An electrochemical testing device combining infrared spectroscopy and online electrochemical mass spectrometry

Abstract

An electrochemical testing device for combining infrared spectroscopy with online electrochemical mass spectrometry, comprising a counter electrode module located at an upper layer, a flow electrolytic cell cavity module located at a middle layer, and an infrared spectroscopy interface module located at a lower layer; the flow electrolytic cell cavity module comprises an electrolytic cell cavity, a positive electrode chamber, a positive electrode liquid inlet, a positive electrode liquid outlet, a mass spectrometer injection port, a sample delivery port, a reference electrode interface, a working electrode, and a reference electrode, the mass spectrometer injection port is used to separate gas, and the gas flows out from the sample delivery port; the counter electrode module comprises a negative electrode cover, a negative electrode chamber, a negative electrode liquid inlet, a negative electrode liquid outlet, a counter electrode interface, and a counter electrode; the positive electrode chamber and the negative electrode chamber are separated by an ion exchange membrane; the infrared spectroscopy interface module comprises a prism and an infrared optical window. The present invention can integrate the signal collection of infrared spectroscopy with the collection of mass spectrometry, so that the collected signals can achieve the same frequency, and the working electrode and the counter electrode can be separated, belonging to the field of electrochemical testing technology.

Description

Technical Field

[0001] The invention relates to the technical field of electrochemical detection, and in particular to an electrochemical testing device combining infrared spectroscopy with online electrochemical mass spectrometry. Background Art

[0002] Among modern experimental testing methods, in-situ testing can obtain important information in molecules, which is conducive to in-depth understanding and recognition of the mechanism of chemical reactions. It has been applied to many scientific research fields, especially suitable for the study of electrochemical reactions.

[0003] Conventional infrared spectroscopy uses the transmission method and uses pressed sheets or coatings for measurement. It is difficult to test some special samples (such as samples that are difficult to dissolve, melt, or crush). The attenuated total reflection (ATR) infrared technology is applied to the Fourier transform infrared spectrometer, resulting in the Fourier transform attenuated total reflection infrared spectrometer. Its basic working principle is that the infrared light emitted from the light source passes through a crystal with a large refractive index and then projects onto the surface of the sample with a small refractive index. When the incident angle is greater than the critical angle, the incident light will produce total reflection. In this process, the infrared light penetrates to a certain depth inside the sample surface and then returns to the surface. The sample selectively absorbs in the frequency region of the incident light, and the intensity of the reflected light is weakened, producing an infrared spectrum similar to the transmission absorption, thereby obtaining the structural information of the chemical composition of the sample surface.

[0004] In addition, online electrochemical mass spectrometry can accurately quantify the gases consumed and generated by the electrochemical reaction system during the reaction process, which is an important means to study the reversible main reaction and irreversible side reactions of the battery. For example, when lithium-ion batteries have side reactions, they are usually accompanied by the generation of gases, such as H 2 ,CO,CO 2 Therefore, by measuring the type and content of gases, combined with power calculation and isotope tracking, the changes in positive and negative electrode materials, electrolytes or SEI films during the operation of lithium-ion batteries can be further clarified. 2 Catalytic reduction is also an important electrocatalytic reaction. The improvement of catalyst activity and selectivity is very important for CO 2 The practical application of catalytic reduction is of great significance.

[0005] At present, conventional methods can only obtain a series of information after the electrochemical reaction, and cannot analyze the chemical bonds, molecular structures, transition states and changes of substances during the electrochemical reaction. In-situ spectroscopy technology can continue to analyze the intermediate products intuitively, and it is receiving more and more attention. Combining attenuated total reflection Fourier transform infrared spectroscopy and online electrochemical mass spectrometry into one device can obtain both infrared signals and mass spectrometry signals. Among them, in-situ electrochemical infrared spectroscopy can analyze the intermediate products of the adsorption layer of the electrode reaction, while in-situ electrochemical mass spectrometry can analyze the gas products produced at the electrode interface. This multi-scale detection method is of great significance for exploring the reaction mechanism of various electrochemical reactions.

