Device and test method for measuring high-temperature discharge amount of material under rapid heating condition

Abstract

The invention discloses a device for measuring the high-temperature degassing amount of a material under a rapid heating condition and a test method, and aims to provide an efficient and accurate measurement means to meet the requirements of material scientific research and industrial application on high-temperature degassing amount test. The device mainly comprises a heating cavity, a heating control system, a vacuum system, a temperature measuring system, a pressure measuring system, a gas collecting system and a data collecting and processing system. According to the invention, a diffusion cavity design in a traditional method is canceled, and the heating system is directly contacted with the sample cavity, so that the heating efficiency is improved, and the system structure is simplified; nonlinear change of the resistance value along with the temperature in the Joule heating process is compensated through a real-time resistance feedback regulation and control mechanism, high-temperature uniform temperature rise control is achieved, rapid and accurate measurement of the high-temperature deflation amount of the material can be achieved, and the requirements of modern scientific research and industrial fields for high-temperature performance testing are met.

Description

Technical Field

[0001] The present invention relates to a device and a testing method for measuring the amount of gas released by a material at high temperature under rapid heating conditions. The device belongs to the field of materials science and testing technology, and is particularly used to measure the amount of gas released by a material under high temperature conditions. The device is widely used in fields such as materials research, aerospace, and the electronics industry, and is particularly suitable for occasions where the amount of gas released by a material at high temperature needs to be measured quickly and accurately. Background Art

[0002] With the continuous advancement of materials science, especially in high-tech fields such as aerospace and electronics, studying the performance of materials under high-temperature conditions has become increasingly important. Many materials release gases at high temperatures, and these gases have a significant impact on their performance, lifespan, and even structural safety. In certain application scenarios, the thermal behavior of materials can change significantly in a very short period of time, making rapid and accurate measurement of high-temperature outgassing crucial. Traditional devices have slow heating rates and are often unable to simulate the rapid thermal loads experienced in high-temperature environments. In particular, some new high-performance materials can exhibit significant differences in their gas release behavior at different heating rates, making an excessively slow heating process inaccurately reflect their performance under extreme conditions. Furthermore, some existing high-temperature outgassing measurement devices require an additional diffusion chamber to separate the heating and measurement regions. While this design can somewhat mitigate the impact of temperature fluctuations in the heating region on the measurement region, it also presents a number of challenges. First, the presence of a diffusion chamber increases the complexity of the device, making the system larger and more difficult to operate. Second, the temperature difference between the diffusion chamber and the measurement region can lead to uneven heat transfer, affecting the actual heating state of the material and, consequently, compromising measurement accuracy. Furthermore, the complexity of the device also leads to longer system response times, hindering rapid and accurate high-temperature outgassing measurements. In this case, traditional heating methods can lead to significant discrepancies between test results and actual application environments. Therefore, rapid heating testing has become a key requirement in the study of high-temperature material properties. Summary of the Invention

[0003] The technical problem solved by the present invention is: to overcome the shortcomings of the existing technology and provide a device and a testing method for measuring the amount of gas released by materials at high temperatures under rapid heating conditions, so as to achieve rapid and accurate measurement of the amount of gas released by materials at high temperatures. The specific technical solution includes the following parts.

[0004] The technical solution of the present invention is: in the first aspect, a device for measuring the amount of gas released by a material at high temperature under rapid heating conditions, comprising:

[0005] A heating chamber is provided, wherein a test sample is filled therein, and both ends of the test sample are in contact with graphite electrodes; one end of the heating chamber is connected to a pressure measurement system via a sealing flange, and the other end is connected to a vacuum system, a gas collection system, and a pressure relief valve via a sealing flange; an exhaust valve is installed between the heating chamber and the vacuum system; and an isolation valve is installed between the heating chamber and the gas collection system; both ends of the graphite electrodes on both sides of the heating chamber are connected to the inner end surface of the sealing flange via high-temperature resistant springs, thereby realizing a conductive path for heating the test sample under the control of a heating control system;

[0006] A vacuum system, used to create a vacuum environment for the heating chamber;

[0007] A temperature measurement system is used to measure the temperature of the test sample position and send the temperature signal to the heating control system and the data acquisition and processing system;

[0008] A pressure measurement system is used to measure the pressure inside the heating chamber and send the pressure signal to the data acquisition and processing system;

[0009] Gas collection system, used to collect the gas released during the testing process of the test sample;

[0010] Data acquisition and processing system, used to collect data from the temperature measurement system and pressure measurement system in real time;

[0011] The heating control system is used to control the temperature of the graphite electrode according to the input temperature signal.

[0012] Furthermore, the graphite electrode is a hollow tubular structure with a resistance value of ≤5Ω.

[0013] Furthermore, the graphite electrode conducts a current of up to 200A, ensuring that the test sample is heated to the preset temperature within milliseconds, with a maximum heating rate of not less than 10 5 ℃ / s, the maximum temperature is not less than 1000℃.

