An adiabatic thermal sample cell structure and testing method for multiphase and multicomponent samples

By employing a dumbbell-shaped sample cell structure, an independent heating wire assembly, and an intelligent measurement and control system, the problems of uneven temperature field distribution and uncontrollable gas introduction and collection in multiphase and multicomponent sample testing have been solved, enabling accurate and safe testing of multiphase and multicomponent samples.

CN120352472BActive Publication Date: 2025-10-31CHINA JILIANG UNIV
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Patent Information

Application Number
CN202510510608.7
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-04-23
Publication Date
2025-10-31
Estimated Expiration
2045-04-23

AI Technical Summary

Technical Problem

Existing adiabatic thermal techniques are difficult to effectively test multiphase and multicomponent samples, especially high-nickel lithium-ion batteries and ternary cathode materials, due to problems such as uneven temperature field distribution, uncontrollable gas introduction and collection, and deviations in the measurement and control system.

Method used

The sample cell adopts a dumbbell-shaped structure, combined with an independent heating wire assembly, a gas pipeline system, and an intelligent measurement and control system, to achieve temperature uniformity and gas separation inside the sample cell. By monitoring and adjusting the sample cell parameters in real time, the accuracy and safety of the test are ensured.

Benefits of technology

It improves the accuracy and repeatability of multiphase and multicomponent sample testing, solves the problems of uneven temperature field distribution and uncontrollable gas introduction and collection, provides data support for the interaction between different substances in multiphase and multicomponent systems, and ensures efficient and stable operation of the test.

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Abstract

This invention relates to the field of adiabatic thermal technology, specifically to an adiabatic thermal sample cell structure and testing method for multiphase and multicomponent samples. The invention aims to solve problems such as difficulties in testing multiphase and multicomponent samples, uneven temperature fields within the sample cell, uncontrollable gas introduction and collection, and deviations in the measurement and control system. The invention consists of a dumbbell-shaped sample cell structure, independent heating wire assemblies, a gas pipeline system, and an intelligent measurement and control system. The dumbbell-shaped sample cell expands the internal space, solving the challenges of testing multiphase and multicomponent samples; the independent heating wire assemblies are wound around both sides of the sample cell, allowing for individual heating and temperature control, compensating for heat loss, and solving the problem of uneven temperature fields; the gas pipeline system connects to the sample cell, enabling phase separation and controllable gas introduction and collection; the intelligent measurement and control system regulates the entire measurement and control system, providing data support and safety assurance for the test.
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Description

Technical Field

[0001] This invention relates to the field of adiabatic thermal technology, specifically to an adiabatic thermal sample cell structure and testing method for multiphase and multicomponent samples. Background Technology

[0002] With the rapid development of materials science, adiabatic calorimetry, as a high-precision calorimetric method for studying the thermal stability of materials, has been widely used in materials science, energy research, and other fields. Adiabatic calorimetry can provide a near-perfect adiabatic environment, effectively avoiding interference from environmental heat exchange. Existing adiabatic calorimetry techniques are mostly designed for single-phase (such as solid or liquid) samples, while precise studies of the thermal stability of common multiphase, multi-component samples (such as high-nickel lithium-ion batteries and ternary cathode materials) are lacking. Therefore, researching an adiabatic calorimetry technique for multiphase, multi-component samples is particularly important.

[0003] Traditional adiabatic calorimetry techniques typically employ a single sample cell structure, monitoring the real-time response of a single-phase sample by controlling the temperature of the entire calorimetric system. Multiphase and multi-component samples, due to the vastly different physicochemical properties of their phases and the complex interactions between components, present significant challenges to the accurate measurement of material thermal stability. Furthermore, multiphase and multi-component materials are prone to phase transitions during heating, and traditional adiabatic calorimetry techniques cannot meet the homogeneity testing requirements for these samples.

