WO2024039071A1 - Dispositif microfluidique rotatif, ensemble microfluidique rotatif, système de synthèse de nanoparticules, procédé de préparation de nanoparticules métalliques, nanoparticules métalliques préparées à partir de celui-ci, et substrat de diffusion raman à surface améliorée - Google Patents

Dispositif microfluidique rotatif, ensemble microfluidique rotatif, système de synthèse de nanoparticules, procédé de préparation de nanoparticules métalliques, nanoparticules métalliques préparées à partir de celui-ci, et substrat de diffusion raman à surface améliorée Download PDF

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WO2024039071A1
WO2024039071A1 PCT/KR2023/009786 KR2023009786W WO2024039071A1 WO 2024039071 A1 WO2024039071 A1 WO 2024039071A1 KR 2023009786 W KR2023009786 W KR 2023009786W WO 2024039071 A1 WO2024039071 A1 WO 2024039071A1
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chamber
channel
chambers
unit
microfluidic device
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PCT/KR2023/009786
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English (en)
Korean (ko)
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서태석
응우엔 반힙
Original Assignee
경희대학교 산학협력단
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Priority claimed from KR1020230088203A external-priority patent/KR20240024010A/ko
Application filed by 경희대학교 산학협력단 filed Critical 경희대학교 산학협력단
Publication of WO2024039071A1 publication Critical patent/WO2024039071A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/14—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic in rotating dishes or pans
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/65—Raman scattering

Definitions

  • the present invention relates to a rotary microfluidic device, and more specifically, a rotary microfluidic device, a rotary microfluidic assembly, a nanoparticle synthesis system, a method for producing metal nanoparticles, metal nanoparticles produced therefrom, and surface-enhanced Raman. It concerns scattering substrates.
  • the microfluidic structure that makes up a microfluidic device includes a chamber that can trap a small amount of fluid, a channel through which the fluid can flow, a valve that can control the flow of the fluid, and a device that can receive the fluid and perform a certain function.
  • Various functional units, etc. may be included.
  • the microfluidic device may be equipped with, for example, a rotating microfluidic device.
  • a synthesis method using a batch reactor is generally used.
  • This synthesis method using a batch reactor is not only greatly affected by various conditions such as reaction temperature and reagent concentration, but also consumes a lot of pipettes and reagents more than necessary, resulting in a lot of time, labor, and cost.
  • a problem of consumption occurred. For example, in order to synthesize 60 nanoparticles, numerous reagents, beakers, and time and manpower were required to individually adjust the concentrations of the reagents, making the synthesis process of nanoparticles with various shapes inefficient.
  • the purpose of the present invention is to provide a rotary microfluidic device that can reduce the time, cost, and labor required to synthesize nanoparticles.
  • Another object of the present invention is to provide a rotational microfluidic device that can automatically and quickly synthesize highly efficient metal nanoparticles of various shapes without human intervention.
  • Another object of the present invention is to provide a rotary microfluidic assembly including the rotary microfluidic device.
  • Another object of the present invention is to provide a nanoparticle synthesis system including the rotary microfluidic assembly.
  • Another object of the present invention is to provide a method for producing metal nanoparticles using the rotary microfluidic device.
  • Another object of the present invention is to provide metal nanoparticles produced by the above metal nanoparticle production method.
  • Another object of the present invention is to provide a Surface-Enhanced Raman Scattering (SERS) substrate that can improve signal sensitivity in Raman spectroscopy analysis.
  • SERS Surface-Enhanced Raman Scattering
  • One embodiment of the present invention for achieving the above object includes: a first unit unit including a plurality of first chambers having the same volume and connected to each other through a first channel; a second unit unit including a plurality of second chambers having different volumes and connected to each other through a second channel; a third unit unit including a plurality of third chambers having different volumes and connected to each other through a third channel; a fourth unit unit including a plurality of fourth chambers having the same volume and connected to each other through a fourth channel; a reaction chamber including a plurality of fifth chambers connected to the first to fourth chambers; a first connection portion connecting each of the first chamber and the second chamber; a second connection portion connecting each of the second chambers and the fifth chamber; a third connection portion connecting each of the third chamber and the fifth chamber; and a fourth connection part connecting each of the fourth chamber and the fifth chamber, wherein the first to fourth connection parts include a passive valve.
  • the thickness of the first channel is thicker than the thickness of the first connection part
  • the thickness of the second channel is thicker than the thickness of the second connection part
  • the thickness of the third channel is thicker than the thickness of the third connection part
  • the thickness of the fourth channel may be thicker than the thickness of the fourth connection part.
  • each of the first chambers is circumferentially arranged
  • each of the second chambers is circumferentially arranged
  • each of the third chambers is circumferentially arranged
  • each of the fourth chambers is circumferentially arranged.
  • each of the fifth chambers may be arranged circumferentially.
  • the first to fourth channels may have a zigzag shape.
  • the first channel is a channel through which a metal seed solution flows
  • the second channel is a channel through which a reducing agent flows
  • the third channel is a channel through which a diluent flows
  • the fourth channel is a channel through which a growth solution flows. It can be a flowing channel.
  • the passive valve includes a first passive valve and a second passive valve connected to the first passive valve, and the first connection portion includes the first passive valve and the second passive valve. May include a passive valve.
  • the volume gradient of each of the second chambers arranged in the circumferential direction and the volume gradient of each of the third chambers arranged in the circumferential direction are different from each other. can do.
  • Another embodiment of the present invention for achieving the above object includes the rotary microfluidic device; And it is possible to provide a rotary microfluidic assembly including an adhesive layer disposed on at least one surface of the rotary microfluidic device.
