquid through the optical fiber probe to generate a photo-thermal effect;
the sample liquid in the step S2 is distilled water;
and step S2 specifically includes the following steps:
s21, placing distilled water on a glass slide, and then installing a CCD camera with an objective lens and an illumination light source on the upper side and the lower side of the distilled water;
s22, adjusting the insertion position and the insertion mode of the optical fiber probe through a micro-operation platform, adjusting the focal length of an objective lens, and observing by a computer connected with a CCD camera;
s23, turning on a laser, a CCD camera, an illumination light source and a computer, adjusting the focal length of an objective lens, and observing the generation of micro liquid drops by using the computer communicated with the CCD camera;
in step S22, firstly, the fiber probe is inserted into the sample liquid from different horizontal positions through the micro-operation platform, and the change of micro-droplets is observed along with the different horizontal insertion positions of the fiber probe;
then the optical fiber probe is inserted into distilled water from different vertical direction positions through the micro-operation platform, and the change of micro-droplets is observed along with the different vertical insertion positions of the optical fiber probe;
s3, respectively blowing a cold air flow and a hot vapor flow to two sides of the top surface of the sample liquid;
s4, until the heat of a certain area in the sample liquid cannot be transferred or the transfer speed is lower than the set requirement, gathering a large amount of heat in a small range under the continuous action of light energy, and forming a light source heating area;
s5, the temperature of the sample liquid is gradually increased, the sample liquid is subjected to liquid-gas phase transition to form vapor, the vapor is condensed when meeting the temperature lower than the saturation temperature to form micro-droplets, and at the moment, under the combined action of the lifting force of the air flow, the gravity of the micro-droplets and the cold air flow and the hot vapor flow, the micro-droplets have upper-lower pressure difference, so that the micro-droplets are suspended on the surface of the sample liquid.
2. The method of generating droplets according to claim 1, characterized in that: as the laser power increases in step S1, the number, size, and liquid level distance to the sample liquid of the generated microdroplets increase.
3. The method of generating droplets according to claim 2, characterized in that: the laser emits light having a wavelength greater than the average wavelength of the absorption coefficient of the sample fluid.
CN202211162402.2A 2022-09-23 2022-09-23 Micro-droplet generation method and generation device thereof Active CN115569675B (en)

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