Raman spectrum device for CO2 supercritical reaction

Abstract

The utility model provides a Raman spectrum device for CO2 supercritical reaction, which comprises a shell, the shell is divided into an upper shell and a lower shell, the upper shell and the lower shell are fixed through a bolt, the top of the upper shell is provided with a light inlet, the interior of the upper shell is provided with an insulating sleeve for supercritical reaction, the outer side of the insulating sleeve is provided with a heating body, and the heating body is connected with the upper shell. The lower shell is connected with a pressure assembly capable of adjusting CO2 pressure, and the pressure assembly is communicated with the insulating sleeve. According to the utility model, the supercritical reaction is carried out in the insulating sleeve, the heating body and the pressure assembly provide high-temperature and high-pressure conditions, and the Raman spectrometer can carry out Raman data acquisition on an electrode material which is charged and discharged in the supercritical state through the light inlet, so that the aim of detecting a supercritical battery system on line is fulfilled; and the electrochemical reaction change of the electrode material can be actually measured and recorded.

Description

Technical Field

[0001] This utility model relates to the field of supercritical battery technology, specifically to a Raman spectroscopy device for supercritical CO2 reactions. Background Technology

[0002] With the rapid development of renewable energy and the widespread adoption of electric vehicles, the demand for high-energy-density and high-efficiency batteries is increasing. Traditional lithium-ion batteries still have limitations in terms of energy density, charging speed, lifespan, and safety. Supercritical battery systems, due to their superior conductivity, rapid ion migration rate, and high energy density in electrochemical reactions, have become a potential solution to these problems. The unique properties of supercritical fluids (SCFs) under high temperature and pressure make them an ideal electrolyte material. Electrolytes in the supercritical state can significantly improve ion mobility while reducing the battery's internal resistance, thereby enhancing the overall battery performance. Compared to traditional batteries, supercritical batteries can operate over a wider temperature and pressure range, exhibiting better energy conversion efficiency and a longer lifespan.

[0003] Internationally, research on supercritical batteries has made significant progress. Many researchers focus on developing supercritical electrolytes, such as supercritical carbon dioxide and supercritical water, exploring their applications in electrochemical reactions. For example, lithium batteries using supercritical carbon dioxide as an electrolyte have shown excellent electrochemical performance, with studies indicating that their energy density and power density are superior to traditional batteries. Furthermore, researchers are exploring the ionic conductivity mechanism under supercritical conditions, attempting to reveal the behavior of supercritical electrolytes under different operating conditions. Domestically, with the rapid development of battery technology, research on supercritical battery systems has gradually gained attention. In recent years, some universities and research institutions have begun related basic research and application exploration, covering the synthesis of supercritical electrolytes, the analysis of ionic conductivity mechanisms, and the design and optimization of battery components. For example, some research groups have developed high-performance lithium batteries based on supercritical electrolytes, achieving good cycle stability and energy efficiency. Meanwhile, domestic research teams are also exploring the practical application potential of supercritical batteries in electric vehicles, energy storage systems, and other fields.

[0004] However, research on supercritical batteries in China is still in its early stages, with related theories and technologies not yet mature, especially in terms of long-cycle performance and safety. In the future, with advancements in materials science and electrochemistry, supercritical battery systems are expected to provide new solutions for next-generation high-performance battery technologies. As an emerging battery technology, supercritical battery systems are attracting increasing research attention due to their unique working mechanism and superior electrochemical performance. With continued exploration and development in this field in China, supercritical batteries are expected to play a significant role in future energy storage and electric vehicle applications.

[0005] In supercritical reactor studies, reactions typically occur under extreme conditions of high temperature and high pressure, making existing detection technologies often ill-suited to this environment and lacking real-time online monitoring capabilities. This results in the invisibility of the reaction process, forcing researchers to rely on indirect methods to infer reaction conditions, thus affecting the accuracy of the data and the understanding of the process. Utility Model Content

[0006] The technical problem to be solved by this invention is how to provide a device for online monitoring of CO2 under supercritical conditions.

