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

Abstract

The present application provides an integrated chip, a synchronous thermal analysis system, and a method for synchronous thermal analysis, which are applied to the field of micro-nano sensor technology. In the method, a heating area is formed on a resonant disk by heating with a heating element, and a plurality of thermocouples are arranged on the resonant disk to form a thermopile, forming a temperature measurement area for detecting the temperature of the heated area. The hot ends of the thermocouples are connected to the cold ends of the thermocouples on the substrate via wires on a plurality of connecting beams distributed around the resonant disk. This can increase the number of thermocouples in the resonant disk, thereby improving the temperature sensitivity of the integrated chip, enabling the integrated chip to meet the testing requirements of samples with low heat absorption / release or small temperature changes, thereby improving the measurement capability of the synchronous thermal analysis system.

Description

Technical Field

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

[0002] Thermal analysis techniques evaluate the temperature-dependent properties of substances under programmed temperature. These techniques have been widely used in fields such as chemical engineering, food safety, and pharmaceutical analysis. Among these techniques, thermogravimetric analysis (TGA) and differential thermal analysis (DTA) are two widely used characterization techniques. TGA is a classic characterization technique used to measure the mass change of a material during programmed heating in a specific atmosphere. It is often used to study a material's thermal stability and thermal properties such as evaporation, decomposition, dehydration, and oxidation during heating. DTA primarily measures the temperature difference of a material under programmed temperature, enabling the study of endothermic or exothermic properties during phase transitions or chemical reactions. Simultaneous thermal analyzers (STAs), which perform simultaneous thermogravimetric and differential thermal analysis, combine TGA and DTA to provide a comprehensive and multi-dimensional understanding of a material's thermodynamic properties. This is particularly valuable for studying advanced functional materials and supporting the rapid development of related research fields.

[0003] The prior art discloses an instrument structure with an integrated resonant cantilever beam as its core, wherein, through an integrated resonant cantilever beam chip, the resonant frequency of the cantilever beam and the real-time temperature of the sample and other information are simultaneously obtained, thereby obtaining the sample mass change and temperature difference change. In the design of this long strip micro-cantilever beam structure, the sample area is located near the free end of the cantilever beam, and the temperature collection element is a thermocouple pair with the hot end set in the sample area. A wire is 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 relatively small, and the integrated cantilever beam chip is difficult to meet the test requirements of samples with low heat absorption / 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] This application provides the following technical solutions:

[0007] An integrated chip for synchronous thermal analysis provided by the present application includes a substrate, a resonant disk, and a plurality of connecting beams;

[0008] 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;

[0009] One end of the thermocouple on the resonant 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 multiple connecting beams are distributed around the resonant disk, so that the hot ends of multiple thermocouples are respectively connected to the cold ends of the thermocouples through the corresponding wires on the connecting beams.

[0010] Preferably, the heating element comprises one or more heating resistance wires, and the heating resistance wires are wound around the resonant disk.

[0011] Preferably, the thermocouple in the temperature detection element includes one or more of a polysilicon thermocouple, a single crystal silicon thermocouple and a metal thermocouple.

[0012] 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.

[0013] Preferably, a resonance excitation and detection module is provided on the connecting beam, and the resonance excitation and detection module is arranged on one end of the connecting beam close to the substrate.

[0014] Preferably, 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;

[0015] 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.

[0016] Preferably, a cavity is formed on the substrate, one end of the connecting beam is fixed to the edge of the cavity, and the resonant disk is located in the cavity area.

[0017] According to the present application, a synchronous thermal analysis system is provided, comprising 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 any of the above-mentioned integrated chips for synchronous thermal analysis;

[0018] 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 tested;

[0019] 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;

[0020] 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;

[0021] 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.