[0014] Furthermore, the heating chamber is a quartz double-tubular structure, including an inner tube and an outer tube; the inner tube has an inner diameter of 5 to 50 mm and a length of 50 to 500 mm, and is used to hold test samples; the outer tube has an inner diameter of 100 to 500 mm and a length of 100 to 550 mm, and is connected to the inner tube and the vacuum system. The heating chamber is evacuated through the vacuum system, and the air pressure in the heating chamber is reduced to below -0.095 MPa. After closing the isolation valve and the exhaust valve, the air pressure increase within 0.5 h is no more than 0.005 MPa.

[0015] Furthermore, the outer surface of the heating chamber is covered with an insulation layer, and the insulation layer is quartz insulation tiles and insulation felt, with a thermal conductivity of ≤0.1W / (m·K) and a temperature resistance of ≥1200°C.

[0016] Furthermore, when the pressure in the heating chamber exceeds a set value, the pressure relief valve opens to release excess gas, thereby preventing equipment damage or danger caused by excessive pressure.

[0017] Furthermore, the temperature measurement system measures the internal temperature by infrared temperature measurement, and the measurement temperature range is 400-3500°C; and measures the external temperature by thermocouple temperature measurement, and the measurement temperature range is room temperature-1300°C.

[0018] Furthermore, the pressure measurement system is measured by a pressure gauge, and the measurement range of the pressure gauge is 0 to 2 MPa;

[0019] The gas collection container of the gas collection system is a sealed container with a maximum pressure resistance of about 1 MPa, ensuring the safety of the collection process.

[0020] Furthermore, the material of the high-temperature resistant spring is nickel-based alloy, and is also used to compress the space of the test sample inside the heating chamber, so that the effective heating area is more concentrated.

[0021] In a second aspect, a testing method implemented according to the device for measuring the amount of gas released by a material at high temperature under rapid heating conditions includes:

[0022] Place the test sample into the heating chamber to form electrical contact with the graphite electrodes at both ends. If the test sample is a non-conductive material, wrap it with graphite paper to form electrical contact with the graphite electrodes at both ends.

[0023] Connect the heating chamber to the vacuum system, open the isolation valve and the exhaust valve, reduce the air pressure in the heating chamber to below the preset value, and close the isolation valve and the exhaust valve;

[0024] The test sample is heated by a heating control system, and the heating power is adjusted by the PID method during the heating process;

[0025] Through data acquisition and processing by the temperature measurement system, pressure measurement system and data acquisition and processing system, the temperature and pressure data are recorded in real time and the outgassing volume of the test sample is calculated;

[0026] The gas generated by the test sample after heating is collected through the gas collection system, and the residual solids in the heating chamber and the collected gas components are analyzed.

[0027] The advantages of the present invention compared with the prior art are:

[0028] 1. By utilizing the Joule heating effect, this method can rapidly heat a sample to the desired high temperature (maximum temperature ≥1000°C) within milliseconds (maximum heating rate ≥105°C / s). Compared to the slower heating rates of traditional methods, this method can more realistically simulate the behavior of materials during high-speed heating processes, making it particularly suitable for testing requirements requiring rapid heating, thereby better evaluating the material's high-temperature outgassing properties.

[0029] 2. By incorporating a resistance non-uniformity correction mechanism during Joule heating, this invention mitigates the localized overheating and uneven heat distribution associated with traditional Joule heating devices, which are often caused by the rapid change in resistance with temperature during heating. Through real-time resistance monitoring and high-speed current feedback control, this invention effectively improves heating power stability and repeatability, ensuring consistent test conditions and data comparability. This approach is particularly suitable for testing novel materials in environments requiring extremely high heating process stability and high-temperature response characteristics.

[0030] 3. This invention eliminates the diffusion chamber design used in traditional methods and instead directly connects the sample chamber through the heating system, improving heating efficiency and simplifying the system structure. This not only reduces the size and complexity of the equipment, but also reduces heat loss, improving the overall system efficiency. The simplified design makes operation easier, reducing the number of steps and learning costs for users.

[0031] 4. The rapid temperature rise test implemented by the present invention not only shortens the test time but also greatly improves the efficiency of material testing. In particular, it can achieve rapid and efficient testing of a large number of test samples 8 in materials research and industrial applications, meeting the needs of modern high-throughput testing.

[0032] 5. The design of this invention is highly adaptable and can be used to measure outgassing of a variety of materials (such as metals, ceramics, and composites) under different high-temperature conditions. By adjusting the heating rate and temperature range, it can meet different testing requirements and has wide application in aerospace, electronics, materials science, and other fields. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] Various other advantages and benefits will become apparent to those skilled in the art upon reading the detailed description of the preferred embodiment below. The accompanying drawings are for illustration purposes only and are not to be considered as limiting the present invention. The same reference symbols are used throughout the drawings to represent the same components. In the drawings:

[0034] Figure 1This is a schematic diagram of the device for measuring the amount of gas released by a material at high temperature under rapid heating conditions in the present invention, wherein 1 is a heating chamber 1, 2 is a heating control system, 3 is a vacuum system 3, 4 is a temperature measurement system 4, 5 is a pressure measurement system 5, 6 is a gas collection system 6, 7 is a data acquisition and processing system 7, 8 is a test sample 8, 9 is a graphite electrode 9, 10 is a sealing flange 10, 11 is an exhaust valve 11, 12 is an isolation valve 12, 13 is a pressure relief valve 13, and 14 is a high-temperature resistant spring 14.