  • Another embodiment of the present invention for achieving the above object includes a storage unit storing a reaction reagent; a guide portion connected to the storage portion and including a connection portion; an injection unit connected to the connection unit and discharging the reaction reagent; a driving unit connected to the injection unit and supplying the reaction reagent to the injection unit;
  • the rotary microfluidic assembly corresponding to the injection unit; It is possible to provide a nanoparticle synthesis system including a rotating part that rotates the rotary microfluidic assembly.
  • the injection unit may be supported by the connection unit.
  • the nanoparticle synthesis system may further include a control unit that adjusts the position of the injection unit and controls the rotation speed of the rotation unit.
  • the nanoparticle synthesis system according to another embodiment of the present invention may further include a packaging part surrounding at least one of the guide part, the driving part, and the rotating part.
  • Another embodiment of the present invention for achieving the above object is a method for producing metal nanoparticles using a nanoparticle synthesis system, comprising: (S1) injecting a metal seed solution into the first chamber; (S2) injecting a reducing agent into the second chamber; (S3) injecting a diluent into the third chamber; (S4) injecting a growth solution into the fourth chamber; and (S5) rotating the rotary microfluidic assembly;
  • S1 injecting a metal seed solution into the first chamber
  • S2 injecting a reducing agent into the second chamber
  • S3 injecting a diluent into the third chamber
  • S4 injecting a growth solution into the fourth chamber
  • S5 rotating the rotary microfluidic assembly
  • the sum of the volume of the reducing agent contained in the second chamber and the volume of the diluent contained in the third chamber corresponding to the second chamber may be constant.
  • the rotary microfluidic assembly may rotate for 1 to 60 seconds at a rotation speed of 4,000 rpm or more.
  • Another embodiment of the present invention to achieve the above object can provide metal nanoparticles manufactured by the above metal nanoparticle manufacturing method.
  • Another embodiment of the present invention to achieve the above object can provide a Surface-Enhanced Raman Scattering (SERS) substrate on which the metal nanoparticles are coated.
  • SERS Surface-Enhanced Raman Scattering
  • the metal nanoparticle may be a star-shaped gold nanoparticle (Au nanoparticle).
  • At least one reaction chamber and an injection chamber connected to the reaction chamber and including at least one subchamber. and at least one connection part connecting each of the subchambers to each other and connecting the reaction chamber and the injection chamber. It provides a rotary microfluidic device, including, wherein each connection portion includes a passive valve.
  • the reaction chamber may be a chamber in which a synthesis reaction of metal nanoparticles occurs.
  • the injection chamber may be a chamber into which a solution required for the synthesis reaction of metal nanoparticles is injected.
  • the solution required for the synthesis reaction of the metal nanoparticles may be a metal seed solution, a reducing agent, a diluent, a growth solution, etc.
  • the technical idea of the present invention is not limited to this, and solutions necessary for various types of synthetic reactions can be selected.
  • the subchamber may include a plurality of first to fourth chambers according to some embodiments of the present invention.
  • connection unit may include a plurality of first to fourth connection units according to some embodiments of the present invention.
  • the time, cost, and labor required to synthesize nanoparticles under various reaction conditions can be significantly reduced, and high-efficiency metal nanoparticles of various shapes can be quickly and automatically synthesized without human intervention.
  • a rotary microfluidic device can be provided. Metal nanoparticles of various shapes manufactured using these rotary microfluidic devices can be used in the fields of photothermal therapy, drug carriers used for drug delivery, diagnostic fields that improve the sensitivity of biological/chemical sensors, and photoacoustic effects-based fields. It can be widely applied in the biomedical imaging field.
  • Figure 1a shows a rotary microfluidic device according to an embodiment of the present invention including 60 reaction units
  • Figure 1b shows one reaction unit
  • Figure 1c shows the principle of fluid flow in the rotary microfluidic device
  • Figure 1d is a digital photo of a rotating microfluidic device.
  • Figure 2 is an enlarged view of one reaction unit shown in Figure 1b.
  • Figure 3a is a rotary microfluidic assembly according to an embodiment of the present invention
  • Figure 3b is a digital photograph of the rotary microfluidic assembly.
  • Figure 4a is a nanoparticle synthesis system according to an embodiment of the present invention.
  • Figure 4b is a digital photograph of a nanoparticle synthesis system according to an embodiment of the present invention.
  • Figure 5a is a schematic diagram of ascorbic acid and water flowing in the circumferential direction, respectively
  • Figure 5b is a digital photograph showing the concentration gradient of ascorbic acid diluted with water after the rotary microfluidic device is rotated
  • Figure 5c is a diagram for each reaction chamber.
  • Figure 5d is a photograph of the nanoparticle synthesis system
  • Figure 5e is an enlarged photograph of the injection part of the nanoparticle synthesis system
  • Figure 5f is a nanoparticle with the packaging part introduced. This is a photo of the composite system.
  • Figure 6a shows a first step in which a gold seed solution (Au seed solution) is first injected into a plurality of first chambers arranged in the circumferential direction;
  • Figure 6b shows a second step in which ascorbic acid is injected into a plurality of second chambers arranged in the circumferential direction;
  • Figure 6c shows a third step in which water is injected into a plurality of third chambers arranged in the circumferential direction;
  • FIG. 6D shows a fourth step in which the growth solution is injected into a plurality of fourth chambers arranged in the circumferential direction.
  • Figure 6e shows that when the rotation speed of the rotating part was rotated to 1,000 RPM, ascorbic acid, water, and growth solution, excluding the gold seed solution, moved to the reaction chamber.
  • Figure 6f shows that when the rotation speed of the rotating part is increased to 4,000 RPM and rotated, even the gold seed solution is moved to the reaction chamber.
  • Figure 6g shows that the gold seed solution moves to 60 first chambers through the zigzag-shaped first channel with a single injection.
  • Figure 6h shows that the recovery volumes of the gold seed solution and the growth solution were each constant.