[0004] From the perspective of sample cell structure, a single sample cell structure has inherent limitations. Traditional adiabatic thermal testing processes treat the entire sample cell structure as a single unit, and the temperature measured by the temperature sensor is the real-time reaction temperature of the internal sample, which cannot track the single-phase temperature of multiphase, multi-sample (such as gas-solid two-phase) samples. Furthermore, the heat transfer mechanism of a single sample cell structure is imperfect, with an uneven internal temperature field distribution and significant temperature differences between the center and the edges. The point-measurement principle of the temperature sensor also contributes to the bias in material thermal stability testing. For multiphase, multi-component samples, a single sample cell structure cannot guarantee sufficient contact between different phases, limiting the sufficiency of the reaction and thus affecting the accuracy and repeatability of the measurement results.

[0005] From a methodological perspective, traditional adiabatic thermal calorimetry heats the sample cell via heat conduction, which is difficult to control precisely at the heating rate. Furthermore, heat loss occurs during conduction, and temperature sensors cannot accurately capture dynamic changes in phase transitions, critical reaction temperatures, and other information. Traditional adiabatic thermal calorimetry methods have significant limitations, only capable of measuring the thermal performance of single, isolated samples, and unable to effectively explore the influence mechanisms of external substances on the thermal reaction process of the target sample. In multiphase, multi-component systems, especially in lithium-ion battery research, the interactions between different materials are crucial to material performance and the overall battery performance. For example, in the study of electrode material thermal stability, external substances such as ambient gases or electrolyte additives may alter the thermal reaction pathway and kinetic characteristics of the sample. The single sample cell structure and the still-developing testing methods can easily lead to deviations in the material thermal stability test results, thus losing their guiding significance for preventing thermal runaway accidents. Summary of the Invention

[0006] To address the shortcomings of existing technologies, this invention provides an adiabatic thermal sample cell structure and testing method for multiphase and multicomponent samples, solving the problems of difficulty in testing multiphase and multicomponent samples, uneven temperature field distribution inside the sample cell, uncontrollable gas introduction and collection, and deviations in the measurement and control system in existing technologies.

[0007] A first aspect of the present invention provides an adiabatic thermal sample cell structure for multiphase, multi-component samples, comprising:

[0008] The sample cell body has a dumbbell-shaped structure, including two independent sample cell sections for respectively accommodating samples with different phase compositions;

[0009] The heating assembly includes an independent heating wire tightly wound around the outside of the sample cell body for individually heating and controlling the temperature of the sample cell to compensate for heat loss and ensure uniform heating of the sample cell surface.

[0010] A gas pipeline system, which is connected to the main body of the sample cell, is used to introduce and collect gas during the sample reaction process;

[0011] The measurement and control system is used to monitor parameters such as temperature and pressure inside the sample cell in real time, and to adjust the heating components and the gas pipeline system according to the monitoring results.

[0012] A second aspect of the present invention provides an adiabatic thermal testing method for multiphase, multi-component samples, employing the above-described structure, comprising the following steps:

[0013] Step 1. Load the multiphase, multi-component sample into the left cavity of the dumbbell-shaped sample cell, which includes two independent sample cell sections for accommodating samples with different phase compositions respectively.

[0014] Step 2. Close the pressure relief valve and the on / off valve in the gas pipeline system to ensure the airtightness of the entire device;

[0015] Step 3. Set the adiabatic thermal experiment parameters, start the heating component to heat the sample cell, detect the temperature in the sample cell in real time through the temperature sensor, and adjust the output power of the heating component according to the comparison between the measured temperature and the set temperature.

[0016] Step 4. After detecting that the sample has started to react, stop active heating, adjust the output power of the heating component according to the temperature feedback measured by the temperature sensor, and track the temperature change in the sample cell in real time.

[0017] Step 5. Collect the gases generated during the reaction through a gas pipeline system and monitor the pressure changes in the sample cell using a pressure sensor;

[0018] Step 6. After the test, release the pressure and cool down rapidly through the gas pipeline system.