[0022] According to a synchronous thermal analysis method provided by the present application, the synchronous thermal analysis system is applied, including: driving a first integrated chip and a second integrated chip with a first frequency parameter, driving heating regions of the first integrated chip and the second integrated chip to increase temperature with a first temperature parameter after stabilization, collecting the resonant frequency and corresponding temperature of the first integrated chip and the second integrated chip during the heating process, as well as the temperature difference and corresponding temperature of the heating region of the first integrated chip and the second integrated chip during the heating process as baseline data;

[0023] Stop vibrating the first integrated chip and the second integrated chip, remove them from the test chamber, cool them to room temperature, and then apply the sample to be tested to the resonant disk of the first integrated chip;

[0024] moving the first integrated chip and the second integrated chip into the test chamber, driving the heating areas of the first integrated chip and the second integrated chip to heat up with a first frequency parameter, and after stabilization, driving the heating areas of the first integrated chip and the second integrated chip to heat up with the first temperature parameter, collecting the resonant frequency and the corresponding temperature of the first integrated chip and the second integrated chip during the heating process, as well as the temperature difference and the corresponding temperature of the heating areas of the first integrated chip and the second integrated chip during the heating process as detection data;

[0025] The thermogravimetric curve and the differential thermal curve of the sample to be tested are fitted using the reference data and the test data.

[0026] Compared with the prior art, the at least one technical solution adopted in this application can achieve the following beneficial effects:

[0027] The present application forms a heating area on the resonant disk by heating through a heating element, and arranges multiple thermocouples in series on the resonant disk to form a thermopile, forming a temperature measurement area for detecting the temperature of the heating area, and the hot end of the thermocouple is connected to the cold end of the thermocouple on the substrate through wires on multiple connecting beams distributed around the resonant disk. This can increase the number of thermocouples in the resonant 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 / release or small temperature changes, thereby improving the measurement capability of the synchronous thermal analysis system. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] In order to more clearly illustrate the technical solutions of the embodiments of the present application, the following briefly introduces the drawings required for use in the embodiments. Obviously, the drawings described below are only some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without any creative work.

[0029] Figure 1 is a bird's-eye view schematic diagram of the integrated chip for simultaneous thermal analysis of the present application;

[0030] Figure 2 This is a first top view schematic diagram of the integrated chip for simultaneous thermal analysis of the present application;

[0031] Figure 3 is a schematic diagram of the temperature sensitivity test results of this application;

[0032] Figure 4 is a schematic diagram of the test results of the indium (In) melting process in this application;

[0033] Figure 5 This is a second top view schematic diagram of the integrated chip used for synchronous thermal analysis in the present application.

[0034] Figure numerals: 1. resonant excitation and detection module; 2. temperature detection element; 3. heating element; 4. thermal resistance hole; 5. wire; 6. cold end; 7. hot end; 8. substrate. DETAILED DESCRIPTION

[0035] The embodiments of the present application are described in detail below with reference to the accompanying drawings.

[0036] The following describes the embodiments of the present application through specific examples, and those skilled in the art can easily understand other advantages and effects of the present application from the contents disclosed in this specification. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments. The present application can also be implemented or applied through other different specific embodiments, and the details in this specification can also be modified or changed in various ways based on different viewpoints and applications without departing from the spirit of the present application. It should be noted that, in the absence of conflict, the features in the following embodiments and embodiments can be combined with each other. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without making creative work are within the scope of protection of this application.

[0037] It should be noted that various aspects of the embodiments within the scope of the appended claims are described below. It should 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, it should be understood by those skilled in the art that an 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 aspect described herein can be used to implement an apparatus and / or practice a method. In addition, other structures and / or functionalities other than one or more of the aspects described herein can be used to implement this apparatus and / or practice this method.

[0038] It should also be noted that the illustrations provided in the following embodiments are only schematic illustrations of the basic concept of the present application. The illustrations only show components related to the present application and are not drawn according to the number, shape and size of components in actual implementation. In actual implementation, the type, quantity and proportion of each component can be changed at will, and the component layout type may also be more complicated.

[0039] Additionally, in the following description, specific details are provided to provide a thorough understanding of the examples, however, one skilled in the art will appreciate that the examples can be practiced without these specific details.

