Test fixture and test method for proton ceramic electrochemical reaction cell for ammonia synthesis

Abstract

The application belongs to the technical field of electrochemical reaction cell testing, and specifically discloses a testing fixture and a testing method for a proton ceramic electrochemical reaction cell for ammonia synthesis. The fixture comprises a cathode gas inlet ceramic tube and an anode gas inlet ceramic tube. The cathode gas inlet ceramic tube and the anode gas inlet ceramic tube are respectively wound with a first platinum mesh and a second platinum mesh at one end. The first platinum mesh is connected with a first platinum wire, and the second platinum mesh is connected with a second platinum wire. The first platinum wire and the second platinum wire are led out and connected with an external battery testing device. A quartz sleeve and a ceramic sleeve are respectively tightly sealed by stainless steel flanges. The testing fixture and the testing method for the proton ceramic electrochemical reaction cell for ammonia synthesis can ensure that the cathode and the anode have excellent air tightness. While ensuring air tightness and long-term stability, the fixture realizes complete collection of the cathode side reaction tail gas, and can meet the requirements of accurate analysis and detection of ammonia synthesis products.

Description

Technical Field

[0001] This invention relates to the field of electrochemical reaction cell testing technology, and in particular to a proton ceramic electrochemical reaction cell testing fixture and testing method for ammonia synthesis. Background Technology

[0002] Since the 20th century, the Haber-Bosch process has dominated global ammonia production, with an annual output exceeding 180 million tons. However, its equilibrium conversion rate is only 10%–15%, and it is highly dependent on fossil fuel routes such as methane reforming to produce hydrogen, resulting in its energy consumption accounting for 1%–2% of global energy consumption and accompanied by serious CO2 emissions. Faced with increasingly severe energy and environmental challenges, there is an urgent need to develop green and sustainable alternative technologies for ammonia synthesis. Electrochemical ammonia synthesis technology based on proton ceramic electrolytes uses N2 and H2 (or H2O) as raw materials and utilizes renewable electricity to drive the nitrogen reduction reaction. This method breaks through the thermodynamic energy barrier of N2 activation by using electricity, overcoming thermodynamic equilibrium limitations, and allowing the reaction to proceed under milder conditions, offering advantages such as low energy consumption, safe operation, and environmental friendliness. In this system, the directional migration of protons in the electrolyte separates the product NH3 and the feed gas on the cathode and anode sides, effectively avoiding side reactions.

[0003] Currently, most commonly used proton ceramic battery testing fixtures in laboratories only allow hydrogen gas to be introduced to the anode side, while the cathode side is usually directly exposed to the air environment. However, in electrochemical ammonia synthesis research, it is required that hydrogen gas (or water vapor) be continuously supplied to the anode side and nitrogen gas be continuously introduced to the cathode side, with complete collection of the cathode-side gases to meet the needs of subsequent accurate analysis and detection. The existing fixture design makes it difficult to achieve independent control and sealed collection of the atmosphere at both the anode and cathode, and cannot meet the special requirements of atmosphere isolation and product collection in the electrochemical ammonia synthesis reaction, thus restricting the development of related research.

[0004] Therefore, it is necessary to design a dual-gas-path closed-loop proton ceramic electrochemical reaction cell test fixture suitable for ammonia synthesis. This fixture achieves precise separation and stable supply of hydrogen (or water vapor) on the anode side and nitrogen on the cathode side by constructing independent gas-tight chambers on both the anode and cathode sides. Simultaneously, it integrates a highly efficient cathode-side gas extraction and collection structure to ensure complete extraction of reaction tail gas, meeting the requirements for online or offline analysis and detection. Furthermore, the fixture design fully considers gas-tight reliability under high-temperature conditions, current collection efficiency, and ease of assembly and operation, providing a structurally sound, functionally complete, and highly adaptable testing device for electrochemical ammonia synthesis research. Summary of the Invention

[0005] The purpose of this invention is to provide a testing fixture and method for a proton-ceramic electrochemical reaction cell used in ammonia synthesis. This fixture ensures excellent airtightness of both the cathode and anode gas paths, virtually eliminating test failures due to atmosphere cross-contamination or seal failure. While guaranteeing airtight isolation and long-term stability, the fixture also enables complete collection of the reaction tail gas on the cathode side, meeting the requirements for accurate analysis and detection of ammonia synthesis products.

