Scanning micro-quality probe imaging technology
Through scanning micromass probe imaging technology, multi-point excitation of the quartz crystal oscillator is solved, and the problem of difficult to obtain regional information of the material surface micromass changes and viscoelastic distribution in the prior art is solved, and visual image information of micromass changes and viscoelastic changes is realized, which is suitable for the combination of various technical means.
Patent Information
- Application Number
- CN202411722723.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-28
- Publication Date
- 2025-03-18
- Estimated Expiration
- 2044-11-28
AI Technical Summary
The prior art is difficult to obtain regional information on the micromass changes and viscoelastic distribution of material surfaces, and cannot be visually expressed in an imaging manner.
Using scanning micromass probe imaging technology, the quartz crystal oscillator is multi-pointed excitation through very small electrodes to obtain the lattice micromass distribution, and visual image information of micromass changes and viscoelastic changes is obtained through computer processing.
It realizes non-invasive non-destructive testing, can obtain the distribution of micromass changes and viscoelastic changes in situ, provides reaction mechanisms in different regions, is suitable for the combination of multiple technical means, and is widely used in the fields of membrane deposition monitoring, electrochemical electrode processes, etc.
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Figure CN119643909A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the field of probe imaging technology, and in particular to a scanning micro-mass probe imaging technology. Background Art
[0002] Probe microscope is a kind of surface analysis tool, which obtains the surface information of the sample through the interaction between the probe and the sample surface. For example, scanning tunneling microscope: imaging by measuring the tunneling current between the probe and the sample; atomic force microscope: imaging by measuring the van der Waals force between the probe and the sample; Kelvin probe force microscope: imaging by measuring the Kelvin contact potential difference between the probe and the sample; magnetic force microscope: imaging by using the magnetic interaction between the probe and the sample; near-field optical scanning microscope: imaging by using the near-field optical effect; scanning electrochemical microscope: imaging by using the electrochemical information between the probe and the sample; thermal field scanning microscope: imaging by measuring the thermal interaction between the probe and the sample, etc. These probe microscopes have a wide range of applications in physics, chemistry, biology, materials science and microelectronics.
[0003] During physical or chemical processes, materials will undergo mass changes. For example, solidification, evaporation, condensation, sublimation, desorption, dissolution, synthesis reaction, decomposition reaction, substitution reaction, and oxidation-reduction reaction will cause the micro-mass on the surface of the material to increase, decrease, or remain unchanged, and may also cause the viscoelasticity of the material to change. By obtaining and analyzing these micro-mass and viscoelasticity change information, the physical and chemical process mechanism of the material can be inferred.
[0004] The acquisition of surface micro-mass and viscoelastic distribution information can enrich the analysis process, further reveal the mechanisms of materials that are not fully understood in physical and chemical processes, and help scientific research to more deeply understand the complexity of material changes. However, according to the results of literature research, there has been no research and report on this type of probe imaging technology.
[0005] Quartz crystal has piezoelectric properties, that is, when the quartz crystal is subjected to mechanical pressure, the charge center of its internal lattice will shift, resulting in polarization. Conversely, if an electric field is applied to the two electrodes of the quartz crystal, the chip will produce mechanical deformation, a phenomenon called the inverse piezoelectric effect. When an alternating electromagnetic field is applied to the surface of the quartz crystal, the chip will produce mechanical oscillations with a certain resonant frequency. When the surface of the quartz crystal adsorbs or desorbs substances, this mass change will cause the resonant frequency of the chip to change. By measuring the change in resonant frequency, the tiny mass changes and viscoelastic changes on the surface of the chip can be accurately detected. The quartz crystal microbalance technology generated by this principle has a measurement accuracy of nanograms, and the mass change that can be measured theoretically is equivalent to a fraction of a monolayer or atomic layer. This micromass sensor has a simple structure, low cost, and high sensitivity, and is widely used in the fields of chemistry and biology.
[0006] However, the existing technology can only obtain macroscopic and average surface quality change information, and cannot obtain multiple information such as the distribution of quality changes and non-uniformity in the region, nor can it be intuitively expressed in an imaging manner.
[0007] The present invention proposes a scanning micromass probe imaging technology, which uses very small electrodes (probes) to perform multi-point excitation on a quartz crystal oscillator that carries a sample to obtain dot matrix micromass distribution, and obtains visual image information of micromass changes through computers and other auxiliary equipment. Summary of the invention
[0008] The purpose of the present invention is to solve the technical problems existing in the prior art and to provide a scanning micro-mass probe imaging technology.