  • Figure 8a shows gold nanoparticles (hereinafter referred to as 'Au#1, Au#4 in that order) prepared with a rotary microfluidic device when the concentration of ascorbic acid was 0.4mM, 0.9mM, 1.25mM, 1.75mM, 2.75mM and 3.6mM. , Au#6, Au#9, Au#15 and Au#20').
  • Figure 8b contains Au#1, Au#4, Au#6, Au#9, Au#15, and Au#20, respectively, required to manufacture a Surface-Enhanced Raman Scattering (SERS) substrate. This shows the color of the gold nanoparticle solution.
  • SERS Surface-Enhanced Raman Scattering
  • Figure 8c shows a method of manufacturing a Surface-Enhanced Raman Scattering (SERS) substrate according to an embodiment of the present invention.
  • SERS Surface-Enhanced Raman Scattering
  • Figure 8d is a digital photograph of a Surface-Enhanced Raman Scattering (SERS) substrate according to an embodiment of the present invention.
  • SERS Surface-Enhanced Raman Scattering
  • Figure 8e is a FE-SEM photograph of a Surface-Enhanced Raman Scattering (SERS) substrate according to various embodiments of the present invention.
  • Figure 9a shows Raman shift using a surface-enhanced Raman scattering substrate coated with gold nanoparticles (Au#1) to analyze the limit of detection (LOD) of R6G (Rhodamine 6G). It represents the intensity of light.
  • Figure 9b shows Raman shift using a surface-enhanced Raman scattering substrate coated with gold nanoparticles (Au#4) to analyze the limit of detection (LOD) of R6G (Rhodamine 6G). It represents the intensity of light.
  • Figure 9c shows Raman shift using a surface-enhanced Raman scattering substrate coated with gold nanoparticles (Au#6) to analyze the limit of detection (LOD) of R6G (Rhodamine 6G). It represents the intensity of light.
  • Figure 9d shows Raman shift using a surface-enhanced Raman scattering substrate coated with gold nanoparticles (Au#9) to analyze the limit of detection (LOD) of R6G (Rhodamine 6G). It represents the intensity of light.
  • Figure 9e shows Raman shift using a surface-enhanced Raman scattering substrate coated with gold nanoparticles (Au#15) to analyze the limit of detection (LOD) of R6G (Rhodamine 6G). It represents the intensity of light.
  • Figure 9f shows Raman shift using a surface-enhanced Raman scattering substrate coated with gold nanoparticles (Au#20) to analyze the limit of detection (LOD) of R6G (Rhodamine 6G). It represents the intensity of light.
  • Figure 9g shows the Raman spectrum for 10 -7 M of R6G (Rhodamine 6G) of the surface-enhanced Raman scattering substrate into which Au#1, Au#4, Au#6, Au#9, Au#15, and Au#20 were introduced, respectively. It represents the century.
  • the 'rotary microfluidic device' may include a plurality of reaction units.
  • one reaction unit may include first to fourth unit parts, a reaction chamber, and first to fourth connection parts.
  • One embodiment of the present invention includes: a first unit unit including a plurality of first chambers having the same volume and connected to each other through a first channel; a second unit unit including a plurality of second chambers having different volumes and connected to each other through a second channel; a third unit unit including a plurality of third chambers having different volumes and connected to each other through a third channel; a fourth unit unit including a plurality of fourth chambers having the same volume and connected to each other through a fourth channel; a reaction chamber including a plurality of fifth chambers connected to the first to fourth chambers; a first connection portion connecting each of the first chamber and the second chamber; a second connection portion connecting each of the second chambers and the fifth chamber; a third connection portion connecting each of the third chamber and the fifth chamber; and a fourth connection part connecting each of the fourth chamber and the fifth chamber, wherein the first to fourth connection parts include a passive valve.
  • the first to fourth connection parts include a passive valve, so that the capillary pressure by the passive valve is higher than the capillary pressure by each channel when the solution is injected into one chamber. , without moving to the reaction chamber, it can be moved to another chamber connected through a channel.
  • the centrifugal force becomes higher than the capillary pressure and the solution contained in each chamber can move to the reaction chamber. Accordingly, the synthesis reaction of various nanoparticles can proceed quickly in each reaction chamber.
  • a rotary microfluidic device that can be provided can be provided.
  • Metal nanoparticles of various shapes manufactured using these rotary microfluidic devices can be used in the fields of photothermal therapy, drug carriers used for drug delivery, diagnostic fields that improve the sensitivity of biological/chemical sensors, and photoacoustic effects-based fields. It can be applied to the biomedical imaging field.
  • Figure 1a shows a rotary microfluidic device according to an embodiment of the present invention including 60 reaction units
  • Figure 1b shows one reaction unit
  • Figure 1c shows the principle of fluid flow in the rotary microfluidic device
  • Figure 1d is a digital photo of a rotating microfluidic device.
  • Figure 2 is an enlarged view of one reaction unit shown in Figure 1b.
  • the rotary microfluidic device 100 includes first to fourth unit parts (U1, U2, U3, U4), a reaction chamber (RC), and first to fourth connection parts. Includes (C1, C2, C3, C4).
  • the rotary microfluidic device 100 includes a first unit unit U1 including a plurality of first chambers 10 that have the same volume and are connected to each other through a first channel 12.
  • the plurality of first chambers 10 may be arranged along the circumferential direction and may all have the same volume.
  • the first channel may be a channel through which a metal seed solution flows, and the metal seed solution may include, for example, NaBH 4 (0.6mL, 0.01M) solution, HAuCl 4 (0.1mL, 25mM), and a surfactant. (Triton
  • the rotary microfluidic device 100 includes a second unit unit U2 including a plurality of second chambers 20 that have different volumes and are connected to each other through a second channel 22.
  • the plurality of second chambers 20 may be arranged along the circumferential direction.