[0035] Figure 2 This is a graph showing the gas release test results of a magnesium carbonate sample under rapid heating conditions in Example 2 of the present invention. DETAILED DESCRIPTION

[0036] In order to better understand the above technical solution, the technical solution of the present invention is described in detail below with reference to the accompanying drawings and specific embodiments. It should be understood that the embodiments of the present invention and the specific features in the embodiments are detailed descriptions of the technical solution of the present invention, rather than limitations on the technical solution of the present invention. In the absence of conflict, the embodiments of the present invention and the technical features in the embodiments can be combined with each other.

[0037] The following is a further detailed description of a device and a test method for measuring the amount of gas released by a material at high temperature under rapid heating conditions provided by an embodiment of the present invention in conjunction with the accompanying drawings. Specific implementation methods may include:

[0038] A heating chamber 1 is provided with a test sample 8 filled therein, and both ends of the test sample 8 are in contact with a graphite electrode 9; one end of the heating chamber 1 is connected to a pressure measurement system 5 via a sealing flange, and the other end is connected to a vacuum system 3, a gas collection system 6 and a pressure relief valve 13 via a sealing flange; an exhaust valve 11 is provided between the heating chamber 1 and the vacuum system 3; an isolation valve 12 is provided between the heating chamber 1 and the gas collection system 6; both ends of the graphite electrodes 9 on both sides of the heating chamber 1 are connected to the inner end faces of the sealing flanges via high-temperature resistant springs 14, realizing a conductive path for heating the test sample 8 under the control of a heating control system 2; the device eliminates the diffusion chamber design in the traditional method, and directly contacts the sample chamber through the heating system, thereby improving the heating efficiency and simplifying the system structure. The heating chamber 1 is used to load samples and heating electrodes; the heating control system adopts the Joule heating effect, which can provide a short-term high current (200A) to achieve rapid heating of the material, ensuring that the high temperature state required for the test is reached in a very short time, thereby simulating the changes in the degassing behavior of the material during the high-speed heating process; the vacuum system 3 is used to evacuate the heating chamber 1; the temperature measurement system 4 is used to test the temperature of the heating chamber 1; the pressure measurement system 5 is used to test the pressure of the heating chamber 1; the gas collection system 6 is used to collect the gas generated after the test sample 8 is heated, for subsequent analysis of the collected gas composition; the data acquisition and processing system 7 is used to collect test data and calculate the degassing volume.

[0039] During implementation, the present invention further optimizes the temperature control accuracy during Joule heating and proposes a "resistance non-uniformity correction mechanism" to compensate for the problem of unstable heating power caused by changes in material resistance with temperature, thereby ensuring the controllability and repeatability of the heating curve. In order to address the problem of changes in heating power caused by changes in material resistance with temperature during heating, the real-time data collected by the high-frequency sampling voltage probe and the current sensor are used to calculate the sample resistance in real time based on Ohm's law R=V / I, and the sample resistance data is updated in a cycle of 1ms. Based on the resistance change trend, the system adopts closed-loop feedback control logic to automatically adjust the output current according to the current sample resistance, maintain the target heating power constant or change according to the preset heating curve, and avoid local overheating or underheating. For example, when it is detected that the resistance value rises too quickly, the current output is automatically reduced to maintain a stable heating rate.

[0040] Furthermore, the heating control system utilizes the Joule heating effect to conduct current through graphite electrodes 9 at both ends, achieving rapid heating of the test sample 8. The current parameters provide short-term high current, up to 200A, ensuring that the test sample 8 is heated to the required high temperature within milliseconds, with a maximum heating rate of ≥105°C / s and a maximum temperature of ≥1000°C. The graphite electrodes 9 are hollow tubular structures with a resistance of ≤5Ω, effectively conducting current and generating Joule heating, achieving rapid heating of the test sample 8. A PID temperature control system is used to precisely regulate the heating power. The PID controller provides feedback based on the deviation between the real-time measured temperature and the set temperature, controlling the heating power by adjusting the heating current. The PID control algorithm effectively reduces temperature fluctuations and maintains system temperature stability, ensuring that the heating process meets the predetermined heating rate and target temperature. Control parameters can be set on the control panel, and the temperature test error is ≤5%.

