An ATR infrared high-low temperature electrochemical in-situ testing device

Abstract

The application discloses an ATR infrared electrochemical in-situ testing device, which comprises a temperature-adjustable electrochemical testing pool and an ATR optical path accessory, and the electrochemical testing pool is connected to the top of the ATR optical path accessory; the electrochemical testing pool comprises a shell, a testing pool body, a counter electrode, a working electrode, a reference electrode and a cold head structure, the shell is sealingly arranged at the top of the ATR optical path accessory, one end of the testing pool body is arranged in a vacuum chamber of the shell, and the other end is arranged on the ATR optical path accessory; the counter electrode is arranged on the testing pool body arranged in the vacuum chamber; one end of the working electrode is arranged close to the testing pool body by penetrating through the counter electrode, and the other end is connected with the cold head structure; the other end of the cold head structure extends out of the shell; the reference electrode is arranged on the working electrode; and the cold head structure provides temperature adjustment for the testing pool body. The application has the advantages that the electrochemical infrared testing device is improved in signal sensitivity, temperature control capability and functional integration.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of electrochemical testing equipment, in particular to an ATR infrared electrochemical in-situ testing device. BACKGROUND

[0002] Existing electrochemical test equipment plays an important role in material characterization and reaction mechanism research, especially in the field of in-situ infrared characterization of electrochemical reactions. By combining electrochemical testing with spectral analysis techniques, the chemical changes of molecules and interfaces during the reaction process can be monitored in real time. The current widely used techniques include infrared spectroscopy equipment based on traditional transmission mode and electrochemical in-situ infrared cell. Although these techniques have been applied to the study of electrochemical reaction mechanism, material interface chemistry and other aspects, there are still significant shortcomings in signal sensitivity, environmental control ability and experimental flexibility. Especially when analyzing the dynamic behavior of electrochemical reactions under high and low temperature conditions, the existing technology has limitations in device function design and performance optimization. The application of traditional infrared spectroscopy technology in electrochemical reaction characterization mainly adopts transmission or reflection mode, but in actual application, the intensity and resolution of infrared signal are easily limited by solution absorption and background interference, especially in liquid environment, the strong absorption characteristics of water or electrolyte solution significantly weaken the detection ability of target signal. In addition, the existing technology still has shortcomings in the enhancement and analysis of interface molecular vibration signals, which makes the characterization of low concentration or weak signal species more difficult. In order to solve this problem, some researchers try to use attenuated total reflection (ATR) technology to enhance the signal by multiple total reflections of light on the surface of high refractive index crystal. However, the existing ATR optical path design usually lacks deep integration with electrochemical testing, resulting in poor synchronization between infrared signal and electrochemical reaction process, further limiting the applicability of the device in complex reaction research. On the other hand, the existing electrochemical infrared test equipment also has obvious shortcomings in environmental control ability, especially in the application of high and low temperature conditions. The dynamics and thermodynamics of electrochemical reactions are highly sensitive to temperature changes, but most existing devices only support room temperature or limited heating functions, making it difficult to achieve precise real-time control of the temperature in the reaction environment. Even some devices with high temperature regulation function often have problems such as narrow adjustment range, slow heating and cooling rate, and uneven temperature distribution. In addition, there are fewer devices for electrochemical testing under low temperature conditions, and the construction and maintenance technology of low temperature environment is not mature enough, which greatly limits the research ability of electrochemical testing in the field of low temperature electrochemistry or frozen electrochemistry. The existing technology also faces the restrictive problem of in-situ cell design. The traditional in-situ electrochemical cell has room for improvement in terms of sealing, corrosion resistance and convenience of sample replacement, especially under high and low temperature conditions, the thermal expansion and contraction characteristics of the in-situ cell may cause the sealing to decline or the material to deteriorate, affecting the reliability of the experiment. In addition, most in-situ cell structure designs lack deep integration of optical path and electrochemical functions, resulting in low efficiency of spectral signal acquisition or instability of electrochemical parameters, which further weakens the comprehensive performance of the device.