[0006] At present, there are still some challenges in using infrared spectroscopy and online mass spectrometry at the same time. For example, during the electrochemical reaction, a series of electrochemical reactions will occur on the surface of the electrode at the same time, producing various gases or a series of reaction products dissolved in the electrolyte. These gases or reaction products dissolved in the solution will affect the gas analysis of the online electrochemical mass spectrometry, and will also affect the infrared spectrum signal of ATR-FTIR, causing interference with the detection of the working electrode, which brings inconvenience to the research. Summary of the invention

[0007] In view of the technical problems existing in the prior art, the purpose of the present invention is to provide an electrochemical testing device combining infrared spectroscopy with online electrochemical mass spectrometry, which can integrate the signal collection of infrared spectroscopy with the collection of mass spectrometry, so that the collected signals can achieve the same frequency, and the working electrode and the counter electrode can be separated.

[0008] In order to achieve the above object, the present invention adopts the following technical scheme: an electrochemical testing device combining infrared spectroscopy with online electrochemical mass spectrometry, comprising a counter electrode module located at an upper layer, a flow electrolytic cell cavity module located at a middle layer, and an infrared spectroscopy interface module located at a lower layer;

[0009] The flow electrolytic cell chamber module comprises an electrolytic cell chamber, a cathode chamber, a cathode liquid inlet, a cathode liquid outlet, a mass spectrometer inlet, a sample delivery port, a reference electrode interface, a working electrode and a reference electrode. The cathode chamber is arranged on the electrolytic cell chamber, the cathode liquid inlet, the cathode liquid outlet, the sample delivery port and the reference electrode interface are all connected to the cathode chamber, the mass spectrometer inlet is located between the sample delivery port and the cathode chamber, the reference electrode interface is used to install the reference electrode, the working electrode is located at the bottom of the cathode chamber, the cathode electrolyte flows in through the cathode liquid inlet and flows out through the cathode liquid outlet, the mass spectrometer inlet is annular and comprises a support sheet and a mass spectrometer filter membrane, the mass spectrometer inlet is used to separate the gas in the cathode electrolyte, and the gas flows out from the sample delivery port;

[0010] The counter electrode module comprises a negative electrode cover, a negative electrode chamber, a negative electrode liquid inlet, a negative electrode liquid outlet, a counter electrode interface and a counter electrode, wherein the negative electrode chamber is arranged on the negative electrode cover, the negative electrode liquid inlet, the negative electrode liquid outlet and the counter electrode interface are all connected to the negative electrode chamber, the negative electrode electrolyte flows into the negative electrode chamber through the negative electrode liquid inlet and flows out through the negative electrode liquid outlet, and the counter electrode interface is used to install the counter electrode;

[0011] The positive electrode chamber is located below the negative electrode chamber, and the positive electrode chamber and the negative electrode chamber are separated by an ion exchange membrane;

[0012] The infrared spectrum interface module comprises a prism and an infrared optical window. The infrared optical window is located at the bottom of the working electrode, and the prism is located below the infrared optical window.

[0013] With this structure, the ion exchange membrane can isolate the working electrode and the counter electrode chamber, allowing specific ions in the electrolyte to pass freely, ensuring that the working electrode and the counter electrode reactions are not disturbed, and the gas can be quickly collected through the mass spectrometer injection port and the sample delivery port. Therefore, this device is convenient for isolating the electrochemical reaction of the working electrode and the counter electrode, facilitating efficient collection of the gas of the working electrode and infrared monitoring of the surface products and products, and preventing the electrochemical reaction of the counter electrode from affecting the accuracy of the detection. At the same time, it is convenient for monitoring continuous Faraday reactions and can control fluid dynamics when measuring the formation rate and conversion frequency of the reaction products.

[0014] This can be expanded to HER, ORR and even full fuel cell research.

[0015] As a preferred embodiment, the support sheet is an annular stainless steel foam body, and the mass spectrometer filter membrane is an annular porous polytetrafluoroethylene film.

[0016] As a preferred embodiment, the positive electrode chamber includes an upper chamber, a lower chamber and a capillary channel, the upper chamber is separated from the negative electrode chamber by an ion exchange membrane, the working electrode is located at the bottom of the lower chamber, the upper chamber and the lower chamber are connected by a capillary channel, the positive electrode liquid outlet is located at the bottom of the upper chamber, and the positive electrode liquid outlet and the mass spectrometer inlet are located at the top of the lower chamber.

[0017] As a preference, there are multiple capillary channels, the upper ends of the capillary channels are connected to the outer edge of the upper chamber, the lower ends of the capillary channels are connected to the outer edge of the lower chamber, the positive electrode liquid outlet is located at the center of the bottom end of the upper chamber, and the positive electrode liquid outlet is located at the center of the top end of the lower chamber.