[0041] Furthermore, the heating chamber 1 is a quartz double-tube structure, the inner diameter of the inner tube is about 5-50 mm, and the length is about 50-500 mm, which is used to hold the test sample 8, and the test sample 8 is quickly heated up by the heating control system of claim 2; the inner diameter of the outer tube is about 100-500 mm, and the length is about 100-550 mm, which is connected to the inner tube and the vacuum system 3, and the system can be evacuated by a vacuum pump, and the vacuum gauge in the heating chamber 1 can be reduced to below -0.095 MPa. After closing the isolation valve and the vacuum valve, the gauge pressure increase within 0.5 h is no more than 0.005 MPa, providing better sealing protection for the test environment; the quartz material has good high temperature resistance and transparency, which is convenient for observing the ablation state and realizing infrared temperature measurement.

[0042] Furthermore, the outer surface of the heating chamber 1 is covered with an insulation layer, which is quartz insulation tiles and insulation felt, with a thermal conductivity of ≤0.1W / (m·K) and a temperature resistance of ≥1200°C, providing insulation protection for the test environment.

[0043] Furthermore, the heating chamber 1 is connected to a safety pressure relief valve 13. When the pressure within the heating chamber 1 exceeds a set value (1 MPa), the pressure relief valve 13 automatically opens, releasing excess gas, thereby preventing damage to the equipment or danger caused by excessive pressure. This pressure relief valve 13 effectively prevents dangers caused by excessive pressure, ensuring safety during the test process. In particular, when the test sample 8 decomposes and releases gas during the experiment, it helps to balance the pressure fluctuations caused by gas expansion, ensuring the long-term stable operation of the equipment.

[0044] Furthermore, the temperature measurement system 4 measures the internal temperature by infrared temperature measurement, and the measurement temperature range is 400~3500℃; measures the external temperature by thermocouple temperature measurement, and the measurement temperature range is room temperature~1300℃; the pressure measurement system 5 measures by a pressure gauge, and the measurement range of the pressure gauge is 0~2MPa.

[0045] Furthermore, the gas collection container of the gas collection system 6 is a sealed container that can withstand the pressure of high-temperature gas, with a maximum pressure of approximately 1 MPa, ensuring the safety of the collection process.

[0046] Furthermore, the data acquisition and processing system acquires temperature and pressure data in real time at a frequency of 1 to 200 Hz for data processing and analysis, and calculates the outgassing volume of the test sample 8 .

[0047] On the other hand, the present invention provides a method for measuring the amount of gas released by a material at high temperature under rapid heating conditions, using the above-mentioned testing device, comprising the following steps:

[0048] Step 1: Place the conductive test sample 8 to be tested into the heating chamber 1 as described in claim 1 and form good electrical contact with the graphite electrodes 9 at both ends. If the test sample 8 to be tested is a non-conductive material, it can be wrapped with graphite paper to form electrical contact with the graphite electrodes 9 at both ends, and the resistance value is ≤10Ω;

[0049] Step 2: Connect the heating chamber 1 to the vacuum system 3, open the isolation valve and the vacuum valve, start the vacuum pump, and reduce the vacuum gauge in the heating chamber 1 to below -0.095 MPa. After closing the isolation valve and the vacuum valve, the gauge pressure should not increase by more than 0.005 MPa within 0.5 h.

[0050] Step 3: Provide a short-term high current (up to 200A) through the heating control system to achieve rapid heating of the test sample 8. Use a PID temperature control system to accurately adjust the heating power. The PID controller performs feedback adjustment based on the deviation between the real-time measured temperature and the set temperature, and controls the heating power by adjusting the heating current. The PID control algorithm can effectively reduce temperature fluctuations and maintain the stability of the system temperature, thereby ensuring that the heating process meets the predetermined heating rate and target temperature. The control parameters can be set on the control panel, and the temperature test error is ≤5%;

[0051] Step 4: Record the temperature and pressure data in real time through the data acquisition and processing system, with a sampling frequency of 1 to 200 Hz, and calculate the outgassing volume of the test sample 8;

[0052] Step 5: The gas generated by the heated test sample 8 is collected through the gas collection system 6 , and the residual solids in the heating chamber 1 and the collected gas components are analyzed.

[0053] Furthermore, in the step 2, after vacuuming, the heating chamber 1 may be heated to 150° C. to 250° C., kept warm, and then vacuumed again to remove the material and water vapor in the heating chamber 1 .

[0054] Furthermore, in step 4, the outgassing volume is calculated based on the collected temperature and pressure data, and the formula is as follows:

[0055]

[0056] Where n is the amount of gas to be measured, P is the measured pressure, V is the effective volume of the heating chamber 1, R is the ideal gas constant, and T is the measured temperature.

[0057] Furthermore, in step five, the gas collected by the gas collection system 6 can be analyzed by gas chromatography, gas molecular absorption spectroscopy or mass spectrometry; and the residual solid can be analyzed by X-ray diffraction, thermal analysis or the like.