[0006] To achieve the above objectives, the present invention provides a test fixture for a proton ceramic electrochemical reaction cell used in ammonia synthesis, comprising a cathode inlet ceramic tube and an anode inlet ceramic tube. One end of the cathode inlet ceramic tube and the anode inlet ceramic tube are respectively wound with a first platinum mesh and a second platinum mesh, which serve as current collectors and are in close contact with the cathode and anode of a button cell. A first platinum wire is connected to the first platinum mesh, and a second platinum wire is connected to the second platinum mesh. The first platinum wire and the second platinum wire are led out and connected to an external battery testing device. A ceramic sleeve is fitted over the anode inlet ceramic tube, and a quartz sleeve is fitted over the ceramic sleeve.

[0007] Preferably, one end of the quartz sleeve is sealed by pressing together a first stainless steel flange and a second stainless steel flange, with a first high-temperature resistant O-ring provided between the first and second stainless steel flanges; one end of the ceramic sleeve is sealed by pressing together a second stainless steel flange and a third stainless steel flange, with a second high-temperature resistant O-ring provided between the second and third stainless steel flanges; the other end of the ceramic sleeve is sealed and fixed to the anode side of the button battery by high-temperature adhesive, thereby achieving physical isolation between the anode and cathode atmospheres.

[0008] Preferably, the first stainless steel flange, the second stainless steel flange, and the third stainless steel flange are connected in sequence.

[0009] Preferably, both the first and second high-temperature resistant O-rings are made of high-temperature resistant rubber.

[0010] Preferably, one end of the anode inlet ceramic tube extends into the ceramic sleeve, and the second platinum mesh wound around its end contacts the anode of the button cell. The anode inlet ceramic tube is used to continuously introduce hydrogen or water vapor, and the gas inside the ceramic sleeve is discharged through the anode outlet tube, forming an independent gas path on the anode side. One end of the cathode inlet ceramic tube extends into the quartz sleeve, and the first platinum mesh wound around its end contacts the cathode of the button cell. The cathode inlet ceramic tube is used to continuously introduce nitrogen, and the gas inside the quartz sleeve is discharged through the cathode outlet ceramic tube and connected to a collection device containing ammonia absorbent, forming an independent gas path on the cathode side.

[0011] Preferably, the cathode inlet ceramic tube, anode inlet ceramic tube, ceramic sleeve, and quartz sleeve are all made of high-temperature resistant ceramic or quartz materials.

[0012] This invention also provides a testing method for a proton ceramic electrochemical reaction cell test fixture for ammonia synthesis, comprising the following steps: S1. The anode inlet ceramic tube is inserted into the ceramic sleeve, and the second platinum mesh is placed at the end of the ceramic sleeve. S2. The second and third stainless steel flanges are fitted into the ceramic sleeve, and a second high-temperature O-ring is placed between the second and third stainless steel flanges and pre-tightened for fixation. S3. The button cell anode side is sealed with high-temperature adhesive to the end of the ceramic sleeve, and the second platinum mesh is bonded to the button cell anode. S4. The quartz sleeve is inserted into the ceramic sleeve and connected to the second stainless steel flange. The first stainless steel flange is then fitted onto the other end of the quartz sleeve, and a first high-temperature O-ring is placed between the first and second stainless steel flanges. S5. The cathode inlet ceramic tube is inserted into the quartz sleeve, and the first platinum mesh is attached to the button cell cathode. S6. Tighten the first stainless steel flange and the third stainless steel flange in sequence to complete the airtight seal; lead out the first platinum wire and the second platinum wire and connect them to the external battery testing equipment; connect the anode gas outlet pipe and the cathode gas outlet ceramic pipe to the gas analysis or collection device respectively. S7. Fix the fixture to the vertical high-temperature furnace, introduce pure hydrogen or water vapor into the anode chamber, and introduce pure nitrogen into the cathode chamber for testing.

