CN111024675A - Raman spectrum-confocal differential interference difference microscope combined analysis system - Google Patents
Raman spectrum-confocal differential interference difference microscope combined analysis system Download PDFInfo
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Abstract
The invention relates to a Raman spectrum-confocal differential interference difference microscope combined analysis system, which is characterized by comprising: the electrochemical in-situ reaction device is used for in-situ test in the electrode charging and discharging process and is provided with an optical window; the Raman spectrum system is used for realizing in-situ Raman spectrum testing of the electrochemical process of the electrode by irradiating the optical window; and the confocal differential interference difference microscope is used for acquiring optical imaging of the electrode in the electrochemical process by irradiating the optical window. The invention can realize in-situ Raman spectrum test and high-resolution optical imaging in the electrode process, and ensure synchronous detection of material structure and chemical components, thereby obtaining richer interface electrochemical reaction information.
Description
Technical Field
The invention relates to a Raman spectrum-confocal differential interference difference microscope combined analysis system which can synchronously analyze and detect chemical components and material structures in an electrode process in real time in situ and relates to the technical field of electrochemical energy storage devices.
Background
With the increasing prominence of energy problems, research and development of electrochemical energy storage technology have become hot spots, especially lithium ion batteries and secondary batteries such as sodium ions and potassium ions. Much research is currently focused on improving the cycle life and electrochemical performance of such batteries, and optimizing storage devices. The electrode/electrolyte interface is an important component of the secondary battery, systematically explores the reaction mechanism, the dynamic behavior and the decay mechanism of the electrochemical charge-discharge process of the battery interface, and is the premise for further improving the battery performance. However, the research of the work at home and abroad is flexible, most of research means are in an ex-situ characterization stage, and the microstructure or substance components of the interface electrochemical process cannot be detected in real time. How to carry out in-situ research on an electrode/electrolyte interface of a battery to obtain more accurate and reliable test data makes the problem to be solved urgently.
In recent years, confocal differential interference microscopy (LCM-DIM) has become a new optical microscopic imaging technology due to its advantages of high spatial resolution, high temporal resolution (scan speed 0.25 sec/frame), and non-interference in space, which are in the order of nanometer of Z axis. Therefore, the LCM-DIM can rapidly observe the dynamic process of the solid-liquid interface of the electrode/electrolyte on a nanometer scale in situ in real time.
However, the optical imaging technology with high resolution can only measure the surface topography of the sample, and cannot perform functional identification on the material composition by the in-situ technology of spectroscopy. Meanwhile, a single spectroscopy technology can only detect the substance elements or molecular structures of the sample to be detected in situ, but cannot monitor the microstructure of the sample in real time.
Disclosure of Invention
In view of the above problems, an object of the present invention is to provide a raman spectroscopy-confocal differential interference microscopy combined analysis system capable of efficiently characterizing the characteristics of a cell interface.
In order to achieve the purpose, the invention adopts the following technical scheme: a raman spectroscopy-confocal differential interference microscopy combined analysis system, the system comprising:
the electrochemical in-situ reaction device is used for in-situ test in the electrode charging and discharging process and is provided with an optical window;
the Raman spectrum system is used for realizing in-situ Raman spectrum testing of the electrochemical process of the electrode by irradiating the optical window to obtain the molecular structure and the chemical components of the working electrode under different voltages;
and the confocal differential interference difference microscope system is used for acquiring optical imaging of the electrode in the electrochemical process by irradiating the optical window.
In some embodiments of the present invention, the electrochemical in-situ reaction device comprises a first packaging shell, a second packaging shell and a flat cell; the first packaging shell and the second packaging shell are fixedly connected through bolts; the flat battery is fixedly arranged between the first shell and the second packaging shell, a working electrode of the flat battery is communicated with the second packaging shell, and a counter electrode of the flat battery is communicated with the first packaging shell.
