Integrated chip for synchronous thermal analysis and synchronous thermal analysis system and method

Abstract

The invention provides an integrated chip for synchronous thermal analysis, a synchronous thermal analysis system and a synchronous thermal analysis method, and is applied to the technical field of micro-nano sensors. A heating area is formed on a resonance disc through heating of a heating element, a plurality of thermocouples are arranged on the resonance disc to form a thermopile, and a temperature measurement area for detecting the temperature of the heating area is formed; the hot ends of the thermocouples are connected to the cold ends of the thermocouples on the substrate through the wires on the plurality of connecting beams distributed around the resonance disc, so that the number of the thermocouples in the resonance disc can be increased, and the temperature sensitivity of the integrated chip can be improved; therefore, the integrated chip can meet the sample test requirements of low heat absorption / release or small temperature change, so that the measurement capability of a synchronous thermal analysis system is improved.

Description

Technical Field

[0001] The present application relates to the technical field of micro-nano sensors, and particularly relates to an integrated chip for synchronous thermal analysis, a synchronous thermal analysis system, and a method. Background Art

[0002] Thermal analysis technology is a technology for evaluating the temperature-dependent properties of substances under programmed temperature control. These technologies have been widely used in many fields such as chemical engineering, food safety, and drug analysis. Among these technologies, thermogravimetric analysis (TGA) and differential thermal analysis (DTA) are two widely used characterization technologies. TGA is a classical characterization technology used to measure the mass change of materials during programmed heating in a specific atmosphere, and is often used to study the thermal stability of materials and thermal properties such as evaporation, decomposition, dehydration, and oxidation of materials during heating. DTA mainly measures the temperature difference of materials under programmed temperature control, enabling people to study the endothermic or exothermic properties of materials during phase changes or chemical reactions. A synchronous thermal analyzer (STA) that realizes simultaneous thermogravimetric-differential thermal analysis combines TGA and DTA, and can comprehensively and multi-dimensionally understand the thermodynamic properties of materials. This is particularly valuable for studying advanced functional materials and supporting the rapid development of related research fields.

[0003] In the prior art, an instrument structure with an integrated resonant cantilever beam as the core is disclosed. Among them, through the integrated resonant cantilever beam chip, information such as the resonant frequency of the cantilever beam and the real-time temperature of the sample are obtained simultaneously, so as to obtain the mass change of the sample and the change of the temperature difference. In the design of this long-strip micro-cantilever beam structure, the sample area is near the free end of the cantilever beam, and the temperature acquisition element is a thermocouple pair with the hot end set in the sample area. Wires are arranged between the free end and the fixed end of the micro-cantilever beam, so that the cold end of the thermocouple is set in the non-heating area. However, due to the structural design of the micro-cantilever beam, the number of thermocouples is small, and it is difficult for this integrated cantilever beam chip to meet the test requirements of samples with low heat absorption / heat release, that is, small temperature changes.

[0004] Based on this, a new technical solution is needed. Summary of the Invention

[0005] In view of this, the present application provides an integrated chip for synchronous thermal analysis, a synchronous thermal analysis system, and a method.

[0006] The present application provides the following technical solutions: An integrated chip for synchronous thermal analysis provided according to the present application includes a substrate, a resonant disk, and a plurality of connecting beams; A heating element is provided on the resonant disk so that the heating element forms a heating area on the resonant disk through heating; a temperature detection element is also provided on the resonant disk, and the temperature detection element includes a plurality of thermocouples. The plurality of thermocouples are connected in series on the resonant disk to form a thermopile, so that the thermopile forms a temperature measurement area for detecting the temperature of the heating area on the resonant disk; One end of the thermocouple on the resonant disk is the hot end, the cold end of the thermocouple is on the substrate, the connecting beam is fixed on the substrate, and a plurality of the connecting beams are distributed around the resonant disk, so that the hot ends of the plurality of thermocouples are respectively connected to the cold ends of the thermocouples through wires on the corresponding connecting beams.

[0007] Preferably, the heating element includes one or more heating resistance wires, and the heating resistance wires are wound around the resonant disk.