[0013] The advantages and beneficial effects of the above-mentioned proton ceramic electrochemical reaction cell test fixture and test method for ammonia synthesis in this invention are as follows: 1. This invention proposes a dual-sided independent airtight chamber to achieve precise isolation and stable supply of anode and cathode atmospheres, complete collection of cathode exhaust gas, and meet the requirements for accurate product detection.

[0014] 2. The multi-stage stainless steel flange and high-temperature O-ring sealing structure of this invention have excellent airtightness at high temperatures and no problems of atmosphere cross-contamination or sealing failure.

[0015] 3. The present invention features platinum mesh current collection and platinum wire current output, resulting in high current collection efficiency and stable contact.

[0016] 4. The present invention has a simple structure, readily available materials, and convenient assembly and disassembly. It is suitable for testing solid oxide batteries that require independent control of atmosphere on both sides in electrochemical ammonia synthesis and other applications.

[0017] The technical solution of the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. Attached Figure Description

[0018] Figure 1 This is a schematic diagram of the electrochemical reaction cell test fixture of the present invention; Figure 2This is a schematic cross-sectional view of the electrochemical reaction cell test fixture of the present invention; Figure 3 The XRD pattern of the SFM powder in this embodiment of the invention; Figure 4 This is a cross-sectional SEM image of the anode-supported proton ceramic battery in an embodiment of the present invention; Figure 5 These are the EIS spectra of the batteries at different temperatures in the embodiments of the present invention; Figure 6 These are the IV curves of the battery at different temperatures in the embodiments of the present invention; Figure 7 (a) shows the UV-Vis absorption spectra of ammonia gas at different concentrations determined by the indophenol determination method in this embodiment of the invention, and (b) shows the calibration curve for estimating ammonia gas concentration in this embodiment of the invention. Figure 8 The ammonia yield of the battery at different temperatures in the embodiments of the present invention are shown.

[0019] Figure Labels 1. First platinum wire; 2. Cathode outlet ceramic tube; 3. First platinum mesh; 4. Button cell; 5. Second platinum mesh; 6. Second platinum wire; 7. Ammonia absorbent; 8. Cathode inlet ceramic tube; 9. Quartz sleeve; 10. Anode inlet ceramic tube; 11. Ceramic sleeve; 12. First stainless steel flange; 13. First high-temperature resistant O-ring seal; 14. Second high-temperature resistant O-ring seal; 15. Second stainless steel flange; 16. Third stainless steel flange; 17. Anode outlet pipe. Detailed Implementation

[0020] The technical solution of the present invention will be further described below through embodiments.

[0021] Unless otherwise defined, the technical or scientific terms used in this invention shall have the ordinary meaning as understood by one of ordinary skill in the art to which this invention pertains.

[0022] The following examples are not intended to limit the invention, but are only for illustration. Unless otherwise specified, the experimental methods used in the following examples are generally performed under conventional conditions. Unless otherwise specified, the materials and reagents used in the following examples are commercially available.

[0023] Example 1 A proton ceramic electrochemical reaction cell test fixture for ammonia synthesis includes a cathode inlet ceramic tube 8 and an anode inlet ceramic tube 10. One end of the cathode inlet ceramic tube 8 and the anode inlet ceramic tube 10 are respectively wound with a first platinum mesh 3 and a second platinum mesh 5, which serve as current collectors and are in close contact with the cathode and anode of the button cell 4. A first platinum wire 1 is connected to the first platinum mesh 3, and a second platinum wire 6 is connected to the second platinum mesh 5. The first platinum wire 1 and the second platinum wire 6 are led out and connected to an external battery testing device. A ceramic sleeve 11 is fitted outside the anode inlet ceramic tube 10, and a quartz sleeve 9 is fitted outside the ceramic sleeve 11.

[0024] One end of the quartz sleeve 9 is sealed by pressing together the first stainless steel flange 12 and the second stainless steel flange 15, and a first high-temperature resistant O-ring 13 is provided between the first stainless steel flange 12 and the second stainless steel flange 15; one end of the ceramic sleeve 11 is sealed by pressing together the second stainless steel flange 15 and the third stainless steel flange 16, and a second high-temperature resistant O-ring 14 is provided between the second stainless steel flange 15 and the third stainless steel flange 16; the other end of the ceramic sleeve 11 is sealed and fixed to the anode side of the button battery 4 by high-temperature adhesive, so as to achieve physical isolation between the anode side and the cathode side atmosphere.