  • the plurality of second chambers 20 include a 2-1 chamber 20-1 and a 2-2 chamber having the same or different volume as the 2-1 chamber 20-1. It may include a chamber 20-2.
  • the 2-1 chamber 20-1 and the 2-2 chamber 20-2 are different, the number of reaction conditions increases and metal nanoparticles of various shapes can be synthesized.
  • the 2-1 chamber 20-1 and the 2-2 chamber 20-2 may be directly connected through one second channel 22, and two or more second channels 22 It can also be indirectly connected through .
  • the second channel 22 may be a channel through which a reducing agent flows, and specifically, it may be a channel through which ascorbic acid flows.
  • the rotary microfluidic device 100 includes a third unit unit U3 including a plurality of third chambers 30 that have different volumes and are connected to each other through a third channel 32.
  • the plurality of third chambers 30 may be arranged along the circumferential direction.
  • the plurality of third chambers 30 include a 3-1 chamber (30-1) and a 2-2 chamber (20-2) corresponding to the 2-1 chamber (20-1). It may include a corresponding 3-2 chamber (30-2).
  • the volume of the 3-1 chamber 30-1 and the volume of the 3-2 chamber 30-2 may be the same or different from each other.
  • the 3-1 chamber 30-1 and the 3-2 chamber 30-2 may be directly connected through one third channel 32, and two or more third channels 32 It can also be indirectly connected through .
  • the third channel may be a channel through which a diluent flows, and specifically, it may be a channel through which water flows.
  • the sum of the volume of the 2-1 chamber (20-1) and the volume of the 3-1 chamber (30-1) may be constant, and the 2-2
  • the sum of the volume of the chamber 20-2 and the volume of the third-2 chamber 30-2 may be constant.
  • the rotary microfluidic device 100 includes a fourth unit unit U4 including a plurality of fourth chambers 40 that have the same volume and are connected to each other through a fourth channel 42.
  • the plurality of fourth chambers 40 may be arranged along the circumferential direction and may all have the same volume.
  • the fourth channel may be a channel through which a growth solution flows.
  • the growth solution may contain metal ions, surfactants, etc., specifically HAuCl 4 (25mM), AgNO 3 (50mM), and It may be a mixture of nonionic surfactant (e.g., 0.3M Triton-X) in a volume ratio of 1:10:166.
  • the rotary microfluidic device 100 includes a reaction chamber (RC) including a plurality of fifth chambers 50 connected to the first to fourth chambers 10, 20, 30, and 40. .
  • a reaction chamber including a plurality of fifth chambers 50 connected to the first to fourth chambers 10, 20, 30, and 40.
  • the centrifugal force becomes higher than the capillary pressure caused by the passive valve, and the metal seed solution, reducing agent, diluent, and growth solution contained in each chamber all flow into the metal.
  • It may be a chamber in which nanoparticles are synthesized.
  • the rotary microfluidic device 100 includes a first connection portion C1 connecting each of the first chamber 10 and the second chamber 20.
  • the first chamber 10 and the second chamber 20 may correspond to each other within one reaction unit through the first connection part C1.
  • the passive valve (pv) may include a first passive valve and a second passive valve connected to the first passive valve.
  • the first connection part C1 may include the first passive valve and the second passive valve.
  • the capillary pressure due to the passive valves may be much higher than the capillary pressure due to the first channel 12. Accordingly, when the metal seed solution is injected into the first chamber 10 only once, the metal seed solution does not move to the reaction chamber but can move to another first chamber 10 through the first channel 12.
  • the thickness of the first channel 12 may be thicker than the thickness of the first connection portion C1.
  • the fluid flowing through the first connection part C1 may receive a relatively large amount of resistance. Due to these structural characteristics, the capillary pressure by the passive valve is further strengthened, allowing the metal seed solution to move through the first channel 12 from one first chamber to another first chamber.
  • the rotary microfluidic device 100 includes a second connection portion C2 connecting each of the second chamber and the fifth chamber.
  • the second chamber 20 and the fifth chamber 50 may correspond to each other within one reaction unit through the second connection portion C2.
  • the thickness of the second channel 22 may be thicker than the thickness of the second connection portion C2.
  • the fluid flowing through the second connection part C2 may receive more resistance. Due to these structural characteristics, the capillary pressure is further strengthened by the passive valve, allowing the reducing agent to move from one second chamber to another second chamber.
  • the rotary microfluidic device 100 includes a third connection portion C3 connecting each of the third chamber 30 and the fifth chamber 50.
  • the third chamber 30 and the fifth chamber 50 may correspond to each other within one reaction unit through a third connection portion C3.
  • the thickness of the third channel 32 may be thicker than the thickness of the third connection portion C3.
  • the fluid flowing through the third connection part C3 may receive more resistance. Due to these structural characteristics, the capillary pressure is further strengthened by the passive valve, allowing the diluent to move from one third chamber to another third chamber.
  • the rotary microfluidic device 100 includes a fourth connection portion C4 connecting each of the fourth chamber 40 and the fifth chamber 50.
  • the fourth chamber 40 and the fifth chamber 50 may correspond to each other within one reaction unit through the fourth connection portion C4.
  • the thickness of the fourth channel 42 may be thicker than the thickness of the fourth connection portion C4. As the thickness of the fourth channel 42 is designed to be thicker than the thickness of the fourth connection part C4, the fluid flowing through the fourth connection part C4 may receive more resistance. Due to these structural characteristics, the capillary pressure is further strengthened by the passive valve, allowing the growth solution to move from one fourth chamber to another fourth chamber.