[0008] Preferably, the thermocouples in the temperature detection element include one or more of polysilicon thermocouples, single-crystal silicon thermocouples, and metal thermocouples.

[0009] Preferably, one end of the connecting beam is connected to the substrate, and the other end of the connecting beam is connected to the resonant disk.

[0010] Preferably, a resonance excitation and detection module is provided on the connecting beam, and the resonance excitation and detection module is arranged at one end of the connecting beam close to the substrate.

[0011] Preferably, the resonance excitation and detection module includes a resonance excitation element and a resonance detection element; the resonance excitation element includes resonance driving resistors, and a plurality of resonance driving resistors are connected in series, so that the resonance excitation element is used to form resonance; The resonance detection element includes a Wheatstone bridge composed of a plurality of single-crystal silicon piezoresistors, so that the resonance detection element is used to collect the resonance frequency of the resonant disk.

[0012] Preferably, a groove cavity is formed on the substrate, one end of the connecting beam is fixed on the edge of the groove cavity, and the resonant disk is in the groove cavity area.

[0013] According to a synchronous thermal analysis system provided by the present application, it includes a first integrated chip, a second integrated chip, a control module, a data acquisition module, a test cavity, and a calculation module; the first integrated chip and the second integrated chip adopt any one of the above-mentioned integrated chips for synchronous thermal analysis; The first integrated chip and the second integrated chip are placed in the test cavity; the resonant disk of the first integrated chip is coated with a sample to be detected; The control module is connected to the first integrated chip and the second integrated chip, so that the control module controls heating of the heating area and controls the resonance excitation and detection module to form resonance; The data acquisition module is connected to the first integrated chip and the second integrated chip, so that the data acquisition module acquires the current temperature of the heating area detected by the temperature detection element and the resonance frequency acquired by the resonance excitation and detection module; The calculation module is connected to the data acquisition module, so that the calculation module calculates the data acquired by the data acquisition module to form a calculation result.

[0014] According to a synchronous thermal analysis method provided by the present application, applying the synchronous thermal analysis system includes: driving the first integrated chip and the second integrated chip with a first frequency parameter, and after stabilization, driving the heating area of the first integrated chip and the second integrated chip to increase in temperature with a first temperature parameter, acquiring the resonance frequency and the corresponding temperature during the temperature increase process of the first integrated chip and the second integrated chip, and the temperature difference of the heating area and the corresponding temperature during the temperature increase process of the first integrated chip and the second integrated chip as reference data; Stop the vibration of the first integrated chip and the second integrated chip, move them out of the test chamber, and after cooling to room temperature, coat the sample to be detected on the resonance disk of the first integrated chip; Move the first integrated chip and the second integrated chip into the test chamber, drive the heating area of the first integrated chip and the second integrated chip to increase in temperature with a first frequency parameter, and after stabilization, drive the heating area of the first integrated chip and the second integrated chip to increase in temperature with the first temperature parameter, acquire the resonance frequency and the corresponding temperature during the temperature increase process of the first integrated chip and the second integrated chip, and the temperature difference of the heating area and the corresponding temperature during the temperature increase process of the first integrated chip and the second integrated chip as detection data; Fit the thermogravimetric curve and differential thermal curve of the sample to be detected through the reference data and the detection data.

[0015] Compared with the prior art, the beneficial effects that can be achieved by at least one of the above technical solutions adopted in the present application at least include: In the present application, a heating area is formed on the resonance disk by heating with a heating element, a plurality of thermocouples connected in series are arranged on the resonance disk to form a thermopile for detecting the temperature of the heating area, and the hot ends of the thermocouples are connected to the cold ends of the thermocouples on the substrate through wires on a plurality of connecting beams distributed around the resonance disk, which can increase the number of thermocouples in the resonance disk and improve the temperature sensitivity of the integrated chip, so that the integrated chip can meet the test requirements of samples with low heat absorption / heat release or small temperature changes, thereby improving the measurement ability of the synchronous thermal analysis system. Description of the Drawings

[0016] To more clearly illustrate the technical solutions of the embodiments of the present application, the accompanying drawings required for the embodiments will be briefly introduced below. Obviously, the accompanying drawings in the following description are only some embodiments of the present application. For those of ordinary skill in the art, without creative efforts, other accompanying drawings can be obtained based on these drawings.