[0018] Preferably, the material of the prism is sapphire glass, calcium fluoride or potassium bromide.

[0019] As a preferred embodiment, the infrared optical window is Si 3 N 4 Crystal thin film, the working electrode is on Si 3 N 4A gold coating deposited on a crystalline film or a conductive carbon material layer deposited on a mass spectrometer filter membrane.

[0020] As a preference, the reference electrode is a silver chloride electrode, a mercury oxide electrode or a reversible hydrogen electrode, and the counter electrode is a platinum wire electrode, a nickel mesh electrode, a graphite rod electrode or a carbon mesh electrode.

[0021] As a preference, the infrared spectrum interface module further comprises a prism cover, the upper end of the prism cover is provided with a groove, the bottom of the groove is provided with a through hole, the infrared optical window and the working electrode are installed in the groove, and the prism is installed in the through hole.

[0022] As a preferred embodiment, it also includes an ion exchange membrane cover, in which the ion exchange membrane is installed, and a first sealing ring is provided between the ion exchange membrane cover and the electrolytic cell cavity, and between the working electrode and the electrolytic cell cavity, respectively, and a second sealing ring is provided between the ion exchange membrane cover and the negative electrode cover, and both the first sealing ring and the second sealing ring are fluororubber rings.

[0023] As a preferred embodiment, it further comprises a plurality of connecting pipes, which are respectively connected to the negative electrode liquid inlet, the negative electrode liquid outlet, the positive electrode liquid inlet, the positive electrode liquid outlet and the sample delivery port, and a third sealing ring is provided between the connecting pipe and the electrolytic cell cavity or the negative electrode cover, and the third sealing ring is a fluororubber ring;

[0024] The connecting pipeline is composed of a first screw with a hole and a hollow steel pipe. The first screw with a hole is fixedly sleeved on the outer side of the hollow steel pipe. The first screw with a hole connects the electrolytic cell cavity and the negative electrode cover through threads.

[0025] As a preferred embodiment, the materials of the electrolytic cell cavity and the negative electrode cover are both PEEK.

[0026] In general, the present invention has the following advantages:

[0027] (1) The present invention realizes the combination of infrared and mass spectrometry, and can be used to simultaneously capture electrochemical signals, infrared signals and mass spectrometry signals under electrochemical reaction conditions.

[0028] (2) The mass spectrometer gas inlet is designed in an annular shape and is placed as close to the working electrode as possible to achieve rapid gas collection and synchronize the infrared spectrum signal with the mass spectrum signal.

[0029] (3) The working electrode and the counter electrode are isolated by designing a double-thin-layer flow electrolytic cell, so that the reaction of the counter electrode will not affect the signal acquisition of the working electrode.

[0030] (4) The device is simple and sturdy to assemble, has a wide range of applications, and is easy to operate, which is of great significance for studying the mechanism of electrochemical reactions. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] Figure 1The working principle diagram is as follows.

[0032] Figure 2 Detailed schematic diagram of the mass spectrometer injection port from a top view.

[0033] Figure 3 Schematic diagram of the working electrode structure in Example 1.

[0034] Figure 4 Schematic diagram of the working electrode structure in Example 2.

[0035] Figure 5 It is a stereogram of the present invention.

[0036] Figure 6 It is a top view of the present invention.

[0037] Figure 7 for Figure 6 Middle AA section view.

[0038] Figure 8 for Figure 7 A magnified view of a portion of the area.

[0039] Fig. 9 for Figure 6 Middle BB cross-section.

[0040] Fig.10 for Fig. 9 A magnified view of a portion of the area.

[0041] Fig.11 for Figure 6 Middle CC section.

[0042] Fig.12 for Figure 6 Middle DD section view.

[0043] Fig.13 A top view of the electrode module.

[0044] Fig.14 for Fig.13 Middle EE section view.

[0045] Fig.15 A top view of the flow electrolysis cell chamber module.

[0046] Fig.16 for Fig.15 Middle FF cross-section.

[0047] Fig.17 A top view of the prism cover.

[0048] Fig.18 for Fig.17 Middle GG cross-section.

[0049] Fig.19 A perspective view of an ion exchange membrane cover.

[0050] Fig. 20 It is an exploded view of the present invention.