[0019] The beneficial effects of this invention are:

[0020] 1. This invention, by introducing a dumbbell-shaped sample cell structure, significantly increases the internal space of the sample cell, facilitating phase separation during multiphase and multi-component sample reactions. This effectively expands the sample testing range of the adiabatic heating system, providing possibilities for exploring the interactions between different substances in multiphase and multi-component systems. Compared to existing technologies that primarily target single-phase sample testing, this invention solves the problem of difficulties in testing multiphase and multi-component samples.

[0021] 2. This invention achieves more uniform heating of the sample cell surface by winding independent heating wire assemblies, reducing the impact of temperature gradients on test results; furthermore, the individual temperature control of the heating wire assemblies on both sides of the sample cell effectively compensates for heat loss caused by heat exchange. Compared to the inherent defects of insufficient temperature control in existing technologies, the problem of uneven temperature field distribution inside the sample cell is effectively solved.

[0022] 3. This invention, by adding a gas pipeline at the sample cell outlet, effectively achieves the separation of different phase media in the thermal stability testing of multiphase and multicomponent samples, facilitating subsequent component analysis of the reaction products. Furthermore, the newly added gas pipeline system allows the introduction of other media during the reaction process via gas interfaces, facilitating the investigation of their influence mechanisms on the sample's thermal reaction. Compared to the inherent drawback of existing technologies where collecting reaction gases is difficult, the addition of the gas pipeline system solves the problem of uncontrollable gas component introduction and collection.

[0023] 4. This invention provides complete data support and safety assurance for the entire adiabatic thermal testing process of multiphase and multi-component samples by adding an intelligent measurement and control system to monitor key parameters such as temperature and pressure on both sides of the dumbbell-shaped sample cell structure in real time, as well as the parameter differences between different phase media during the reaction process, thus ensuring the efficient and stable operation of the adiabatic thermal test. Attached Figure Description

[0024] For ease of explanation, the present invention will be described in detail with reference to the following drawings.

[0025] Figure 1 This is a schematic diagram of the dumbbell-shaped sample cell structure of the adiabatic heating system according to an embodiment of the present invention;

[0026] Figure 2 This is a schematic diagram of the gas pipeline of the adiabatic heating system according to an embodiment of the present invention;

[0027] Figure 3 This is a schematic diagram of the temperature control of the independent heating wire assembly of the adiabatic heating system according to an embodiment of the present invention;

[0028] Figure 4 This is a schematic diagram of the adiabatic thermal measurement and control system according to an embodiment of the present invention;

[0029] Figure 5 This is a schematic diagram of the temperature of the sample cell on the left side in the thermal runaway of lithium iron phosphate according to an embodiment of the present invention.

[0030] Figure 6 This is a schematic diagram of the pressure in the sample cell on the right side of the lithium iron phosphate thermal runaway according to an embodiment of the present invention. Detailed Implementation

[0031] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the invention. All other embodiments obtained by those skilled in the art based on the embodiments of this invention without inventive effort are within the scope of protection of this invention.

[0032] The following detailed description, in conjunction with the accompanying drawings and specific embodiments, provides an adiabatic thermal sample cell structure and testing method for multiphase, multi-component samples provided by the present invention.

[0033] Please see Figure 1 This application proposes an adiabatic thermal sample cell structure for multiphase and multicomponent samples, including a dumbbell-shaped sample cell structure, an independent heating wire assembly, a gas pipeline system, and an intelligent measurement and control system.

[0034] The dumbbell-shaped sample cell is the core structure, the independent heating wire assembly is tightly wound around the outside of the dumbbell-shaped sample cell sphere, the gas pipeline system is connected to the dumbbell-shaped sample cell, and the intelligent measurement and control system is used for testing and regulating the overall calorimetric structure.