In some embodiments of the present invention, the first package housing comprises a first insulating plate, a first conductive plate, a second insulating plate, and a first sealing ring; the second packaging shell comprises a second conductive plate, a third insulating plate, a quartz plate, a second sealing ring and a third sealing ring; the flat cell comprises a working electrode, a solid electrolyte membrane, a counter electrode and a pressurizing fixing piece;
the first insulating plate is fixedly connected with a first conductive plate, and a battery jar is arranged at the bottom of the first conductive plate; the pressurizing fixing piece, the counter electrode, the solid electrolyte membrane and the working electrode are arranged in the battery jar from top to bottom in sequence; a second insulating plate and a first sealing ring are arranged at the bottom of the first conducting plate positioned outside the battery jar;
the bottom of the second insulating plate is provided with the second conductive plate corresponding to the battery jar, and the second conductive plate is provided with a first optical window; the bottom of the second conductive plate is provided with the third insulating plate, and the third insulating plate is provided with a second window corresponding to the first optical window;
the quartz plate is arranged between the first optical window and the second optical window through a second sealing ring and a third sealing ring.
In some embodiments of the invention, the raman spectroscopy system comprises a laser light source, a first color filter, a dichroic mirror, a microscope objective, a first half mirror, a first lens, a second color filter, a first reflecting mirror, a second lens, a raman spectrometer and a CCD detector; the laser signal generated by the laser light source is transmitted to the dichroic mirror through the first color filter, the dichroic mirror splits the laser signal, the laser signal reflected by the dichroic mirror is transmitted to the microscope objective, the microscope objective faces the second optical window, the microscope objective focuses the laser signal on the working electrode, the Raman signal generated by the working electrode is collected by the microscope objective, then is reflected by the first semi-transparent semi-reflector through the dichroic mirror, and is coupled into the Raman spectrometer for Raman signal detection through the first lens, the second color filter, the first reflector and the second lens in sequence; the CCD detector is used for assisting in observing the surface of the working electrode.
In some embodiments of the present invention, the confocal differential interference difference microscope system includes an illumination source, a second reflecting mirror, a polarizer, a second half mirror, an optical system, a third reflecting mirror, a nomas prism, a confocal aperture pinhole, an analyzer, and a photomultiplier tube;
light emitted by the irradiation light source is reflected by the second reflecting mirror and enters the polarizer to generate linearly polarized light, linearly polarized light is reflected by the second semi-transparent semi-reflecting mirror and enters the optical system to adjust the direction of a light path, and the linearly polarized light is reflected by the third reflecting mirror to the Nomeski prism to be decomposed into two beams of light with mutually vertical polarization directions; two bunches of light penetrate first semi-transparent semi-reflecting mirror, dichroic mirror and microobjective in proper order and shine working electrode, two light beams that reflect through working electrode loop through microobjective, dichroic mirror and first semi-transparent semi-reflecting mirror and send to nomas prism, nomas prism makes two bunches of light compound collineations again, then passes through third speculum, optical system group, second semi-transparent semi-reflecting mirror, confocal diaphragm pinhole and analyzer in proper order and is received by photomultiplier, obtains working electrode's optical imaging through handling.
In some embodiments of the present invention, the laser light source has a wavelength of 532 nm.
In some embodiments of the present invention, the illumination source is a superluminescent light emitting diode.
Due to the adoption of the technical scheme, the invention has the following advantages:
1. the Raman spectrum-confocal differential interference difference microscope combined analysis system perfectly combines a Raman spectrometer system and a confocal differential interference difference microscope system, has the functions of a Raman spectrometer and high-resolution optical imaging, and can obtain related substance components at the same position while analyzing the surface appearance structure of a sample to be detected;
2. the invention aims at an electrochemical system in an energy storage device, and makes up for the in-situ characterization means of the electrode process and the vacancy of an in-situ electrochemical reaction device;
in conclusion, the method can realize in-situ tracking of high spatial resolution and high time resolution in the electrode process, and can realize synchronous monitoring of the interface structure and the corresponding species analysis, thereby obtaining richer electrochemical interface reaction information.
