CN112557371B - Nanoscopic multiphase interface transient observation device and method based on laser effect - Google Patents
Nanoscopic multiphase interface transient observation device and method based on laser effect Download PDFInfo
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Abstract
The invention discloses a nanoscopic multiphase interface transient observation device based on laser action, which comprises: the micro-pin fin heat dissipation structure chip is placed on a micro-detection scanning platform, a micro-cylinder array, a lens structure and an optical fiber coupler are arranged in the micro-pin fin heat dissipation structure chip, a suspension solution containing gold nanoparticles is communicated in a micro-channel of the micro-cylinder array, the micro-pin fin heat dissipation structure chip and the micro-detection scanning platform are placed in a cassette, laser pulses emitted by a double-pulse width laser align to the lens structure under the action of the optical fiber coupler, the laser pulses enter the micro-cylinder array from the side surface after being focused to irradiate the gold nanoparticles in the suspension solution, and the multi-phase interface transient state formed after the gold nanoparticles are irradiated by the laser pulses is observed in a dark field environment. The device can carry out high-resolution dark field observation on the nanoscopic multiphase interface transient state generated in the microcolumn array and can control the temperature of the microcolumn array. The invention also provides a nanoscopic multiphase interface transient observation method based on the laser effect.
Description
Technical Field
The invention belongs to the technical field of micro-scale observation. More specifically, the invention relates to a nanoscopic multiphase interface transient observation device based on laser action and a method thereof.
Background
The noble metal nano particles can become an ideal nano heat source when emitting light under the action of the plasma resonance wavelength. The large amount of energy of the femtosecond laser pulse can produce an intense, transient and limited temperature rise around the luminescent plasmonic nanoparticles, eventually leading to transient bubble nucleation. The first application of plasmon-induced Microbubbles (MBs) involves generating surface MB on a metal film as an effective lens for surface plasmon waves in a microfluidic environment. In this configuration, the plasmon resonance of the nanoparticle assembly is located around 530 nm. When such systems are illuminated locally at this wavelength, efficient light absorption occurs at the glass-water interface where the nanoparticles reside, which can produce a temperature increase in the surrounding water. If the light intensity is strong enough, MB is generated at the interface.
Through the surface plasmon effect of the gold nanoparticles, the laser pulse duration and the laser power of the relationship between the surface resonance frequency intensity and the irradiation time power are measured, and bubbles can be generated and maintained without melting the nanorods. Photothermal processes at this power and pulse duration.
The following bottleneck problems exist for the nanoscopic scale multiphase interface transient observation:
1. transient analysis methods and test approaches for characterizing material properties at the macro-scale are no longer applicable at the nano-scale.
2. The nano-scale observation means such as SEM, TEM and FIB need to observe the solid sample in a high-cleanness environment.
3. Transient processes occur often on the order of picoseconds at nanoscopic multiphase interfaces.
4. Bright field microscopy observation achieves at best sub-micron resolution, subject to diffraction limits and working distance limitations.
5. And in the process of observing the multi-phase interface transient state, the position of an observed object is not easy to capture and control.
6. Finite element models on a macroscopic scale (such as hydrodynamic NS equations) are often limited in nanoscale by challenges that do not hold up to continuity assumptions.
And the nanoscopic multiphase interface molecular dynamics model lacks effective experimental data support, and model correction can be performed only through static macroscopic physical quantities.
Disclosure of Invention
An object of the present invention is to solve at least the above problems and/or disadvantages and to provide at least the advantages described hereinafter.
It is still another object of the present invention to provide a nanoscopic multiphase interface transient observation device based on laser action, which can perform high-resolution dark field observation on nanoscopic multiphase interface transients generated in a microcolumn array, and at the same time, can control the temperature of the microcolumn array, thereby improving experimental efficiency.
Still another object of the present invention is to provide a method for observing a nanoscopic multiphase interface transient state based on a laser effect, which can obtain a nanoscopic multiphase interface with high resolution and can easily capture an observed object.
To achieve these objects and other advantages and in accordance with the purpose of the invention, as embodied and broadly described herein, there is provided a nanoscopic multiphase interface transient observation device based on laser action, comprising:
the micro-needle fin heat dissipation structure chip is placed on the microscopic detection scanning platform, a micro-column array, a lens structure connected with the micro-column array and an optical fiber coupler used for connecting one end of an optical fiber are arranged in the micro-needle fin heat dissipation structure chip, wherein a micro-channel of the micro-column array is communicated with a suspension solution containing gold nanoparticles, and the micro-needle fin heat dissipation structure chip and the microscopic detection scanning platform are placed in a cassette;
and the laser pulse emitted by the double-pulse-width laser directly aligns to the lens structure under the action of the optical fiber coupler through the optical fiber, enters the micro-column array from the side after being focused, irradiates the gold nanoparticles in the suspension solution, and observes a multiphase interface transient state formed after the gold nanoparticles are irradiated by the laser pulse through a microscope in a dark field environment.
