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

Abstract

The invention discloses an ATR infrared electrochemical in-situ testing device which comprises a temperature-adjustable electrochemical testing cell and an ATR light path accessory, and the electrochemical testing cell is connected to the top of the ATR light path accessory; the electrochemical testing cell comprises a shell, a testing cell body, a counter electrode, a working electrode, a reference electrode and a cold head structure, the shell is arranged at the top of the ATR light path accessory in a sealed mode, one end of the testing cell body is arranged in a vacuum cavity of the shell, the other end of the testing cell body is arranged on the ATR light path accessory, the counter electrode is arranged on the testing cell body arranged in the vacuum cavity, and the working electrode is arranged on the working electrode. One end of the working electrode penetrates through the counter electrode and is close to the test cell body, the other end of the working electrode is connected with the cold head structure, the other end of the cold head structure extends out of the shell, a reference electrode is arranged on the working electrode, and the cold head structure provides temperature adjustment for the test cell body. The electrochemical infrared testing device has the advantages that the performance of the electrochemical infrared testing device on signal sensitivity, temperature control capability and function integration is improved.

Description

Technical Field

[0001] The present invention relates to the technical field of electrochemical testing equipment, and particularly to an ATR infrared electrochemical in-situ testing device. Background Technique

[0002] Existing electrochemical testing equipment has played 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 spectroscopic analysis techniques, the chemical changes of molecules and interfaces during the reaction can be monitored in real time. Currently widely used techniques include infrared spectroscopic equipment based on traditional transmission mode and in-situ infrared cells for electrochemistry. Although these techniques have been applied to study electrochemical reaction mechanisms, material interface chemistry, etc., there are still significant deficiencies in signal sensitivity, environmental regulation ability, and experimental flexibility. Especially when analyzing the dynamic behavior of electrochemical reactions under high and low temperature conditions, there are various limitations in the equipment function design and performance optimization of existing technologies. The application of traditional infrared spectroscopic techniques in electrochemical reaction characterization mainly uses transmission or reflection modes. However, in practical applications, the intensity and resolution of infrared signals are easily limited by solution absorption and background interference. Especially in the liquid phase environment, the strong absorption characteristics of water or electrolyte solutions significantly weaken the detection ability of target signals. In addition, existing technologies still have deficiencies in enhancing and analyzing interfacial molecular vibration signals, which makes the characterization of low-concentration or weak-signal species more difficult. To solve this problem, some researchers have tried to use attenuated total reflection (ATR) techniques, which enhance signals by multiple total reflections of light on the surface of a high-refractive-index crystal. However, the existing ATR optical path designs usually lack deep integration with electrochemical testing, resulting in poor synchronization between infrared signals and the electrochemical reaction process, further limiting the applicability of the equipment in complex reaction research. On the other hand, existing electrochemical infrared testing equipment also has obvious deficiencies in environmental regulation ability, especially in applications under high and low temperature conditions. The kinetic and thermodynamic properties of electrochemical reactions are highly sensitive to temperature changes, but most existing equipment only supports room temperature or limited heating functions and it is difficult to achieve precise real-time control of the temperature in the reaction environment. Even if some equipment has high-temperature regulation functions, there are often problems such as narrow regulation range, slow heating and cooling rates, and uneven temperature distribution. In addition, equipment for electrochemical testing under low temperature conditions is even scarcer, and the technology for constructing and maintaining a low temperature environment is not yet mature, greatly limiting the research ability of electrochemical testing in the fields related to low-temperature electrochemical behavior or cryo-electrochemistry. Existing technologies also face restrictive problems in in-situ cell design. There is room for improvement in the sealing, corrosion resistance, and sample replacement convenience of traditional in-situ electrochemical cells. Especially in high and low temperature environments, the thermal expansion and contraction characteristics of in-situ cells may lead to a decrease in sealing performance or material deterioration, thus affecting the reliability of experiments. In addition, most in-situ cell structure designs lack deep integration of optical path and electrochemical functions, resulting in low efficiency of obtaining spectral signals or instability of electrochemical parameters. This functional separation further weakens the comprehensive performance of the equipment.