[0009] To achieve the above-mentioned purpose, the technical solution provided by the present invention is: a scanning micro-mass probe imaging technology, including a probe, a probe moving module, an optical microscopy measurement module, an oscillation excitation module, a probe position measurement module, a quartz crystal oscillator, an oscillation signal acquisition module, a high-speed switch, an integrated test cell, a software processing module, and a sample; the probe is placed vertically and has a dual-electrode mode with electrodes S1 and S2 at the top, and the sample is coated on the quartz crystal oscillator;
[0010] The probe is used to generate an electromagnetic field signal for exciting the micro-area oscillation of the quartz crystal oscillator and to receive the electromagnetic field signal for the oscillation attenuation of the quartz crystal oscillator;
[0011] The probe moving module can move in three directions: x, y, and z;
[0012] The optical microscopy measurement module is used to measure the vertical distance between the probe and the quartz crystal oscillator;
[0013] The oscillation excitation module is used to emit a high-frequency oscillation signal to excite the quartz crystal oscillator to generate micro-area oscillation via the probe;
[0014] The probe position measurement module is used to measure the probe position dot matrix coordinate information;
[0015] The high-speed switch is used to quickly cut off the excitation signal of the oscillation excitation module;
[0016] The oscillation signal acquisition module is used to collect the amplitude and oscillation frequency of the quartz crystal oscillator;
[0017] The integrated test cell is one of a gas phase test cell, a liquid phase test cell, an electrochemical test cell, and a photoelectrochemical test cell, and is used to provide a reaction environment for causing changes in the micro-mass Δm and the viscoelasticity ΔQ of the sample;
[0018] The software processing module embeds the envelope fitting equation, underdamping fitting equation, and Sauerbrey equation operation to obtain the Δm of the i×j lattice respectively. xiyj and ΔQ xiyj Information, where i is the number of test points in the x-axis direction, and j is the number of test rows in the y-axis direction; further processing is performed to obtain the distribution image of the micro-mass and dissipation factor of the surface sample of the quartz crystal oscillator.
[0019] Preferably, the oscillation excitation module emits a signal to the probe that is in accordance with the fundamental frequency f of the quartz crystal oscillator. 0 The same high-frequency oscillation signal is generated; when the probe gradually approaches the quartz crystal oscillator along the Z axis, the optical microscope measurement module displays and measures the relative position of the probe and the quartz crystal oscillator; when the probe contacts the quartz crystal oscillator, the probe movement module stops the probe approach; at this time, the probe top electrode S1 and electrode S2 convert the signal emitted by the oscillation excitation module into an electromagnetic field signal that excites the micro-region oscillation of the quartz crystal oscillator, and the oscillation signal acquisition module acquires the oscillation amplitude and frequency of the quartz crystal oscillator coated with the sample at this time; the probe position measurement module obtains the coordinate position (x i ,y j );
[0020] When the micro-area oscillation of the quartz crystal oscillator is stable, the high-speed switch quickly cuts off the oscillation excitation module signal. At this time, the process of the quartz crystal oscillator presents an under-damped attenuated electromagnetic field signal. The probe top electrode S1 and electrode S2 serve as the receiving electrodes of the electromagnetic field to receive the attenuated signal. The oscillation signal acquisition module receives the attenuated signal at a frequency not less than 2 times the fundamental frequency f. 0 The attenuation signal is collected at a sampling rate of , and the above steps are repeated by moving the probe in the x and y planes to obtain the Δm of the i×j point matrix xiyj and ΔQ xiyj The software processing module processes the information to obtain the distribution image of micro-mass and viscoelasticity of the sample on the surface of the quartz crystal.
[0021] Preferably, when the integrated test cell is a gas phase test cell, the quartz crystal oscillator coated with the sample is installed at the bottom of the gas phase test cell; a first joint and a second joint are provided on the gas phase test cell, and the research gas is introduced into the gas phase test cell through the first joint, and the research gas reacts with the sample to cause changes in micro-mass and viscoelasticity, and finally the gas is discharged from the second joint.