Preferably, the nanoscopic multiphase interface transient observation device based on laser action further includes:
the optical fiber is a Y-shaped optical fiber, a third end of the Y-shaped optical fiber is connected to the first spectrometer, the surface of the gold nanoparticle is irradiated and excited by laser pulse to generate a Raman scattering signal, and the generated Raman scattering signal returns to the first spectrometer through the Y-shaped optical fiber so as to monitor the spectrum of the backscattered light;
and the high-speed camera is connected with the first interface of the microscope beam splitter and is used for shooting the multiphase interface transient state formed after the gold nanoparticles are irradiated by the laser pulse.
Preferably, the nanoscopic multiphase interface transient observation device based on laser action further includes:
the second spectrometer is connected with the second interface of the microscope beam splitter, the surface of the gold nanoparticle is irradiated and excited by laser pulse to generate a Raman scattering signal, and the generated Raman scattering signal enters the second spectrometer through the second interface of the microscope beam splitter so as to monitor the spectrum of forward scattered light;
and the high-speed camera is connected with the first interface of the microscope beam splitter and is used for shooting the multiphase interface transient state formed after the gold nanoparticles are irradiated by the laser pulse.
Preferably, the nanoscopic multiphase interface transient observation device based on laser action further includes:
the optical fiber is a Y-shaped optical fiber, a third end of the Y-shaped optical fiber is connected to the first spectrometer, the surface of the gold nanoparticle is irradiated and excited by laser pulse to generate a Raman scattering signal, and the generated Raman scattering signal returns to the first spectrometer through the Y-shaped optical fiber so as to monitor the spectrum of the backscattered light;
the second spectrometer is connected with the second interface of the microscope beam splitter, the surface of the gold nanoparticle is irradiated and excited by laser pulse to generate a Raman scattering signal, and the generated Raman scattering signal enters the second spectrometer through the second interface of the microscope beam splitter so as to monitor the spectrum of forward scattered light;
and the high-speed camera is connected with the first interface of the microscope beam splitter and is used for shooting the multiphase interface transient state formed after the gold nanoparticles are irradiated by the laser pulse.
Preferably, the nanoscopic multiphase interface transient observation device based on the laser effect, the microneedle fin heat dissipation structure chip is arranged in the following manner: the micro-needle fin heat dissipation structure chip comprises an upper chip and a lower chip, a groove is arranged in the middle of the upper surface of the lower chip, a plurality of micro-column arrays which are arranged in order are arranged in the groove, and the lens structure and the optical fiber coupler are sequentially arranged beside the groove; and plating a metal layer of chromium and gold on the lower surface of the upper chip so as to be combined with the lower chip.
Preferably, the nanoscopic multiphase interface transient observation device based on laser action is characterized by further comprising a dielectrophoresis control loop, which comprises: the micro-column array comprises a first plane microelectrode arranged on the upper interface of the micro-column array, a second plane microelectrode arranged on the lower interface of the micro-column array and an alternating current power supply; one end of the alternating current power supply is connected with the first planar microelectrode, and the other end of the alternating current power supply is connected with the alternating current power supply of the second planar microelectrode; the first planar microelectrode, the second planar microelectrode and the alternating current power supply form a control loop, and gold nanoparticles suspended in flowing liquid in the micro-channel are gathered in an objective observation area of the microscope and kept still.
Preferably, the nanoscopic multiphase interface transient observation device based on the laser effect further comprises a base in a groove shape, the microneedle fin heat dissipation structure chip is just arranged in the groove of the base to keep balance and stability, wherein openings are arranged on two opposite groove edges of the base so that the optical fiber can pass through the openings to be connected with the optical fiber coupler; the middle positions of the other two opposite sides of the base are respectively concave inwards to form notches, so that the bottom surface of the micro-needle fin heat dissipation structure chip can be connected with the outside.
Preferably, the nanoscopic multiphase interface transient observation device based on the laser effect is characterized in that a suspension solution containing gold nanoparticles is introduced into a micro channel of the micro-column array, and the specific setting mode is as follows: a cooling system is provided, the cooling system comprising:
a liquid storage tank storing a suspension solution containing gold nanoparticles;
the liquid phase pump is connected with the liquid storage tank;
a water inlet and a water outlet, which are arranged on the lower chip and are positioned below the micro-column array, wherein a first water pipe connected with the liquid phase pump is connected to the water inlet through a notch on the base;
the collecting groove is connected with a second water pipe, and the second water pipe is connected to the water outlet through another notch on the base;
and the suspension solution in the liquid storage tank enters a micro channel of the micro-column array through the water inlet under the action of the liquid phase pump, cools the micro-needle fin heat dissipation structure chip, and then enters the collecting tank from the water outlet.
Preferably, the nanoscopic multiphase interface transient observation device based on the laser effect, the thicknesses of the upper chip and the lower chip are both 0.35mm, the micro-cylinder array is uniformly arranged in a size of 5 × 10, the micro-cylinders in the micro-cylinder array are in any one or more of a hexagon, a circle, a square or a triangle, the lens structure is a three-sided cylindrical mirror, the optical fiber coupler is a long wedge-shaped optical fiber coupler, the base is made of polytetrafluoroethylene, the second plane arranged on the lower interface of the micro-cylinder array is a micro-electrode array, and the number of the second plane is 5-10.