[0017] Figure 1 is an aerial view schematic diagram of the integrated chip for synchronous thermal analysis of the present application; Figure 2 is a first top view schematic diagram of the integrated chip for synchronous thermal analysis of the present application; Figure 3 is a schematic diagram of the test results of the temperature sensitivity of the present application; Figure 4 is a schematic diagram of the test results of the melting process of indium (In) in the present application; Figure 5 is a second top view schematic diagram of the integrated chip for synchronous thermal analysis of the present application.

[0018] Reference numerals: 1, resonance excitation and detection module; 2, temperature detection element; 3, heating element; 4, heat insulation hole; 5, wire; 6, cold end; 7, hot end; 8, substrate. Specific embodiments

[0019] The embodiments of the present application will be described in detail below with reference to the accompanying drawings.

[0020] The following specific examples illustrate the implementation manners of the present application. Those skilled in the art can easily understand other advantages and effects of the present application from the content disclosed in this specification. Obviously, the described embodiments are only some embodiments of the present application, rather than all embodiments. The present application can also be implemented or applied through other different specific implementation manners. Various details in this specification can also be modified or changed based on different viewpoints and applications without departing from the spirit of the present application. It should be noted that, without conflict, the following embodiments and the features in the embodiments can be combined with each other. All other embodiments obtained by those of ordinary skill in the art based on the embodiments in the present application without creative efforts belong to the scope of protection of the present application.

[0021] It should be noted that the following description pertains to various aspects of embodiments within the scope of the appended claims. It will be apparent that the aspects described herein can be embodied in a wide variety of forms, and any specific structure and / or function described herein is merely illustrative. Based on this application, those skilled in the art should understand that one aspect described herein can be implemented independently of any other aspect, and two or more of these aspects can be combined in various ways. For example, any number and aspects set forth herein can be used to implement the device and / or practice the method. Additionally, this device can be implemented and this method can be practiced using other structures and / or functionality in addition to one or more of the aspects set forth herein.

[0022] It should also be noted that the diagrams provided in the following embodiments only schematically illustrate the basic concept of this application. The diagrams only show the components related to this application and are not drawn according to the number, shape, and size of the components in actual implementation. The type, quantity, and proportion of each component in actual implementation can be arbitrarily changed, and the component layout type may also be more complex.

[0023] Furthermore, in the following description, specific details are provided to facilitate a thorough understanding of the examples. However, those skilled in the art will understand that the examples can be practiced without these specific details.

[0024] Through in-depth research and improvement exploration of the synchronous thermal analyzer and the synchronous thermal analysis method, the applicant found that: the working principle of existing commercial STAs is to use a high-precision electronic balance to monitor the mass change of the sample under programmed temperature control, and at the same time use a temperature measurement system to record the temperature difference change between the sample and the reference sample. Such instruments have problems such as large sample consumption, long analysis time, high energy consumption, and difficulty in coupling. To solve the pain points of existing instruments, the Chinese patent literature with the publication number CN117907146A discloses a chip-type synchronous thermal analyzer and a synchronous thermal analysis method, which is an instrument structure with an integrated resonant cantilever beam as the core and a corresponding test method. The core is to obtain information such as the resonant frequency of the cantilever beam and the real-time temperature of the sample through the integrated resonant cantilever beam chip, so as to obtain the sample mass change and the temperature difference change. However, the integrated resonant cantilever beam chip disclosed in this patent adopts a long-strip micro-cantilever beam structure design, the sample area is located near the free end of the cantilever beam, and the temperature acquisition element is a thermocouple pair with the hot end set in the sample area. Since the cold end of the thermocouple needs to be set in the non-heating area, wires need to be arranged between the free end and the fixed end of the micro-cantilever beam. Limited by the heat-blocking hole structure of the micro-cantilever beam, the space left for the wires is limited, so only 2 thermocouples can be arranged to form a thermopile. The temperature measurement ability (temperature sensitivity) of the thermopile is proportional to the number of thermocouples. Therefore, the chip disclosed in this patent has a temperature sensitivity of only 0.7 mV / K, which is difficult to meet the test requirements of samples with low heat absorption / heat release (small temperature change).