[0022] Preferably, when the integrated test cell is a liquid phase test cell, the quartz crystal oscillator coated with the sample is installed at the bottom of the liquid phase test cell, and a first joint and a second joint are provided on the liquid phase test cell. Liquid is introduced into the liquid phase test cell through the first joint, the liquid reacts with the sample to cause micro-mass changes, and finally the liquid is discharged from the second joint.
[0023] Preferably, when the integrated test cell is an electrochemical test cell, a transparent conductive oxide film is deposited on the surface of the quartz crystal oscillator, and the quartz crystal oscillator is installed at the bottom of the electrochemical test cell, and the sample is deposited on the quartz crystal oscillator in advance or deposited on the quartz crystal oscillator during the photoelectrochemical reaction process; a three-electrode system is arranged in the electrochemical test cell, and the three-electrode system is connected to an external electrochemical workstation.
[0024] Preferably, when the integrated test cell is a photoelectrochemical test cell, a transparent conductive oxide film is deposited on the surface of the quartz crystal oscillator, and the quartz crystal oscillator is installed at the bottom of the photoelectrochemical test cell, and the sample is deposited on the quartz crystal oscillator in advance or deposited on the quartz crystal oscillator during the electrochemical reaction process; a three-electrode system is arranged in the electrochemical test cell, and the three-electrode system is connected to an external electrochemical workstation; an external spectrometer emits a light beam to irradiate the sample, and simultaneously receives and analyzes the light beam reflected / transmitted back by the sample.
[0025] Preferably, the working electrode in the three-electrode system is a quartz crystal or a sample deposited on the surface of the quartz crystal; the counter electrode in the three-electrode system is one of the precious metal electrodes of gold, silver, platinum, palladium, iridium and their alloys; the reference electrode in the three-electrode system is one of the reference electrodes selected from the group consisting of a hydrogen electrode, a calomel electrode, a silver-silver chloride electrode, a mercury-mercury oxide electrode and a mercury-mercurous sulfate electrode; the transparent conductive oxide film is one of the group consisting of an indium tin oxide film, an aluminum-doped zinc oxide film, a fluorine-doped tin oxide film, an antimony-doped tin oxide film, a gallium-doped zinc oxide film, a zinc oxide film doped with other elements and a titanium oxide-based film.
[0026] Preferably, the electrode S1 and the electrode S2 are coils or metal sheets; the quartz crystal oscillator is a thin sheet of quartz material with piezoelectric properties.
[0027] Beneficial effects of the present invention:
[0028] The scanning micro-mass probe imaging technology in the present invention is a non-invasive non-destructive testing technology that does not affect the reaction system. It can perform multi-point, line and surface scanning to detect the micro-mass and viscoelastic properties of the sample. It can obtain the distribution of micro-mass changes and viscoelastic changes in situ, and obtain the reaction mechanism of different regions. It can be used in combination with a variety of technical means to obtain more reaction process information. It can be widely used in film deposition monitoring, electrochemical electrode processes, surface electrochemistry and catalytic electrochemistry, environmental monitoring, drug and biomolecule detection and other research. BRIEF DESCRIPTION OF THE DRAWINGS
[0029] The drawings described herein are used to provide further understanding of the present invention and constitute a part of the present invention. The exemplary embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute improper limitations on the present invention.
[0030] Figure 1 It is a schematic diagram of the overall structure of the present invention;
[0031] Figure 2 is a diagram of the top structure of the probe of the present invention;
[0032] Figure 3 is a schematic diagram of an electrochemical test cell in the present invention;
[0033] Figure 4 Schematic diagram of the photoelectrochemical test cell in the present invention;
[0034] Figure 5 It is the micro-mass and viscoelastic lattice image of the i×j lattice in the present invention.
[0035] Figure annotation:
[0036] 1-probe, 2-probe moving module, 3-optical microscopy measurement module, 4-oscillation excitation module, 5-probe position measurement module, 6-quartz crystal oscillator, 7-oscillation signal acquisition module, 8-high-speed switch, 9-integrated test cell, 10-software processing module, 11-sample, 12-inlet connector, 13-outlet connector, 14-electrochemical test cell, 15-transparent conductive oxide film, 16-counter electrode, 17-reference electrode, 18-electrochemical workstation, 19-spectrum tester. DETAILED DESCRIPTION
[0037] This section will describe in detail the specific embodiments of the present invention. The preferred embodiments of the present invention are shown in the accompanying drawings. The purpose of the accompanying drawings is to supplement the description of the text part of the specification with graphics, so that people can intuitively and vividly understand each technical feature and the overall technical solution of the present invention, but it cannot be understood as a limitation on the scope of protection of the present invention.