[0003] In summary, there are multiple deficiencies in the current application of electrochemical infrared testing equipment under high and low temperature conditions, including limitations in infrared signal enhancement ability, insufficient temperature control range, room for optimization of the in-situ cell structure, and insufficient equipment function integration. These problems not only affect the performance of the equipment and the flexibility of experiments, but also limit the application of the equipment in more complex and extensive research scenarios. Summary of the Invention

[0004] The technical problem to be solved by the present invention is how to improve the performance of electrochemical infrared testing equipment and the flexibility of experiments.

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

[0006] An ATR infrared electrochemical in-situ testing device includes a temperature-adjustable electrochemical testing cell and an ATR optical path accessory, and the electrochemical testing cell is connected to the top of the ATR optical path accessory;

[0007] The electrochemical testing cell includes a housing, a testing cell body, a counter electrode, a working electrode, a reference electrode, and a cold head structure. The housing is hermetically arranged on the top of the ATR optical path accessory. One end of the testing cell body is arranged in the vacuum chamber of the housing, and the other end is arranged on the ATR optical path accessory. A counter electrode is arranged on the testing cell body arranged in the vacuum chamber. One end of the working electrode penetrates through the counter electrode and is close to the testing cell body, and the other end is connected to the cold head structure. The other end of the cold head structure extends out of the housing. A reference electrode is arranged on the working electrode, and the cold head structure provides temperature regulation for the testing cell body.

[0008] The temperature of the working electrode and the testing cell body is effectively regulated through the cold head structure to achieve the effect of precise temperature control. At the same time, the inside of the housing is set as a vacuum chamber to play a temperature insulation function for the equipment inside the housing, so as to realize the temperature insulation effect of the cold head structure part. At the same time, the electrochemical testing cell and the ATR optical path accessory are combined to realize infrared spectroelectrochemical testing, and then the integration of the high and low temperature system, the electrochemical system, and the infrared spectroscopy system into one body is realized, improving the performance of the testing equipment and the flexibility of experiments.

[0009] Based on the ATR optical path structure, an innovative high and low temperature control system, and an improved in-situ cell design, the present invention significantly improves the performance of electrochemical infrared testing equipment in terms of signal sensitivity, temperature control ability, and function integration. Compared with the prior art, this equipment solves key problems such as signal interference, insufficient temperature control range, and poor structural stability, provides a comprehensive and efficient technical means, opens up new possibilities for the study of electrochemical reactions under high and low temperature conditions, and has wide applicability and significant performance improvement of the equipment.

[0010] Preferably, the cold head structure includes 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 housing 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 housing and is connected to the nitrogen output end of the cold head. An annular gap is formed 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 provided on the housing.

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

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

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

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

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

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

[0019] Compared with the prior art, the beneficial effects of the present invention are as follows:

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

[0021] Figure 1 is a schematic structural diagram of an embodiment of the present invention;

[0022] Figure 2 is a partial cross - sectional view of an embodiment of the present invention;

[0023] Figure 3 is a cross - sectional view of the electrochemical test cell of an embodiment of the present invention. Detailed Embodiments

[0024] For the convenience of those skilled in the art to understand the technical solution of the present invention, the technical solution of the present invention will be further described below in conjunction with the accompanying drawings of the specification.

[0025] In this application, unless otherwise clearly defined and limited, terms such as "installed", "connected", "linked", "fixed", etc. shall be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or integrated; it can be a mechanical connection, an electrical connection, or a communication connection; it can be directly connected, or indirectly connected through an intermediate medium, and can be the communication inside two components or the interaction relationship between two components. For those of ordinary skill in the art, the specific meanings of the above terms in this application can be understood according to specific circumstances.

[0026] The terms "first" and "second" are only used for descriptive purposes and cannot be understood as indicating or implying relative importance or implicitly specifying the quantity of the indicated technical features. Thus, the features defined with "first" and "second" may explicitly or implicitly include one or more of such features. In the description of this application, the meaning of "a plurality" is two or more unless otherwise specifically defined.

[0027] Refer to Figures 1 to 3 , this embodiment discloses an ATR infrared electrochemical in-situ testing device, including an electrochemistry testing cell 1 with adjustable temperature and an ATR optical path accessory 2. The electrochemistry testing cell 1 is connected to the top of the ATR optical path accessory 2. In this embodiment, the ATR optical path accessory 2 can be purchased in the market.