[0025] Based on this, the following will describe the technical solutions provided by the embodiments of the present application in conjunction with the accompanying drawings.

[0026] An embodiment of this specification proposes an integrated chip for synchronous thermal analysis, as Figure 1 、 Figure 2 and Figure 5 shown, including a substrate 8, a resonant disk, and a plurality of connecting beams. A heating element 3 is provided on the resonant disk so that the heating element 3 forms a heating area on the resonant disk through heating; a temperature detection element 2 is also provided on the resonant disk. The temperature detection element 2 includes a plurality of thermocouples, and the plurality of thermocouples are connected in series on the resonant disk to form a thermopile, so that the thermopile forms a temperature measurement area for detecting the temperature of the heating area on the resonant disk. The resonant disk is used for coating the sample to be detected, and the heating area and the temperature measurement area are used for coating the sample to be detected. The heating area and the temperature measurement area can coincide. The sample to be detected is, for example, indium. The heating element 3 can be distributed around the center of the resonant disk, and the hot ends 7 of the thermocouples can be located at the center of the resonant disk to form a thermopile. Using a thermopile for temperature measurement, increasing the number of thermocouples to improve the temperature detection ability.

[0027] One end of the thermocouple is at the hot end 7 of the resonant disk, the cold end 6 of the thermocouple is on the substrate 8, the connecting beams are fixed on the substrate 8, and a plurality of connecting beams are distributed around the resonant disk so that the hot ends 7 of the plurality of thermocouples are respectively connected to the cold end 6 of the thermocouple through the wires 5 on the corresponding connecting beams.

[0028] In one embodiment, the heating element 3 includes one or more heating resistance wires, and the heating resistance wires are wound around the resonant disk.

[0029] In one embodiment, the thermocouple in the temperature detection element 2 includes one or more of a polysilicon thermocouple, a single-crystal silicon thermocouple, and a metal thermocouple. For example, the temperature detection element 2 is a thermopile composed of a plurality of polysilicon thermocouples, single-crystal silicon thermocouples, metal thermocouples, etc.

[0030] In one embodiment, one end of the connecting beam is connected to the substrate, and the other end of the connecting beam is connected to the resonant disk. The cold end and the hot end are respectively arranged near the two ends of the connecting beam.

[0031] In one embodiment, heat-blocking holes 4 are provided on the connecting beam, and the heat-blocking holes 4 are located between the resonance excitation and detection module 1 and the resonant disk, and the wires 5 are arranged on both sides of the heat-blocking holes 4 on the connecting beam.

[0032] In one embodiment, a groove cavity is formed on the substrate 8, one end of the connecting beam is fixed on the edge of the groove cavity, and the resonant disk is in the groove cavity area.

[0033] In one embodiment, a resonance excitation and detection module 1 is provided on the connecting beam, and the resonance excitation and detection module 1 is arranged at one end of the connecting beam close to the substrate 8.

[0034] In one embodiment, the resonance excitation and detection module 1 includes a resonance excitation element and a resonance detection element; the resonance excitation element includes resonance driving resistors, and a plurality of resonance driving resistors are connected in series so that the resonance excitation element is used to form resonance; the resonance detection element includes a Wheatstone bridge composed of a plurality of single-crystal silicon piezoresistors so that the resonance detection element is used to collect the resonance frequency of the resonant disk.