[0040] Through in-depth research and improvement exploration on synchronous thermal analyzers and synchronous thermal analysis methods, the applicant found that the working principle of existing commercial STA is to use a high-precision electronic balance to monitor the mass change of the sample under programmed temperature control, and use a temperature measurement system to record the temperature difference between the sample and the reference sample. This type of instrument has problems such as large sample consumption, long analysis time, high energy consumption, and difficulty in combination. In order to solve the pain points of existing instruments, the Chinese invention patent document with publication number CN117907146A discloses a chip-type synchronous thermal analyzer and 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 of this is to obtain information such as the resonant frequency of the cantilever beam and the real-time temperature of the sample through an integrated resonant cantilever beam chip, thereby obtaining the sample mass change and temperature difference change. However, the integrated resonant cantilever beam chip disclosed in the patent adopts a long 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. Because the cold end of the thermocouple needs to be placed in the non-heating zone, a wire needs to be arranged between the free end and the fixed end of the microcantilever. Due to the heat-resistant hole structure of the microcantilever, the space left for the wire is limited, so only two thermocouples can be arranged to form a thermopile. The temperature measurement capability (temperature sensitivity) of the thermopile is proportional to the number of thermocouples. Therefore, the temperature sensitivity of the chip disclosed in this patent is only 0.7 mV / K, which is difficult to meet the testing requirements of samples with low heat absorption / release (small temperature changes).

[0041] Based on this, the technical solutions provided by the various embodiments of the present application are described below in conjunction with the accompanying drawings.

[0042] The embodiments of this specification propose an integrated chip for synchronous thermal analysis, such as Figure 1 、 Figure 2 as well as Figure 5 As shown, it includes 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 by heating. A temperature detection element 2 is also provided on the resonant disk. The temperature detection element 2 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 on the resonant disk for detecting the temperature of the heating area. The resonant disk is used to coat the sample to be tested, and the heating area and the temperature measurement area are used to coat the sample to be tested. The heating area and the temperature measurement area can overlap. The sample to be tested is, for example, indium. The heating element 3 can be distributed around the center of the resonant disk, and the hot end 7 of the thermocouple can be located in the center of the resonant disk to form a thermopile. The thermopile is used to measure temperature and the number of thermocouples is increased to improve the temperature detection capability.

[0043] One end of the thermocouple on the resonant disk is the hot end 7, and the cold end 6 of the thermocouple is on the substrate 8. The connecting beam is fixed on the substrate 8, and multiple connecting beams are distributed around the resonant disk so that the hot ends 7 of multiple thermocouples are respectively connected to the cold ends 6 of the thermocouples through the corresponding wires 5 on the connecting beams.

[0044] 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.

[0045] In one embodiment, the thermocouple in the temperature detection element 2 includes one or more of polysilicon thermocouples, single crystal silicon thermocouples, and metal thermocouples. For example, the temperature detection element 2 is a thermopile composed of multiple polysilicon thermocouples, single crystal silicon thermocouples, and metal thermocouples.

[0046] 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.

[0047] In one embodiment, a heat-resistance hole 4 is provided on the connecting beam, and the heat-resistance hole 4 is located between the resonance excitation and detection module 1 and the resonance disk, and the wires 5 are arranged on both sides of the heat-resistance hole 4 on the connecting beam.

[0048] In one embodiment, a cavity is formed on the substrate 8, one end of the connecting beam is fixed to the edge of the cavity, and the resonant disk is located in the cavity area.

[0049] 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 provided on one end of the connecting beam close to the substrate 8 .

[0050] In one embodiment, the resonant excitation and detection module 1 includes a resonant excitation element and a resonant detection element; the resonant excitation element includes a resonant driving resistor, and multiple resonant driving resistors are arranged in series so that the resonant excitation element is used to form resonance; the resonant detection element includes a Wheatstone bridge composed of multiple single crystal silicon piezoresistors, so that the resonant detection element is used to collect the resonant frequency of the resonant disk.