Preferably, the nanoscopic multiphase interface transient observation device based on the laser effect is characterized in that the wavelength of the double-pulse-width laser is 532nm, the picosecond pulse width is 20ps, the nanosecond pulse width is 10ns, the seed source output power is 10mW, the first spectrometer and the second spectrometer acquire spectral images by using the minimum gate width of 8ms, and the microscope adopts a 5-time objective lens and a 20-time objective lens.
Preferably, the nanoscopic multiphase interface transient observation device based on laser action connects the first spectrometer, the second spectrometer and the high-speed camera to a computer respectively, so as to observe a spectrogram and a recorded multiphase interface transient image on the computer.
The object of the invention can be further realized by a nanoscopic multiphase interface transient observation method based on laser action, which comprises the following steps:
adjusting the microscope, and starting the high-speed camera to clearly observe an image on the computer;
placing the micro-needle fin heat radiation structure chip and the microscopic detection scanning platform in a cassette;
starting a liquid phase pump to pump out the suspension solution containing the gold nanoparticles from the storage tank and enter a micro-channel of the micro-column array;
starting a double-pulse-width laser, firstly irradiating the gold nanoparticles in the micro-column array micro-channel by using a first beam of picosecond laser pulse, causing the gold nanoparticles to be distorted in a high-power peak value short time, then irradiating the gold nanoparticles by using a second beam of nanosecond laser pulse, and irradiating weak laser power to form a signal;
recording the surface appearance and the contact surface of the gold nanoparticles to generate picosecond scale transient change by using a high-speed camera; and (3) collecting a backward scattering Raman spectrum with a picosecond response rate through a first spectrometer, and/or collecting a forward scattering Raman spectrum with a picosecond response rate through a second spectrometer, and analyzing the transient change of the gold nanoparticle form.
Preferably, the nanoscopic multiphase interface transient observation method based on the laser effect comprises the following steps of:
adjusting the focusing of a lens at the front end of the 20-time objective lens to align the 20-time objective lens to a region to be detected and observe a clear image on a host;
observing a visual field range of 200 Mum multiplied by 200 Mum by using an optical fiber with a core diameter of 1000 Mum and a 5-time objective lens, and then observing a visual field range of 40 Mum multiplied by 40 Mum by using the optical fiber with the core diameter of 200 Mum and the 5-time objective lens;
then, the field of view of 50 μm.times.50 μm was observed using an optical fiber having a core diameter of 1000 μm and a 20-fold objective lens, and then the field of view of 10 μm.times.10 μm was observed using an optical fiber having a core diameter of 200 μm and a 20-fold objective lens.
The invention at least comprises the following beneficial effects:
the micro-pin fin heat dissipation structure chip is internally provided with a micro-column array, a lens structure connected with the micro-column array and an optical fiber coupler used for connecting one end of an optical fiber, namely, the optical fiber coupler, the lens structure and the micro-column array are integrated on the micro-pin fin heat dissipation structure chip to form a whole. Laser pulses through the optical fibers can directly aim at and focus into the micro-column array from the side face of the micro-needle fin heat dissipation structure chip, and irradiate the suspension solution containing the gold nanoparticles. By the design, the light path is stable, and the experimental efficiency can be greatly improved. The microneedle fin heat dissipation structure chip and the microscopic detection scanning platform are placed in a cassette, namely, observed in a dark field environment. And under a dark field environment, picosecond laser irradiation is adopted to enable the gold nanoparticles to maintain a metastable thermal equilibrium state. Because laser pulses enter the micro-column array from the side surface, by adopting the oblique illumination mode, excellent imaging contrast can be obtained through the spatial separation of incident light and scattered light of a sample, and the resolution ratio of the gold nanoparticles can be improved by 2-3 orders of magnitude. In addition, by analyzing raman spectra of forward scattering and backward scattering, the morphology of gold nanoparticles can be studied in depth.
And secondly, a suspension solution containing gold nanoparticles is communicated in a micro-channel of the micro-column array and is realized through a cooling system, so that the temperature in the micro-column cavity can be controlled at high precision. Therefore, the high-heat-conductivity and high-transparency micro-needle fin heat dissipation structure chip can control the temperature in the micro-flow chamber and can perform high-resolution dark-field observation on the gas-liquid interface in the micro-flow chamber. And the dielectrophoresis control loop is arranged to control the movement of the gold nanoparticles.
And thirdly, for the scattering of light caused by the nonuniformity of the gas-liquid phase interface, reconstructing the three-dimensional morphology of bubbles on the surface of the gold nanoparticles by high-speed microscopic photography, spectrometer spectral analysis and calculation software on a computer in a dark field environment, realizing three-dimensional super-resolution imaging of the nanoscale solid-liquid-gas heat transfer interface and providing a basis for the verification of a molecular dynamics model. The observation problem of the nano-scale heat transfer interface morphology in the field of heat transfer research is solved, and a brand new observation means is explored for the micro-nano-scale heat transfer basic research.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Drawings
FIG. 1 is a schematic structural diagram of a nanoscopic multiphase interface transient observation device based on laser action according to an embodiment of the present invention;
FIG. 2 is a schematic diagram illustrating the relationship between the structures of a nanoscopic multiphase interface transient observation device based on laser action according to an embodiment of the present invention;
fig. 3 is a schematic structural diagram of a microneedle fin heat dissipation structure chip in a nanoscopic multiphase interface transient observation device based on laser action according to an embodiment of the present invention;
FIG. 4 is a schematic diagram illustrating the structural relationship of an intermediate electrophoresis control loop of a nanoscopic multiphase interface transient observation device based on laser action according to an embodiment of the present invention;
FIG. 5 is a schematic structural diagram of a base in a nanoscopic multiphase interface transient observation device based on laser action according to another embodiment of the present invention;
FIG. 6 is a top view of a laser pulse passing through a lens structure in a nanoscopic multiphase interface transient observation device based on laser action according to another embodiment of the present invention;
fig. 7 is a side view of a laser pulse passing through a lens structure in a nanoscopic multiphase interface transient observation device based on laser action according to another embodiment of the present invention.