[0035] This application is a MEMS integrated chip for synchronous thermal analysis. Here, MEMS, the full name is Micro-Electro-Mechanical Systems, that is, micro-electromechanical systems. In order to improve the problem of the relatively low temperature sensitivity of the existing synchronous thermal analysis chip based on a resonant microcantilever beam, this application discloses a disk-shaped MEMS integrated synchronous thermal analysis chip. The center of this chip is a disk structure, and it is connected to the substrate 8 through 4 bridge-like structures, similar to the arrangement of 4 cantilever beam structures facing each other in pairs and sharing a sample area (the central disk). Due to having more wiring space for the thermocouple wires 5, the disk structure serves as the sample area, and the number of temperature-measuring thermocouples integrated on it can reach 8, thereby greatly improving the temperature measurement sensitivity. Other structures are similar to those of the microcantilever beam. A heating element 3 composed of metal coils is still integrated on the disk. Resonant excitation and frequency detection elements are integrated near the fixed-end positions of the 4 bridge-like structures, which can excite the entire structure to resonate and obtain the resonant frequency.

[0036] As Figure 2 and Figure 3 shown, using the disk-shaped MEMS integrated synchronous thermal analysis chip to replace the microcantilever beam integrated synchronous thermal analysis chip, the number of thermocouples is increased from 2 to 8, thereby increasing the temperature sensitivity by 4 times, which can meet the synchronous thermal analysis test requirements of most samples. The test process is similar to that of a chip-type synchronous thermal analyzer and synchronous thermal analysis method with the publication number CN117907146A. As Figure 4 shown, the DTA test results of the indium melting process are provided. Compared with the former patent, the signal peak is much larger.

[0037] This MEMS integrated chip mainly has three major types of components: a micro-heater component, a thermocouple temperature detection component, and a resonant drive / detection component: The micro-heater spirally winds around the upper right, lower right, upper left, and lower left sides of the resonant disk to provide the operating temperature for the device. The thermocouple temperature detection component consists of 16 pairs of polysilicon-metal thermocouples. Its hot ends 7 are concentrated at the center of the resonant disk, and the cold ends 6 are arranged at the roots of the connecting beams. The temperature change of the hot ends 7 is read through the Seebeck effect. The resonant drive resistors are arranged at the roots of the four connecting beams and are connected in series. The disk is driven to resonate through the thermal effect. The resonant detection resistors consist of four single-crystalline silicon piezoresistors to form a Wheatstone bridge at the roots of the connecting beams, closer to the center compared to the drive resistors. Combining with a phase-locked loop circuit to track the resonant frequency of the resonant disk. This application can improve the temperature sensitivity of the synchronous thermal analysis MEMS chip, thereby improving the measurement ability of the chip-type synchronous thermal analyzer.

[0038] This embodiment of the specification also discloses a synchronous thermal analysis system, including a first integrated chip, a second integrated chip, a control module, a data acquisition module, a test chamber, and a calculation module; the first integrated chip and the second integrated chip adopt any of the above-mentioned integrated chips for synchronous thermal analysis.

[0039] The first integrated chip and the second integrated chip are placed in the test chamber; the resonant disk of the first integrated chip is coated with the sample to be detected; the control module is connected to the first integrated chip and the second integrated chip, so that the control module controls the heating of the heating area and controls the resonant excitation and the detection module 1 to form resonance; the data acquisition module is connected to the first integrated chip and the second integrated chip, so that the data acquisition module acquires the current temperature of the heating area detected by the temperature detection element 2 and the resonant frequency acquired by the resonant excitation and the detection module 1; the calculation module is connected to the data acquisition module, so that the calculation module calculates the data acquired by the data acquisition module to form a calculation result.

[0040] The control module controls the connection of the heating element 3 to perform heating; the control module controls the connection of the resonant excitation element to form resonance; the data acquisition module is connected to the resonance detection element.

[0041] The synchronous thermal analysis system further includes an atmosphere adjustment module, the atmosphere adjustment module communicates with the test chamber, and the atmosphere adjustment module is connected to the control module, so that the atmosphere adjustment module adjusts the atmosphere in the test chamber under the control of the control module.

[0042] The synchronous thermal analysis system further includes an input / output module, the input / output module is respectively connected to the control module and the calculation module, and is used to receive inputs to adjust the control parameters of the control module, and output the calculation results of the calculation module.