[0035] The dumbbell-shaped sample cell is entirely located inside the adiabatic thermal cavity, and its structure is either a double-sphere dumbbell or a double-cylinder dumbbell. The overall structure of the dumbbell-shaped sample cell includes: externally embedded independent heating wire assemblies 1 and 5; titanium alloy sample cells 2 and 6 with consistent structural dimensions; internal cavity structures 3 and 7 for samples of different phases; and connecting pipes 4. The two independent sample cells enable adiabatic analysis of samples with different phase compositions; one side is used for analyzing gas-liquid or gas-solid phases, while the other side is used for collecting and testing the gas phase. This unique structural design expands the internal space of the sample cell, enabling simultaneous synergistic reaction studies of multiphase, multi-component samples and other introduced substances.

[0036] The independent heating wire assembly is located on the outer surface of the dumbbell-shaped sample cell sphere or cylinder. For spherical sample cells, the heating wire is wound along a specific helical trajectory, starting from one end of the helix and rising along the outside of the sphere with a constant pitch until it covers the entire surface. For cylindrical sample cells, the heating wire is wound in an evenly spaced spiral pattern to cover the cylindrical surface, ensuring a constant distance between any two adjacent turns of the heating wire along the sample cell axis. The independent heating wire assembly is used for individual heating and temperature control of both sides of the dumbbell-shaped sample cell structure, compensating for heat loss due to heat conduction in real time. Its unique winding method ensures uniform heating of the outer surface of the sample cell junction.

[0037] In this embodiment, heat loss compensation for multiphase and multicomponent sample reaction process is achieved by using externally embedded independent heating wire assemblies 1 and 5. The independent heating wire assemblies 1 and 5 are made of nickel-chromium alloy heating wire with stable structure and strong corrosion resistance, which greatly extends the service life of the overall sample cell structure. The heating wire assembly is evenly wound around the outer wall of the sample cell, which greatly avoids the risk of local overheating.

[0038] This embodiment effectively expands the reaction space of multiphase and multicomponent samples by using sample cells 2 and 6 with consistent structural dimensions. Sample cells 2 and 6 are made of titanium alloy material with good high-temperature resistance and strong fatigue resistance, and the titanium alloy density is 4.5 g / cm³. 3 It has an operating temperature of up to 600℃, which meets the testing requirements of conventional multiphase and multicomponent samples.

[0039] This embodiment utilizes cavity structures 3 and 7, which incorporate samples of different phases, to achieve sample separation, facilitating the study of reactant collection and phase interaction mechanisms in multiphase, multi-component samples. The connecting pipe 4 is made of titanium alloy, the same material as sample cells 2 and 6, reducing the impact of heat transfer within the dumbbell-shaped sample cell structure. Furthermore, when the multiphase, multi-component sample reaction produces gas, the connecting pipe 4 can guide the gas produced in the left sample cell 2 into the right sample cell 6. If the pressure in the right sample cell 6 exceeds a certain safety threshold, the connecting pipe 4 can balance the internal pressure of the sample cell structure, ensuring the safe conduct of thermal stability testing of the multiphase, multi-component sample.

[0040] Please see Figure 2 This embodiment proposes a gas pipeline for testing multiphase and multi-component samples based on a dumbbell-shaped sample cell structure. The overall structure of the gas pipeline includes: a cooling gas cylinder 8, a blowing gas cylinder 9, a gas collecting cylinder 10, pressure sensors 11 and 12, four-way connectors 13 and 14, a pressure relief valve 15, and on / off gas valves 16, 17, and 18.

[0041] In this embodiment, two four-way connectors 13 and 14 are used to ensure the smooth flow of gas throughout the gas path structure. The four-way connectors 13 and 14 are closed structures, with plugs or temperature sensors connected to the upper ends of the connectors according to testing requirements; the lower sides of the four-way connectors connect to both sides of the dumbbell-shaped sample cell, and the reaction pressure on both sides of the dumbbell-shaped sample cell is monitored in real time by two pressure sensors 11 and 12.