Drawings
The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Like reference numerals refer to like parts throughout the drawings. In the drawings:
FIG. 1 is a diagram of an optical path structure of a combined Raman spectroscopy-confocal differential interference microscopy analysis system according to this embodiment;
fig. 2 is a schematic structural diagram of the electrochemical in-situ reaction device according to the embodiment.
Detailed Description
Exemplary embodiments of the present invention will be described in more detail below with reference to the accompanying drawings. While exemplary embodiments of the invention are shown in the drawings, it should be understood that the invention can be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
It is to be understood that the terminology used herein is for the purpose of describing particular example embodiments only, and is not intended to be limiting. As used herein, the singular forms "a", "an" and "the" may be intended to include the plural forms as well, unless the context clearly indicates otherwise. The terms "comprises," "comprising," "including," and "having" are inclusive and therefore specify the presence of stated features, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, steps, operations, elements, components, and/or groups thereof. The method steps, processes, and operations described herein are not to be construed as necessarily requiring their performance in the particular order described or illustrated, unless specifically identified as an order of performance. It should also be understood that additional or alternative steps may be used.
As shown in fig. 1, the raman spectroscopy-confocal differential interference microscopy analysis system provided in this embodiment includes an electrochemical in-situ reaction device 1, a raman spectroscopy system, and a confocal differential interference microscopy system, wherein the electrochemical in-situ reaction device 1 is disposed on a test platform 2.
The electrochemical in-situ reaction device 1 is used for in-situ test in the electrode charging and discharging process and is provided with an optical window;
the Raman spectrum system is used for realizing in-situ Raman spectrum testing of the electrochemical process of the electrode by irradiating the optical window to obtain the molecular structure and the chemical components of the working electrode under different voltages;
the confocal differential interference difference microscope system is used for obtaining optical imaging of the electrochemical process of the electrode by irradiating the optical window to obtain the microstructure of the working electrode under different voltages.
Specifically, the raman spectroscopy system includes a laser light source 3, a color filter 4, a dichroic mirror 5, a microscope objective 6, a half mirror 7, a lens 8, a color filter 9, a reflecting mirror 10, a lens 11, a raman spectrometer 12, and a CCD detector 13.
Laser signals generated by a laser light source 3 are transmitted to a dichroic mirror 5 through a color filter 4, the dichroic mirror 5 splits the laser signals, the laser signals reflected by the dichroic mirror 5 are transmitted to a microscope objective 6, the microscope objective 6 is over against an optical window of the electrochemical in-situ reaction device 1 to be detected on the test bench 2, the microscope objective 6 focuses the laser signals on working electrodes of the electrochemical in-situ reaction device 1 to be detected, and meanwhile, a CCD detector 13 is used for assisting in observing the surfaces of the working electrodes. Incident light is scattered by substance molecules on the surface of the electrode, Raman spectrum signals scattered back are collected by the microscope objective 6 and then penetrate through the dichroic mirror 5, Raman signals transmitted by the dichroic mirror 5 are reflected by the semi-transparent semi-reflecting mirror 7, and are coupled into the Raman spectrometer 12 through the lens 8, the color filter 9, the reflecting mirror 10 and the lens 11 in sequence to be subjected to Raman signal detection, and the molecular structure and chemical components of the electrode to be detected under different voltages can be rapidly represented. Wherein, the dichroic mirror 5 is used for reflecting the laser signal and transmitting the Raman signal; the function of the half-transmitting and half-reflecting mirror 7 is to reflect the generated Raman signal; in addition, the microscope objective 6, the dichroic mirror 5 and the semi-transparent and semi-reflective mirror 7 are sequentially arranged below the test bench 2 from top to bottom, and the center lines of the microscope objective 6, the dichroic mirror 5 and the semi-transparent and semi-reflective mirror 7 are positioned on the same vertical line, so that the obtained raman signal can smoothly pass through the raman signal.
Specifically, the confocal differential interference contrast microscope system includes a superluminescent light emitting diode 14, a reflector 15, a polarizer 16, a half-mirror 17, an optical train 18, a reflector 19, a nomas prism 20, a confocal aperture 21, an analyzer 22, and a photomultiplier 23.