[0043] The control module inputs a voltage control signal to the resonant excitation element and the heating element 3, and the data acquisition module acquires the frequency signal and the temperature signal corresponding to the resonance detection element and the temperature detection element 2, and adjusts the input voltage control signal according to the acquired frequency signal and temperature signal, so as to achieve precise temperature control, improve the analysis accuracy.

[0044] In this application, the size of the first integrated chip for coating the sample to be detected and the second integrated chip without coating the sample to be detected is in the micron level, and the sample loading capacity of the integrated chip is in the nanogram level; in addition, the self-heating programmed temperature rise method is adopted for the sample on the integrated chip, which can realize reaction and real-time measurement on the first integrated chip at a faster heating rate. Not only the heating rate is several times higher than that of the existing commercial thermal analysis instruments, but also the analysis accuracy is higher. At the same time, the accuracy of the sample analysis result will not be affected by the sample amount and the gas environment. In this application, the self-heating programmed temperature rise method in the micro-integrated chip is adopted, abandoning the existing large-volume heating cavity device, realizing simultaneous multi-channel measurement thermal analysis of multiple chips with different samples loaded respectively with different heating programs synchronously, greatly shortening the time-consuming, and further improving the efficiency of thermal analysis measurement.

[0045] The resonant excitation element can be configured as a thermal excitation circuit built with single crystal silicon resistors; the resonant detection element can be configured as a Wheatstone bridge circuit built with single crystal silicon resistors to further improve its working performance.

[0046] The heating element 3 can be configured as a high temperature resistant metal heating wire, and the wound coil can improve its heating efficiency.

[0047] The temperature detection element 2 can be configured as a temperature measuring thermocouple arranged in a crystalline silicon thermocouple pair. The polycrystalline silicon thermocouple pair can use P-type and N-type polycrystalline silicon as thermocouple materials, and its Seebeck coefficient is much higher than that of a traditional metal structure thermocouple.

[0048] The frequency signal and temperature signal corresponding to the resonance detection element and the temperature detection element 2 are specific physical quantities, such as voltage values, which can be converted into corresponding frequency values ​​and temperature values ​​by using a calculation module through a mapping relationship between a preset physical quantity and frequency or temperature.

[0049] The atmosphere adjustment module may include a gas chamber and a vacuum pump, and the gas chamber and the vacuum pump are respectively connected to the test chamber module by gas. The test chamber is used to maintain the detection environment atmosphere, and the atmosphere adjustment module is used to adjust the atmosphere in the test chamber. Different environmental atmospheres can be adjusted by the atmosphere adjustment module according to different analysis projects, so as to meet the needs of different analysis projects. In thermogravimetric analysis, the types of environmental atmospheres may involve protective atmospheres such as nitrogen, argon, and helium, or oxidizing atmospheres such as oxygen and air and other special atmospheres, or vacuum atmospheres, etc. In differential thermal analysis, the types of environmental atmospheres may involve oxidizing, reducing, and inert atmospheres, etc. Atmospheres of different properties have a certain influence on thermogravimetric curves or differential thermal curves.

[0050] The present embodiment also provides a synchronous thermal analysis method, which uses the above-mentioned synchronous thermal analysis system, including: driving the first integrated chip and the second integrated chip with a first frequency parameter, and driving the heating area of ​​the first integrated chip and the second integrated chip to heat up with a first temperature parameter after stabilization, collecting the resonant frequency and the corresponding temperature of the first integrated chip and the second integrated chip during the heating process, and the temperature difference and the corresponding temperature of the heating area of ​​the first integrated chip and the second integrated chip during the heating process as reference data.

[0051] The first integrated chip and the second integrated chip stop vibrating, and are removed from the test cavity. After cooling to room temperature, the sample to be tested is coated on the resonance disk of the first integrated chip.

[0052] Move the first integrated chip and the second integrated chip into the test chamber, drive the heating regions of the first integrated chip and the second integrated chip to increase in temperature with a first frequency parameter, and after stabilization, drive the heating regions of the first integrated chip and the second integrated chip to increase in temperature with a first temperature parameter. Collect the resonant frequencies and corresponding temperatures during the temperature increase of the first integrated chip and the second integrated chip, as well as the temperature difference between the heating regions and the corresponding temperatures during the temperature increase of the first integrated chip and the second integrated chip as detection data.