[0028] The electrochemistry testing cell 1 includes a housing 11, a testing cell body 12, a counter electrode 13, a working electrode 14, a reference electrode 15, and a cold head structure 16. The housing 11 is hermetically arranged on the top of the ATR optical path accessory 2. One end of the testing cell body 12 is arranged in the vacuum chamber of the housing 11, and the other end is arranged on the ATR optical path accessory 2. A counter electrode 13 is arranged on the testing cell body 12 arranged in the vacuum chamber. One end of the working electrode 14 penetrates through the counter electrode 13 and is close to the testing 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 housing 11. A reference electrode 15 is arranged on the working electrode 14. The temperature of the working electrode 14 and the testing cell body 12 is effectively regulated through the cold head structure 16 to achieve the effect of precise temperature control. At the same time, the inside of the housing 11 is set as a vacuum chamber to play a temperature insulation function for the equipment inside the housing 11 to realize the temperature preservation function of the cold head structure 16 part. At the same time, the electrochemistry testing cell 1 and the ATR optical path accessory 2 are cooperated to realize infrared spectroscopic electrochemistry testing, and then the integration of the high and low temperature system, the electrochemistry system, and the infrared spectroscopy system into one body is realized, improving the performance of the testing equipment and the flexibility of the experiment.

[0029] An observation window 111 is opened on the housing 11 for convenient observation.

[0030] A vacuum interface 112 and an external electrode interface 113 are provided on the housing 11. The housing 11 is connected to an external vacuum pump through the vacuum interface 112 to create a vacuum environment inside the housing 11 for heat insulation. The counter electrode 13, the working electrode 14, and the reference electrode 15 are connected to the external electrode interface 113 through battery electrode wires and then connected to an electrical testing device through external electrode wires. At the same time, the electrochemical testing cell 1 is used for electrochemical electrical performance testing, and physical property analysis is carried out through an infrared spectrometer, and the required data can be measured.

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

[0032] An inlet and an outlet are opened on the test cell body 12, and the height of the inlet is lower than that of the outlet to meet the requirement of liquid circulation inside the entire test cell body 12.

[0033] Furthermore, in order to adapt to high - and low - temperature environments and the acid - base environment during 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, etc.

[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. An annular gap is formed 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 a vacuum layer is between them. The heating element is arranged on the outer wall of the cold head 161 to heat 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 is the innermost pipe diameter. Through the vertical liquid nitrogen filling method, it directly reaches the contact point of the cold head 161 to cool the cold head 161, enabling it to quickly reach the required low-temperature point. The opening at the upper end of the cold head 161 is directly connected to the outer wall diameter of the nitrogen outlet pipe 163. The liquid nitrogen is extracted by the extraction device connected to the nitrogen outlet pipe 163, and the time of the liquid nitrogen at the cold head 161 is controlled by different extraction speeds to achieve the low-temperature control method. At the same time, a heating element is provided on the cold head 161. On the one hand, it can reduce its thermal resistance. On the other hand, during the electroheating process of the heating wire, heat can be quickly transferred to the cold head 161 to achieve its temperature-rising function. Through the regulation of the liquid nitrogen extraction speed and the power regulation of the heating element, the rapid temperature regulation function of the cold head 161 can be achieved. The cold head 161 is directly embedded in the working electrode 14, and when used in combination, the temperature range inside the entire electrochemical test cell 1 can be changed from -50 to 100 °C.

[0036] The working principle of this embodiment is as follows: First, the working electrode 14, the reference electrode 15, and the 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 the counter electrode 13 need to be installed), and they are 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 fastened to the working electrode 14. The internal electrode wires of the connecting device are connected. The side sealing cover plate of the housing 11 is covered, and it is connected to an external vacuum pump through the vacuum interface 112 to create a vacuum environment inside the housing 11 for heat insulation. It is connected to an external liquid nitrogen tank through the nitrogen inlet pipe 162 to provide a cold source for the cold head 161. Temperature control is achieved through the corresponding control software. The counter electrode 13, the working electrode 14, and the reference electrode 15 are connected to the external electrode interface 113 through the battery electrode wires and are connected to the electrical testing equipment through the external electrode wires. At the same time, the electrochemical test cell 1 is used for electrochemical electrical performance testing, and physical property analysis is carried out through an infrared spectrometer, and the required data can be measured.