[0042] Preferably, the left side of the four-way connector 13 is connected to the outside air and the cooling gas cylinder 8 via a pressure relief valve 15 and a gas switching valve 16, respectively. It should be noted that during normal thermal stability testing, both the gas switching valve 16 and the pressure relief valve 15 are closed. After the thermal stability test of the multiphase, multi-component sample is completed, the pressure relief valve 15 is opened and the gas switching valve 16 is closed, allowing the gas pipeline system to be directly connected to the atmospheric environment, achieving the effect of pressure release at the end of the reaction; the pressure relief valve 15 is closed and the gas switching valve 16 is opened, allowing cooling gas to be introduced into the gas pipeline from the cooling gas cylinder 8 (the built-in gas is usually nitrogen), achieving rapid cooling after the reaction.

[0043] Preferably, the right side of the four-way connector 14 is connected to the gas collecting cylinder 10 and the blowing cylinder 9 via gas valves 17 and 18, respectively. When multiphase and multi-component sample testing requires analysis of the gas-producing components, the gas valve 17 is opened and the gas valve 18 is closed. The gas produced by the reaction flows through the gas pipeline to the gas collecting cylinder 10, thereby achieving the effect of collecting the gas produced by the reaction and using it to analyze the influence of other gas phase components on the thermal runaway of the existing sample. When multiphase and multi-component sample adiabatic thermal testing requires studying the influence mechanism of gas phase substances on the existing reaction, the gas valve 17 is closed and the gas valve 18 is opened. The gas phase substances are blown into the gas pipeline from the blowing cylinder 9 and enter the dumbbell-shaped sample cell through the four-way connector 14, achieving the effect of gas phase substances intervening in the adiabatic thermal reaction.

[0044] Please see Figure 3 In this embodiment, precise temperature control of multiphase and multicomponent sample reaction is achieved by using externally embedded independent heating wire assemblies 1 and 5.

[0045] The temperature control logic of the independent heating wire assembly is as follows:

[0046] (1) Add the multiphase and multicomponent sample to be tested into the left sample cell and initialize the temperature control parameters;

[0047] (2) Real-time feedback of the power of the independent heating wire on the outer surface of the left sample cell based on the temperature difference between the preset temperature and the temperature measured by the temperature sensor; detection of whether the reaction has occurred after the step temperature is reached;

[0048] (3) After the reaction occurs, the independent heating wire on the outer surface of the left sample cell is controlled to heat and track the sample reaction temperature until the reaction ends.

[0049] (4) The heating wire on the outer surface of the sample cell on the right side controls the temperature by following the temperature of the gas phase inside the cavity throughout the experiment.

[0050] The specific temperature control steps are as follows: Initial temperature control parameters such as the starting interval temperature, starting interval temperature rise rate, step size, step holding time, and reaction detection threshold are set. When the sample temperature is lower than the starting interval temperature, the heating wire of the adiabatic furnace body heats the furnace body according to the starting interval temperature rise rate. The difference between the temperature measured by the temperature sensor and the target temperature of the starting interval is fed back to the output power of the embedded heating wire assemblies 1 and 5 in real time. When the temperature measured by the temperature sensor meets the holding temperature condition, the output of the embedded heating wire assemblies 1 and 5 is maintained at a constant temperature, and the holding temperature indicator starts counting. By real-time feedback of the sample's heating rate, if the sample's heating rate is higher than the reaction detection threshold, a reaction is determined to have occurred. At this time, the output of the embedded heating wire is controlled to track the sample temperature until the reaction ends. If the holding temperature count does not detect a reaction within the set holding time, the next step target temperature is calculated. Each step temperature control logic follows the starting interval step until the adiabatic thermal test ends.

