System and method for rapidly testing performance of solar thermochemical cycle material
By integrating gas switching, heating, and analysis subsystems, and utilizing Joule heating with ring-shaped graphite electrodes and vacuum chamber protection, the problem of slow heating and cooling rates in traditional equipment has been solved. This enables rapid and accurate testing of the properties of solar thermochemical cycle materials, adapts to large-size samples, and ensures system stability and data reliability.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- SOUTHERN UNIVERSITY OF SCIENCE AND TECHNOLOGY
- Filing Date
- 2025-12-17
- Publication Date
- 2026-04-28
AI Technical Summary
In existing technologies, testing methods that maintain stable material properties are time-consuming and difficult to use for characterizing the kinetic characteristics of large-sized samples. In particular, in solar thermochemical cycle systems, the heating and cooling rates of traditional equipment are slow and cannot meet the needs of rapid testing.
By integrating a gas switching subsystem, a heating subsystem, and a gas analysis subsystem, and utilizing a ring-shaped graphite electrode for Joule heating combined with vacuum chamber protection, it achieves rapid and uniform testing of large samples with a heating and cooling rate exceeding 1000℃/min. The gas atmosphere switching and temperature control are precise, simulating a real cyclic environment.
It enables rapid and accurate material performance testing, shortens testing time from days/weeks to hours, adapts to different sample morphologies, ensures stable system operation, and provides high data reliability. It is suitable for samples ranging from trace powders to macroscopic bulk samples.
Smart Images
Figure CN121933563A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of energy materials technology, and in particular to a rapid testing system and method for the performance of materials used in solar thermochemical cycles. Background Technology
[0002] For a practical thermochemical cycle system, in addition to requirements on the redox properties of materials, maintaining stable material properties is also crucial for the long-term efficient operation of the system. Therefore, rapidly achieving multi-cycle testing of material properties is helpful for the design, development, and screening of thermochemical cycle materials.
[0003] Current testing methods for maintaining stable material properties, such as tube furnace heating and thermogravimetric analysis, have very slow heating and cooling rates, typically only 5-20 °C / min; for multi-cycle testing, the time cost is significant. Infrared heating furnaces can provide heating and cooling rates as high as 400 °C / min, but due to the small core heating area, there are limitations on the mass (usually <1g) and morphology (generally only powder) of the material sample, making it difficult to characterize the kinetic characteristics of thermochemically cycled materials in actual reactors.
[0004] Therefore, existing technologies need to be improved. Summary of the Invention
[0005] In view of the shortcomings of the prior art, the purpose of this invention is to provide a rapid testing system and method for the properties of solar thermochemical cycle materials, aiming to solve the problems that existing testing systems are time-consuming and difficult to use for characterizing the kinetic characteristics of large-size samples.
[0006] The technical solution of the present invention is as follows: In a first aspect, the present invention provides a rapid testing system for the properties of materials used in solar thermochemical cycles, comprising: The gas switching subsystem is used to achieve timed cyclic switching of the gas atmosphere; The heating subsystem includes a reaction chamber for containing a test sample, a ring-shaped graphite electrode sleeved outside the reaction chamber, a vacuum chamber disposed outside the ring-shaped graphite electrode, and a temperature controller connected to the ring-shaped graphite electrode. The ring-shaped graphite electrode is used to heat the reaction chamber by Joule heating, and the temperature controller is used to control the heating power of the ring-shaped graphite electrode. The gas analysis subsystem is used for real-time monitoring and analysis of gas components and concentrations during the testing process; The outlet of the gas switching subsystem is connected to the inlet of the reaction chamber, and the outlet of the reaction chamber is connected to the inlet of the gas analysis subsystem.
[0007] It should be noted that the reaction chamber can be made of a quartz tube, and the diameter of the tube and the size of the annular graphite electrode can be adjusted to change the size of the uniform heating area and adapt to test material samples of different qualities or morphologies.
[0008] Optionally, the gas switching subsystem includes at least two parallel gas supply lines; each gas supply line includes: Solenoid valves are installed on each of the aforementioned gas supply lines to control the opening and closing of the corresponding gas lines; The intelligent relay is electrically connected to each of the solenoid valves and is used to perform timed cyclic control of the circuit channels of the multiple solenoid valves to achieve automatic timed switching of the gas atmosphere.
[0009] Optionally, the gas switching subsystem further includes a gas flow controller, which is installed on each of the gas supply pipelines to precisely control the flow rate of each gas.