[0051] Among them, 1 is the counter electrode, 2 is the long bolt, 3 is the hollow steel pipe, 4 is the first screw with a hole, 5 is the third sealing ring, 6 is the negative electrode cover, 7 is the second screw with a hole, 8 is the fourth sealing ring, 9 is the second sealing ring, 10 is the ion exchange membrane, 11 is the first sealing ring, 12 is the ion exchange membrane cover, 13 is the reference electrode, 14 is the electrolytic cell chamber, 15 is the stainless steel foam, 16 is the mass spectrometer filter membrane, 17 is the prism cover, 18 is the prism, 19 is the working electrode and the infrared optical window, 20 is the sample material, 601 is the negative electrode chamber, 1401 is the upper chamber, 1402 is the lower chamber, 1403 is the capillary channel, 1901 is the gold plating, 1902 is the Si 3 N 4 Film, 1903 is a conductive carbon material layer. DETAILED DESCRIPTION

[0052] The present invention will be further described in detail below with reference to the accompanying drawings and specific implementation methods.

[0053] Embodiment 1

[0054] like Figures 5 to 20 As shown, an electrochemical testing device for combining infrared spectroscopy with online electrochemical mass spectrometry comprises a counter electrode module located at an upper layer, a flow electrolytic cell cavity module located at a middle layer, and an infrared spectroscopy interface module located at a lower layer;

[0055] The flow electrolytic cell chamber module comprises an electrolytic cell chamber, a cathode chamber, a cathode liquid inlet, a cathode liquid outlet, a mass spectrometer inlet, a sample delivery port, a reference electrode interface, a working electrode and a reference electrode. The cathode chamber is arranged on the electrolytic cell chamber, the cathode liquid inlet, the cathode liquid outlet, the sample delivery port and the reference electrode interface are all connected to the cathode chamber, the mass spectrometer inlet is located between the sample delivery port and the cathode chamber, the reference electrode interface is used to install the reference electrode, the working electrode is located at the bottom of the cathode chamber, the cathode electrolyte flows in through the cathode liquid inlet and flows out through the cathode liquid outlet, the mass spectrometer inlet is annular and comprises a support sheet and a mass spectrometer filter membrane, the mass spectrometer inlet is used to separate the gas in the cathode electrolyte, and the gas flows out from the sample delivery port;

[0056] The counter electrode module comprises a negative electrode cover, a negative electrode chamber, a negative electrode liquid inlet, a negative electrode liquid outlet, a counter electrode interface and a counter electrode, wherein the negative electrode chamber is arranged on the negative electrode cover, the negative electrode liquid inlet, the negative electrode liquid outlet and the counter electrode interface are all connected to the negative electrode chamber, the negative electrode electrolyte flows into the negative electrode chamber through the negative electrode liquid inlet and flows out through the negative electrode liquid outlet, and the counter electrode interface is used to install the counter electrode;

[0057] The positive electrode chamber is located below the negative electrode chamber, and the positive electrode chamber and the negative electrode chamber are separated by an ion exchange membrane;

[0058] The infrared spectrum interface module comprises a prism and an infrared optical window. The infrared optical window is located at the bottom of the working electrode, and the prism is located below the infrared optical window.

[0059] The supporting sheet is a ring-shaped stainless steel foam body, and the mass spectrometer filter membrane is a ring-shaped porous polytetrafluoroethylene film.

[0060] The positive electrode chamber includes an upper chamber, a lower chamber and a capillary channel. The upper chamber is separated from the negative electrode chamber by an ion exchange membrane. The working electrode is located at the bottom of the lower chamber. The upper chamber and the lower chamber are connected by a capillary channel. The positive electrode liquid outlet is located at the bottom of the upper chamber, and the positive electrode liquid outlet and the mass spectrometer inlet are located at the top of the lower chamber.

[0061] There are multiple capillary channels, the upper ends of the capillary channels are connected to the outer edge of the upper chamber, the lower ends of the capillary channels are connected to the outer edge of the lower chamber, the positive electrode liquid outlet is located at the center of the bottom end of the upper chamber, and the positive electrode liquid outlet is located at the center of the top end of the lower chamber.