[0038] The present invention proposes a scanning micromass probe imaging technology, which uses very small electrodes (probes) to perform multi-point excitation on a quartz crystal oscillator that carries a sample, obtains the dot matrix micromass and viscoelastic distribution, and obtains visual image information of micromass changes and viscoelasticity through computers and other auxiliary equipment.
[0039] Reference Figure 1-Figure 5 The preferred embodiment of the present invention is a scanning micro-mass probe imaging technology, comprising a probe 1, a probe moving module 2, an optical microscopy measurement module 3, an oscillation excitation module 4, a probe position measurement module 5, a quartz crystal oscillator 6, an oscillation signal acquisition module 7, a high-speed switch 8, an integrated test cell 9, a software processing module 10, and a sample 11; the probe 1 is placed vertically and has a dual-electrode mode with electrodes S1 and S2 at the top, and the sample 11 is coated on the quartz crystal oscillator 6; the electrodes S1 and S2 are coils or metal sheets; the quartz crystal oscillator 6 is a thin sheet of quartz material with piezoelectric properties.
[0040] The probe 1 is used to generate an electromagnetic field signal for exciting the micro-region oscillation of the quartz crystal oscillator 6 and to receive an electromagnetic field signal for attenuating the oscillation of the quartz crystal oscillator 6;
[0041] The probe moving module 2 can move in three directions: x, y, and z;
[0042] The optical microscopic measurement module 3 is used to measure the vertical distance between the probe 1 and the quartz crystal oscillator 6;
[0043] The oscillation excitation module 4 is used to emit a high-frequency oscillation signal to excite the quartz crystal oscillator 6 to generate micro-area oscillation via the probe 1;
[0044] The probe position measurement module 5 is used to measure the position lattice coordinate information of the probe 1;
[0045] The high-speed switch 8 is used to quickly cut off the excitation signal of the oscillation excitation module 4;
[0046] The oscillation signal acquisition module 7 is used to collect the amplitude and oscillation frequency of the quartz crystal oscillator 6;
[0047] The integrated test cell 9 is one of a gas phase test cell, a liquid phase test cell, an electrochemical test cell 14, and a photoelectrochemical test cell, and is used to provide a reaction environment for causing changes in the micro-mass Δm and the viscoelasticity ΔQ of the sample 11;
[0048] The software processing module 10 embeds the envelope fitting equation, the underdamping fitting equation, and the Sauerbrey equation operation to obtain the Δm of the i×j lattice respectively. xiyj and ΔQ xiyj Information, where i is the number of test points in the x-axis direction, and j is the number of test rows in the y-axis direction; further processing is performed to obtain a distribution image of the micro-mass and dissipation factor of the surface sample 11 of the quartz crystal oscillator 6.
[0049] Example 1
[0050] When the integrated test cell 9 is a gas phase test cell, the quartz crystal oscillator 6 coated with the sample 11 is installed at the bottom of the gas phase test cell; the gas phase test cell is provided with a first joint 12 and a second joint 13, and the research gas is introduced into the gas phase test cell through the first joint 12, and the research gas reacts with the sample 11 to cause micro-mass changes, and finally the gas is discharged from the second joint 13.