[0051] Please see Figure 4In this embodiment, the furnace heating wire assembly 21, pressure sensors 11 and 12, and temperature sensors 19 and 20 work together to complete the feedback control of the entire measurement and control system. The specific control logic is as follows: Temperature sensors 19 and 20, and pressure sensors 11 and 12 monitor the temperature and pressure changes on both sides of the dumbbell-shaped sample cell in real time. When the adiabatic thermal test of the multiphase multicomponent sample begins, the furnace heating wire assembly 21 starts working first. The heat loss generated during the heating process is compensated by the output of the external heating wire assemblies 1 and 5. The real-time temperature changes measured by temperature sensors 19 and 20 are fed back to the control system. The system outputs feedback based on the temperature detection value and the set value, thereby changing the output power of the heating wire to achieve the effect of feedback control. When the real-time pressure value measured by pressure sensors 11 and 12 changes, the corresponding output is sent to the gas pipeline system to realize the pressure regulation of the entire measurement and control system.

[0052] This embodiment proposes a dumbbell-shaped sample cell structure for multiphase and multicomponent samples and implements feedback control for the entire measurement and control system. Furthermore, this embodiment also proposes a standard testing method for multiphase and multicomponent samples, as described below:

[0053] Step 1: Close the pressure relief valve 15 and switch the air valves 16, 17, and 18 to ensure the airtightness of the entire device.

[0054] Step 2: Load the weighed multiphase multicomponent sample into the left cavity 3 of the dumbbell-shaped sample cell, open the gas valve 17, and keep the gas valves 16 and 18 and the pressure relief valve 15 closed. The dumbbell-shaped sample cell is fixed to the four-way connectors 13 and 14 through the compression fitting.

[0055] Step 3: The measurement and control system sets the adiabatic thermal experiment parameters, the furnace heating wire assembly 21 starts heating, and the temperature sensors 19 and 20 detect the temperature inside the dumbbell-shaped sample cell in real time. Based on the comparison between the measured temperature and the set temperature, the output power of the external independent heating wires 1 and 5 is adjusted.

[0056] Step 4: When the reaction of the multiphase multicomponent sample is detected, the furnace heating wire assembly 21 and the external independent heating wire assemblies 1 and 5 stop active heating. Based on the temperature measured by temperature sensors 19 and 20, the output power of the external heating wires 1 and 5 is fed back, and the temperature on both sides of the dumbbell-shaped sample cell is tracked in real time.

[0057] Step 5: Pressure sensors 11 and 12 detect the pressure changes on both sides of the dumbbell-shaped sample cell respectively. The reaction gas enters the gas collecting bottle 10 sequentially through the connecting pipe 4, sample cell 6, four-way connector 14, and gas valve 17.

[0058] Step 6: After the adiabatic thermal test of the multiphase and multicomponent sample is completed, close the gas valves 16, 17, and 18, and open the pressure relief valve 15 to achieve the pressure relief effect.

[0059] Step 7: Close the pressure relief valve 15, switch the gas valves 17 and 18, and open the switch the gas valve 16. Cooling gas enters the dumbbell-shaped sample cell from the cooling gas cylinder 8 through the four-way connector 13 to achieve rapid cooling.

[0060] To verify the above design, this application further provides the following simulated thermal runaway experiment.

[0061] This application presents a simulation experiment on lithium iron phosphate materials based on a modified dumbbell-shaped sample cell structure and testing method. The lithium iron phosphate electrolytic material was placed in the left sample cell cavity, and the initial temperature control parameters were set as follows: start-up temperature 50℃, start-up isothermal time 120 min, step temperature increment 5℃, step temperature increment rate 5℃ / min, step isothermal time 90 min, reaction judgment threshold 0.03℃ / min, and reaction termination temperature 350℃. (See attached...) Figure 5 .

[0062] like Figure 6 As shown, the results indicate that the initial reaction temperature of the left sample cell was 101.2℃, the adiabatic temperature rise was 295.4℃, and the gas generated during the reaction entered the right sample cell through the dumbbell-shaped sample cell structure. The adiabatic pressure rise of the right sample cell was 0.023 MPa, which achieved the separation of different phases of the multiphase and multi-component sample, facilitating subsequent analysis of gas components.

[0063] The above description is an embodiment of the present invention. It should be noted that, for those skilled in the art, various modifications and improvements can be made without departing from the principle of the present invention, and these should also be considered within the scope of protection of the present invention.