[0053] Fit the thermogravimetric curve and differential thermal curve of the sample to be detected through the reference data and the detection data.

[0054] This synchronous thermal analysis method further includes: dispersing the solid sample to be detected in a solvent to form a liquid mixture, treating the mixture with ultrasonic waves, and dripping the treated mixture onto the area of the first integrated chip to be coated with the sample to be detected through a micromanipulator and drying it. The above solvent can include one or all of anhydrous ethanol and deionized water, and the solvent can be freely selected according to the needs of the analysis project; the mixture after ultrasonic treatment can be a suspension or a solution.

[0055] This synchronous thermal analysis method further includes: driving the first integrated chip and the second integrated chip to increase in temperature with a first speed parameter and a first temperature parameter to remove the impurities adsorbed on the first integrated chip and the second integrated chip. By placing the first integrated chip and the second integrated chip in the test chamber for self-cleaning, the accuracy of subsequent analysis can be improved.

[0056] Among them, the method for fitting the thermogravimetric curve of the sample to be detected includes: Subtract the vibration frequency value of the first integrated chip corresponding to the temperature in the reference data from the vibration frequency value of the first integrated chip corresponding to the temperature change in the detection data to obtain the vibration frequency conversion value corresponding to the temperature change.

[0057] Convert the conversion value of the vibration frequency corresponding to the temperature change into the mass of the sample to be detected according to the relationship between the vibration frequency and the mass of the sample to be detected.

[0058] Calculate the percentage of weight loss of the mass of the sample to be detected corresponding to the temperature change.

[0059] Fit the thermogravimetric curve of the sample to be detected according to the percentage of weight loss of the mass of the sample to be detected corresponding to the temperature change.

[0060] Among them, the method for fitting the differential thermal curve of the sample to be detected includes: Subtract the temperature difference between the first integrated chip and the second integrated chip corresponding to the temperature in the reference data from the temperature difference between the first integrated chip and the second integrated chip corresponding to the temperature change in the detection data to obtain the fitting value of the temperature difference corresponding to the temperature change.

[0061] According to the fitted value of the temperature difference between the first integrated chip and the second integrated chip corresponding to the change in temperature, the differential thermal curve of the sample to be detected is fitted.

[0062] During the analysis of the thermogravimetric curve, the mass of the sample to be detected needs to be obtained by coating the vibration frequency of the first integrated chip of the sample to be detected. Similarly, the corresponding mass value can be obtained by using the mapping relationship between the preset frequency value and the mass of the sample to be detected and performing conversion using the calculation module.

[0063] In this specification, for the same and similar parts among the various embodiments, reference can be made to each other. Each embodiment focuses on the differences from other embodiments. In particular, for the embodiments described later, the description is relatively simple, and for the relevant parts, reference can be made to the partial description of the foregoing embodiments.

[0064] As described above, the above is only the specific implementation manner of the present application, but the protection scope of the present application is not limited thereto. Any changes or substitutions that can be easily thought of by those skilled in the art within the technical scope disclosed in the present application should be covered by the protection scope of the present application. Therefore, the protection scope of the present application should be subject to the protection scope of the claims.

Claims

1. An integrated chip for synchronous thermal analysis, characterized in that: It includes a substrate, a resonant disk, and a plurality of connecting beams; The resonant disk is provided with a heating element, so that the heating element forms a heating area on the resonant disk by heating; the resonant disk is also provided with a temperature detection element, and the temperature detection element includes a plurality of thermocouples, and the plurality of thermocouples are connected in series on the resonant disk to form a thermopile, so that the thermopile forms a temperature measurement area on the resonant disk for detecting the temperature of the heating area; One end of the thermocouple on the resonance disk is the hot end, and the cold end of the thermocouple is on the substrate. The connecting beam is fixed on the substrate, and a plurality of the connecting beams are distributed around the resonance disk, so that the hot ends of the plurality of thermocouples are respectively connected to the cold ends of the thermocouples through the corresponding wires on the connecting beams.