Detailed Description
The present invention is further described in detail below with reference to the attached drawings so that those skilled in the art can implement the invention by referring to the description text.
It will be understood that terms such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
As shown in fig. 1 to 3, an embodiment of the present invention provides a nanoscopic multiphase interface transient observation device based on laser effect, including: a micro-needle fin heat dissipation structure chip 1, which is placed on a microscopic detection scanning platform 210, wherein a micro-column array 110, a lens structure 120 connected with the micro-column array 110, and an optical fiber coupler 130 for connecting one end of an optical fiber 3 are arranged in the micro-needle fin heat dissipation structure chip 1, wherein a micro-channel between micro-columns in the micro-column array 110 is communicated with a suspension solution containing gold nanoparticles, and the micro-needle fin heat dissipation structure chip 1 and the microscopic detection scanning platform 210 are placed in a cassette 4; the double-pulse-width laser 5 is connected with the other end of the optical fiber 3, laser pulses emitted by the double-pulse-width laser 5 directly aim at the lens structure 120 through the optical fiber 3 under the action of the optical fiber coupler 130 to be focused and then enter the micro-column array 110 from the side surface, and irradiate gold nanoparticles in a suspension solution; and under a dark field environment, observing a multiphase interface transient state formed after the gold nanoparticles are irradiated by laser pulses through a microscope.
When the double-pulse-width laser 5 is used for irradiating the gold nanoparticles, short-pulse-width laser pulses are firstly excited to generate signals, long-pulse-width laser pulses are secondarily excited to achieve signal enhancement, a light source adopted by the double-pulse-width laser is a double-pulse-width seed source (ps, ns), the wavelength is 532nm, the picosecond pulse width is 20ps, the nanosecond pulse width is 10ns, and the seed source output power is 10 mW. After laser pulses generated by the double-pulse-width laser pass through the lens structure 120, the laser pulses are converged to a certain extent from a top view as shown in fig. 6, and are diverged to a certain extent from a side view as shown in fig. 7, so that irradiation excitation can be well performed on gold nanoparticles in a suspension solution.
In the above embodiment, the micropin fin heat dissipation structure chip 1 is provided with the micropin array 110, the lens structure 120 connected to the micropin array, and the optical fiber coupler 130 for connecting an end of the optical fiber, that is, the optical fiber coupler 130, the lens structure 120, and the micropin array 110 are integrated on the micropin fin heat dissipation structure chip 1. The laser pulse passing through the optical fiber 3 can be directly aligned and focused to enter the micro-column array 110 to irradiate the gold nanoparticles, so that the light path is stable, and the experimental efficiency is greatly improved. The coolant for cooling the micropin fin heat dissipation structure chip 1 is provided in the micro flow channel of the micropin array 110, and the temperature in the micropin chamber can be controlled with high accuracy. The microneedle fin heat dissipation structure chip and the microscopic detection scanning platform are placed in a cassette, namely, observed in a dark field environment. And under a dark field environment, picosecond laser irradiation is adopted to enable the gold nanoparticles to maintain a metastable thermal equilibrium state. Because laser pulses enter the micro-column array from the side surface, by adopting the oblique illumination mode, excellent imaging contrast can be obtained through the spatial separation of incident light and scattered light of a sample, and the resolution ratio of the gold nanoparticles can be improved by 2-3 orders of magnitude.
In order to obtain a spectrum of backscattered light generated after the gold nanoparticles are excited by laser pulse irradiation and record a formed multiphase interface transient image, in one embodiment, the nanoscopic multiphase interface transient observation device based on laser action further includes: the optical fiber 3 is a Y-shaped optical fiber, the third end of the Y-shaped optical fiber is connected to the first spectrometer 6, the surface of the gold nanoparticle is irradiated and excited by laser pulse to generate a Raman scattering signal, and the generated Raman scattering signal returns to the first spectrometer 6 through the Y-shaped optical fiber so as to monitor the spectrum of the backscattered light; and the high-speed camera 7 is connected with the first interface 221 of the optical splitter 220 of the microscope 2 and is used for shooting the multiphase interface transient state formed after the gold nanoparticles are irradiated by the laser pulse.
In the above embodiment, the optical fiber is set as a Y-type optical fiber, the laser pulse generated by the double-pulse-width laser excites the surface of the gold nanoparticle to generate a raman scattering signal, and simultaneously, the scattering signal returns to the first spectrometer as it is, and the spectrum of the backscattered light is detected. In specific operation, the high-speed camera 7 takes image parameters of an observation object at a frame rate of 340fps using pixels 2048 × 1048. The first spectrometer 6 collects spectral images using a minimum gate width of 8ms, and the objective 230 of the microscope 2 uses a 5-fold objective and a 20-fold objective.