[0003] In summary, there are several deficiencies in the application of electrochemical infrared test equipment under high and low temperature conditions, including the limitation of infrared signal enhancement capability, the deficiency of temperature control range, the optimization space of in-situ cell structure, and the deficiency of equipment function integration. These problems not only affect the performance of the equipment and the flexibility of the experiment, but also limit the application of the equipment in more complex and more extensive research scenarios. SUMMARY

[0004] The technical problem to be solved by the present application is how to improve the performance of the electrochemical infrared test equipment and the flexibility of the experiment.

[0005] To solve the above technical problems, the present application provides the following technical solutions:

[0006] An ATR infrared electrochemical in-situ test device, comprising a temperature-adjustable electrochemical test cell and an ATR optical path accessory, the electrochemical test cell being connected at the top of the ATR optical path accessory;

[0007] The electrochemical test cell comprises a shell, a test cell body, a counter electrode, a working electrode, a reference electrode, and a cold head structure. The shell is sealingly arranged at the top of the ATR optical path accessory. The test cell body is arranged in a vacuum chamber in the shell at one end and on the ATR optical path accessory at the other end. The counter electrode is arranged on the test cell body in the vacuum chamber. The working electrode is arranged in the test cell body near the counter electrode at one end and connected with the cold head structure at the other end. The cold head structure extends out of the shell at the other end. The reference electrode is arranged on the working electrode. The cold head structure provides temperature adjustment for the test cell body.

[0008] The cold head structure effectively adjusts the temperature of the working electrode and the test cell body, achieving precise temperature control. The shell is arranged as a vacuum chamber, providing temperature insulation for the equipment inside the shell, and achieving temperature preservation of the cold head structure. The electrochemical test cell and the ATR optical path accessory cooperate to realize infrared spectroscopic electrochemical test, thereby integrating high and low temperature systems, electrochemical systems, and infrared spectroscopic systems, improving the performance of the test equipment and the flexibility of the experiment.

[0009] Based on the ATR optical path structure, the innovative high and low temperature control system, and the improved in-situ cell design, the present application significantly improves the performance of the electrochemical infrared test equipment in signal sensitivity, temperature control ability, and functional integration. Compared with the prior art, the present application solves the key problems of signal interference, insufficient temperature control range, and poor structural stability, providing a comprehensive and efficient technical means, opening up new possibilities for electrochemical reaction research under high and low temperature conditions, and improving the wide applicability and performance of the equipment.

[0010] Preferably, the cold head structure comprises a cold head, a nitrogen inlet pipe, a nitrogen outlet pipe, an outer cylinder and a heating element, the cold head is connected to the working electrode, one end of the nitrogen inlet pipe extends into the shell and is connected to the cold head, the nitrogen outlet pipe is sleeved outside the nitrogen inlet pipe and one end thereof extends into the shell and is connected to the nitrogen outlet end of the cold head, there is an annular gap between the inner wall of the nitrogen outlet pipe and the outer wall of the nitrogen inlet pipe to form a nitrogen outlet cavity, the outer cylinder is sleeved outside the nitrogen outlet pipe, and the heating element is arranged on the outer wall of the cold head for heating.

[0011] Preferably, the heating element is a heating wire.

[0012] Preferably, an observation window is formed in the shell.

[0013] Preferably, a vacuum interface and an electrode external interface are arranged on the shell.

[0014] Preferably, the test cell body has a "mountain" shape structure.

[0015] Preferably, an infrared window is formed in the bottom of the test cell body.

[0016] Preferably, a liquid inlet and a liquid outlet are formed in the test cell body.

[0017] Preferably, the height of the liquid inlet is lower than that of the liquid outlet.

[0018] Preferably, the material of the test cell body is PEEK or PTFE.

[0019] Compared with the prior art, the present application has the following advantages:

[0020] Based on the ATR optical path structure, the innovative high-low temperature control system and the improved in-situ cell design, the present application significantly improves the performance of the electrochemical infrared test equipment in signal sensitivity, temperature control ability and functional integration. Compared with the prior art, the present application solves the key problems of signal interference, insufficient temperature control range and poor structural stability, and provides a comprehensive and efficient technical means, which opens up new possibilities for the study of electrochemical reactions under high and low temperature conditions, and the wide applicability and significant performance improvement of the equipment. BRIEF DESCRIPTION OF DRAWINGS

[0021] Fig. 1 FIG. 1 is a structural schematic diagram of an embodiment of the present application;

[0022] Fig. 2 FIG. 2 is a partial sectional view of an embodiment of the present application;

[0023] Fig. 3 FIG. 3 is a sectional view of an electrochemical test cell according to an embodiment of the present application. DETAILED DESCRIPTION

[0024] In order to facilitate those skilled in the art to understand the technical solutions of the present application, the technical solutions of the present application will be further described in conjunction with the drawings in the specification.