Light emitted by the superluminescent light emitting diode 14 is reflected by the reflecting mirror 15 to enter the polarizer 16, the polarizer 16 is used for enabling the light emitted by the superluminescent light emitting diode 14 to generate linear polarization, linearly polarized light is reflected by the semi-transmitting and semi-reflecting mirror 17 to enter the optical system 18 for adjusting the direction of an optical path, and then the linearly polarized light is reflected by the reflecting mirror 19 to be split into two beams of light with mutually vertical polarization directions through the Nomesis prism 20. The two beams of light sequentially penetrate through the half-mirror 7, the dichroic mirror 5 and the microscope objective 6 with a small transverse offset and enter the surface of a working electrode of the electrochemical in-situ reaction device 1 to be measured, because the height of an incident point is different to form an optical path difference, the two beams of light reflected by the working electrode sequentially pass through the microscope objective 6, the dichroic mirror 5, the half-mirror 7 and the Nomuski prism 20, the Nomuski prism 20 enables the two beams of light to be recombined and collinear, the light generates another part of optical path difference in the process of passing through the Nomuski prism, and then the light sequentially passes through the reflecting mirror 19, the optical system 18, the half-mirror 17, the confocal aperture pinhole 21 and the analyzer 22 to be received by the photomultiplier 23, wherein the analyzer 22 is used for combining the two beams of light into two beams of light with the same polarization direction to enable the two beams of light to interfere with each other, and at the moment, the phase difference formed by the two total optical path differences between the surface of a sample and the total optical path difference of the Nomuski Dark contrast, which reflects the difference between the surface structure and the convex-concave direction of the sample, finally forms surface 3D imaging. The interference signal received by the photomultiplier 23 is converted into an electric signal to be processed, and structural conversion imaging of the electrode surface in the electrochemical environment is obtained. Wherein, the dichroic mirror 5 of the confocal differential interference difference microscope system is used for allowing the light beam signal to directly transmit; the half mirror 7 has the function of directly transmitting a light beam signal in a confocal differential interference difference microscope system. The central lines of the microscope objective 6, the dichroic mirror 5, the semi-transparent semi-reflecting mirror 7 and the nomas prism 20 in the confocal differential interference difference microscope system are positioned on the same vertical line to ensure the smoothness of the optical path, wherein the optical system 18 can adopt a reflecting mirror to adjust the direction of the optical path.
In summary, the raman spectroscopy system and the confocal differential interference difference microscopy system of the embodiment share the dichroic mirror 5 and the half-mirror 7, so that the raman spectroscopy system and the confocal differential interference difference microscopy system are used together, and share the test bench 2 and the microscope objective 6, so that the raman spectroscopy and the high-resolution optical imaging data are collected at the same position of the electrochemical in-situ reaction device, and the related substance components can be obtained at the same position while the surface topography of the sample to be detected is analyzed.
Specifically, as shown in fig. 2, the electrochemical in-situ reaction device 1 includes a first packaging case, a second packaging case, and a flat cell.
The first packaging shell and the second packaging shell are fixedly connected through bolts, and the flat battery is fixed and sealed through extrusion force between the first packaging shell and the second packaging shell. The working electrode of the flat battery is communicated with the second packaging shell, and the counter electrode of the flat battery is communicated with the first packaging shell.