[0025] The first stainless steel flange 12, the second stainless steel flange 15, and the third stainless steel flange 16 are connected in sequence.

[0026] The first high-temperature resistant O-ring 13 and the second high-temperature resistant O-ring 14 are both made of high-temperature resistant rubber.

[0027] One end of the anode inlet ceramic tube 10 extends into the ceramic sleeve 11, and the second platinum mesh 5 wrapped around its end contacts the anode of the button cell 4. The anode inlet ceramic tube 10 is used to continuously introduce hydrogen or water vapor. The gas in the ceramic sleeve 11 is discharged through the anode outlet tube 17, forming an independent gas path on the anode side. One end of the cathode inlet ceramic tube 8 extends into the quartz sleeve 9, and the first platinum mesh 3 wrapped around its end contacts the cathode of the button cell 4. The cathode inlet ceramic tube 8 is used to continuously introduce nitrogen. The gas in the quartz sleeve 9 is discharged through the cathode outlet ceramic tube 2 and connected to a collection device containing ammonia absorbent 7, forming an independent gas path on the cathode side.

[0028] The cathode inlet ceramic tube 8, the anode inlet ceramic tube 10, the ceramic sleeve 11, and the quartz sleeve 9 are all made of high-temperature resistant ceramic or quartz materials.

[0029] The test method for the proton ceramic electrochemical reaction cell test fixture for ammonia synthesis includes the following steps: First, the anode inlet ceramic tube 10 is inserted into the ceramic sleeve 11, with the second platinum mesh 5 positioned at one end of the ceramic sleeve 11. Then, the second stainless steel flange 15 and the third stainless steel flange 16 are sequentially fitted onto the outside of the ceramic sleeve 11, and a second high-temperature resistant O-ring sealant 14 is placed between the second and third stainless steel flanges 15 and 16. Pre-tightening the third stainless steel flange 16 achieves initial fixation of the ceramic sleeve 11. Next, the anode side of the button battery 4 is sealed and fixed to that end of the ceramic sleeve 11 with high-temperature adhesive, ensuring close contact between the second platinum mesh 5 and the battery anode. Finally, the quartz sleeve 9 is fitted onto the outside of the ceramic sleeve 11, with one end of the quartz sleeve 9 aligned with the second stainless steel flange 15. A first high-temperature resistant O-ring seal 13 is placed between the first stainless steel flange 12 and the second stainless steel flange 15, and the first stainless steel flange 12 is fitted onto the other end of the quartz sleeve 9. Then, the cathode gas inlet ceramic tube 8 is inserted from this end of the quartz sleeve 9, so that the first platinum mesh 3 is tightly attached to the cathode of the button cell 4. Finally, the first stainless steel flange 12 and the third stainless steel flange 16 are pressed in sequence, and the first high-temperature resistant O-ring seal 13 and the second high-temperature resistant O-ring seal 14 achieve an airtight seal between the two ends of the quartz sleeve 9 and the ceramic sleeve 11. The first platinum wire 1 and the second platinum wire 6 are led out and connected to the external battery testing equipment, and the anode gas outlet tube 17 and the cathode gas outlet ceramic tube 2 are respectively connected to the gas analysis or collection device.

[0030] Fix the fixture to the vertical high-temperature furnace, introduce pure hydrogen or water vapor into the anode chamber, and introduce pure nitrogen into the cathode chamber for testing.

[0031] The gas passage is set up as follows: Figure 1 and Figure 2 As shown, one end of the anode inlet ceramic tube 10 extends into the ceramic sleeve 11, and the second platinum mesh 5 wound around its end contacts the anode of the button cell 4. The anode inlet ceramic tube 10 is used to continuously introduce hydrogen or water vapor to provide a reaction atmosphere for the anode side. The gas inside the ceramic sleeve 11 is discharged through the anode outlet tube 17, forming an independent gas path on the anode side. One end of the cathode inlet ceramic tube 8 extends into the quartz sleeve 9, and the first platinum mesh 3 wound around its end contacts the cathode of the button cell 4. The cathode inlet ceramic tube 8 is used to continuously introduce nitrogen to provide a reaction atmosphere for the cathode side. The gas inside the quartz sleeve 9 is discharged through the cathode outlet ceramic tube 2 and connected to a collection device containing ammonia absorbent 7, forming an independent gas path on the cathode side. This structural design allows the reaction tail gas on the cathode side to be completely extracted and collected, meeting the needs of subsequent accurate analysis and detection.