2. The integrated chip for synchronous thermal analysis according to claim 1, characterized in that: The heating element includes one or more heating resistance wires, and the heating resistance wires are wound around the resonance disk.

3. The integrated chip for synchronous thermal analysis according to claim 1, characterized in that: The thermocouple in the temperature detection element includes one or more of a polysilicon thermocouple, a single crystal silicon thermocouple and a metal thermocouple.

4. The integrated chip for synchronous thermal analysis according to claim 1, characterized in that: One end of the connecting beam is connected to the substrate, and the other end of the connecting beam is connected to the resonance disk.

5. The integrated chip for simultaneous thermal analysis according to claim 1, characterized in that: A resonance excitation and detection module is provided on the connection beam, and the resonance excitation and detection module is arranged on one end of the connection beam close to the substrate.

6. The integrated chip for simultaneous thermal analysis according to claim 5, characterized in that: The resonance excitation and detection module includes a resonance excitation element and a resonance detection element; the resonance excitation element includes a resonance drive resistor, and a plurality of resonance drive resistors are arranged in series so that the resonance excitation element is used to form resonance; The resonance detection element includes a Wheatstone bridge composed of a plurality of single crystal silicon piezoresistors, so that the resonance detection element is used to collect the resonance frequency of the resonance disk.

7. The integrated chip for simultaneous thermal analysis according to claim 5, characterized in that: The connecting beam is provided with a heat-resistance hole, and the heat-resistance hole is located between the resonance excitation and detection module and the resonance disk, and the wire is arranged on both sides of the heat-resistance hole on the connecting beam.

8. The integrated chip for simultaneous thermal analysis according to claim 4, characterized in that: A cavity is formed on the substrate, one end of the connecting beam is fixed to the edge of the cavity, and the resonance disk is located in the cavity area.

9. A synchronous thermal analysis system, characterized in that: It comprises a first integrated chip, a second integrated chip, a control module, a data acquisition module, a test chamber and a computing module; the first integrated chip and the second integrated chip are the integrated chips for synchronous thermal analysis described in any one of claims 5 to 7; The first integrated chip and the second integrated chip are placed in the test cavity; the resonance disk of the first integrated chip is used to coat the sample to be tested; The control module is connected to the first integrated chip and the second integrated chip, so that the control module controls the heating of the heating area and controls the resonance excitation and detection module to form resonance; The data acquisition module is connected to the first integrated chip and the second integrated chip so that the data acquisition module acquires the current temperature of the heating area detected by the temperature detection element and the resonant frequency acquired by the resonant excitation and detection module; The calculation module is connected to the data acquisition module so that the calculation module calculates the data collected by the data acquisition module to form a calculation result.

10. A synchronous thermal analysis method, characterized in that: The synchronous thermal analysis system of claim 9 comprises: driving the first integrated chip and the second integrated chip with a first frequency parameter, driving the heating area of ​​the first integrated chip and the second integrated chip to heat up with a first temperature parameter after stabilization, collecting the resonant frequency and the corresponding temperature of the first integrated chip and the second integrated chip during the heating process, and the temperature difference and the corresponding temperature of the heating area of ​​the first integrated chip and the second integrated chip during the heating process as the reference data; Stop vibrating the first integrated chip and the second integrated chip, remove them from the test chamber, and apply the sample to be tested to the resonance disk of the first integrated chip after cooling to room temperature; The first integrated chip and the second integrated chip are moved into the test chamber, and the heating regions of the first integrated chip and the second integrated chip are driven to heat up with the first frequency parameter, and after stabilization, the heating regions of the first integrated chip and the second integrated chip are driven to heat up with the first temperature parameter, and the resonant frequency and the corresponding temperature during the heating process of the first integrated chip and the second integrated chip, as well as the temperature difference and the corresponding temperature of the heating region during the heating process of the first integrated chip and the second integrated chip are collected as detection data; The thermogravimetric curve and the differential thermal curve of the sample to be tested are fitted by using the reference data and the test data.

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