[0010] Optionally, the heating subsystem further includes an infrared thermometer for real-time monitoring of the sample temperature within the reaction chamber; the temperature controller is communicatively connected to the infrared thermometer to form a closed-loop temperature control circuit.
[0011] It should be noted that the temperature controller in this embodiment can adjust the heating power of the annular graphite electrode in real time according to the feedback signal of the infrared thermometer, so as to achieve rapid temperature control with a heating and cooling rate of more than 1000℃ / min.
[0012] Optionally, the heating subsystem further includes a water chiller and a vacuum pump, wherein the water chiller is used to cool the vacuum chamber and the vacuum pump is used to evacuate the vacuum chamber to remove oxidizing gases therein.
[0013] Optionally, the gas analysis subsystem is an infrared flue gas analyzer.
[0014] Secondly, the present invention provides a method for rapid testing of the performance of materials used in solar thermochemical cycles, comprising the following steps: S1. Place the material sample to be tested into the reaction chamber; according to the test requirements, set the temperature program in the temperature controller, and set the gas atmosphere switching program corresponding to each temperature stage in the gas switching subsystem. S2. Start the vacuum pump to evacuate the vacuum chamber and remove the oxidizing gas therein; then, introduce the initial reaction gas into the reaction chamber through the gas switching subsystem. S3. Start the heating program of the temperature controller to perform Joule heating on the sample through the annular graphite electrode; at the same time, start the gas analysis subsystem to continuously monitor and record the gas composition. S4. After the test, acquire and analyze temperature-time data and gas composition-time data to evaluate material performance.
[0015] Beneficial Effects: This invention provides a rapid testing system and method for the performance of materials in a solar thermochemical cycle. Through a core heating structure of "reaction chamber - ring-shaped graphite electrode - vacuum chamber," integrated with an automatic switching gas switching subsystem at the front end and a closed-loop gas analysis subsystem at the back end, this invention synergistically produces the following overall beneficial effects: Fast: Extremely fast heating and cooling rates (>1000°C / min), reducing the total time for multi-cycle testing from "days / weeks" to "hours".
[0016] Accuracy: It allows for precise programmable control of the coordinated changes in temperature and atmosphere, highly simulating real-world cyclic environments, and providing accurate and reliable data.
[0017] Wide range: It can test samples ranging from trace powders to macroscopic bulk materials, breaking through the sample limitations of existing rapid testing equipment.
[0018] Stability: The vacuum protection design ensures the long-term stable operation of the system core. Attached Figure Description
[0019] Figure 1 This is a schematic diagram of the structure of the rapid testing system for the performance of solar thermochemical cycle materials according to Embodiment 1 of the present invention. Detailed Implementation
[0020] This invention provides a rapid testing system and method for the performance of materials used in solar thermochemical cycles. To make the objectives, technical solutions, and effects of this invention clearer and more explicit, the invention is further described in detail below. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the invention.
[0021] Solar-driven two-step thermochemical cycle decomposition of H2O / CO2 to produce H2 / CO is an effective route for renewable fuel synthesis. Compared to direct pyrolysis of H2O / CO2, the introduction of metal oxides in this two-step thermochemical cycle can effectively reduce the reaction temperature and achieve product separation. Currently, cerium oxide, a representative material, possesses good redox properties and stability; however, its high reduction temperature requirement (>1500℃) leads to significant sensible heat loss during the cycle, limiting the fuel efficiency of the thermochemical cycle. Emerging perovskite metal oxides offer significant material design potential. By controlling the doping elements and their proportions to achieve appropriate enthalpy and high entropy, the reaction temperature during reduction can be effectively reduced, thus becoming a possible pathway to improve the fuel efficiency of thermochemical cycles. For a practical thermochemical cycle system, in addition to requirements for the redox properties of the materials, maintaining stable material performance is also crucial for the long-term efficient operation of the system.
[0022] Current testing methods for maintaining stable material properties either have slow heating rates, resulting in high time costs, or small core heating areas, making them unsuitable for characterizing large-sized samples.
[0023] Therefore, it is necessary to develop a material performance testing system that can achieve large-mass sample loading and meet the requirements of rapid heating and cooling.