[0032] The working mechanism of the flange and sealing structure is as follows: Through the sequential connection and compression of the first stainless steel flange 12, the second stainless steel flange 15, and the third stainless steel flange 16, axial compression is achieved on the internal ceramic pipes and sealing rings. This causes the first high-temperature resistant O-ring 13 and the second high-temperature resistant O-ring 14 to undergo elastic deformation, thereby filling the tiny gap between the flange and the pipes, achieving reliable airtightness at high temperatures. Simultaneously, this flange compression structure ensures the relative positions of the ceramic pipes are fixed, allowing the first platinum mesh 3 and the second platinum mesh 5 to maintain good contact pressure with the battery electrodes, ensuring the stability of current collection during testing. This fixture has a reasonable structural design, readily available materials, and is easy to disassemble and assemble, making it particularly suitable for electrochemical ammonia synthesis research requiring independent control of both atmospheres and exhaust gas collection.

[0033] Example 2 Taking the testing of an anode-supported proton ceramic battery in electrochemical ammonia synthesis as an example, the present invention will be described in detail below with reference to the accompanying drawings.

[0034] I. Preparation and assembly of anode-supported proton ceramic batteries.

[0035] First, an anode-supported proton ceramic battery was prepared, including an anode support, an anode functional layer, an electrolyte, and a cathode.

[0036] Anode support: First, weigh out a certain amount of NiO and BaZr. 0.1 Ce 0.7 Y 0.1 Yb 0.1 O3 (BZCYYb) powder, with a mass ratio of 6:4, is then mixed with starch, ensuring the starch mass is 15% of the NiO-BZCYYb powder mass. The mixture is placed in a ball mill jar, anhydrous ethanol is added, and the mill is operated at 200 rpm. -1 Ball milling for 12 hours. Then drying in an oven to obtain support powder. The support powder was placed in a circular mold, held under 10 MPa pressure for 1 minute, and then demolded to obtain support blank. The blank was then placed in a muffle furnace for pre-sintering at 1000℃.

[0037] Anode functional layer: Weigh a certain amount of NiO and BZCYYb powder (mass ratio 6:4) into a ball mill jar, and add a certain amount of anhydrous ethanol, polyethylene glycol, polyvinyl butyral, triethanolamine and dimethyl phthalate. Then, mill at 250 rpm. -1 The anode functional layer was ball-milled at a certain speed for 12 hours to obtain the anode functional layer dropper solution. The anode dropper solution was used to drop the solution onto the surface of the support and dried at room temperature. Then, it was placed in a muffle furnace and slowly heated to 600°C to remove organic matter.

[0038] Electrolytes: Weigh a measured amount of BZCYYb powder into a ball mill jar, and add measured amounts of anhydrous ethanol, polyethylene glycol, polyvinyl butyral, triethanolamine, and dimethyl phthalate. Then, mill at 250 rpm. -1 The electrolyte coating solution was obtained by ball milling at a certain speed for 12 hours. The electrolyte coating solution was then applied to the surface of the anode functional layer using a dropper and dried at room temperature. Subsequently, the layer was placed in a muffle furnace and sintered at 1300℃ to obtain a half cell.