[0051] In this embodiment, the oscillation excitation module 4 sends a signal to the probe 1 that is in accordance with the fundamental frequency f of the quartz crystal oscillator 6. 0 The same high-frequency oscillation signal; when the probe 1 gradually approaches the quartz crystal oscillator 6 along the Z axis, the optical microscope measurement module 3 displays and measures the relative position of the probe 1 and the quartz crystal oscillator 6; when the probe 1 contacts the quartz crystal oscillator 6, the probe moving module 2 stops the probe 1 from approaching; at this time, the top electrodes S1 and S2 of the probe 1 convert the signal emitted by the oscillation excitation module 4 into an electromagnetic field signal that excites the micro-region oscillation of the quartz crystal oscillator 6, and the oscillation signal acquisition module 7 acquires the oscillation amplitude and frequency of the quartz crystal oscillator 6 coated with the sample 11 at this time; the probe position measurement module 5 obtains the coordinate position (x i ,y j );
[0052] When the micro-area oscillation of the quartz crystal oscillator 6 is stable, the high-speed switch 8 quickly cuts off the signal of the oscillation excitation module 4. At this time, the process of the quartz crystal oscillator 6 presents an under-damped attenuated electromagnetic field signal. The top electrode S1 and the electrode S2 of the probe 1 receive the attenuated signal as the receiving electrodes of the electromagnetic field. The oscillation signal acquisition module 7 receives the attenuated signal at a frequency not less than 2 times the fundamental frequency f 0 The attenuation signal is collected at a sampling rate of 10, and the attenuation time constant t is obtained by the envelope fitting equation embedded in the software processing module 10. x1y1 , the frequency f is obtained by fitting the underdamped waveform equation x1y1 . Through Δf x1y1 =f 0 -f x1y1 , obtain the micro-area change frequency Δf x1y1 ; Then use the Sauerbrey equation to convert Δf x1y1 Transformed into the micro-mass change Δm of sample 11 x1y1 ; by ΔQ x1y1 =t x1y1 ×f x1y1 Obtain the dissipation factor ΔQ of the micro-region viscoelastic change x1y1 . Probe 1 is moved to the next position (x) by probe moving module 2 2 ,y 1 ), by repeating the above steps, we can obtain Δm x2y1 .
[0053] And so on, we can get y 1 Δm of the row xiy1 and ΔQ xiy1 , (i is the number of test points in the x-axis direction), change y j (j is the number of test rows in the y-axis direction), and finally we get Figure 5 Δm of the i×j lattice shown xiyj and ΔQ xiyj The information is used to form the i and j dot matrix. The software processing module 10 further processes and obtains the distribution image of the micro-mass and viscoelasticity of the sample 11 in the surface area of the quartz crystal oscillator 6.
[0054] Example 2
[0055] When the integrated test cell 9 is a liquid phase test cell, the quartz crystal oscillator 6 coated with the sample 11 is installed at the bottom of the liquid phase test cell. The liquid phase test cell is provided with a first joint 12 and a second joint 13. Liquid is introduced into the liquid phase test cell through the first joint 12. The liquid reacts with the sample 11 to cause micro-mass changes. Finally, the liquid is discharged from the second joint 13. The micro-mass imaging steps are the same as those in implementation 1.
[0056] Example 3
[0057] When the integrated test cell 9 is a photoelectrochemical test cell, a quartz crystal oscillator 6 with a transparent conductive oxide film 15 deposited on the surface is installed at the bottom of the photo / electrochemical test cell, and the sample 11 can be deposited on the quartz crystal oscillator 6 in advance or deposited on the quartz crystal oscillator 6 during the photo / electrochemical reaction process; a three-electrode system is arranged in the photo / electrochemical test cell 14, and the three-electrode system is connected to an external electrochemical workstation 18, and an external spectrometer 19 can emit a light beam to illuminate the sample 11, and at the same time receive and analyze the light beam reflected / transmitted back by the sample 11.
[0058] Example 4
[0059] When the integrated test cell 9 is an electrochemical test cell 14, a transparent conductive oxide film 15 is deposited on the surface of the quartz crystal oscillator 6 and installed at the bottom of the electrochemical test cell, and the sample 11 is deposited on the quartz crystal oscillator 6 in advance or deposited on the quartz crystal oscillator 6 during the electrochemical reaction process; a three-electrode system is arranged in the electrochemical test cell 14, and the three-electrode system is connected to an external electrochemical workstation 18.
[0060] Furthermore, the working electrode in the three-electrode system is a quartz crystal oscillator 6 or a sample 11 deposited on the surface of the quartz crystal oscillator 6; the counter electrode 16 in the three-electrode system is one of the precious metal electrodes of gold, silver, platinum, palladium, iridium and their alloy electrodes; the reference electrode 17 in the three-electrode system is a reference electrode selected from the group consisting of a hydrogen electrode, a calomel electrode, a silver-silver chloride electrode, a mercury oxide electrode and a mercury sulfate electrode; the transparent conductive oxide film 15 is an indium tin oxide (ITO) film, an aluminum-doped zinc oxide (AZO) film, a fluorine-doped tin oxide (FTO) film, an antimony-doped tin oxide (ATO) film, a gallium-doped zinc oxide (GZO) film, a zinc oxide (ZnO) film doped with other elements, a titanium oxide (TiO 2 ) is a kind of base film.