[0024] This embodiment provides a rapid testing system for the properties of materials used in solar thermochemical cycles, such as... Figure 1 As shown, it includes: Gas switching subsystem 1 is used to realize timed cyclic switching of gas atmosphere; The heating subsystem 2 includes a reaction chamber 21 for containing a test sample, an annular graphite electrode 22 sleeved outside the reaction chamber 21, a vacuum chamber 23 disposed outside the annular graphite electrode 22, and a temperature controller 24 connected to the annular graphite electrode 22. The annular graphite electrode 22 is used to heat the reaction chamber 21 by Joule heating, and the temperature controller 24 is used to control the heating power of the annular graphite electrode 22. Gas analysis subsystem 3 is used for real-time monitoring and analysis of gas components and concentrations during the testing process; The outlet of the gas switching subsystem 1 is connected to the inlet of the reaction chamber 21, and the outlet of the reaction chamber 21 is connected to the inlet of the gas analysis subsystem 3.
[0025] It should be noted that this embodiment consists of three functional subsystems connected in a specific way to form an organic whole. The unique structure of the heating subsystem 2, characterized by a three-layer structure of "reaction chamber 21 - annular graphite electrode 22 - vacuum chamber 23," enables rapid, uniform, and large-sample testing. The use of "annular graphite electrode" for "Joule heating" is fundamentally different from the radiant heating of traditional tube furnaces and infrared lamps, and is the basis for achieving ultra-high-speed heating and cooling (>1000℃ / min). The dedicated vacuum chamber 23 encloses the graphite electrode, which prevents oxidation and ablation at high temperatures, greatly extending the lifespan of the core heating element; secondly, it creates a low-pressure insulating environment, reducing heat dissipation and improving thermal efficiency while protecting external components and the environment. This embodiment connects the three stages of "atmosphere control - programmed heating - product analysis" to construct a complete, closed-loop experimental platform specifically for testing the performance of solar thermochemical cycle materials, distinguishing it from general-purpose or single-function testing equipment (such as standalone thermogravimetric analyzers or tube furnaces). This embodiment uses Joule heating to solve the problem of "how to quickly and repeatedly simulate a complete, atmosphere-alternating chemical cycle process," which differs from the problem-oriented approach of using Joule heating to quickly reach high temperatures. Therefore, this embodiment is the first to apply Joule heating technology to "multi-cycle, automated, high-throughput testing of the performance of solar thermochemical cycle materials," and has designed a completely new system architecture and collaborative control method for this purpose.
[0026] Furthermore, the reaction chamber 21 can be made of a quartz tube, the diameter of which and the size of the annular graphite electrode 22 can be adjusted to change the size of the uniform heating area and adapt to test material samples of different qualities or morphologies.
[0027] In one embodiment, the gas switching subsystem 1 includes at least two parallel gas supply lines; each gas supply line includes: Solenoid valve 11 is installed on each of the gas supply pipelines and is used to control the opening and closing of the corresponding gas path; The intelligent relay 12 is electrically connected to each of the solenoid valves 11 and is used to perform timed cyclic control of the circuit channels of the multiple solenoid valves 11 to realize automatic timed switching of the gas atmosphere.
[0028] This embodiment employs a modular electrical control scheme consisting of "12 intelligent relays + 11 solenoid valves". The intelligent relays, acting as programmable timing controllers, directly drive the switching of the solenoid valves with their multiple output signals, thereby precisely controlling the on / off sequence of each gas path. Compared to using expensive dynamic gas distribution instruments or relying on manual switching, this scheme provides a low-cost, highly reliable, intuitively programmable solution that is easy to synchronize with temperature controllers. It is the key execution component for achieving "fully automated" and "multi-cycle" testing processes, significantly reducing labor costs and operational errors.
[0029] In one embodiment, the gas switching subsystem 1 further includes a gas flow controller 13, which is disposed on each of the gas supply pipelines for precisely controlling the flow rate of each gas.
[0030] This embodiment further introduces a gas flow controller 13, typically a mass flow controller (MFC). It can receive analog signals to achieve continuous, precise, and stable regulation of the gas flow rate. With the addition of the gas flow controller 13, the system can not only control the "type" and "sequence" of the gas, but also precisely control the "flow rate." This is crucial for material performance testing, as the space velocity (flow rate / catalyst mass) of the reactant gas is a key parameter affecting reaction kinetics and apparent properties. This feature ensures the accuracy of test conditions and the repeatability and comparability of experimental data, enhancing the scientific value of the test results.
[0031] In one embodiment, the heating subsystem 2 further includes an infrared thermometer 25 for real-time monitoring of the sample temperature inside the reaction chamber 21; the temperature controller 24 is communicatively connected to the infrared thermometer 25 to form a closed-loop temperature control circuit.