[0058] Example 1

[0059] In the solution provided in the embodiment of the present invention, Figure 1 As shown, this embodiment provides a test device for measuring the amount of gas released by a material at high temperature under rapid heating conditions, comprising a heating chamber 1, a heating control system 2, a vacuum system 3, a temperature measurement system 4, a pressure measurement system 5, a gas collection system 6, and a data acquisition and processing system 7. The heating chamber 1 is filled with a test sample 8, the ends of which are in contact with graphite electrodes 9. The ends of the heating chamber 1 are connected to the vacuum system 3, the pressure measurement system 5, and the gas collection system 6 via sealing flanges 10. An exhaust valve 11 is installed between the heating chamber 1 and the vacuum system 3; an isolation valve 12 is installed between the heating chamber 1 and the gas collection system 6; and a pressure relief valve 13 is connected to the heating chamber 1 to ensure test safety.

[0060] The heating control system 2 utilizes the Joule heating effect to conduct current through the graphite electrodes 9 at both ends to achieve rapid heating of the test sample 8. The current parameter can provide a short-term high current, up to 200A, ensuring that the test sample 8 is heated to the required high temperature within milliseconds, with a maximum heating rate of 10 5℃ / s, the maximum temperature is 2000℃; the graphite electrode 9 is a hollow tubular structure with a resistance value of 3Ω, which can effectively conduct current and generate Joule heat to achieve rapid heating of the test sample 8. A PID temperature control system is used to accurately adjust the heating power. The PID controller performs feedback adjustment based on the deviation between the real-time measured temperature and the set temperature, and controls the heating power by adjusting the heating current. The PID control algorithm can effectively reduce temperature fluctuations and maintain the stability of the system temperature, thereby ensuring that the heating process meets the predetermined heating rate and target temperature. The control parameters can be set on the control panel, and the temperature test error is 3-5%;

[0061] The heating chamber 1 is a quartz double-tube structure. The inner tube has an inner diameter of about 10 mm, a length of about 50 mm, and an effective volume of 32 ml. It is used to hold the test sample 8 and achieve rapid heating of the test sample 8 through the heating control system; the outer tube has an inner diameter of about 100 mm and a length of about 100 mm. It is connected to the inner tube and the vacuum system 3. The system can be evacuated by a vacuum pump, and the vacuum gauge in the heating chamber 1 can be reduced to -0.098 MPa. After closing the isolation valve and the vacuum valve, the gauge pressure increases by 0.002 MPa within 0.5 h, providing better sealing protection for the test environment; the quartz material has good high-temperature resistance and transparency, which is convenient for observing the ablation state and realizing infrared temperature measurement.

[0062] The outer surface of the heating chamber 1 is covered with an insulation layer, which is quartz or alumina insulation tiles and insulation felt. The thermal conductivity is 0.05W / (m·K) and the maximum temperature resistance is ≥1200, providing insulation protection for the test environment.

[0063] Heating chamber 1 is connected to a safety pressure relief valve 13. When the pressure within heating chamber 1 exceeds a set value (1 MPa), valve 13 automatically opens, releasing excess gas, thereby preventing damage to the equipment or other hazards caused by excessive pressure. This valve effectively prevents hazards caused by excessive pressure, ensuring safety during testing. In particular, when test sample 8 decomposes and releases gas during the experiment, it helps balance pressure fluctuations caused by gas expansion, ensuring long-term stable operation of the equipment.

[0064] The temperature measurement system 4 measures the internal temperature by infrared temperature measurement, and the measurement temperature range is 400-3500°C; the external temperature is measured by thermocouple temperature measurement, and the measurement temperature range is room temperature to 1300°C; the pressure measurement system 5 measures by a pressure gauge, and the measurement range of the pressure gauge is 0-2MPa.

[0065] The gas collection container of the gas collection system 6 is a sealed container that can withstand the pressure of high-temperature gas. The maximum pressure it can withstand is about 1 MPa, ensuring the safety of the collection process.

[0066] The data acquisition and processing system collects temperature and pressure data in real time at a frequency of 1 to 200 Hz for data processing and analysis, and calculates the outgassing volume of the test sample 8.

[0067] Example 2

[0068] This embodiment provides a test method for measuring the amount of gas released by a material at high temperature under rapid heating conditions, using the test device of Example 1, and comprising the following steps:

[0069] Step 1: Weigh 0.5g of magnesium carbonate powder, wrap it with graphite paper and place it in the heating chamber 1 to form good electrical contact with the graphite electrodes 9 at both ends, and add graphite plugs at both ends.

[0070] Step 2: Connect the heating chamber 1 to the vacuum system 3 and start the vacuum pump to reduce the vacuum gauge in the heating chamber 1 to -0.098MPa. After closing the isolation valve and the vacuum valve, the gauge pressure will increase by 0.002MPa within 0.5h. Then, heat the heating chamber 1 to about 200℃ and keep it warm for 10 minutes to remove moisture from the material and the heating chamber 1 to prevent moisture from affecting the test results. Then evacuate the heating chamber 1 to a pressure of -0.095MPa. After closing the isolation valve and the vacuum valve, the gauge pressure will increase by 0.003MPa within 0.5h.