[0061] Furthermore, when the integrated test cell 9 is an electrochemical test cell 14 and a photoelectrochemical cell, the micromass imaging step is different from that in implementation 2 in that the imaging process is synchronously imaged during the electrochemical process under the control of the electrochemical workstation 18, and the remaining principles and steps are the same as those in implementation 1.
[0062] The scanning micro-mass probe imaging technology in the present invention is a non-invasive non-destructive testing technology that does not affect the reaction system. It can perform multi-point, line and surface scanning to detect the micro-mass and viscoelastic properties of the sample, obtain the distribution of micro-mass changes and viscoelastic changes in situ, and obtain the reaction mechanism of different regions. It can be used in combination with a variety of technical means to obtain more reaction process information and can be widely used in film deposition monitoring, electrochemical electrode processes, surface electrochemistry and catalytic electrochemistry, environmental monitoring, drug and biomolecule detection and other research.
[0063] Under the premise that no conflict occurs, those skilled in the art may freely combine and superimpose the above-mentioned additional technical features.
[0064] The above description is only a preferred implementation mode of the present invention. Any technical solution that achieves the purpose of the present invention by substantially the same means belongs to the protection scope of the present invention.
Claims
1. A scanning micro-mass probe imaging technology, characterized in that: The invention comprises a probe (1), a probe moving module (2), an optical microscopic measurement module (3), an oscillation excitation module (4), a probe position measurement module (5), a quartz crystal oscillator (6), an oscillation signal acquisition module (7), a high-speed switch (8), an integrated test cell (9), a software processing module (10), and a sample (11); the probe (1) is placed vertically and has a dual-electrode mode with an electrode S1 and an electrode S2 at the top, and the sample (11) is coated on the quartz crystal oscillator (6); The probe (1) is used to generate an electromagnetic field signal for exciting the micro-region oscillation of the quartz crystal oscillator (6) and to receive the electromagnetic field signal of the oscillation attenuation of the quartz crystal oscillator (6); The probe moving module (2) can move in three directions: x, y and z. The optical microscopic measurement module (3) is used to measure the vertical distance between the probe (1) and the quartz crystal oscillator (6); The oscillation excitation module (4) is used to emit a high-frequency oscillation signal to excite the quartz crystal oscillator (6) via the probe (1) to generate micro-region oscillation; The probe position measurement module (5) is used to measure the position matrix coordinate information of the probe (1); The high-speed switch (8) is used to quickly cut off the excitation signal of the oscillation excitation module (4); The oscillation signal acquisition module (7) is used to collect the amplitude and oscillation frequency of the quartz crystal oscillator (6); The integrated test cell (9) is one of a gas phase test cell, a liquid phase test cell, an electrochemical test cell (14), and a photoelectrochemical test cell, and is used to provide a reaction environment for causing changes in the micro-mass Δm and the viscoelasticity ΔQ of the sample (11); The software processing module (10) embeds the envelope fitting equation, the underdamping fitting equation, and the Sauerbrey equation operation to obtain the Δm of the i×j lattice respectively. xiyj and ΔQ xiyj Information, wherein i is the number of test points in the x-axis direction and j is the number of test rows in the y-axis direction; and further processing is performed to obtain a distribution image of the micro-mass and dissipation factor of the surface sample (11) of the quartz crystal oscillator (6).
2. The scanning micro-mass probe imaging technique according to claim 1, characterized in that: The oscillation excitation module (4) sends a high-frequency oscillation signal to the probe (1) that is the same as the fundamental frequency f0 of the quartz crystal oscillator (6); when the probe (1) gradually approaches the quartz crystal oscillator (6) along the Z axis, the optical microscopic measurement module (3) displays and measures the relative position of the probe (1) and the quartz crystal oscillator (6); when the probe (1) contacts the quartz crystal oscillator (6), the probe moving module (2) stops the probe (1) from approaching; at this time, the top electrode S1 and the electrode S2 of the probe (1) convert the signal sent by the oscillation excitation module (4) into an electromagnetic field signal that excites the micro-region oscillation of the quartz crystal oscillator (6), and the oscillation signal acquisition module (7) acquires the oscillation amplitude and frequency of the quartz crystal oscillator (6) coated with the sample (11) at this time; the probe position measurement module (5) obtains the coordinate position (x i ,y j ); When the micro-region oscillation of the quartz crystal oscillator (6) is stable, the high-speed switch (8) quickly cuts off the signal of the oscillation excitation module (4). At this time, the process of the quartz crystal oscillator (6) presents an underdamped attenuated electromagnetic field signal. The top electrode S1 and the electrode S2 of the probe (1) receive the attenuated signal as the receiving electrodes of the electromagnetic field. The oscillation signal acquisition module (7) acquires the attenuated signal at a sampling rate of not less than 2 times the fundamental frequency f0. The above steps are repeated by moving the probe (1) in the x and y planes to obtain Δm of the i×j lattice. xiyj and ΔQ xiyj The software processing module (10) processes the information to obtain a distribution image of micro-mass and viscoelasticity occurring on the surface sample (11) of the quartz crystal oscillator (6).