[0062] like Figure 1 to Figure 3 The figure shows the working principle diagram of the device. In the figure, a is the negative electrode inlet flow, b is the negative electrode outlet flow, c is the positive electrode inlet flow, d is the positive electrode outlet flow, e is the separated gas, f is the infrared beam, and RE is the reference electrode. The positive electrode electrolyte flows into the upper chamber through the positive electrode inlet, flows to the outer edge of the upper chamber through the capillary channel to the lower chamber, and flows from the outer edge of the lower chamber to the center through the annular area where the mass spectrometer injection port is located. The gas separated by the mass spectrometer injection port flows out from the sample delivery port, and the positive electrode electrolyte flows out from the positive electrode outlet in the center. The mass spectrometer injection port can be designed according to actual conditions, so that the porous polytetrafluoroethylene film is as close to the working electrode below as possible to achieve rapid gas adoption.

[0063] The materials of the prism are sapphire glass, calcium fluoride or potassium bromide.

[0064] Infrared optical window is Si 3 N 4 Crystal thin film, the working electrode is on Si 3 N 4 Gold layer deposited on a crystalline film.

[0065] The reference electrode is a silver chloride electrode, a mercury oxide electrode or a reversible hydrogen electrode, and the counter electrode is a platinum wire electrode, a nickel mesh electrode, a graphite rod electrode or a carbon mesh electrode.

[0066] The infrared spectrum interface module also includes a prism cover, the upper end of the prism cover is provided with a groove, the bottom of the groove is provided with a through hole, the infrared optical window and the working electrode are installed in the groove, and the prism is installed in the through hole.

[0067] It also includes an ion exchange membrane cover, in which the ion exchange membrane is installed. A first sealing ring is provided between the ion exchange membrane cover and the electrolytic cell cavity, and between the working electrode and the electrolytic cell cavity, respectively. A second sealing ring is provided between the ion exchange membrane cover and the negative electrode cover. Both the first sealing ring and the second sealing ring are fluororubber rings.

[0068] It also includes a plurality of connecting pipes, which are respectively connected to the negative electrode liquid inlet, the negative electrode liquid outlet, the positive electrode liquid inlet, the positive electrode liquid outlet and the sample delivery port, and a third sealing ring is provided between the connecting pipe and the electrolytic cell cavity or the negative electrode cover, and the third sealing ring is a fluororubber ring;

[0069] The connecting pipeline is composed of a first screw with a hole and a hollow steel pipe. The first screw with a hole is fixedly sleeved on the outer side of the hollow steel pipe. The first screw with a hole connects the electrolytic cell cavity and the negative electrode cover through threads.

[0070] The counter electrode is installed on the counter electrode interface through the second perforated screw, and the reference electrode is installed on the reference electrode interface through the second perforated screw. A fourth sealing ring is provided between the second perforated screw and the electrolytic cell cavity or the negative electrode cover. The second perforated screw is an M6 perforated screw, and the fourth sealing ring is a fluororubber ring with an outer diameter of 5 mm and a wire diameter of 1 mm.

[0071] The hollow steel tube is a hollow steel tube with a diameter of 0.25 inches, the first screw with a hole is a 0.25-inch v1_0 model first screw with a hole, and the third sealing ring is a fluororubber ring with an outer diameter of 10 mm and a wire diameter of 2 mm. The second sealing ring is a fluororubber ring with an outer diameter of 18 mm and a wire diameter of 2 mm, and the first sealing ring is a fluororubber ring with an outer diameter of 26 mm and a wire diameter of 4 mm.

[0072] In actual use, all connecting pipes, reference electrodes and counter electrodes can be replaced with other pipes, electrodes or devices of similar specifications, and the gas collected by the reaction can be introduced into the mass spectrometer for detection.

[0073] The materials of the electrolytic cell chamber and the negative electrode cover are both PEEK. The material of the prism cover is stainless steel 316L.

[0074] The electrolytic cell chamber, the negative electrode cover and the prism cover are detachably connected by long bolts. The long bolts are M6 long bolts.

[0075] Embodiment 2

[0076] like Figure 4 As shown, the working electrode is a conductive carbon material layer deposited on a porous polytetrafluoroethylene film.

[0077] The sample material to be tested is coated on the conductive carbon material layer.

[0078] The parts not mentioned in this embodiment are the same as those in the first embodiment.

[0079] Embodiment 3

[0080] An electrochemical testing device combining infrared spectroscopy and online electrochemical mass spectrometry is used to test the oxygen evolution reaction (OER) in water decomposition. The specific steps are as follows:

[0081] 1. Assemble the bottom optical path system: Place the prism in the holder of the prism cover and install it to ensure normal use of the optical path.