Preferably, the first packaging shell comprises a first insulating plate 1-1, a first conducting plate 1-2, a second insulating plate 1-3 and a first sealing ring 1-4, and a battery jar is arranged at the bottom of the first conducting plate 1-2;
the second packaging shell comprises a second conductive plate 1-5, a third insulating plate 1-6, quartz plates 1-7, a second sealing ring 1-8 and a third sealing ring 1-9;
the flat cell comprises working electrodes 1-10, diaphragms (or solid electrolyte membranes) 1-11, counter electrodes 1-12, pressurizing fixtures 1-13 and cell tanks 1-14, wherein the specific installation process of the electrochemical in-situ reaction device is as follows:
firstly, assembling a first packaging shell, namely fixing a first insulating plate 1-1 and a first conducting plate 1-2 through screws, and then placing a second insulating plate 1-3 and a first sealing ring 1-4 on the first conducting plate 1-2 on the outer side of a battery jar;
assembling a second packaging shell, namely sequentially assembling a second conductive plate 1-5, a second sealing ring 1-9, a quartz plate 1-7, a third sealing ring 1-8 and a third insulating plate 1-6 in sequence, and fixing the second conductive plate 1-5 and the third insulating plate 1-6 through screws, wherein optical windows are correspondingly arranged on the second conductive plate 1-5 and the third insulating plate 1-6;
thirdly, sequentially placing the pressurizing and fixing members 1-13, the counter electrode 1-12, the diaphragm (or the solid electrolyte membrane) 1-11 and the working electrode 1-10 in the battery jar 1-14 of the first conductive plate 1-2, and then placing the assembled second packaging shell on the first packaging shell; finally, screws 1-15 penetrating through fixing holes of a third insulating plate 1-6, a second conducting plate 1-5, a second insulating plate 1-3, a first conducting plate 1-2 and a first insulating plate 1-1 are fixed through nuts 1-16 to assemble the device shown in the figure 2, wherein a pressurizing fixing piece 1-13 is in contact with the bottom of the first conducting plate, a working electrode is in contact with the top of the second conducting plate 1-5, leads are respectively connected from the first conducting plate 1-2 and the second conducting plate 1-5 and are connected with an electrochemical analyzer to perform electrochemical testing, the device is placed on a testing table 2, and in-situ Raman spectrum testing and high-resolution optical observation of the electrochemical process of the electrode can be achieved through an optical window at the second conducting plate 1-5.
In some embodiments of the present invention, the first conductive plate 1-2 and the second conductive plate 1-5 are made of stainless steel, and are provided with screw through holes correspondingly; the first insulating plate 1-1, the second insulating plate 1-3 and the third insulating plate 1-6 are all made of polytetrafluoroethylene materials, and are correspondingly provided with screw through holes.
In some embodiments of the present invention, the raman spectroscopy system employs a 532nm laser source 3 and the confocal differential interference contrast microscopy system employs a superluminescent light emitting diode 14 as the illumination source.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the above embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the embodiments of the invention without departing from the spirit and scope of the invention, which is to be covered by the claims.
Claims (7)
1. A combined raman spectroscopy-confocal differential interference microscopy analysis system, comprising:
the electrochemical in-situ reaction device is used for in-situ test in the electrode charging and discharging process and is provided with an optical window;
the Raman spectrum system is used for realizing in-situ Raman spectrum testing of the electrochemical process of the electrode by irradiating the optical window to obtain the molecular structure and the chemical components of the working electrode under different voltages;
and the confocal differential interference difference microscope system is used for acquiring optical imaging of the electrode in the electrochemical process by irradiating the optical window.
2. The combined Raman spectroscopy and confocal differential interference and difference microscope analysis system according to claim 1, wherein the electrochemical in-situ reaction device comprises a first packaging shell, a second packaging shell and a flat-plate battery; the first packaging shell and the second packaging shell are fixedly connected through bolts; the flat battery is fixedly arranged between the first shell and the second packaging shell, a working electrode of the flat battery is communicated with the second packaging shell, and a counter electrode of the flat battery is communicated with the first packaging shell.
3. The combined raman spectroscopy and confocal differential interference microscopy analysis system of claim 2, wherein the first encapsulating housing comprises a first insulating plate, a first electrically conductive plate, a second insulating plate, and a first sealing ring; the second packaging shell comprises a second conductive plate, a third insulating plate, a quartz plate, a second sealing ring and a third sealing ring; the flat cell comprises a working electrode, a solid electrolyte membrane, a counter electrode and a pressurizing fixing piece;
the first insulating plate is fixedly connected with a first conductive plate, and a battery jar is arranged at the bottom of the first conductive plate; the pressurizing fixing piece, the counter electrode, the solid electrolyte membrane and the working electrode are arranged in the battery jar from top to bottom in sequence; a second insulating plate and a first sealing ring are arranged at the bottom of the first conducting plate positioned outside the battery jar;
the bottom of the second insulating plate is provided with the second conductive plate corresponding to the battery jar, and the second conductive plate is provided with a first optical window; the bottom of the second conductive plate is provided with the third insulating plate, and the third insulating plate is provided with a second window corresponding to the first optical window;
the quartz plate is arranged between the first optical window and the second optical window through a second sealing ring and a third sealing ring.