[0039] Cathode: First, Sr2Fe cathode powder was prepared using the glycine method. 1.5 Mo 0.5 O6 (SFM), weigh out Sr(NO3)2, Fe(NO3)3·6H2O and (NH4)6Mo7O according to the stoichiometric ratio. 24 Dissolve 4H₂O in deionized water and stir. Then, add glycine and citric acid monohydrate in a stoichiometric ratio (metal ion:glycine:citric acid monohydrate = 1:2:1.5). Stir the solution at 80°C until it becomes gel-like. Place the gel in an oven and heat at 200°C to obtain a dry, fluffy precursor. Finally, calcine the precursor in a muffle furnace at 1100°C to obtain SFM powder (XRD results are shown in [reference needed]). Figure 3 SFM and BZCYYb powders were mixed in a 6:4 ratio, and a binder (a mixture of ethyl cellulose and turpentine percolate) was added. The mixture was then ball-milled to obtain a cathode slurry. Finally, the cathode slurry was coated onto the surface of the half-cell, dried, and then sintered in a muffle furnace at 1050°C to obtain the desired anode-supported single cell. A cross-sectional SEM image of the cell is shown below. Figure 4 .

[0040] II. Electrochemical Testing.

[0041] After the test fixture was assembled, the battery performance was tested. The test fixture was fixed in a vertical high-temperature furnace by an iron frame (the heating and cooling rate was controlled by a temperature controller at 5℃ / min). Pure hydrogen gas was introduced into the anode chamber at a rate of 45 mL / min, and pure nitrogen gas was introduced into the cathode chamber at a rate of 15 mL / min. The test temperatures were 600℃, 500℃, 400℃, and 300℃.

[0042] The electrochemical performance of the battery was tested using an electrochemical workstation (Gamry), including electrochemical impedance spectroscopy and IV curves. The electrochemical impedance spectroscopy results show ( Figure 5 The battery polarization resistance shows a continuous increasing trend with decreasing temperature, and the polarization resistances at 600℃, 500℃, 400℃, and 300℃ are 15.9 Ωcm. 2 30.Ωcm 2 60.0Ωcm 2 and 491.6Ωcm 2IV curve results ( Figure 6 This indicates that the current density decreases continuously with decreasing temperature. At a voltage of -0.6V, the current densities at 600℃, 500℃, 400℃, and 300℃ are 656.5 mA / cm², respectively. -2 403.4mAcm -2 170.3mAcm -2 and 20.1mAcm -2 .

[0043] After the electrochemical nitrogen reduction reaction (NRR) proceeded for 30 minutes, the generated NH3 was completely absorbed by 10 mL of 0.01 mol / L HCl solution. Subsequently, the NH4-containing solution was purified using the indophenol blue method. + The 0.01 mol / L HCl absorption solution was used for detection and quantitative analysis. The specific procedure was as follows: First, 2 mL of the solution was transferred from the 0.01 mol / L HCl absorption solution, then 2 mL of colorimetric solution (1 mol / L NaOH solution containing 5 wt% salicylic acid and 5 wt% sodium citrate) was added. Subsequently, 1 mL of oxidizing solution prepared with 0.05 mol / L NaClO and 0.2 mL of catalyst solution (1 wt% sodium nitrosoferricyanide, Na2[Fe(CN)5NO]·2H2O) were added sequentially. After the mixed solution was allowed to stand at room temperature in the dark for 1 hour, it was detected at a wavelength of 655 nm using a Lambda 35 UV-Vis spectrophotometer. The yield of NH3 was determined using a standard curve calibrated with NH4Cl solution (y = 0.5615x + 0.0432, R...). 2 Quantitative calculations were performed using the formula (=0.999), see [link / reference]. Figure 7 The ammonia yields obtained at different temperatures using the SFM electrode in this test are shown in the figure. Figure 8 The highest ammonia yield of 70.09 μg·h was achieved at 600℃ and -0.6V. -1 ·cm -2 .

[0044] Therefore, the above-mentioned proton ceramic electrochemical reaction cell test fixture and test method for ammonia synthesis in this invention can ensure excellent airtightness of the cathode and anode gas paths, and almost eliminate the possibility of test failure due to atmosphere cross-contamination or seal failure. While ensuring airtight isolation and long-term stability, the fixture achieves complete collection of the reaction tail gas on the cathode side, which can meet the requirements for accurate analysis and detection of ammonia synthesis products.

[0045] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and not to limit them. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can still be made to the technical solutions of the present invention, and these modifications or equivalent substitutions cannot cause the modified technical solutions to deviate from the spirit and scope of the technical solutions of the present invention.