[0025] In this application, unless otherwise expressly specified and limited, the terms "installation," "connection," "linking," and "fixing," etc., should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part; they can refer to a mechanical connection, an electrical connection, or a communication connection; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal communication of two components or the interaction between two components. Those skilled in the art can understand the specific meaning of the above terms in this application according to the specific circumstances.

[0026] The terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of technical features indicated. Therefore, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of this application, "multiple" means two or more, unless otherwise explicitly specified.

[0027] See Figs. 1 to 3 This embodiment discloses an ATR infrared electrochemical in-situ testing device, including a temperature-adjustable electrochemical test cell 1 and an ATR optical path accessory 2. The electrochemical test cell 1 is connected to the top of the ATR optical path accessory 2. In this embodiment, the ATR optical path accessory 2 is commercially available.

[0028] The electrochemical test cell 1 includes a shell 11, a test cell body 12, a counter electrode 13, a working electrode 14, a reference electrode 15, and a cold head structure 16. The shell 11 is sealed on top of the ATR optical path accessory 2. One end of the test cell body 12 is located inside the vacuum chamber of the shell 11, and the other end is located on the ATR optical path accessory 2. The counter electrode 13 is located on the test cell body 12 located inside the vacuum chamber. One end of the working electrode 14 passes through the counter electrode 13 and is located close to the test cell body 12, and the other end is connected to the cold head structure 16. The other end of the cold head structure 16 extends out of the shell 11. The reference electrode 15 is located on the working electrode 14. The temperature of the working electrode 14 and the test cell body 12 is effectively regulated by the cold head structure 16 to achieve precise temperature control. At the same time, the interior of the shell 11 is set as a vacuum chamber, which serves as a temperature insulation function for the internal equipment of the shell 11, thereby achieving the temperature insulation function of the cold head structure 16. Simultaneously, the electrochemical test cell 1 and the ATR optical path accessory 2 are used together to realize infrared spectroscopy electrochemical testing, thereby integrating the high and low temperature system, the electrochemical system, and the infrared spectroscopy system into one, improving the performance of the testing equipment and the flexibility of the experiment.

[0029] An observation window 111 is provided on the housing 11 for easy observation.

[0030] A vacuum interface 112 and an external electrode interface 113 are provided on the housing 11. The vacuum interface 112 is connected to an external vacuum pump to provide a vacuum environment inside the housing 11 for heat insulation. The counter electrode 13, working electrode 14, and reference electrode 15 are connected to the external electrode interface 113 through battery electrode wires and connected to electrical testing equipment through external electrode wires. At the same time, the electrochemical test cell 1 is used to perform electrochemical and electrical performance tests, and the physical properties are analyzed by an infrared spectrometer to obtain the required data.

[0031] The test cell body 12 is the main location where the electrochemical reaction occurs. It has a "mountain" shaped structure. The counter electrode 13, working electrode 14, and reference electrode 15 are all distributed around the "mountain". Various commercial electrodes and flexible tubing used for liquid flow can be externally mounted. An infrared window (not shown in the figure) is opened at the bottom of the test cell body 12. The material of the infrared window needs to meet the transmission requirements of the infrared spectrum. Therefore, the material selection includes, but is not limited to, crystalline silicon, germanium, zinc selenide, calcium fluoride, barium fluoride, diamond, etc.

[0032] The test pool body 12 is provided with an inlet and an outlet, wherein the height of the inlet is lower than the height of the outlet, so as to meet the requirements of liquid circulation inside the entire test pool body 12.

[0033] Furthermore, in order to adapt to high and low temperature environments and acid and alkali environments in the electrochemical reaction process, the material selection of the test cell body 12 needs to meet the characteristics of high and low temperature resistance, corrosion resistance and easy processing. Therefore, the material selection of the test cell body 12 includes, but is not limited to, various engineering plastics, such as PEEK or PTFE.