[0071] Step 3: Set the heating temperature to 1000°C within 5 seconds and then maintain it for 10 seconds;

[0072] Step 4: Use the data acquisition and processing system to record temperature and pressure data in real time at a sampling frequency of 50 Hz. Calculate the outgassing volume of test sample 8 based on the measured data.

[0073] The test results are as follows Figure 2 The final pressure of the sample involved in this embodiment at 1000°C is 0.42 MPa. It is calculated that the total amount of gas released during the heating process is 1.3×10 -3 mol.

[0074] Step 5: The gas generated after the test sample 8 is heated is collected through the gas collection system 6. The generated gas can be detected by gas chromatography to be CO2; the residual solid X-ray diffraction detection component is MgO, and the accuracy of the single reaction product test is verified by thermal analysis. The reaction ratio of this reaction tested by this equipment is 21%, and the reaction ratio obtained by thermogravimetric analysis of residual magnesium carbonate at the same temperature is 20%, which is basically consistent with the results of the rapid heating test method.

[0075] Example 3

[0076] This embodiment provides a test method for measuring the amount of gas released by a material at high temperature under rapid heating conditions, using the test device of Example 1, and comprising the following steps:

[0077] Step 1: Weigh 0.2g of phenolic resin powder, wrap it with graphite paper and put it into the heating chamber 1 to form good electrical contact with the graphite electrodes 9 at both ends, and add graphite plugs at both ends.

[0078] Step 2: Connect heating chamber 1 to vacuum system 3, open the isolation valve, and start the vacuum pump. The vacuum gauge in heating chamber 1 should be reduced to -0.095 MPa. After closing the isolation valve and vacuum valve, the gauge pressure should increase by 0.003 MPa within 0.5 hours. Next, heat heating chamber 1 to approximately 250°C and maintain this temperature for 10 minutes to remove moisture from the material and heating chamber 1, preventing it from affecting the test results. Evacuate heating chamber 1 to a pressure of -0.097 MPa. After closing the isolation valve and vacuum valve, the gauge pressure should increase by 0.002 MPa within 0.5 hours.

[0079] Step 3: Set the heating temperature to 600°C within 3 seconds, keep warm for 10 seconds, then reach 800°C within 2 seconds, keep warm for 10 seconds, then reach 1500°C within 2 seconds, keep warm for 10 seconds.

[0080] Step 4: The temperature and pressure data were recorded in real time by the data acquisition and processing system with a sampling frequency of 100 Hz. The final pressure of the sample at 1500°C was 0.59 MPa. The total amount of gas released during the heating process was calculated to be 1.6×10 -3 mol.

[0081] Step 5: Open the isolation valve, collect the gas generated after the test sample 8 is heated, and perform mass spectrometry analysis on the gas components. The products are water, methane, methanol, carbon monoxide, carbon dioxide, benzene, phenol, o-cresol, p-cresol, o-o-xylenol, etc.

[0082] Example 4

[0083] This embodiment provides a test device for measuring the amount of gas released by a material at high temperature under rapid heating conditions, comprising a heating chamber 1, a heating control system 2, a vacuum system 3, a temperature measurement system 4, a pressure measurement system 5, a gas collection system 6, and a data acquisition and processing system 7. The heating chamber 1 is filled with a test sample 8, the ends of which are in contact with graphite electrodes 9. The ends of the heating chamber 1 are connected to the vacuum system 3, the pressure measurement system 5, and the gas collection system 6 via sealing flanges 10. An exhaust valve 11 is installed between the heating chamber 1 and the vacuum system 3; an isolation valve 12 is installed between the heating chamber 1 and the gas collection system 6; and a pressure relief valve 13 is connected to the heating chamber 1 to ensure test safety.

[0084] The heating control system 1 utilizes the Joule heating effect to conduct current through the graphite electrodes 9 at both ends to achieve rapid heating of the test sample 8. The current parameters can provide a short-term high current, up to 200A, ensuring that the test sample 8 is heated to the required high temperature within milliseconds. The maximum heating rate is 10 5 ℃ / s, the maximum temperature is 3500℃; the graphite electrode 9 is a hollow tubular structure with a resistance of 4Ω, which can effectively conduct current and generate Joule heat to achieve rapid heating of the test sample 8. A PID temperature control system is used to accurately adjust the heating power. The PID controller performs feedback adjustment based on the deviation between the real-time measured temperature and the set temperature, and controls the heating power by adjusting the heating current. The PID control algorithm can effectively reduce temperature fluctuations and maintain the stability of the system temperature, thereby ensuring that the heating process meets the predetermined heating rate and target temperature. The control parameters can be set on the control panel, and the temperature test error is 2-5%;

[0085] The heating chamber 1 is a quartz double-tube structure with an effective volume of 720 ml. The inner diameter of the inner tube is about 30 mm and the length is about 200 mm. It is used to hold the test sample 8, and the test sample 8 is quickly heated up by the heating control system of claim 2; the inner diameter of the outer tube is about 300 mm and the length is about 250 mm. It is connected to the inner tube and the vacuum system 3. The system can be evacuated by a vacuum pump, and the vacuum gauge in the heating chamber 1 can be reduced to -0.098 MPa. After closing the isolation valve and the vacuum valve, the gauge pressure increases by 0.002 MPa within 0.5 h, providing better sealing protection for the test environment; the quartz material has good high temperature resistance and transparency, which is convenient for observing the ablation state and realizing infrared temperature measurement.