4. The combined Raman spectroscopy and confocal differential interference difference microscope analysis system according to claim 3, wherein the Raman spectroscopy system comprises a laser light source, a first color filter, a dichroic mirror, a microscope objective, a first half mirror, a first lens, a second color filter, a first reflecting mirror, a second lens, a Raman spectrometer and a CCD detector;
the laser signal generated by the laser light source is transmitted to the dichroic mirror through the first color filter, the dichroic mirror splits the laser signal, the laser signal reflected by the dichroic mirror is transmitted to the microscope objective, the microscope objective faces the second optical window, the microscope objective focuses the laser signal on the working electrode, the Raman signal generated by the working electrode is collected by the microscope objective, then is reflected by the first semi-transparent semi-reflector through the dichroic mirror, and is coupled into the Raman spectrometer for Raman signal detection through the first lens, the second color filter, the first reflector and the second lens in sequence; the CCD detector is used for assisting in observing the surface of the working electrode.
5. The combined Raman spectroscopy and confocal differential interference microscopy analysis system according to claim 4, wherein the confocal differential interference microscopy system comprises an illumination source, a second reflecting mirror, a polarizer, a second half mirror, an optical train, a third reflecting mirror, a Nomesis prism, a confocal aperture pinhole, an analyzer, and a photomultiplier tube;
light emitted by the irradiation light source is reflected by the second reflecting mirror and enters the polarizer to generate linearly polarized light, linearly polarized light is reflected by the second semi-transparent semi-reflecting mirror and enters the optical system to adjust the direction of a light path, and the linearly polarized light is reflected by the third reflecting mirror to the Nomeski prism to be decomposed into two beams of light with mutually vertical polarization directions; two bunches of light penetrate first semi-transparent semi-reflecting mirror, dichroic mirror and microobjective in proper order and shine working electrode, two light beams that reflect through working electrode loop through microobjective, dichroic mirror and first semi-transparent semi-reflecting mirror and send to nomas prism, nomas prism makes two bunches of light compound collineations again, then passes through third speculum, optical system group, second semi-transparent semi-reflecting mirror, confocal diaphragm pinhole and analyzer in proper order and is received by photomultiplier, obtains working electrode's optical imaging through handling.
6. The combined Raman spectroscopy and confocal differential interference microscopy analysis system of claim 4, wherein the laser source has a wavelength of 532 nm.
7. The combined Raman spectroscopy and confocal differential interference microscopy analysis system of claim 5, wherein the illumination source is a superluminescent light emitting diode.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114778513A (en) * | 2022-03-31 | 2022-07-22 | 中国科学院青岛生物能源与过程研究所 | Raman spectrometer for synchronous micro-area electrochemical detection and method for synchronously collecting electrochemical and Raman spectrum signals in cell micro-area |
| CN115356327A (en) * | 2022-10-19 | 2022-11-18 | 北京市农林科学院智能装备技术研究中心 | Nutrient solution detection device, method and system |
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2020
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114778513A (en) * | 2022-03-31 | 2022-07-22 | 中国科学院青岛生物能源与过程研究所 | Raman spectrometer for synchronous micro-area electrochemical detection and method for synchronously collecting electrochemical and Raman spectrum signals in cell micro-area |
| CN115356327A (en) * | 2022-10-19 | 2022-11-18 | 北京市农林科学院智能装备技术研究中心 | Nutrient solution detection device, method and system |
| CN115356327B (en) * | 2022-10-19 | 2023-04-21 | 北京市农林科学院智能装备技术研究中心 | Nutrient solution detection device, method and system |
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