In order to obtain the spectrum of the forward scattered light generated after the gold nanoparticles are excited by the laser pulse irradiation, as shown in fig. 2, in one embodiment of the present invention, the nanoscopic multiphase interface transient observation device based on laser action further includes: and the second spectrometer 11 is connected with the second interface 222 of the microscope beam splitter 220, the surface of the gold nanoparticle is irradiated and excited by laser pulse to generate a raman scattering signal, and the generated raman scattering signal enters the second spectrometer 11 through the second interface 222 of the microscope beam splitter 220 so as to monitor the spectrum of the forward scattering light. The second spectrometer is connected to the second interface 222 of the microscope spectrometer 220 to collect the vertically scattered light, and the spectrometer 220 can divide the vertically scattered light into "0, 100%", "100%, 0", "50%, 50%", and collect the spectral and image parameters, respectively.
In one embodiment, as shown in fig. 2, the nanoscopic multiphase interface transient observation device based on laser action further includes: the optical fiber 3 is a Y-shaped optical fiber, the third end of the Y-shaped optical fiber is connected to the first spectrometer 6, the surface of the gold nanoparticle is irradiated and excited by laser pulse to generate a Raman scattering signal, and the generated Raman scattering signal returns to the first spectrometer 6 through the Y-shaped optical fiber so as to monitor the spectrum of the backscattered light; the second spectrometer 11 is connected with the second interface 222 of the microscope beam splitter 220, the surface of the gold nanoparticle is irradiated and excited by laser pulse to generate a raman scattering signal, and the generated raman scattering signal enters the second spectrometer 11 through the second interface 222 of the microscope beam splitter 220 so as to monitor the spectrum of the forward scattering light;
in the above embodiment, both the spectrum of the backward scattering light and the spectrum of the forward scattering light can be obtained, so that the obtained spectral data are more comprehensive, and a sufficient data source is provided for further analysis and research.
In order to facilitate the arrangement of the micro-pillar array 110, the lens structure 120 and the optical fiber coupler 130 in the micro-pin fin heat dissipation structure chip, in a specific embodiment of the present invention, the nano-observation multiphase interface transient observation device based on a laser effect is specifically arranged in the manner that: the micro pin fin heat dissipation structure chip 1 comprises an upper chip 101 and a lower chip 102, a groove is arranged in the middle of the upper surface of the lower chip 102, a plurality of micro columns which are arranged in order are arranged in the groove, and the lens structure 120 and the optical fiber coupler 130 are sequentially arranged beside the groove; and plating a chromium and gold metal layer on the lower surface of the upper chip 101, and combining the lower chip with a gold coating of chromium, gold and gold 20+200nm by a gold-gold bonding process. In the specific manufacturing process, the thicknesses of the upper chip and the lower chip are both 0.35mm, the micro-cylinder array 110 is uniformly arranged by 5 × 10, the micro-cylinders are in any shape of hexagon, circle, square or triangle, the lens structure 120 is a three-sided cylindrical mirror, and the optical fiber coupler 130 is a long wedge-shaped optical fiber coupler. The thickness of the microneedle fin heat sink structure chip 1, the number of the micro pillars, and the shape of the micro pillars are not limited to those exemplified in the present embodiment, and the parameters listed in the present embodiment may be preferred parameters.
In one embodiment, as shown in fig. 4, the nanoscopic multiphase interface transient observation device based on laser effect further includes a dielectrophoresis control loop, which includes: a first planar microelectrode 12 arranged at the upper interface of the micropillar array 110, a second planar microelectrode 13 arranged at the lower interface of the micropillar array, and an alternating current power supply 14; one end of the alternating current power supply is connected with the first planar microelectrode 12, and the other end of the alternating current power supply is connected with the second planar microelectrode 14; the first planar microelectrode 12, the second planar microelectrode 13 and the alternating current power supply 14 form a control loop, and gold nanoparticles suspended in flowing liquid in the micro-channel are gathered in an observation area of an objective lens of the microscope and kept still.
In the above embodiment, since the gold nanoparticles are suspended in the flowing liquid, in order to keep the gold nanoparticles as immobile as possible and improve the experimental effect, the electrokinetic technique of dielectrophoresis is employed, and an alternating current electric field is used to aggregate the gold nanoparticles. Therefore, the gold nanoparticles suspended in the flowing liquid are gathered in the observation area of the objective lens and kept still by arranging the micro-thin plane electrodes on the upper and lower interfaces of the micro-channel. The second planar microelectrode 13 arranged on the lower interface of the micropillar array is a microelectrode array, the number of the microelectrode array is preferably 5-10, and the microelectrode array can be specifically arranged according to actual conditions. As to how to arrange the second planar microelectrode array on the lower interface of the micro channel, the embodiment of the present invention is not particularly limited as long as the function can be achieved, for example, a polytetrafluoroethylene plate 15 is arranged on each of the upper and lower interfaces of the microcolumn array, and the first planar microelectrode and the second planar microelectrode are arranged on the polytetrafluoroethylene plate 15.