[0032] In this embodiment, the infrared thermometer 25 serves as a temperature sensor and is communicatively connected to the temperature controller 24, forming a closed-loop control circuit of "measurement-comparison-adjustment". This embodiment uses an infrared thermometer, avoiding the lag and inconvenience of contact temperature measurement methods such as thermocouples in ultra-rapid temperature change scenarios, resulting in faster response and better suitability for the characteristics of this system. Closed-loop control enables the system to operate strictly according to preset complex temperature curves (such as multi-stage heating and cooling, and isothermal control), rather than simply providing heating power. This is a prerequisite for simulating specific temperature processes in real thermochemical cycles. While pursuing extremely high heating and cooling rates, closed-loop control can prevent temperature overshoot or runaway, ensuring the safety of the testing process and the validity of the data.
[0033] It should be noted that the temperature controller 24 in this embodiment can adjust the heating power of the annular graphite electrode 22 in real time according to the feedback signal of the infrared thermometer 25, so as to achieve rapid temperature control with a heating and cooling rate of more than 1000℃ / min.
[0034] In one embodiment, the heating subsystem 2 further includes a water chiller 26 and a vacuum pump 27, wherein the water chiller 26 is used to cool the vacuum chamber 23, and the vacuum pump 27 is used to evacuate the vacuum chamber 23 to remove oxidizing gases therein.
[0035] The vacuum pump in this embodiment can not only "remove oxidizing gases", but also establish and maintain the low-pressure environment required by the vacuum chamber 23. The water chiller 26 actively cools the vacuum chamber, playing a triple role: protecting the sealing materials and structure of the vacuum chamber and preventing overheating damage; serving as an additional heat dissipation means to help achieve a faster cooling rate when rapid cooling is required; and maintaining the stability of the external ambient temperature of the system to ensure the normal operation of other electronic components.
[0036] In one embodiment, the gas analysis subsystem 3 is an infrared flue gas analyzer.
[0037] This embodiment uses an infrared flue gas analyzer that can continuously, online, and rapidly measure the concentration of key gas components such as H2O, CO2, and CO. The equipment is relatively mature and reliable.
[0038] This embodiment also provides a method for rapid testing of the performance of materials used in solar thermochemical cycles, including the following steps: S1. Parameter setting: Place the sample of the material to be tested into the reaction chamber 21; according to the test requirements, set the temperature program in the temperature controller 24, and set the gas atmosphere switching program corresponding to each temperature stage in the gas switching subsystem 1. S2. Initialization of the reaction environment: Start the vacuum pump 27 to evacuate the vacuum chamber 23 and remove the oxidizing gas therein; then, introduce the initial reaction gas into the reaction chamber 21 through the gas switching subsystem 1. S3. Automatic Cyclic Test: The heating program of the temperature controller 24 is started, and the sample is Joule heated through the annular graphite electrode 22; at the same time, the gas analysis subsystem 3 is started to continuously monitor and record the gas composition. During the test, the temperature controller 24 controls the power of the annular graphite electrode 22 according to the set program to achieve rapid heating and cooling of the sample; at the same time, the gas switching subsystem 1 automatically and periodically switches the type of gas introduced into the reaction chamber 21 according to its set switching program to match the current temperature stage. S4. Data Acquisition and Analysis: After the test, acquire and analyze temperature-time data and gas composition-time data to evaluate material performance.
[0039] In summary, this invention provides a rapid testing system and method for the performance of materials used in solar thermochemical cycles. The invention comprises three functional subsystems connected in a specific manner to form an organic whole. The unique structure of the heating subsystem 2—a three-layer structure characterized by a reaction chamber 21, a ring-shaped graphite electrode 22, and a vacuum chamber 23—enables rapid, uniform, and large-sample testing. The use of a ring-shaped graphite electrode for Joule heating is fundamentally different from the radiant heating of traditional tube furnaces and infrared lamps, and is the basis for achieving ultra-high-speed heating and cooling (>1000℃ / min). The dedicated vacuum chamber 23 encloses the graphite electrode, preventing oxidation and ablation at high temperatures, significantly extending the lifespan of the core heating element; and creating a low-pressure, insulated environment, reducing heat dissipation, thus improving thermal efficiency and protecting external components and the environment. This embodiment connects the three stages of "atmosphere control - programmed heating - product analysis" to construct a complete, closed-loop experimental platform specifically for testing the performance of solar thermochemical cycle materials, distinguishing it from general-purpose or single-function testing equipment (such as standalone thermogravimetric analyzers or tube furnaces). This embodiment uses Joule heating to address the problem of "how to quickly and repeatedly simulate a complete, atmosphere-alternating chemical cycle process," which differs from the problem of how to quickly reach high temperatures using Joule heating. Therefore, this embodiment innovatively applies Joule heating technology to "multi-cycle, automated, high-throughput testing of the performance of solar thermochemical cycle materials," and designs a novel system architecture and collaborative control method for this purpose. Furthermore, the reaction chamber 21 can be made of a quartz tube, and its diameter and the size of the annular graphite electrode 22 are adjustable to change the size of the uniform heating area, adapting to test material samples of different qualities or morphologies.