Claims

1. A test fixture for a proton-ceramic electrochemical reaction cell used in ammonia synthesis, characterized in that: The device includes a cathode inlet ceramic tube and an anode inlet ceramic tube. One end of each ceramic tube is wound with a first platinum mesh and a second platinum mesh, respectively, serving as current collectors that are in close contact with the cathode and anode of the button cell. A first platinum wire is connected to the first platinum mesh, and a second platinum wire is connected to the second platinum mesh. The first and second platinum wires are led out and connected to external battery testing equipment. A ceramic sleeve is fitted over the anode inlet ceramic tube, and a quartz sleeve is fitted over the ceramic sleeve.

2. The proton-ceramic electrochemical reaction cell test fixture for ammonia synthesis according to claim 1, characterized in that: One end of the quartz sleeve is sealed by pressing together a first stainless steel flange and a second stainless steel flange, with a first high-temperature resistant O-ring between the first and second stainless steel flanges; one end of the ceramic sleeve is sealed by pressing together a second stainless steel flange and a third stainless steel flange, with a second high-temperature resistant O-ring between the second and third stainless steel flanges; the other end of the ceramic sleeve is sealed and fixed to the anode side of the button cell by high-temperature adhesive, achieving physical isolation between the anode and cathode atmospheres.

3. The proton-ceramic electrochemical reaction cell test fixture for ammonia synthesis according to claim 2, characterized in that: The first stainless steel flange, the second stainless steel flange, and the third stainless steel flange are connected in sequence.

4. The proton-ceramic electrochemical reaction cell test fixture for ammonia synthesis according to claim 2, characterized in that: Both the first and second high-temperature resistant O-rings are made of high-temperature resistant rubber.

5. The proton-ceramic electrochemical reaction cell test fixture for ammonia synthesis according to claim 1, characterized in that: One end of the anode inlet ceramic tube extends into the ceramic sleeve, and the second platinum mesh wound around its end contacts the anode of the button cell. The anode inlet ceramic tube is used to continuously introduce hydrogen or water vapor, and the gas inside the ceramic sleeve is discharged through the anode outlet tube, forming an independent gas path on the anode side. One end of the cathode inlet ceramic tube extends into the quartz sleeve, and the first platinum mesh wound around its end contacts the cathode of the button cell. The cathode inlet ceramic tube is used to continuously introduce nitrogen, and the gas inside the quartz sleeve is discharged through the cathode outlet ceramic tube and connected to a collection device containing ammonia absorbent, forming an independent gas path on the cathode side.

6. The proton-ceramic electrochemical reaction cell test fixture for ammonia synthesis according to claim 1, characterized in that: The cathode inlet ceramic tube, anode inlet ceramic tube, ceramic sleeve, and quartz sleeve are all made of high-temperature resistant ceramic or quartz materials.

7. The test method for the proton-ceramic electrochemical reaction cell test fixture for ammonia synthesis according to any one of claims 1-6, characterized in that, Includes the following steps: S1. The anode inlet ceramic tube is inserted into the ceramic sleeve, and the second platinum mesh is placed at the end of the ceramic sleeve. S2. The second and third stainless steel flanges are fitted into the ceramic sleeve, and a second high-temperature O-ring is placed between the second and third stainless steel flanges and pre-tightened for fixation. S3. The button cell anode side is sealed with high-temperature adhesive to the end of the ceramic sleeve, and the second platinum mesh is bonded to the button cell anode. S4. The quartz sleeve is inserted into the ceramic sleeve and connected to the second stainless steel flange. The first stainless steel flange is then fitted onto the other end of the quartz sleeve, and a first high-temperature O-ring is placed between the first and second stainless steel flanges. S5. The cathode inlet ceramic tube is inserted into the quartz sleeve, and the first platinum mesh is attached to the button cell cathode. S6. Tighten the first stainless steel flange and the third stainless steel flange in sequence to complete the airtight seal; lead out the first platinum wire and the second platinum wire and connect them to the external battery testing equipment; connect the anode gas outlet pipe and the cathode gas outlet ceramic pipe to the gas analysis or collection device respectively. S7. Fix the fixture to the vertical high-temperature furnace, introduce pure hydrogen or water vapor into the anode chamber, and introduce pure nitrogen into the cathode chamber for testing.

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