In one embodiment, as shown in fig. 5, the nanoscopic multiphase interface transient observation device based on the laser effect further includes a base 8 in a groove shape, and the microneedle fin heat dissipation structure chip 1 is just disposed in the groove of the base 8 to keep balance and stability, so as to fix the microneedle fin heat dissipation structure chip 1. Wherein, openings 810 are provided on two opposite groove edges of the base 8, so that the optical fiber 3 can pass through the openings 810 to connect with the optical fiber coupler 130; the middle positions of the other two opposite sides of the base 8 are respectively concave inwards to form notches 820, so that the bottom surface of the micro-needle fin heat dissipation structure chip 1 can be connected with the outside, and the stability and balance of the micro-needle fin heat dissipation structure chip 1 can be ensured, for example, an electric wire connected with the second planar microelectrode is connected with an alternating current power supply through the notches 820. The base 8 is made of polytetrafluoroethylene, namely acrylic material.
In order to facilitate the control of the cooling liquid in the micro channels in the micro-pillar array, in one embodiment of the present invention, the nanoscopic multiphase interface transient observation device based on laser action is configured to set the cooling liquid for cooling the micro-needle fin heat dissipation structure chip in the micro channels between the micro-pillars in the micro-pillar array 110, and the specific configuration manner is as follows: a cooling system is provided, the cooling system comprising: a reservoir 910 storing a cooling liquid 960; a liquid phase pump 920 connected to the reservoir 910; a water inlet and outlet 140 (one of which is used as a water inlet and the other is used as a water outlet) which is arranged on the lower-layer microneedle fin heat dissipation structure chip 102 and is positioned below the micro-pillar array 110, and a first water pipe 930 connected with the liquid phase pump 920 is connected to the water inlet through a notch on the base 8; the collecting tank 940 is connected with a second water pipe 950, the second water pipe 950 is connected to the water outlet through another notch on the base 8, and when the collecting tank is specifically arranged, the water inlet and the water outlet can be connected with the first water pipe and the second water pipe through an M3 nut and an adapter port welded on the back of the lower microneedle fin heat dissipation structure chip; and the cooling liquid in the liquid storage tank enters a micro channel between the micro columns through the water inlet under the action of the liquid phase pump, cools the micro needle fin heat dissipation structure chip, and then enters the collecting tank from the water outlet. During specific operation, the micro-needle fin heat dissipation structure chip 1 is always kept horizontal, cooling liquid 960 (deionized water) is pumped out from the liquid storage tank 910 by a high-pressure liquid phase pump (XYYHY Y-600), the flow rate of the cooling liquid can be adjusted by changing the power of the cooling liquid, the cooling liquid enters the micro-flow channel after being accurately adjusted by a needle valve (Swagelok SS-1VS8) and is subjected to heat exchange, and finally the cooling liquid flows into the collection tank.
In one embodiment, the nanoscopic multiphase interface transient observation device based on laser action connects the first spectrometer 6, the second spectrometer 11 and the high-speed camera 7 to the computer 10 respectively, so as to observe a spectrogram and a recorded multiphase interface transient image on the computer 10. Connecting the high speed camera 7, the first spectrometer 6 and the second spectrometer 11 to the computer 10 also facilitates processing of spectrograms and images using computational tools on the host computer.
In another embodiment provided by the invention, the implementation of the nanoscopic multiphase interface transient observation method based on the laser effect is further provided, and the method comprises the following steps:
adjusting the microscope, turning on the high-speed camera 7 so that the image is clearly observed on the computer 10;
placing the micro-needle fin heat radiation structure chip 1 and the microscopic detection scanning platform 210 in a cassette 4;
starting the liquid phase pump 920 to pump out the suspension solution containing the gold nanoparticles from the storage tank and enter a micro-channel of the micro-column array;
starting a double-pulse-width laser 5, firstly irradiating the gold nanoparticles in the micro-column array micro-channel by using a first beam of picosecond laser pulse, causing the gold nanoparticles to be distorted in a high-power peak value short time, then irradiating the gold nanoparticles by using a second beam of nanosecond laser pulse, and irradiating with weak laser power to form a signal;
recording the surface appearance and the contact surface of the gold nanoparticles to generate picosecond scale transient change by using a high-speed camera 7; and (3) collecting backward scattering Raman spectrums with the picosecond response rate through the first spectrometer 6 and/or collecting forward scattering Raman spectrums with the picosecond response rate through the second spectrometer 11, and analyzing the transient changes of the gold nanoparticle forms.
In the above embodiment, a high-speed camera (Flare 2M360-CL) is combined with a microscope, a transparent glass cover plate bonded on the top of a micro flow channel is used to observe the boiling state of metal nano particles under the irradiation of laser pulses, all images are shot in a fixed window size with a sampling frequency of 340FPS, and data are processed and collected by CoreView software on a computer after being stacked and cached. The shooting observation is respectively carried out under the dark field environment and the natural light environment, the resolution can be improved under the dark field environment, and the resolution can be improved by one to two orders of magnitude. In the specific experimental process, CNN modeling analysis is carried out on the signals of the multiple gold nanoparticles subjected to repeated experiments, and the whole-process observation of the gold nanoparticle photothermal effect with the resolution of 20-50 picoseconds can be obtained.