  • Each of the first chambers 10 is arranged in a circumferential direction
  • each of the second chambers 20 is arranged in a circumferential direction
  • each of the third chambers 30 is arranged in a circumferential direction
  • each of the The fourth chamber 40 may be arranged in the circumferential direction
  • each of the fifth chambers 50 may be arranged in the circumferential direction. That is, one first chamber may be arranged in a circumferential direction with another first chamber, one second chamber may be arranged in a circumferential direction with another second chamber, and one third chamber may be arranged in a circumferential direction with another third chamber. and may be arranged in a circumferential direction, one fourth chamber may be arranged in a circumferential direction with another fourth chamber, and one fifth chamber may be arranged in a circumferential direction with another fifth chamber.
  • the first to fourth channels 12, 22, 32, and 42 may have a zigzag shape.
  • the capillary pressure by the passive valve is further strengthened, so that the solution injected only once into each chamber does not flow to the reaction chamber (RC) and flows into each of the first to fourth channels.
  • Each solution can flow through.
  • the volume gradient of each of the second chambers 20 arranged in the circumferential direction and the volume gradient of each of the third chambers 30 arranged in the circumferential direction. may be different from each other.
  • the plurality of second chambers 20 sequentially arranged in the circumferential direction may increase in volume along the clockwise direction
  • the plurality of third chambers 30 continuously arranged in the circumferential direction may increase in volume along the clockwise direction.
  • Volume may decrease.
  • the plurality of second chambers 20 sequentially arranged in the circumferential direction may decrease in volume in a clockwise direction
  • the plurality of third chambers 30 continuously arranged in the circumferential direction may decrease in volume in a clockwise direction.
  • the volume may increase accordingly.
  • the total sum of the volume of the diluent and the volume of the reducing agent can be maintained constant, and various concentrations of the reducing agent can be implemented to quickly produce nanoparticles with various shapes. .
  • Figure 3a is a rotary microfluidic assembly according to an embodiment of the present invention
  • Figure 3b is a digital photograph of the rotary microfluidic assembly.
  • another embodiment of the present invention includes the rotary microfluidic device 100 and an adhesive layer 120 disposed on at least one surface of the rotary microfluidic device 100.
  • a typical microfluidic assembly 200 may be provided.
  • the adhesive layer 120 may include a pressure-sensitive adhesive, which is a non-reactive adhesive that forms an adhesive bond when pressure is applied. By using the pressure-sensitive adhesive, an adhesive layer can be easily formed on at least one side of the rotary microfluidic assembly.
  • the adhesive layer 120 may be disposed on both sides of the rotary microfluidic device 100.
  • the adhesive layer 120 may include a first adhesive layer 120a and a second adhesive layer 120b opposite the first adhesive layer 120a.
  • the thickness of the first and second adhesive layers 120a and 120b may each independently be 10 to 80 ⁇ m.
  • the rotary microfluidic device 100 may have a radius of 6.0 to 10.0 cm and a thickness of 3 to 10 mm.
  • the technical idea of the present invention is not limited to this, and the radius and thickness of the rotary microfluidic device may be appropriately modified.
  • Figure 4a is a nanoparticle synthesis system according to an embodiment of the present invention.
  • Figure 4b is a digital photograph of a nanoparticle synthesis system according to an embodiment of the present invention.
  • the nanoparticle synthesis system 300 includes a storage part 310, a guide part 320, an injection part 322, a driving part 330, and a rotary microfluidic assembly 200. ) and a rotating part 340.
  • the storage unit 310 is a member that stores reaction reagents necessary for synthesizing nanoparticles.
  • the storage unit 310 may include first to fourth storage units, and each of the first to fourth storage units may include a metal seed solution, a reducing agent, a diluent, and a growth solution.
  • the guide unit 320 is connected to the storage unit 310 and may include a connection unit 325.
  • the connection unit 325 may be indirectly connected to the storage unit 310 through the driving unit 330.
  • Reaction reagents may be injected into the rotary microfluidic assembly 200 through the injection unit 322.
  • the guide part 320 may include a metal rod 328 extending long in the height direction, a ball screw 326, a stepper motor 324, and a connection part 325.
  • the metal rod 328 is spaced apart from the main body 320bd of the guide portion 320 in the lateral direction and may extend long in the height direction.
  • the ball screw 326 is spaced apart from the main body 320bd of the guide portion 320 in the lateral direction and may extend long in the height direction.
  • connection portion 325 may have a shape corresponding to that of the metal rod 328 and the ball screw 326, and may surround the metal rod 328 and the ball screw 326. A portion of the connection portion 325 may surround the metal rod 328 and the ball screw 326, while the other portion may protrude in the direction in which the rotary microfluidic assembly 200 is disposed. Additionally, the connection portion 325 may move in the height direction (eg, z-axis direction) of the metal rod 328 and the ball screw 326.
  • the connection part 325 may function as a holder arm supporting the injection part 322. Accordingly, the injection part 322 connected to the connection part 325 can also move along the height direction.
  • the injection unit 322 is connected to the connection unit 325 and can discharge the reaction reagent. Specifically, the injection part 322 may be supported by the connection part 325.
  • the driving unit 330 connects the storage unit 310 and the guide unit 320, and can supply the reaction reagent to the injection unit 322.
  • the driving unit 330 may include a port valve 332 and a pump 334.
  • the port valve 332 may perform the function of controlling the flow of the reaction reagent fluid within the driving unit, and the pump 334 may function to move the reaction reagent stored in the storage unit 310 to the driving unit 330. can be performed.
  • the stepper motor 324 may provide power necessary for the up/down movement of the connection part 325.
  • the stepper motor 324 may be placed below the guide unit 320.
  • the nanoparticle synthesis system 300 may include a first connector (CN1) connecting the storage unit 310 and the driving unit 330, and the injection unit 322 and the driving unit ( 330) may include a second connector CN2.
  • the reaction reagents contained in the storage unit 310 may be moved to the driving unit 330 through the first connection pipe (CN1) and then to the injection unit 322 through the second connection pipe (CN2).