[0051] The present application is a MEMS integrated chip for synchronous thermal analysis, where MEMS stands for Micro-Electro-Mechanical Systems. To address the low temperature sensitivity of existing synchronous thermal analysis chips based on resonant microcantilevers, the present application discloses a disc-shaped MEMS integrated synchronous thermal analysis chip. The chip has a disc structure at its center, connected to a substrate 8 via four bridge structures, similar to four cantilever beam structures arranged in pairs relative to each other and sharing a common sample area (the central disc). Because there is more space for wiring thermocouple wires 5, the disc structure serves as the sample area, and up to eight temperature-measuring thermocouples can be integrated thereon, significantly improving temperature measurement sensitivity. The remaining structures are similar to those of the microcantilever. The disc still integrates a heating element 3 composed of a metal coil, and the four bridge structures are integrated with resonant excitation and frequency detection elements near the fixed ends, which can excite the entire structure to resonate and obtain the resonant frequency.

[0052] like Figure 2 and Figure 3 As shown, a disc-shaped MEMS integrated synchronous thermal analysis chip is used instead of a micro-cantilever integrated synchronous thermal analysis chip, increasing the number of thermocouples 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 a chip-type synchronous thermal analyzer and synchronous thermal analysis method with publication number CN117907146A. Figure 4 As shown, the DTA test results of the indium melting process are provided. Compared with the previous patent, the signal peak is much larger.

[0053] The MEMS integrated chip mainly consists of three types of components: microheater elements, thermocouple temperature detection elements, and resonant drive / detection elements: the microheater coils are wound around the upper right, lower right, upper left, and lower left sides of the resonant disk to provide the device with an operating temperature. The thermocouple temperature detection element consists of 16 pairs of polysilicon-metal thermocouples, with the hot end 7 concentrated at the center of the resonant disk and the cold end 6 set at the root of the connecting beam. The temperature change of the hot end 7 is read through the Seebeck effect. The resonant drive resistor is set at the root of the four connecting beams and connected in series. The disk is driven to resonate through the thermal effect. The resonant detection resistor is composed of four single-crystal silicon piezoresistors forming a Wheatstone bridge, which is located at the root of the connecting beam and is closer to the center than the drive resistor. Combined with a phase-locked loop circuit, the resonant frequency of the resonant disk is tracked. The present application can improve the temperature sensitivity of the synchronous thermal analysis MEMS chip, thereby improving the measurement capability of the chip-type synchronous thermal analyzer.

[0054] The embodiments of this specification also disclose 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 computing module; the first integrated chip and the second integrated chip are any of the above-mentioned integrated chips for synchronous thermal analysis.

[0055] 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 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 resonant excitation and 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 collects the current temperature of the heating area detected by the temperature detection element 2 and the resonant frequency collected by the resonant excitation and detection module 1; 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.

[0056] The control module controls the connection of the heating element 3 to perform heating; the control module controls the connection of the resonance excitation element to form resonance; and the data acquisition module controls the connection of the resonance detection element.

[0057] The synchronous thermal analysis system further includes an atmosphere adjustment module, which is connected to the test chamber and the control module, so that the atmosphere adjustment module adjusts the atmosphere in the test chamber under the control of the control module.

[0058] The synchronous thermal analysis system also includes an input and output module, which is connected to the control module and the calculation module respectively, and is used to receive input to adjust the control parameters of the control module and output the calculation results of the calculation module.

[0059] The control module inputs voltage control signals to the resonant excitation element and the heating element 3. The data acquisition module collects the frequency signals and temperature signals corresponding to the resonant detection element and the temperature detection element 2, and adjusts the input voltage control signal according to the collected frequency signals and temperature signals to achieve precise temperature control and improve the analysis accuracy.