[0007] This utility model solves the above-mentioned technical problems through the following technical means:

[0008] This invention provides a Raman spectroscopy device for supercritical CO2 reactions, comprising a housing, which is divided into an upper housing and a lower housing, which are fixed together by bolts. The upper housing has a light inlet at the top and an insulating sleeve for supercritical reactions inside. A heating element is provided on the outside of the insulating sleeve. The lower housing is connected to a pressure assembly that can adjust the CO2 pressure, and the pressure assembly is in communication with the insulating sleeve.

[0009] Beneficial effects: This invention achieves the purpose of online detection of supercritical battery systems by conducting supercritical reactions in an insulating sleeve, using a heating element and pressure components to provide high temperature and high pressure conditions, and using a Raman spectrometer through an input port to collect Raman data on electrode materials undergoing charging and discharging in supercritical conditions. It can also accurately measure and record changes in the electrochemical reactions of electrode materials.

[0010] Preferably, the bottom of the light inlet is provided with an optical window, which is fixed to the top of the insulating sleeve by a fastener.

[0011] Preferably, the insulating sleeve has a metal boss and a spring inside that can fix the electrode material, and the spring is sleeved on the surface of the metal boss.

[0012] Preferably, the heating element is fixed on the surface of the heat insulation plate.

[0013] Preferably, heat insulation cotton is provided between the heating element and the heat insulation plate.

[0014] Preferably, the upper housing is equipped with a temperature sensor, which is a platinum thermoelectric temperature sensor.

[0015] Preferably, the pressure assembly includes an air inlet connector and an air outlet connector, which are fixed on both sides of the lower housing.

[0016] Preferably, the upper housing and the lower housing are sealed together by an insulating gasket.

[0017] Preferably, the housing is cylindrical and made of 316L stainless steel or molybdenum.

[0018] Beneficial effects: By setting the shell to a cylindrical shape, this utility model can achieve high temperature and high pressure reaction conditions for the entire device, and can maximize the uniformity of high pressure conditions and the pressure bearing capacity of the shell; the shell material is 316L stainless steel or molybdenum, which not only has a certain hardness, but also conducts electricity and has good corrosion resistance.

[0019] Preferably, the optical window is made of high-transparency sapphire.

[0020] Beneficial effects: This utility model uses a high-transparency sapphire window material, which can adapt to high temperature and high pressure conditions, withstand pressure, and has high light transmittance.

[0021] The advantages of this utility model are:

[0022] This invention, through a pressure component, a heating element, and a temperature sensor, can directly obtain more accurate reaction parameters at high temperatures and high pressures in supercritical reactions. This real-time capability greatly enhances the control over the electrochemical reaction process, enabling researchers to adjust experimental conditions and optimize the reaction process in a timely manner.

[0023] In extreme environments, traditional sensors are prone to drift and instability due to atmospheric influences. However, this device effectively reduces the impact of the external environment on its performance by embedding the temperature sensor inside the upper housing, ensuring more reliable temperature sensor measurement results under high temperature and high pressure conditions, thereby improving the stability of the entire detection system.

[0024] This novel device, by incorporating an optical window in the upper housing, enables online imaging and spectroscopic analysis of electrode materials under supercritical conditions. This allows researchers to observe dynamic changes within the insulating sleeve in real time, gaining a deeper understanding of the reaction process. This intuitive visualization provides crucial support for exploring the reaction mechanism, helping researchers quickly identify and adjust problems during practical operations. Attached Figure Description

[0025] Figure 1 This is a schematic diagram of a Raman spectroscopy device for supercritical CO2 reactions in one of the embodiments;

[0026] Figure 2 This is a cross-sectional view of a Raman spectroscopy device used for supercritical CO2 reactions in the embodiment. Detailed Implementation

[0027] To make the objectives, technical solutions, and advantages of the embodiments of this utility model clearer, the technical solutions of the embodiments of this utility model will be clearly and completely described below in conjunction with the embodiments of this utility model. Obviously, the described embodiments are only some embodiments of this utility model, not all embodiments. Based on the embodiments of this utility model, all other embodiments obtained by those skilled in the art without creative effort are within the protection scope of this utility model.