In one embodiment, the nanoscopic multiphase interface transient observation method based on laser action comprises the following steps:
adjusting the focusing of a lens at the front end of the 20-time objective lens to align the 20-time objective lens to a region to be detected and observe a clear image on a computer;
observing a visual field range of 200 Mum multiplied by 200 Mum by using an optical fiber with a core diameter of 1000 Mum and a 5-time objective lens, and then observing a visual field range of 40 Mum multiplied by 40 Mum by using the optical fiber with the core diameter of 200 Mum and the 5-time objective lens;
then, the field of view of 50 μm.times.50 μm was observed using an optical fiber having a core diameter of 1000 μm and a 20-fold objective lens, and then the field of view of 10 μm.times.10 μm was observed using an optical fiber having a core diameter of 200 μm and a 20-fold objective lens.
The number of apparatuses and the scale of the process described herein are intended to simplify the description of the present invention. The application, modification and variation of the present nanoscopic multiphase interface transient observation device based on laser action will be apparent to those skilled in the art.
As described above, the invention can carry out high-resolution dark field observation on the nanoscopic multiphase interface transient state in the micro-column array, and can control the temperature in the micro-column array structure and improve the experimental efficiency.
While embodiments of the invention have been disclosed above, it is not intended to be limited to the uses set forth in the specification and examples. It can be applied to all kinds of fields suitable for the present invention. Additional modifications will readily occur to those skilled in the art. It is therefore intended that the invention not be limited to the exact details and illustrations described and illustrated herein, but fall within the scope of the appended claims and equivalents thereof.
Claims (12)
1. A nanoscopic multiphase interface transient observation device based on laser action is characterized by comprising:
the micro-needle fin heat dissipation structure chip is placed on a microscopic detection scanning platform, a micro-column array, a lens structure connected with the micro-column array and an optical fiber coupler used for connecting one end of an optical fiber are arranged in the micro-needle fin heat dissipation structure chip, wherein a suspension solution containing gold nanoparticles is communicated in a micro-channel of the micro-column array, the micro-needle fin heat dissipation structure chip and the microscopic detection scanning platform are placed in a cassette, and the micro-needle fin heat dissipation structure chip is arranged in a mode that: the micro-needle fin heat dissipation structure chip comprises an upper chip and a lower chip, a groove is arranged in the middle of the upper surface of the lower chip, a plurality of micro-column arrays which are arranged in order are arranged in the groove, and the lens structure and the optical fiber coupler are sequentially arranged beside the groove; plating a metal layer of chromium and gold on the lower surface of the upper chip so as to be combined with the lower chip;
and the laser pulse emitted by the double-pulse-width laser directly aligns to the lens structure under the action of the optical fiber coupler through the optical fiber, enters the micro-column array from the side after being focused, irradiates the gold nanoparticles in the suspension solution, and observes a multiphase interface transient state formed after the gold nanoparticles are irradiated by the laser pulse through a microscope in a dark field environment.
2. The laser-based nanoscopic multiphase interface transient observation device of claim 1, further comprising:
the optical fiber is a Y-shaped optical fiber, a third end of the Y-shaped optical fiber is connected to the first spectrometer, the surface of the gold nanoparticle is irradiated and excited by laser pulse to generate a Raman scattering signal, and the generated Raman scattering signal returns to the first spectrometer through the Y-shaped optical fiber so as to monitor the spectrum of the backscattered light;
and the high-speed camera is connected with a first interface of the microscope beam splitter and is used for shooting the multiphase interface transient state formed after the gold nanoparticles are irradiated by the laser pulse.
3. The laser-based nanoscopic multiphase interface transient observation device of claim 1, further comprising:
the second spectrometer is connected with a second interface of the microscope beam splitter, the surface of the gold nanoparticle is irradiated and excited by laser pulse to generate a Raman scattering signal, and the generated Raman scattering signal enters the second spectrometer through the second interface of the microscope beam splitter so as to monitor the spectrum of the forward scattering light;
and the high-speed camera is connected with the first interface of the microscope beam splitter and is used for shooting the multiphase interface transient state formed after the gold nanoparticles are irradiated by the laser pulse.
4. The laser-based nanoscopic multiphase interface transient observation device of claim 1, further comprising:
the optical fiber is a Y-shaped optical fiber, a third end of the Y-shaped optical fiber is connected to the first spectrometer, the surface of the gold nanoparticle is irradiated and excited by laser pulse to generate a Raman scattering signal, and the generated Raman scattering signal returns to the first spectrometer through the Y-shaped optical fiber so as to monitor the spectrum of the backscattered light;
the second spectrometer is connected with a second interface of the microscope beam splitter, the surface of the gold nanoparticle is irradiated and excited by laser pulse to generate a Raman scattering signal, and the generated Raman scattering signal enters the second spectrometer through the second interface of the microscope beam splitter so as to monitor the spectrum of the forward scattering light;
and the high-speed camera is connected with the first interface of the microscope beam splitter and is used for shooting the multiphase interface transient state formed after the gold nanoparticles are irradiated by the laser pulse.