[0034] The cold head structure 16 includes a cold head 161, a nitrogen inlet pipe 162, a nitrogen outlet pipe 163, an outer cylinder 164, and a heating element. The cold head 161 is connected to the working electrode 14. One end of the nitrogen inlet pipe 162 extends into the housing 11 and is connected to the cold head 161. The nitrogen outlet pipe 163 is sleeved outside the nitrogen inlet pipe 162 and one end extends into the housing 11 and is connected to the nitrogen output end of the cold head 161. There is an annular gap between the inner wall of the nitrogen outlet pipe 163 and the outer wall of the nitrogen inlet pipe 162 to form a nitrogen outlet cavity. The outer cylinder is sleeved outside the nitrogen outlet pipe 163, and there is a vacuum layer between them. The heating element is disposed on the outer wall of the cold head 161 for heating the cold head 161. In this embodiment, the heating element is a heating wire wound around the outer wall of the cold head 161.

[0035] The nitrogen inlet pipe 162 has the innermost diameter and directly injects liquid nitrogen into the contact point of the cold head 161 via a vertical injection method. This cools the cold head 161, allowing it to quickly reach the required low temperature. The opening at the top of the cold head 161 is directly connected to the outer wall of the nitrogen outlet pipe 163. Liquid nitrogen is extracted using a pumping device connected to the nitrogen outlet pipe 163, and the time the liquid nitrogen spends at the cold head 161 is controlled by varying the pumping speed, thus achieving low-temperature control. Simultaneously, a heating element is installed on the cold head 161. This reduces thermal resistance, and the heating wire, through electrical heating, quickly transfers heat to the cold head 161, raising its temperature. By adjusting the liquid nitrogen pumping speed and the power of the heating element, rapid temperature control of the cold head 161 can be achieved. The cold head 161 is directly embedded in the working electrode 14, and when used in conjunction, it allows for temperature variations within the entire electrochemical test cell 1 from -50°C to 100°C.

[0036] The working principle of this embodiment is as follows: First, the working electrode 14, reference electrode 15, and counter electrode 13 are assembled according to the general assembly steps of the electrochemical test cell 1 (if it is a battery system, only the working electrode 14 and counter electrode 13 need to be installed), and fixed on the ATR optical path accessory 1. The cold head structure 16 is inserted into the center of the electrochemical test cell 1 from above and the cold head 161 is rotated until it is firmly fixed to the working electrode 14. The internal electrode wires are connected, and the side sealing cover of the housing 11 is covered. The vacuum interface 112 is connected to an external vacuum pump to provide a vacuum environment inside the housing 11 for heat insulation. The nitrogen inlet pipe 162 is connected to an external liquid nitrogen tank to provide a cold source for the cold head 161. Temperature control is achieved through the corresponding control software. The counter electrode 13, working electrode 14, and reference electrode 15 are connected to the electrode external interface 113 through the battery electrode wires and connected to the electrical testing equipment through the electrode external wires. At the same time, the electrochemical test cell 1 is used to perform electrochemical and electrical performance tests, and the physical properties are analyzed by an infrared spectrometer to obtain the required data.

[0037] This embodiment discloses an ATR infrared electrochemical in-situ testing device. Based on the ATR optical path structure, it effectively enhances the intensity and quality of the infrared signal, significantly reducing the signal attenuation problem caused by solution absorption interference in the liquid phase environment compared to traditional transmission or reflection modes. Secondly, this embodiment achieves a significant breakthrough in temperature control, proposing a high and low temperature control system capable of covering a wide temperature range from low to high temperatures and achieving real-time and precise temperature adjustment during the reaction process. Traditional equipment often only supports limited heating functions, making it difficult to meet testing needs under extreme temperature conditions, especially in low-temperature environments where it is almost impossible to operate. This device not only expands the temperature control range but also significantly improves the heating and cooling rates and temperature distribution uniformity through optimized heating and cooling device design, thus providing a more flexible and reliable experimental method for studying electrochemical reaction behavior under high and low temperature conditions. Furthermore, this real-time temperature control system can maintain experimental stability under rapidly changing temperature conditions, making the study of electrochemical characteristics in dynamic temperature environments possible. The in-situ cell design of this device has also been significantly improved, overcoming the shortcomings of traditional equipment in terms of sealing, temperature resistance, and structural stability. Meanwhile, the optical channel of the in-situ cell is deeply integrated with the electrochemical testing unit, achieving a simultaneous improvement in signal acquisition efficiency and electrochemical parameter stability.