[0037] An ATR infrared electrochemical in-situ testing device disclosed in this embodiment, based on the ATR optical path structure, effectively enhances the intensity and quality of infrared signals. Compared with the traditional transmission or reflection mode, it significantly reduces the problem of signal attenuation caused by solution absorption interference in the liquid phase environment. Secondly, this embodiment has made an important breakthrough in temperature control. It proposes a high and low temperature control system that can cover a wide temperature range from low to high and achieve real-time and precise temperature adjustment during the reaction process. Traditional equipment often only supports limited heating functions and is difficult to meet the testing requirements under extreme temperature conditions, especially almost inoperable in low temperature environments. This device not only expands the temperature control range but also significantly improves the heating and cooling rate and temperature distribution uniformity by optimizing the design of the heating and cooling devices, thus providing a more flexible and reliable experimental means for the study of electrochemical reaction behaviors under high and low temperature conditions. In addition, this real-time temperature control system can also maintain the stability of the experiment under rapidly changing temperature conditions, making it possible to study the electrochemical characteristics in a dynamic temperature environment. The in-situ cell design of the device in this application has also been significantly improved, overcoming the deficiencies of traditional equipment in terms of sealing, temperature resistance, and structural stability. At the same time, 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, based on the ATR optical path structure, the innovative high and low temperature control system, and the improved in-situ cell design, this application significantly improves the performance of the electrochemical infrared testing equipment in terms of signal sensitivity, temperature control ability, and functional integration. Compared with the prior art, this device 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 the study of electrochemical reactions under high and low temperature conditions. The wide applicability and significant performance improvement of the device make it have important application prospects in many fields such as electrochemical mechanism research, interfacial chemical analysis, and material characterization.

[0039] For those skilled in the art, it is obvious that the present invention is not limited to the details of the above exemplary embodiments, and can be implemented in other specific forms without departing from the spirit or basic characteristics of the present invention. Therefore, from any point of view, the embodiments should be regarded as exemplary and non-limiting. The scope of the present invention is defined by the appended claims rather than the above description. Therefore, it is intended to include all changes within the meaning and scope of the equivalent elements of the claims in the present invention, and any reference signs in the claims should not be regarded as limiting the claimed rights.

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

Claims

1. An in-situ ATR infrared electrochemical testing device, characterized in that: It includes an electrochemistry test cell with adjustable temperature and an ATR optical path accessory. The electrochemistry test cell is connected to the top of the ATR optical path accessory; The electrochemistry test cell includes a housing, a test cell body, a counter electrode, a working electrode, a reference electrode, and a cold head structure. The housing is hermetically set on the top of the ATR optical path accessory. One end of the test cell body is set in the vacuum chamber of the housing, and the other end is set on the ATR optical path accessory. The counter electrode is set on the test cell body in the vacuum chamber. One end of the working electrode penetrates through the counter electrode and is close to the test cell body, and the other end is connected to the cold head structure. The other end of the cold head structure extends out of the housing. The reference electrode is set on the working electrode. The cold head structure provides temperature regulation for the test cell body.

2. The ATR infrared electrochemical in-situ testing device according to claim 1, characterized in that: The cold head structure includes 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 housing and is connected to the cold head. The nitrogen outlet pipe is sleeved outside the nitrogen inlet pipe and one end extends into the housing and is connected to the nitrogen output end of the cold head. An annular gap is formed between the inner wall of the nitrogen outlet pipe and the outer wall of the nitrogen inlet pipe to form a nitrogen outlet chamber. The outer cylinder is sleeved outside the nitrogen outlet pipe. The heating element is set on the outer wall of the cold head for heating.

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

4. An ATR infrared electrochemistry in-situ testing device according to claim 1, characterized in that: An observation window is opened on the housing.

5. An ATR infrared electrochemistry in-situ testing device according to claim 1, wherein: A vacuum interface and an external electrode interface are set on the housing.

6. The ATR infrared electrochemistry in-situ testing device according to claim 1, characterized in that: The test cell body is in a "mountain" - shaped structure.

7. An in-situ ATR infrared electrochemical testing device according to claim 1, characterized in that: An infrared window is opened at the bottom of the test cell body.

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

9. An ATR infrared electrochemistry in-situ testing device according to claim 8, characterized in that: The height of the liquid inlet is lower than the height of the liquid outlet.

10. The ATR infrared electrochemistry in-situ test device according to claim 1, characterized in that: The material of the test cell body is PEEK or PTFE.

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