[0028] In the description of this utility model, it should be noted that the terms "center," "upper," "lower," "left," "right," "vertical," "horizontal," "inner," and "outer," etc., indicating the orientation or positional relationship, are based on the orientation or positional relationship shown in the accompanying drawings and are only for the convenience of describing this utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of this utility model. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and should not be construed as indicating or implying relative importance. It should be noted that unless otherwise explicitly specified and limited, the terms "installation," "connection," and "joining" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this utility model according to the specific circumstances.

[0029] according to Figure 1-2 As shown, this embodiment provides a Raman spectroscopy device for supercritical CO2 reactions, including a housing, which is the chamber for the supercritical reaction. In order to achieve the high temperature and high pressure reaction conditions of the entire device, the housing is cylindrical in shape, and the internal chamber is also cylindrical. This can maximize the uniformity of high pressure conditions and the pressure-bearing capacity of the housing. The housing is designed to withstand high pressure and have good thermal conductivity. Therefore, the materials selected for the housing include, but are not limited to, various pressure-resistant metal materials, such as 316L stainless steel, molybdenum, etc. These materials not only have a certain degree of hardness, but also have good electrical conductivity and corrosion resistance.

[0030] The housing is divided into an upper housing 10 and a lower housing 20. The upper housing 10 and the lower housing 20 are fixed by bolts and sealed in the middle with an insulating gasket 17. The bolt holes are provided with insulating sleeves 13 to ensure that the electrode material does not short-circuit during charging and discharging.

[0031] The upper housing 10 has a light inlet 12 at the top center and an optical window 121 at the bottom. In order to adapt to high temperature and high pressure conditions and meet the optical light transmission requirements, the optical window 121 used in this embodiment is made of high-transparency sapphire, which can withstand pressure and has high light transmittance. Furthermore, a stainless steel reflective material is provided on the outside of the optical window 121 to avoid interference from thermal radiation imaging.

[0032] The upper housing 10 is also provided with a temperature sensor 11 on its side. The temperature sensor 11 is a platinum thermoelectric temperature sensor, and its interior is provided with an insulating sleeve 14 for supercritical reaction. The insulating sleeve 14 is barrel-shaped and the material can be, but is not limited to, various plastic materials, such as polytetrafluoroethylene (PTFE) and PEEK. A heating element 15 is provided on the outside of the insulating sleeve 14. The heating element 15 is annular, so that the heating temperature is concentrated around the insulating sleeve 14, thereby not affecting the imaging effect of the optical window 141. The heating element 15 is fixed to the surface of the heat insulation plate 16. The heat insulation plate 16 is annular and its function is to prevent the temperature of the heating element 15 from being conducted downward to the lower housing 20. Heat insulation cotton is provided between the heating element 15 and the heat insulation plate 16. The heat insulation cotton is used to fix the heating element 15 and reduce the heat conduction to the heat insulation plate 15. The insulating sleeve 14 is provided with a metal boss 141 for fixing the electrode material and a spring 142. The spring 142 is sleeved on the surface of the metal boss 141.

[0033] The heating element 15 can be selected from, but is not limited to, conventional heating resistance wires and heating plates. Placed inside the upper housing 10, the heating element 15 not only provides heating but also insulation. Simultaneously, the upper housing 10 is equipped with a temperature sensor 11, with a control accuracy of ±1℃. Temperature information can also be accurately and quickly acquired in real time via software. The heating element 15 can heat the electrode material within a temperature range of RT-50℃.