  • the injection portion 322 may be the distal end of the second connection pipe CN2.
  • the rotary microfluidic assembly 200 may correspond to the injection unit 322.
  • the reaction reagents required for synthesizing nanoparticles injected through the injection unit 322 may be injected into each chamber of the rotary microfluidic assembly.
  • the reaction reagents required for synthesizing nanoparticles injected through the injection unit 322 may be injected into each chamber of the rotary microfluidic assembly.
  • four injection units may be provided, and each reaction reagent may be placed in the first to fourth chambers (see FIG. 2) corresponding to the four injection units. This can be input.
  • the nanoparticle synthesis system 300 includes a rotating part 340 that rotates the rotary microfluidic assembly 200.
  • the rotating unit 340 may include a rotating motor 341, a support member 343, and a heater 345.
  • the rotation motor 341 may provide power to rotate the rotational microfluidic assembly 200, and the support member 343 may perform a function of supporting the heater 345. (345) can perform the function of controlling the synthesis temperature of nanoparticles.
  • the nanoparticle synthesis system 300 may further include a control unit that adjusts the position of the injection unit 322 and controls the rotation speed of the rotation unit 340.
  • the control unit may be a hardware device that operates an in-house program, and more specifically, the hardware device may be a computer.
  • the nanoparticle synthesis system 300 may further include a packaging part 390 surrounding at least one of the guide part 320, the driving part 330, and the rotating part 340, , Specifically, it can surround all of the guide part 320, the driving part 330, and the rotating part 340.
  • a packaging part 390 is provided to pack at least one of the guide part 320, the driving part 330, and the rotating part 340, a nanoparticle synthesis system with portable characteristics can be provided. .
  • Figure 5a is a schematic diagram of ascorbic acid and water flowing in the circumferential direction, respectively
  • Figure 5b is a digital photograph showing the concentration gradient of ascorbic acid diluted with water after the rotary microfluidic device is rotated
  • Figure 5c is a diagram for each reaction chamber.
  • Figure 5d is a photograph of the nanoparticle synthesis system
  • Figure 5e is an enlarged photograph of the injection part of the nanoparticle synthesis system
  • Figure 5f is a nanoparticle with the packaging part introduced. This is a photo of the composite system.
  • ascorbic acid was introduced into 60 chambers sequentially arranged in the circumferential direction with a single injection, and water was similarly introduced into 60 chambers corresponding to the 60 chambers containing ascorbic acid with a single injection. It has been done.
  • the sum of the volume of ascorbic acid and the volume of water per reaction unit was kept constant at 40 ⁇ L, but the volumes of ascorbic acid and water were adjusted by varying the depth of each chamber.
  • the diluted solution of ascorbic acid and water introduced into the reaction chamber can be analyzed through UV-vis absorbance spectroscopy.
  • the ultraviolet-visible absorption spectroscopy is an analysis method that determines the concentration of a sample based on absorbance, which is the amount of light absorbed by a diluted solution of ascorbic acid and water.
  • absorbance the amount of light absorbed by a diluted solution of ascorbic acid and water.
  • the nanoparticle synthesis system in the nanoparticle synthesis system according to an embodiment of the present invention, four types of reaction reagents stored in a solution storage are moved by a pump to four needle injectors. You can move.
  • the injection unit can be driven in the z-axis direction by a linear guide manufactured using a 3D printing method, and four types of reaction reagents can be injected into each chamber of the rotary microfluidic assembly through the injection unit.
  • a portable nanoparticle synthesis system can be provided by packing the linear guide part and the pump with a packaging part manufactured by a 3D printing method.
  • Another embodiment of the present invention can provide a method for producing metal nanoparticles using the nanoparticle synthesis system.
  • the method for producing metal nanoparticles may include (S1) injecting a metal seed solution into the first chamber.
  • the means for injecting the metal seed solution in step (S1) may be an injection unit of the nanoparticle synthesis system.
  • a single metal seed solution injected into one first chamber through the injection unit may be injected into another first chamber through the first channel due to the capillary pressure caused by the passive valve and the difference in thickness between the first channel and the first connection portion. You can.
  • the metal seed solution can be injected into all of the plurality of first chambers having the same volume.
  • the method for producing metal nanoparticles may include (S2) injecting a reducing agent into the second chamber.
  • the means for injecting the reducing agent into the second chamber may be an injection unit of the nanoparticle synthesis system.
  • the reducing agent injected only once into one second chamber through the injection unit may be injected into another second chamber through the second channel due to the capillary pressure caused by the passive valve and the difference in thickness between the second channel and the second connection portion.
  • a plurality of second chambers having different volumes may be provided to implement various concentrations of the reducing agent.
  • the method for producing metal nanoparticles according to an embodiment of the present invention may include (S3) injecting a diluent into the third chamber.
  • the means for injecting the diluent into the third chamber may be an injection unit of the nanoparticle synthesis system.
  • the diluent injected only once into one third chamber through the injection unit may be injected into another third chamber through the third channel due to the capillary pressure caused by the passive valve and the difference in thickness between the third channel and the third connection.
  • a plurality of third chambers having different volumes may be provided to variously control the concentration of the reducing agent as a diluent.
  • the method for producing metal nanoparticles includes (S4) injecting a growth solution into the fourth chamber.
  • the means for injecting the growth solution into the fourth chamber may be an injection unit of the nanoparticle synthesis system.
  • the reaction solution injected only once into one fourth chamber through the injection unit can be injected into another fourth chamber through the fourth channel due to the capillary pressure caused by the passive valve and the difference in thickness between the fourth channel and the fourth connection. .
  • the method for producing metal nanoparticles includes (S5) rotating the rotary microfluidic assembly.
  • the means for rotating the rotary microfluidic assembly may be a rotating part, and specifically, may be a conventional motor in the relevant technical field.