3. The scanning micro-mass probe imaging technique according to claim 1, characterized in that: When the integrated test cell (9) is a gas phase test cell, a quartz crystal oscillator (6) coated with a sample (11) is installed at the bottom of the gas phase test cell; a first joint (12) and a second joint (13) are provided on the gas phase test cell, and a research gas is introduced into the gas phase test cell through the first joint (12), and the research gas reacts with the sample (11) to cause changes in micro-mass and viscoelasticity, and finally the gas is discharged through the second joint (13).
4. The scanning micro-mass probe imaging technique according to claim 1, characterized in that: When the integrated test cell (9) is a liquid phase test cell, the quartz crystal oscillator (6) coated with the sample (11) is installed at the bottom of the liquid phase test cell, and a first joint (12) and a second joint (13) are provided on the liquid phase test cell. Liquid is introduced into the liquid phase test cell through the first joint (12), the liquid reacts with the sample (11) to cause a micro-mass change, and finally the liquid is discharged through the second joint (13).
5. The scanning micro-mass probe imaging technique according to claim 1, characterized in that: When the integrated test cell (9) is an electrochemical test cell (14), a transparent conductive oxide film (15) is deposited on the surface of a quartz crystal oscillator (6), and the quartz crystal oscillator (6) is installed at the bottom of the electrochemical test cell. The sample (11) is deposited on the quartz crystal oscillator (6) in advance or is deposited on the quartz crystal oscillator (6) during a photoelectrochemical reaction process. A three-electrode system is provided in the electrochemical test cell (14), and the three-electrode system is connected to an external electrochemical workstation (18).
6. The scanning micro-mass probe imaging technique according to claim 1, characterized in that: When the integrated test cell (9) is a photoelectrochemical test cell, a transparent conductive oxide film (15) is deposited on the surface of a quartz crystal oscillator (6), and the quartz crystal oscillator (6) is installed at the bottom of the photoelectrochemical test cell. The sample (11) is deposited on the quartz crystal oscillator (6) in advance or deposited on the quartz crystal oscillator (6) during the electrochemical reaction process. A three-electrode system is arranged in the electrochemical test cell (14), and the three-electrode system is connected to an external electrochemical workstation (18). An external spectrum tester (19) emits a light beam to illuminate the sample (11), and simultaneously receives and analyzes a light beam reflected / transmitted back by the sample (11).
7. A scanning micro-mass probe imaging technique according to claim 5 or 6, characterized in that: The working electrode in the three-electrode system is a quartz crystal oscillator (6) or a sample (11) deposited on the surface of the quartz crystal oscillator (6); the counter electrode (16) in the three-electrode system is one of the precious metal electrodes of gold, silver, platinum, palladium, iridium and their alloy electrodes; the reference electrode (17) in the three-electrode system is one of the reference electrodes selected from the group consisting of a hydrogen electrode, a calomel electrode, a silver-silver chloride electrode, a mercury oxide electrode and a mercury sulfate electrode; and the transparent conductive oxide film (15) is one of the group consisting of an indium tin oxide film, an aluminum-doped zinc oxide film, a fluorine-doped tin oxide film, an antimony-doped tin oxide film, a gallium-doped zinc oxide film, a zinc oxide film doped with other elements and a titanium oxide-based film.
8. The scanning micro-mass probe imaging technique according to claim 1, characterized in that: The electrode S1 and the electrode S2 are coils or metal sheets; the quartz crystal oscillator sheet (6) is a thin sheet of quartz material with piezoelectric properties.
Citation Information
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