[0038] In summary, this application, based on the ATR optical path structure, innovative high and low temperature control system, and improved in-situ cell design, significantly enhances the performance of electrochemical infrared testing equipment in terms of signal sensitivity, temperature control capability, and functional integration. Compared to existing technologies, this equipment solves key problems such as signal interference, insufficient temperature control range, and poor structural stability, providing a comprehensive and efficient technical means and opening up new possibilities for electrochemical reaction research under high and low temperature conditions. The equipment's wide applicability and significant performance improvement make it promising for applications in multiple fields such as electrochemical mechanism research, interfacial chemical analysis, and materials characterization.

[0039] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention can be implemented in other specific forms without departing from its spirit or essential characteristics. Therefore, the embodiments should be considered illustrative and non-limiting in all respects, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, all variations falling within the meaning and scope of equivalents of the claims are intended to be included within the present invention, and no reference numerals in the claims should be construed as limiting the scope of the claims.

[0040] The above embodiments are merely examples of implementation methods of the invention. The scope of protection of the present invention is not limited to the above embodiments. For those skilled in the art, several modifications and improvements can be made without departing from the concept of the present invention, and these all fall within the scope of protection of the present invention.

Claims

1. An ATR infrared electrochemical in-situ testing device, characterized by: The electrochemical test cell and the ATR optical path accessory are connected at the top of the ATR optical path accessory. The electrochemical test cell comprises a shell, a test cell body, a counter electrode, a working electrode, a reference electrode and a cold head structure, the shell is sealingly arranged at the top of the ATR optical path accessory, one end of the test cell body is arranged in a vacuum chamber of the shell, and the other end is arranged on the ATR optical path accessory, the counter electrode is arranged on the test cell body arranged in the vacuum chamber, one end of the working electrode is arranged close to the test cell body through the counter electrode, and the other end is connected with the cold head structure, the other end of the cold head structure extends out of the shell, the reference electrode is arranged on the working electrode, and the cold head structure provides temperature adjustment for the test cell body. The cold head structure comprises a cold head, a nitrogen inlet pipe, a nitrogen outlet pipe, an outer cylinder and a heating element, the cold head is connected with the working electrode, one end of the nitrogen inlet pipe extends into the shell and is connected with the cold head, the nitrogen outlet pipe is sleeved outside the nitrogen inlet pipe and one end thereof extends into the shell and is connected with a nitrogen gas output end of the cold head, there is an annular gap between the inner wall of the nitrogen outlet pipe and the outer wall of the nitrogen inlet pipe to form a nitrogen outlet cavity, the outer cylinder is sleeved outside the nitrogen outlet pipe, and the heating element is arranged on the outer wall of the cold head for heating.

2. An ATR infrared electrochemical in situ testing device according to claim 1, characterized in that: The heating element is a heating wire.

3. An ATR infrared electrochemical in situ testing device according to claim 1, characterized in that: An observation window is arranged on the shell.

4. The ATR infrared electrochemical in situ testing apparatus according to claim 1, characterized in that: A vacuum interface and an electrode external interface are arranged on the shell.

5. The ATR infrared electrochemical in situ testing apparatus according to claim 1, wherein: The test cell body has a "mountain" shape structure.

6. An ATR infrared electrochemical in situ testing apparatus according to claim 1, characterized in that: An infrared window is arranged at the bottom of the test cell body.

7. An ATR infrared electrochemical in situ testing apparatus according to claim 1, characterized in that: A liquid inlet and a liquid outlet are arranged on the test cell body.

8. An ATR infrared electrochemical in situ testing apparatus according to claim 7, characterized in that: The height of the liquid inlet is lower than that of the liquid outlet.

9. An ATR infrared electrochemical in situ testing apparatus according to claim 1, characterized in that: The material of the test cell body is PEEK or PTFE.

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