Claims

1. An adiabatic thermal sample cell structure for multiphase, multi-component samples, characterized in that, include: The sample cell body has a dumbbell-shaped structure, including two independent sample cell sections for respectively accommodating samples with different phase compositions; The heating assembly includes an independent heating wire tightly wound around the outside of the sample cell body for individually heating and controlling the temperature of the sample cell to compensate for heat loss and ensure uniform heating of the sample cell surface. A gas pipeline system, which is connected to the main body of the sample cell, is used to introduce and collect gas during the sample reaction process; The measurement and control system is used to monitor the temperature and pressure parameters inside the sample cell in real time, and to adjust the heating components and the gas pipeline system according to the monitoring results. The main body of the sample cell has a double-sphere dumbbell shape or a double-cylinder dumbbell shape. The two independent sample cell sections are used for analyzing gas-liquid or gas-solid phases, as well as for the collection and testing of the gas phase. The independent heating wire is wound around the outer surface of the sphere or cylinder of the sample cell body along a spiral trajectory, and the heating wire starts from one end of the spiral and rises along the outside of the sphere or cylinder with a constant pitch until it covers the entire surface. The gas pipeline system includes a pressure relief valve, two four-way connectors, multiple on / off valves, a gas collecting cylinder, and a cooling gas cylinder. The pressure relief valve and the on / off valves are both connected to the sample cell through four-way connectors for releasing reaction pressure and introducing cooling gas. The measurement and control system includes a temperature sensor and a pressure sensor, which are independently connected to the remaining two sides of the four-way connector to monitor the temperature and pressure changes on both sides of the sample cell in real time.

2. A method for adiabatic thermal testing of multiphase, multi-component samples, employing the structure described in claim 1, characterized in that, Includes the following steps: Step 1. Load the multiphase, multi-component sample into the left cavity of the dumbbell-shaped sample cell, which includes two independent sample cell sections for accommodating samples with different phase compositions respectively. Step 2. Close the pressure relief valve and the on / off valve in the gas pipeline system to ensure the airtightness of the entire device; Step 3. Set the adiabatic thermal experiment parameters, start the heating component to heat the sample cell, detect the temperature in the sample cell in real time through the temperature sensor, and adjust the output power of the heating component according to the comparison between the measured temperature and the set temperature. Step 4. After detecting that the sample has started to react, stop active heating, adjust the output power of the heating component according to the temperature feedback measured by the temperature sensor, and track the temperature change in the sample cell in real time. Step 5. Collect the gases generated during the reaction through a gas pipeline system and monitor the pressure changes in the sample cell using a pressure sensor; Step 6. After the test, release the pressure and cool down rapidly through the gas pipeline system.

3. The adiabatic thermal testing method for multiphase, multi-component samples according to claim 2, characterized in that, In step 3, the adiabatic thermal experiment parameters include the start-up interval temperature, the start-up interval temperature rise rate, the step size, the step isothermal time, and the reaction detection threshold.

4. The adiabatic thermal testing method for multiphase, multi-component samples according to claim 2, characterized in that, In step 4, when the sample heating rate is detected to be higher than the preset reaction detection threshold, it is determined that a reaction has occurred. At this time, the output power of the heating component is controlled to track the sample temperature until the reaction ends.

5. The adiabatic thermal testing method for multiphase, multi-component samples according to claim 2, characterized in that, In step 5, the gas pipeline system includes a pressure relief valve, two four-way connectors, multiple on / off valves, a gas collection cylinder, and a cooling gas cylinder. The reaction product gas enters the gas collection cylinder sequentially through the connecting pipeline, sample cell, four-way connector, and on / off valves.

6. The adiabatic thermal testing method for multiphase, multi-component samples according to claim 5, characterized in that, In step 3, the temperature sensor and pressure sensor are independently connected to both sides of the four-way connector to monitor the temperature and pressure changes on both sides of the sample cell in real time.

Citation Information

Patent Citations

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