[0086] The outer surface of the heating chamber 1 is covered with an insulation layer, which is made of alumina insulation tiles and insulation felt. The thermal conductivity is 0.05W / (m·K) and the maximum temperature resistance is 1600°C, providing insulation protection for the test environment.

[0087] Heating chamber 1 is connected to a safety pressure relief valve 13. When the pressure within heating chamber 1 exceeds a set value (1 MPa), valve 13 automatically opens, releasing excess gas, thereby preventing damage to the equipment or other hazards caused by excessive pressure. This valve effectively prevents hazards caused by excessive pressure, ensuring safety during testing. In particular, when test sample 8 decomposes and releases gas during the experiment, it helps balance pressure fluctuations caused by gas expansion, ensuring long-term stable operation of the equipment.

[0088] The temperature measurement system 4 measures the internal temperature by infrared temperature measurement, and the measurement temperature range is 400-3500°C; the external temperature is measured by thermocouple temperature measurement, and the measurement temperature range is room temperature to 1300°C; the pressure measurement system 5 measures by a pressure gauge, and the measurement range of the pressure gauge is 0-2MPa.

[0089] The gas collection container of the gas collection system 6 is a sealed container that can withstand the pressure of high-temperature gas. The maximum pressure it can withstand is about 1 MPa, ensuring the safety of the collection process.

[0090] The data acquisition and processing system collects temperature and pressure data in real time at a frequency of 1 to 200 Hz for data processing and analysis, and calculates the outgassing volume of the test sample 8.

[0091] Example 5

[0092] This embodiment provides a test method for measuring the amount of gas released by a material at high temperature under rapid heating conditions, using the test device of Example 4, and comprising the following steps:

[0093] Step 1: Weigh 1.5g of carbon fiber reinforced phenolic resin-based composite material powder, wrap it with graphite paper and place it in the heating chamber 1 to form good electrical contact with the graphite electrodes 9 at both ends, and add graphite plugs at both ends.

[0094] Step 2: Connect heating chamber 1 to vacuum system 3, open the isolation valve, and start the vacuum pump. The vacuum gauge in heating chamber 1 should be reduced to -0.096 MPa. After closing the isolation valve and vacuum valve, the gauge pressure should increase by 0.002 MPa within 0.5 hours. Next, heat heating chamber 1 to approximately 150°C and maintain this temperature for 10 minutes to remove moisture from the material and heating chamber 1, preventing it from affecting the test results. Evacuate heating chamber 1 to a pressure of -0.098 MPa. After closing the isolation valve and vacuum valve, the gauge pressure should increase by 0.004 MPa within 0.5 hours.

[0095] Step 3: Set the heating program to reach 3000°C within 0.5s, then reduce to 600°C, and repeat three times;

[0096] Step 4: The temperature and pressure data were recorded in real time by the data acquisition and processing system with a sampling frequency of 200 Hz. The final pressure of the sample at 3000°C was 0.14 MPa. The total amount of gas released during the heating process was calculated to be 3.8×10 -3 mol.

[0097] Step 5: Open the isolation valve, collect the gas generated after the test sample 8 is heated, and perform mass spectrometry analysis on the gas components. The products are water, ethane, ethanol, carbon monoxide, carbon dioxide, benzene, phenol, o-cresol, p-cresol, o-xylenol, 2,4,6-trimethylphenol, etc.

[0098] Obviously, those skilled in the art may make various changes and modifications to the present invention without departing from the spirit and scope of the present invention. Thus, if such changes and modifications fall within the scope of the claims and their equivalents, the present invention is intended to include such changes and modifications.

[0099] The contents not described in detail in the specification of the present invention belong to the common knowledge of those skilled in the art.