[0082] 2. Assemble the three electrodes and all piping systems: After preparing the working electrode, fix the working electrode and the prism to the corresponding positions of the prism cover. Install the reference electrode and the hollow steel pipes corresponding to each liquid flow in the corresponding holes of the electrolytic cell cavity, and tighten them with sealing rings and corresponding screws with holes to ensure sealing. At the same time, insert the stainless steel foam and mass spectrometer filter into the annular groove of the electrolytic cell cavity and fix them. Next, install the negative electrode cover. First, fit the prepared ion exchange membrane with the sealing ring and tighten it on the negative electrode cover through the ion exchange membrane cover. Also install the counter electrode and each hollow steel pipe corresponding to the liquid flow in the negative electrode cover in the corresponding holes of the negative electrode cover. Use sealing rings and corresponding screws with holes to tighten them to ensure sealing. Complete the loading of the three electrodes and all piping systems.

[0083] 3. Assemble the entire electrolytic cell system: Assemble the bottom optical path and the corresponding electrode system together, and use two sealing rings to press the gaps between the prism cover, the electrolytic cell cavity and the negative electrode cover respectively, and then use long bolts to fix them to ensure the sealing of the entire system.

[0084] 4. Start the device: Use a peristaltic pump to set a certain flow rate to pump the negative electrode electrolyte from the negative electrode inlet, and pump it out from the negative electrode outlet after fully soaking the counter electrode. At the same time, set another peristaltic pump to connect the working electrode inlet and working electrode outlet, and also set a certain speed to control the flow of the liquid. The test can be started only after there is no gas in all pipes.

[0085] 5. System test: connect the electrochemical workstation, in-situ mass spectrometer and infrared spectrometer, first use infrared spectrometer and mass spectrometer to test the background signal, then trigger the electrochemical workstation, adopt the working mode of dynamic potential, constant potential or constant current, and obtain the electrochemical reaction signal, mass spectrometry test signal and infrared spectrum signal at the same time. The ion exchange membrane used in this device isolates the working electrode and the counter electrode reaction during the test, which reduces the system error for gas detection and reaction monitoring of mass spectrometry. At the same time, the double-layer flow design allows the electrolyte to enter the edge of the working electrode from the thin double-layer flow and gradually enter the center of the working electrode as it flows. After fully contacting the reaction, it can also fully collect all the gases produced by the reaction through the annular mass spectrometer injection port, instead of only extracting a small amount of sample as a representative test like the existing injection device, which increases the collection rate of the product and reduces the experimental error caused by side reactions.

[0086] 6. After the test is completed, turn off the instrument, turn off the power, and end the test.

[0087] In the above tests, the working electrodes used were catalyst materials and Si 3 N 4 Membrane electrode composition. The reference electrode is Ag-AgCl reference electrode. The counter electrode is a platinum wire electrode.

[0088] The parts not mentioned in this embodiment are the same as those in the first embodiment.

[0089] The above embodiments are preferred implementation modes of the invention, but the implementation modes of the present invention are not limited to the above embodiments. Any other changes, modifications, substitutions, combinations, and simplifications that do not deviate from the spirit and principles of the present invention should be equivalent replacement methods and are included in the protection scope of the present invention.