  • the rotary microfluidic assembly may be rotated for 1 to 60 seconds at a rotation speed of more than 1,000 rpm, and specifically, may be rotated for 1 to 20 seconds at a rotation speed of 4,000 rpm or more. If the rotational speed of the rotating microfluidic assembly is below the above range, the centrifugal force acting on the innermost metal seed solution is lower than the capillary pressure, and the metal seed solution may not be able to move to the reaction chamber.
  • the sum of the volume of the reducing agent contained in the second chamber and the volume of the diluent contained in the third chamber corresponding to the second chamber may be constant.
  • the second chamber and the third chamber corresponding to the second chamber may be provided in one reaction unit.
  • the metal nanoparticles may be, for example, gold nanoparticles, silver nanoparticles, or alloy nanoparticles.
  • the metal nanoparticles can be applied, for example, in the field of photothermal therapy, drug carriers used for drug delivery, diagnostic fields that improve the sensitivity of biological/chemical sensors, and biomedical imaging fields based on photoacoustic effects.
  • Figure 6a shows a first step in which a gold seed solution (Au seed solution) is first injected into a plurality of first chambers arranged in the circumferential direction;
  • Figure 6b shows a second step in which ascorbic acid is injected into a plurality of second chambers arranged in the circumferential direction;
  • Figure 6c shows a third step in which water is injected into a plurality of third chambers arranged in the circumferential direction;
  • FIG. 6D shows a fourth step in which the growth solution is injected into a plurality of fourth chambers arranged in the circumferential direction.
  • Figure 6e shows that when the rotation speed of the rotating part was rotated at 1,000 rpm, ascorbic acid, water, and growth solution, excluding the gold seed solution, moved to the reaction chamber.
  • Figure 6f shows that when the rotation speed of the rotating part is increased to 4,000 rpm and rotated, even the gold seed solution is moved to the reaction chamber.
  • Figure 6g shows that the gold seed solution moves to 60 first chambers through the zigzag-shaped first channel with a single injection.
  • Figure 6h shows that the recovery volumes of the gold seed solution and the growth solution were each constant. Considering that theoretically the volume of the gold seed solution is 10 ⁇ L and the volume of the growth solution is 25 ⁇ L, it can be confirmed that the synthesis reaction of various metal nanoparticles using the rotary microfluidic device was performed accurately.
  • Raman spectroscopy is a method of detecting unknown molecules by utilizing the property of absorbing light energy as much as the vibrational energy of the molecule when the molecule is irradiated with a laser.
  • SERS Surface Enhanced Raman Spectroscopy
  • LSPR localized surface plasmon resonance
  • Another embodiment of the present invention can provide a Surface-Enhanced Raman Scattering (SERS) substrate on which the metal nanoparticles are coated.
  • the metal nanoparticle may be a star-shaped gold nanoparticle (Au nanoparticle).
  • Au nanoparticle As star-shaped gold nanoparticles are coated on a surface-enhanced Raman scattering (SERS) substrate, the sensitivity of the signal in Raman spectroscopy analysis can be significantly improved.
  • the concentration of ascorbic acid to implement the star-shaped gold nanoparticles may be 1.75 to 2.75mM. If the concentration of ascorbic acid is less than the above numerical range, gold nanoparticles in the shape of a circle or polyhedron may be produced and the sensitivity of the signal in Raman spectroscopy analysis may not be sufficiently improved, and if the concentration of ascorbic acid exceeds the above numerical range, star-shaped gold nanoparticles may be produced. As clusters are formed, the sensitivity of the signal in Raman spectroscopy analysis may not be sufficiently improved.
  • Figure 8a shows gold nanoparticles (hereinafter referred to as 'Au#1, Au#4 in that order) prepared with a rotary microfluidic device when the concentration of ascorbic acid was 0.4mM, 0.9mM, 1.25mM, 1.75mM, 2.75mM and 3.6mM. , Au#6, Au#9, Au#15, Au#20').
  • Figure 8b contains Au#1, Au#4, Au#6, Au#9, Au#15, and Au#20, respectively, required to manufacture a Surface-Enhanced Raman Scattering (SERS) substrate. This shows the color of the gold nanoparticle solution.
  • SERS Surface-Enhanced Raman Scattering
  • Figure 8c shows a method of manufacturing a Surface-Enhanced Raman Scattering (SERS) substrate according to an embodiment of the present invention.
  • the method of manufacturing a surface-enhanced Raman scattering substrate according to an embodiment of the present invention includes the steps of treating a glass slide with H 2 O 2 under acid conditions to introduce hydroxide ions to the surface of the glass slide; Modifying the surface of the glass slide into which hydroxide ions (OH - ) have been introduced with 3-aminopropyltriethoxysilane to produce a glass slide into which NH 3 + has been introduced; And the glass slide introduced to the surface of the NH 3 + is immersed in a solution containing gold nanoparticles, then washed with deionized water, and finally, metal nanoparticles are coated on the surface, using Surface-Enhanced Raman Scattering.
  • SERS may include manufacturing a substrate.
  • Figure 8d is a digital photograph of a Surface-Enhanced Raman Scattering (SERS) substrate according to an embodiment of the present invention.
  • Figure 8e is a FE-SEM photograph of a Surface-Enhanced Raman Scattering (SERS) substrate according to various embodiments of the present invention.
  • the detection limit refers to the minimum concentration at which a substance can be said to be detected with considerable confidence.
  • the method for analyzing the surface-enhanced Raman scattering method is, for example, immersing the surface-enhanced Raman scattering substrate in each solution (100 ⁇ L) of 10 -5 to 10 -15 M of R6G (Rhodamine 6G) for 3 hours at room temperature. This may be a method of analyzing dried results, and a Raman spectrometer with an exciting source of 532 nm may be used as analysis equipment.