5. A nanoscopic multiphase interface transient observation device based on laser action as recited in claim 1, further comprising a dielectrophoresis control loop comprising: the micro-column array comprises a first plane microelectrode arranged on the upper interface of the micro-column array, a second plane microelectrode arranged on the lower interface of the micro-column array and an alternating current power supply; one end of the alternating current power supply is connected with the first planar microelectrode, and the other end of the alternating current power supply is connected with the alternating current power supply of the second planar microelectrode; the first planar microelectrode, the second planar microelectrode and the alternating current power supply form a control loop, and gold nanoparticles suspended in flowing liquid in the micro-channel are gathered in an objective observation area of the microscope and kept still.
6. The laser-based nanoscopic multiphase interface transient observation device of claim 5, further comprising a base having a groove shape, wherein the micro-pin fin heat dissipation structure chip is disposed right inside the groove of the base to keep balance and stability, wherein openings are disposed on two opposite groove edges of the base for the optical fiber to pass through the openings to connect to the optical fiber coupler; the middle positions of the other two opposite sides of the base are respectively concave inwards to form notches, so that the bottom surface of the micro-needle fin heat dissipation structure chip can be connected with the outside.
7. The device for observing the transient state of the nanoscopic multiphase interface based on the laser effect as claimed in claim 6, wherein a suspension solution containing gold nanoparticles is passed through the micro flow channels of the micro-column array, and the specific setting mode is as follows: a cooling system is provided, the cooling system comprising:
a liquid storage tank storing a suspension solution containing gold nanoparticles;
the liquid phase pump is connected with the liquid storage tank;
a water inlet and a water outlet, which are arranged on the lower chip and are positioned below the micro-column array, wherein a first water pipe connected with the liquid phase pump is connected to the water inlet through a notch on the base;
the collecting groove is connected with a second water pipe, and the second water pipe is connected to the water outlet through another notch on the base;
and the suspension solution in the liquid storage tank enters a micro channel of the micro-column array through the water inlet under the action of the liquid phase pump, cools the micro-needle fin heat dissipation structure chip, and then enters the collecting tank from the water outlet.
8. The nanoscopic multiphase interface transient state observation device based on the laser effect as claimed in claim 7, wherein the thickness of the upper chip and the lower chip is 0.35mm, the micro-cylinder array is uniformly arranged by 5 × 10, the shape of the micro-cylinder in the micro-cylinder array is any one or more of hexagon, circle, square or triangle, the lens structure is a three-sided cylindrical mirror, the optical fiber coupler is a long wedge-shaped optical fiber coupler, the material of the base is polytetrafluoroethylene, and the second plane micro-electrodes arranged on the lower interface of the micro-cylinder array are micro-electrode arrays, and the number of the second plane micro-electrodes is 5-10.
9. The laser-based nanoscopic multiphase interface transient observation device of claim 4, wherein said dual pulse width laser has a wavelength of 532nm, a picosecond pulse width of 20ps, a nanosecond pulse width of 10ns, a seed source output power of 10mW, said first spectrometer and said second spectrometer collect spectral images using a minimum gate width of 8ms, and said microscope uses a 5 x objective lens and a 20 x objective lens.
10. A nanoscopic multiphase interface transient viewing device as claimed in claim 9 wherein said first spectrometer, said second spectrometer and said high speed camera are each connected to a computer for facilitating observation of a spectrogram and recorded multiphase interface transient images on the computer.
11. The nanoscopic multiphase interface transient observation method based on the laser effect is applied to the nanoscopic multiphase interface transient observation device based on the laser effect, which is characterized by comprising the following steps of:
adjusting the microscope, and starting the high-speed camera to clearly observe an image on the computer;
placing the micro-needle fin heat radiation structure chip and the microscopic detection scanning platform in a cassette;
starting a liquid phase pump to pump out the suspension solution containing the gold nanoparticles from the storage tank and enter a micro-channel of the micro-column array;
starting a double-pulse-width laser, firstly irradiating the gold nanoparticles in the micro-column array micro-channel by using a first beam of picosecond laser pulse, causing the gold nanoparticles to be distorted in a high-power peak value short time, then irradiating the gold nanoparticles by using a second beam of nanosecond laser pulse, and irradiating weak laser power to form a signal;
recording the surface appearance and the contact surface of the gold nanoparticles to generate picosecond scale transient change by using a high-speed camera; and (3) collecting a backward scattering Raman spectrum with a picosecond response rate through a first spectrometer, and/or collecting a forward scattering Raman spectrum with a picosecond response rate through a second spectrometer, and analyzing the transient change of the gold nanoparticle form.
12. The method for transient observation of nanoscopic multiphase interfaces based on laser action according to claim 11, wherein said adjusting the microscope comprises:
adjusting the focusing of a lens at the front end of the 20-time objective lens to align the 20-time objective lens to a region to be detected and observe a clear image on a host;
observing a visual field range of 200 Mum multiplied by 200 Mum by using an optical fiber with a core diameter of 1000 Mum and a 5-time objective lens, and then observing a visual field range of 40 Mum multiplied by 40 Mum by using the optical fiber with the core diameter of 200 Mum and the 5-time objective lens;
then, the field of view of 50 μm.times.50 μm was observed using an optical fiber having a core diameter of 1000 μm and a 20-fold objective lens, and then the field of view of 10 μm.times.10 μm was observed using an optical fiber having a core diameter of 200 μm and a 20-fold objective lens.
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