Claims

1. An electrochemical testing device combining infrared spectroscopy and online electrochemical mass spectrometry, Features: It includes a counter electrode module located at the upper layer, a flow electrolysis cell cavity module located at the middle layer, and an infrared spectrum interface module located at the lower layer; The flow electrolytic cell chamber module comprises an electrolytic cell chamber, a cathode chamber, a cathode liquid inlet, a cathode liquid outlet, a mass spectrometer inlet, a sample delivery port, a reference electrode interface, a working electrode and a reference electrode. The cathode chamber is arranged on the electrolytic cell chamber, the cathode liquid inlet, the cathode liquid outlet, the sample delivery port and the reference electrode interface are all connected to the cathode chamber, the mass spectrometer inlet is located between the sample delivery port and the cathode chamber, the reference electrode interface is used to install the reference electrode, the working electrode is located at the bottom of the cathode chamber, the cathode electrolyte flows in through the cathode liquid inlet and flows out through the cathode liquid outlet, the mass spectrometer inlet is annular and comprises a support sheet and a mass spectrometer filter membrane, the mass spectrometer inlet is used to separate the gas in the cathode electrolyte, and the gas flows out from the sample delivery port; The counter electrode module comprises a negative electrode cover, a negative electrode chamber, a negative electrode liquid inlet, a negative electrode liquid outlet, a counter electrode interface and a counter electrode, wherein the negative electrode chamber is arranged on the negative electrode cover, the negative electrode liquid inlet, the negative electrode liquid outlet and the counter electrode interface are all connected to the negative electrode chamber, the negative electrode electrolyte flows into the negative electrode chamber through the negative electrode liquid inlet and flows out through the negative electrode liquid outlet, and the counter electrode interface is used to install the counter electrode; The positive electrode chamber is located below the negative electrode chamber, and the positive electrode chamber and the negative electrode chamber are separated by an ion exchange membrane; The infrared spectrum interface module includes a prism and an infrared optical window, wherein the infrared optical window is located at the bottom of the working electrode, and the prism is located below the infrared optical window; The support sheet is a ring-shaped stainless steel foam body, and the mass spectrometer filter membrane is a ring-shaped porous polytetrafluoroethylene film; The positive electrode chamber includes an upper chamber, a lower chamber and a capillary channel. The upper chamber is separated from the negative electrode chamber by an ion exchange membrane. The working electrode is located at the bottom of the lower chamber. The upper chamber and the lower chamber are connected by a capillary channel. The positive electrode liquid outlet is located at the bottom of the upper chamber, and the positive electrode liquid outlet and the mass spectrometer inlet are located at the top of the lower chamber.

2. An electrochemical testing device combining infrared spectroscopy and online electrochemical mass spectrometry according to claim 1, Features: There are multiple capillary channels, the upper ends of the capillary channels are connected to the outer edge of the upper chamber, the lower ends of the capillary channels are connected to the outer edge of the lower chamber, the positive electrode liquid outlet is located at the center of the bottom end of the upper chamber, and the positive electrode liquid outlet is located at the center of the top end of the lower chamber.

3. An electrochemical testing device combining infrared spectroscopy and online electrochemical mass spectrometry according to claim 1, Features: The materials of the prism are sapphire glass, calcium fluoride or potassium bromide.

4. An electrochemical testing device combining infrared spectroscopy and online electrochemical mass spectrometry according to claim 1, Features: The infrared optical window is a Si3N4 crystal film, and the working electrode is a gold coating deposited on the Si3N4 crystal film or a conductive carbon material layer deposited on a mass spectrometer filter membrane.

5. An electrochemical testing device combining infrared spectroscopy and online electrochemical mass spectrometry according to claim 1, Features: The reference electrode is a silver chloride electrode, a mercury oxide electrode or a reversible hydrogen electrode, and the counter electrode is a platinum wire electrode, a nickel mesh electrode, a graphite rod electrode or a carbon mesh electrode.

6. An electrochemical testing device combining infrared spectroscopy and online electrochemical mass spectrometry according to claim 1, Features: The infrared spectrum interface module also includes a prism cover, the upper end of the prism cover is provided with a groove, the bottom of the groove is provided with a through hole, the infrared optical window and the working electrode are installed in the groove, and the prism is installed in the through hole.

7. An electrochemical testing device combining infrared spectroscopy and online electrochemical mass spectrometry according to claim 1, Features: It also includes an ion exchange membrane cover, in which the ion exchange membrane is installed. A first sealing ring is provided between the ion exchange membrane cover and the electrolytic cell cavity, and between the working electrode and the electrolytic cell cavity, respectively. A second sealing ring is provided between the ion exchange membrane cover and the negative electrode cover. Both the first sealing ring and the second sealing ring are fluororubber rings.

8. An electrochemical testing device combining infrared spectroscopy and online electrochemical mass spectrometry according to claim 1, Features: It also includes a plurality of connecting pipes, which are respectively connected to the negative electrode liquid inlet, the negative electrode liquid outlet, the positive electrode liquid inlet, the positive electrode liquid outlet and the sample delivery port, and a third sealing ring is provided between the connecting pipe and the electrolytic cell cavity or the negative electrode cover, and the third sealing ring is a fluororubber ring; The connecting pipeline is composed of a first screw with a hole and a hollow steel pipe. The first screw with a hole is fixedly sleeved on the outer side of the hollow steel pipe. The first screw with a hole connects the electrolytic cell cavity and the negative electrode cover through threads.

Images