[0034] To conduct supercritical reaction experiments, the device also requires a pressure test. The lower housing 20 is connected to a pressure assembly capable of adjusting CO2 pressure. This pressure assembly is connected to an insulating sleeve 14, ensuring that CO2 gas enters the insulating sleeve 14 without affecting the electrochemical reaction of the electrode materials. The pressure assembly includes an inlet connector 21 and an outlet connector 22, which are fixed to both sides of the lower housing 20. The materials used for the inlet connector 21 and outlet connector 22 include, but are not limited to, stainless steel, ensuring sealing while also being resistant to high pressure and corrosion. The inlet connector 21 and outlet connector 22 can pressurize the lower housing 20 via a pressurization device. In this embodiment, the maximum pressure withstand capability of the device is no greater than 10 MPa. The outlet connector 22 is equipped with a pressure relief valve to prevent excessive internal pressure from operational errors, which could lead to danger. Simultaneously, the inlet connector 21 is equipped with a gas valve, which locks the pressure of the entire device, enabling long-term, continuous Raman spectral data acquisition of the electrode materials.

[0035] The device in this embodiment is placed in a Raman spectrometer, which can acquire spectral data of electrode materials that are being charged and discharged under supercritical conditions, and realize the real measurement and recording of the changes in the electrochemical reaction of the electrode materials.

[0036] The specific method of using this utility model device is as follows:

[0037] First, loosen and remove the bolts securing the upper and lower housings using a tool. Separate the upper housing 10 from the lower housing 20, and remove the metal boss 141. Then, sequentially fill the electrode material, diaphragm, and lithium sheet into the insulating sleeve 14. Place the metal boss 141 parallel into the insulating sleeve 141 and press it down slightly with your thumb to ensure full contact between the positive and negative electrodes. Next, place the spring 142 onto the surface of the metal boss 141. Finally, secure the upper housing 10 and the lower housing 20 with bolts. Then, connect the gas inlet 21 and gas outlet 22 of the lower housing 20. Plug the power extension cable into the housing and place it on the stage of the Raman spectrometer to complete the electrochemical reaction under supercritical conditions.

[0038] The above embodiments are only used to illustrate the technical solutions of this utility model, and are not intended to limit it. Although this utility model has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of this utility model.

Claims

1. A Raman spectrometer for supercritical CO2 reactions, characterized in that, The device includes a housing, which is divided into an upper housing (10) and a lower housing (20). The upper housing (10) and the lower housing (20) are fixed by bolts. The upper housing (10) has a light inlet (12) at the top and an insulating sleeve (14) for supercritical reaction inside. A heating element (15) is provided on the outside of the insulating sleeve (14). The lower housing (20) is connected to a pressure assembly that can adjust the CO2 pressure. The pressure assembly is connected to the insulating sleeve (14).

2. The Raman spectroscopy apparatus for supercritical CO2 reactions according to claim 1, characterized in that, The bottom of the light inlet (12) is provided with an optical window (121), and the optical window (121) is fixed to the top of the insulating sleeve (14) by a fastener (122).

3. The Raman spectroscopy apparatus for supercritical CO2 reactions according to claim 1, characterized in that, The insulating sleeve (14) is provided with a metal boss (141) and a spring (142) inside, which can fix the electrode material. The spring (142) is sleeved on the surface of the metal boss (141).

4. The Raman spectrometer for supercritical CO2 reactions according to claim 1, characterized in that, The heating element (15) is fixed on the surface of the heat insulation plate (16).

5. The Raman spectroscopy apparatus for supercritical CO2 reactions according to claim 4, characterized in that, Insulating cotton is provided between the heating element (15) and the heat insulation plate (16).

6. The Raman spectrometer for supercritical CO2 reactions according to claim 4, characterized in that, The upper housing (10) is provided with a temperature sensor (11), which is a platinum thermoelectric temperature sensor.

7. The Raman spectrometer for supercritical CO2 reactions according to claim 1, characterized in that, The pressure assembly includes an air inlet connector (21) and an air outlet connector (22), which are fixed on both sides of the lower housing (20).

8. The Raman spectrometer for supercritical CO2 reactions according to claim 1, characterized in that, The upper housing (10) and the lower housing (20) are sealed together by an insulating gasket (17).

9. The Raman spectrometer for supercritical CO2 reactions according to claim 1, characterized in that, The shell is cylindrical and made of 316L stainless steel or molybdenum.

10. The Raman spectroscopy apparatus for supercritical CO2 reactions according to claim 2, characterized in that, The optical window (121) is made of high-transparency sapphire.

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