Claims

1. A device for measuring the amount of gas released by a material at high temperature under rapid heating conditions, characterized in that: include: A heating chamber (1) is provided with a test sample (8) filled therein, and both ends of the test sample (8) are in contact with a graphite electrode (9); one end of the heating chamber (1) is connected to a pressure measurement system (5) via a sealing flange, and the other end is connected to a vacuum system (3), a gas collection system (6) and a pressure relief valve (13) via a sealing flange; an exhaust valve (11) is provided between the heating chamber (1) and the vacuum system (3); an isolation valve (12) is provided between the heating chamber (1) and the gas collection system (6); both ends of the graphite electrodes (9) on both sides of the heating chamber (1) are connected to the inner end surface of the sealing flange via a high-temperature resistant spring (14), thereby realizing a conductive path for heating the test sample (8) under the control of a heating control system (2); A vacuum system (3) for creating a vacuum environment for the heating chamber (1); A temperature measurement system (4) is used to measure the temperature of the test sample (8) and send the temperature signal to the heating control system (2) and the data acquisition and processing system (7); A pressure measurement system (5) for measuring the pressure inside the heating chamber (1) and sending a pressure signal to a data acquisition and processing system (7); a gas collection system (6) for collecting gas released during the testing process of the test sample (8); A data acquisition and processing system (7) for collecting data from the temperature measurement system (4) and the pressure measurement system (5) in real time; A heating control system (2) is used for controlling the graphite electrode (9) to increase its temperature according to an input temperature signal.

2. The device for measuring the amount of gas released by a material at high temperature under rapid heating conditions according to claim 1, characterized in that: The graphite electrode (9) is a hollow tubular structure with a resistance value of ≤5Ω.

3. The device for measuring the amount of gas released by a material at high temperature under rapid heating conditions according to claim 1, characterized in that: The graphite electrode (9) conducts a current of up to 200A, ensuring that the test sample (8) is heated to a preset temperature within milliseconds, with a maximum heating rate of not less than 10 5 ℃ / s, the maximum temperature is not less than 1000℃.

4. The device for measuring the amount of gas released by a material at high temperature under rapid heating conditions according to claim 1, characterized in that: The heating chamber (1) is a quartz double-tube structure, comprising an inner tube and an outer tube; the inner tube has an inner diameter of 5 to 50 mm and a length of 50 to 500 mm, and is used to hold the test sample (8); the outer tube has an inner diameter of 100 to 500 mm and a length of 100 to 550 mm, and is connected to the inner tube and the vacuum system (3). The heating chamber (1) is evacuated by the vacuum system (3), and the air pressure in the heating chamber (1) is reduced to below -0.095 MPa. After closing the isolation valve (12) and the exhaust valve (11), the air pressure increase within 0.5 h is no more than 0.005 MPa.

5. The device for measuring the amount of gas released by a material at high temperature under rapid heating conditions according to claim 1, characterized in that: The outer surface of the heating chamber (1) is covered with a heat-insulating layer, which is made of quartz heat-insulating tiles and heat-insulating felt, has a thermal conductivity of ≤0.1W / (m·K) and a temperature resistance of ≥1200°C.

6. The device for measuring the amount of gas released by a material at high temperature under rapid heating conditions according to claim 1, characterized in that: When the pressure in the heating chamber (1) exceeds a set value, the pressure relief valve (13) opens to release excess gas, thereby preventing equipment damage or danger caused by excessive pressure.

7. The device for measuring the amount of gas released by a material at high temperature under rapid heating conditions according to claim 1, characterized in that: The temperature measurement system (4) measures the internal temperature by infrared temperature measurement, and the measurement temperature range is 400-3500°C; and measures the external temperature by thermocouple temperature measurement, and the measurement temperature range is room temperature-1300°C.

8. The device for measuring the amount of gas released by a material at high temperature under rapid heating conditions according to claim 1, characterized in that: The pressure measurement system (5) is measured by a pressure gauge, and the measurement range of the pressure gauge is 0 to 2 MPa; The gas collection container of the gas collection system (6) is a sealed container with a maximum pressure resistance of approximately 1 MPa, thereby ensuring the safety of the collection process.

9. The device for measuring the amount of gas released by a material at high temperature under rapid heating conditions according to claim 1, characterized in that: The material of the high temperature resistant spring (14) is nickel-based alloy, and is also used to compress the space of the test sample (8) inside the heating chamber (1), so that the effective heating area is more concentrated.

10. The testing method implemented by the device for measuring the amount of gas released by a material at high temperature under rapid heating conditions according to any one of claims 1 to 9, characterized in that: include: The test sample (8) is placed in the heating chamber (1) to form electrical contact with the graphite electrodes (9) at both ends. If the test sample (8) is a non-conductive material, it is wrapped with graphite paper to form electrical contact with the graphite electrodes (9) at both ends; Connect the heating chamber (1) to the vacuum system (3), open the isolation valve (12) and the air extraction valve (11), reduce the air pressure in the heating chamber (1) to below a preset value, and close the isolation valve (12) and the air extraction valve (11); The test sample (8) is heated by a heating control system (2), and the heating power is adjusted by a PID method during the heating process; By collecting and processing data through the temperature measurement system (4), the pressure measurement system (5) and the data acquisition and processing system (7), the temperature and pressure data are recorded in real time, and the outgassing amount of the test sample (8) is calculated; The gas generated after the test sample (8) is heated is collected by a gas collection system (6), and the residual solids in the heating chamber (1) and the collected gas components are analyzed.

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