  • Figure 9a shows Raman shift using a surface-enhanced Raman scattering substrate coated with gold nanoparticles (Au#1) to analyze the limit of detection (LOD) of R6G (Rhodamine 6G). It represents the intensity of light.
  • Figure 9b shows Raman shift using a surface-enhanced Raman scattering substrate coated with gold nanoparticles (Au#4) to analyze the limit of detection (LOD) of R6G (Rhodamine 6G). It represents the intensity of light.
  • each surface-enhanced Raman scattering substrate coated with gold nanoparticles (Au#1, Au#4) having a smooth surface shape has a detection limit of 10 -9 M ( R6G) was confirmed to be visible.
  • Figure 9c shows Raman shift using a surface-enhanced Raman scattering substrate coated with gold nanoparticles (Au#6) to analyze the limit of detection (LOD) of R6G (Rhodamine 6G). It represents the intensity of light.
  • Figure 9d shows Raman shift using a surface-enhanced Raman scattering substrate coated with gold nanoparticles (Au#9) to analyze the limit of detection (LOD) of R6G (Rhodamine 6G). It represents the intensity of light.
  • the surface-enhanced Raman scattering substrate coated with gold nanoparticles (Au#6, Au#9) with some sharp surfaces has a lower detection limit (R6G) of 10 -10 M. It was confirmed that .
  • Figure 9e shows Raman shift using a surface-enhanced Raman scattering substrate coated with gold nanoparticles (Au#15) to analyze the limit of detection (LOD) of R6G (Rhodamine 6G). It represents the intensity of light.
  • the surface-enhanced Raman scattering substrate coated with star-shaped gold nanoparticles (Au#15) on the surface showed a lower detection limit (R6G) of 10 -11 M. From this, it can be inferred that the gold nanoparticles have a star shape and can amplify the light signal in Raman spectroscopy.
  • Figure 9f shows Raman shift using a surface-enhanced Raman scattering substrate coated with gold nanoparticles (Au#20) to analyze the limit of detection (LOD) of R6G (Rhodamine 6G). It represents the intensity of light.
  • Figure 9g shows the Raman spectrum for 10 -7 M of R6G (Rhodamine 6G) of the surface-enhanced Raman scattering substrate into which Au#1, Au#4, Au#6, Au#9, Au#15, and Au#20 were introduced, respectively. It represents the century.
  • first chamber 20 second chamber
  • Nanoparticle synthesis system 310 Storage unit
  • stepper motor 325 connection part
  • driving unit 332 port valve

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Abstract

L'invention concerne un dispositif microfluidique rotatif qui peut réduire le temps, le coût, et la main d'œuvre requis pour synthétiser des nanoparticules. Selon un aspect de la présente invention, un dispositif microfluidique rotatif comprend : une chambre de réaction ; une chambre d'injection raccordée à la chambre de réaction et comprenant une ou plusieurs sous-chambres ; et une ou plusieurs parties de raccordement raccordant les sous-chambres respectives les unes aux autres et raccordant la chambre de réaction et la chambre d'injection l'une à l'autre, chacune des parties de raccordement comprenant une soupape passive.
PCT/KR2023/009786 2022-08-16 2023-07-10 Dispositif microfluidique rotatif, ensemble microfluidique rotatif, système de synthèse de nanoparticules, procédé de préparation de nanoparticules métalliques, nanoparticules métalliques préparées à partir de celui-ci, et substrat de diffusion raman à surface améliorée WO2024039071A1 (fr)

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KR10-2022-0102291 2022-08-16
KR20220102291 2022-08-16
KR10-2023-0088203 2023-07-07
KR1020230088203A KR20240024010A (ko) 2022-08-16 2023-07-07 회전형 마이크로유동 장치, 회전형 마이크로유동 어셈블리,나노입자 합성시스템, 금속나노입자의 제조방법, 이로부터 제조된 금속나노입자 및 표면증강 라만산란 기판

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101239764B1 (ko) * 2007-04-05 2013-03-06 삼성전자주식회사 원심력 기반의 미세유동 시스템 및 상기 미세유동 시스템용바이오 카트리지
KR101738765B1 (ko) * 2015-08-25 2017-06-08 한국과학기술원 나노 입자 합성 고속대량스크리닝용 마이크로 디바이스 및 이를 이용한 나노 입자 합성 방법
CN110496658A (zh) * 2019-09-12 2019-11-26 重庆科技学院 一种联合诊断纸基微流控芯片及制备方法
WO2021185857A2 (fr) * 2020-03-17 2021-09-23 Nordetect Aps Dispositif microfluidique, production d'un dispositif microfluidique et procédé et système pour effectuer des déterminations inorganiques
KR20210133713A (ko) * 2020-04-29 2021-11-08 경희대학교 산학협력단 미세유동장치 및 이를 포함하는 시료 분석 장치

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101239764B1 (ko) * 2007-04-05 2013-03-06 삼성전자주식회사 원심력 기반의 미세유동 시스템 및 상기 미세유동 시스템용바이오 카트리지
KR101738765B1 (ko) * 2015-08-25 2017-06-08 한국과학기술원 나노 입자 합성 고속대량스크리닝용 마이크로 디바이스 및 이를 이용한 나노 입자 합성 방법
CN110496658A (zh) * 2019-09-12 2019-11-26 重庆科技学院 一种联合诊断纸基微流控芯片及制备方法
WO2021185857A2 (fr) * 2020-03-17 2021-09-23 Nordetect Aps Dispositif microfluidique, production d'un dispositif microfluidique et procédé et système pour effectuer des déterminations inorganiques
KR20210133713A (ko) * 2020-04-29 2021-11-08 경희대학교 산학협력단 미세유동장치 및 이를 포함하는 시료 분석 장치

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