[0060] In the present application, the size of the first integrated chip for coating the sample to be detected and the second integrated chip not coated with the sample to be detected are at the micron level, and the sample loading capacity of the integrated chip is at the nanogram level; in addition, the sample on the integrated chip is subjected to a self-heating program heating method, which can realize reaction and real-time measurement on the first integrated chip at a faster heating rate. Not only is the heating rate several times higher than that of existing commercial thermal analysis instruments, but the accuracy of the analysis will also be higher. At the same time, the accuracy of the sample analysis results will not be affected by the sample amount and the gas environment. In the present application, the self-heating program heating method in the micro-integrated chip is adopted, which abandons the existing large-volume heating cavity device, and realizes the simultaneous use of multiple chips with different samples to perform different multi-channel measurement thermal analysis with different heating programs, which greatly shortens the time consumption and further improves the efficiency of thermal analysis measurement.

[0061] 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.

[0062] The heating element 3 can be configured as a high-temperature resistant metal heating wire, and the wound coil can improve its heating efficiency.

[0063] The temperature detection element 2 can be configured as a temperature measuring thermocouple arranged in a crystalline silicon thermocouple pair. The polysilicon thermocouple pair can use P-type and N-type polysilicon as thermocouple materials, and its Seebeck coefficient is much higher than that of traditional metal structure thermocouples.

[0064] The frequency signals and temperature signals corresponding to the resonance detection element and the temperature detection element 2 are specific physical quantities, such as voltage values. The corresponding frequency values ​​and temperature values ​​can be obtained by converting them using a calculation module through a preset mapping relationship between the physical quantity and the frequency or temperature.

[0065] 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 in gas communication. 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, thereby meeting the needs of different analysis projects. In thermogravimetric analysis, the types of environmental atmospheres may include 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 include oxidizing, reducing, and inert atmospheres, etc. Atmospheres of different properties have a certain influence on the thermogravimetric curve or differential thermal curve.

[0066] 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 after stabilization, driving the heating area of ​​the first integrated chip and the second integrated chip to heat up with a first temperature parameter, collecting the resonant frequency and corresponding temperature of the first integrated chip and the second integrated chip during the heating process, as well as the temperature difference and corresponding temperature of the heating area of ​​the first integrated chip and the second integrated chip during the heating process as baseline data.

[0067] The first integrated chip and the second integrated chip stop vibrating, are removed from the test cavity, and are cooled to room temperature before the sample to be tested is coated on the resonance disk of the first integrated chip.

[0068] The first integrated chip and the second integrated chip are moved into the test chamber, and the heating areas of the first integrated chip and the second integrated chip are driven to heat up with the first frequency parameter. After stabilization, the heating areas of the first integrated chip and the second integrated chip are driven to heat up with the first temperature parameter. The resonant frequency and the corresponding temperature of the first integrated chip and the second integrated chip during the heating process, as well as the temperature difference and the corresponding temperature of the heating areas of the first integrated chip and the second integrated chip during the heating process are collected as detection data.

[0069] The thermogravimetric curve and differential thermal curve of the sample to be tested are fitted by using the benchmark data and the test data.

[0070] The simultaneous thermal analysis method further includes dispersing a solid sample to be tested in a solvent to form a liquid mixture, ultrasonically treating the mixture, dripping the treated mixture onto the sample-to-be-tested area of ​​the first integrated chip using a micromanipulator, and drying the mixture. The solvent may include anhydrous ethanol, deionized water, or both, and the solvent may be selected based on the analysis requirements. The ultrasonically treated mixture may be a suspension or a solution.

[0071] The synchronous thermal analysis method further includes: driving the first integrated chip and the second integrated chip to increase temperature at a first speed parameter and a first temperature parameter to remove impurities adsorbed on the first integrated chip and the second integrated chip. The accuracy of subsequent analysis is improved by placing the first integrated chip and the second integrated chip in a test chamber for self-cleaning.

[0072] The method of fitting the thermogravimetric curve of the sample to be tested includes:

[0073] The vibration frequency value of the first integrated chip corresponding to the temperature change in the detection data is subtracted from the vibration frequency value of the first integrated chip corresponding to the corresponding temperature in the reference data to obtain a vibration frequency conversion value corresponding to the temperature change.

[0074] The converted value of the vibration frequency corresponding to the temperature change is converted into the mass of the sample to be detected based on the relationship between the vibration frequency and the mass of the sample to be detected.