[0040] It should be understood that the application of the present invention is not limited to the examples above. Those skilled in the art can make improvements or modifications based on the above description, and all such improvements and modifications should fall within the protection scope of the appended claims.
Claims
1. A rapid testing system for the properties of materials used in solar thermochemical cycles, characterized in that, include: The gas switching subsystem (1) is used to realize the timed cyclic switching of the gas atmosphere; The heating subsystem (2) includes a reaction chamber (21) for containing a test sample, an annular graphite electrode (22) sleeved outside the reaction chamber (21), a vacuum chamber (23) disposed outside the annular graphite electrode (22), and a temperature controller (24) connected to the annular graphite electrode (22). The annular graphite electrode (22) is used to heat the reaction chamber (21) by Joule heating, and the temperature controller (24) is used to control the heating power of the annular graphite electrode (22). The gas analysis subsystem (3) is used for real-time monitoring and analysis of gas components and concentrations during the testing process; The outlet of the gas switching subsystem (1) is connected to the inlet of the reaction chamber (21), and the outlet of the reaction chamber (21) is connected to the inlet of the gas analysis subsystem (3).
2. The rapid testing system for the properties of materials used in solar thermochemical cycles according to claim 1, characterized in that, The gas switching subsystem (1) includes at least two parallel gas supply lines; each gas supply line includes: Solenoid valves (11) are installed on each of the gas supply lines to control the opening and closing of the corresponding gas lines; The intelligent relay (12) is electrically connected to each of the solenoid valves (11) and is used to perform timed cyclic control on the circuit channels of the multiple solenoid valves (11) to realize automatic timed switching of the gas atmosphere.
3. The rapid testing system for the properties of materials used in solar thermochemical cycles according to claim 2, characterized in that, The gas switching subsystem (1) also includes a gas flow controller (13), which is installed on each of the gas supply pipelines to precisely control the flow rate of each gas.
4. The rapid testing system for the properties of materials used in solar thermochemical cycles according to claim 1, characterized in that, The heating subsystem (2) also includes an infrared thermometer (25) for real-time monitoring of the sample temperature in the reaction chamber (21); the temperature controller (24) is communicatively connected to the infrared thermometer (25) to form a closed-loop temperature control circuit.
5. The rapid testing system for the properties of materials used in solar thermochemical cycles according to claim 1, characterized in that, The heating subsystem (2) also includes a water chiller (26) and a vacuum pump (27). The water chiller (26) is used to cool the vacuum chamber (23), and the vacuum pump (27) is used to evacuate the vacuum chamber (23) to remove oxidizing gases therein.
6. The rapid testing system for the properties of materials used in solar thermochemical cycles according to claim 1, characterized in that, The gas analysis subsystem (3) is an infrared flue gas analyzer.
7. A test method for a rapid testing system for the properties of materials used in solar thermochemical cycles, as described in any one of claims 1-6, characterized in that, Includes the following steps: S1. Place the sample of the material to be tested into the reaction chamber (21); according to the test requirements, set the temperature program in the temperature controller (24) and set the gas atmosphere switching program corresponding to each temperature stage in the gas switching subsystem (1); S2. Evacuate the vacuum chamber (23) to remove the oxidizing gas; then, introduce the initial reaction gas into the reaction chamber (21) through the gas switching subsystem (1); S3. Start the heating program of the temperature controller (24) and perform Joule heating on the sample through the annular graphite electrode (22); at the same time, start the gas analysis subsystem (3) to continuously monitor and record the gas composition. S4. After the test, acquire and analyze temperature-time data and gas composition-time data to evaluate material performance.