[0075] Calculate the weight loss percentage of the sample to be tested corresponding to the temperature change.

[0076] The thermogravimetric curve of the sample to be tested is fitted according to the weight loss percentage of the sample to be tested corresponding to the temperature change.

[0077] The method of fitting the differential thermal curve of the sample to be detected includes:

[0078] The temperature difference between the first integrated chip and the second integrated chip corresponding to the temperature change in the detection data is subtracted from the temperature difference between the first integrated chip and the second integrated chip corresponding to the corresponding temperature in the reference data to obtain a fitting value of the temperature difference corresponding to the temperature change.

[0079] The differential thermal curve of the sample to be detected is fitted according to the fitting value of the temperature difference between the first integrated chip and the second integrated chip corresponding to the temperature change.

[0080] During the thermogravimetric curve analysis process, the mass of the sample to be tested needs to be obtained through the vibration frequency of the first integrated chip coated with the sample to be tested. Similarly, the corresponding mass value can be obtained by converting the mapping relationship between the preset frequency value and the mass of the sample to be tested using the calculation module.

[0081] In this specification, the same or similar parts between the various embodiments can be referred to each other, and each embodiment focuses on the differences from other embodiments. In particular, for the embodiments described later, the description is relatively simple, and the relevant parts can be referred to the partial description of the previous embodiments.

[0082] The above description is merely a specific embodiment of the present application, but the scope of protection of the present application is not limited thereto. Any changes or substitutions that can be easily conceived by a person skilled in the art within the technical scope disclosed in the present application should be included in the scope of protection of the present application. Therefore, the scope of protection of the present application should be based on the scope of protection of the claims.

Claims

1. An integrated chip for synchronous thermal analysis, characterized in that: comprising 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 resonant 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 resonant disk, so that the hot ends of the plurality of thermocouples are respectively connected to the cold ends of the thermocouples through the wires on the corresponding connecting beams. 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; A resonance excitation and detection module is provided on the connecting beam, and the resonance excitation and detection module is used to drive the resonance disk to generate resonance and detect its resonance frequency.

2. The integrated chip for simultaneous 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 resonant disk.

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

5. The integrated chip for simultaneous thermal analysis according to claim 4, 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.

6. The integrated chip for simultaneous thermal analysis according to claim 4, characterized in that: A heat-resistance hole is provided on the connecting beam, and the heat-resistance hole is located between the resonance excitation and detection module and the resonance disk, and the wires are arranged on both sides of the heat-resistance hole on the connecting beam.

7. The integrated chip for simultaneous thermal analysis according to claim 1, 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 resonant disk is located in the cavity area.

8. A synchronous thermal analysis system, characterized in that: The device 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 chip for synchronous thermal analysis according to any one of claims 4 to 6; The first integrated chip and the second integrated chip are placed in the test cavity; the resonant 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.

9. A synchronous thermal analysis method, characterized in that: The synchronous thermal analysis system of claim 8 comprises: driving the first integrated chip and the second integrated chip with a first frequency parameter, driving the heating areas 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 corresponding temperature of the first integrated chip and the second integrated chip during the heating process, and collecting the temperature difference and corresponding temperature of the heating areas of the first integrated chip and the second integrated chip during the heating process as baseline data; Stop vibrating the first integrated chip and the second integrated chip, remove them from the test chamber, cool them to room temperature, and then apply the sample to be tested to the resonant disk of the first integrated chip; moving the first integrated chip and the second integrated chip into the test chamber, driving the heating areas of the first integrated chip and the second integrated chip to heat up with a first frequency parameter, and after stabilization, driving the heating areas of the first integrated chip and the second integrated chip to heat up with the first temperature parameter, collecting the resonant frequency and the corresponding temperature of the first integrated chip and the second integrated chip during the heating process, as well as the temperature difference and the corresponding temperature of the heating areas of the first integrated chip and the second integrated chip during the heating process as detection data; The thermogravimetric curve and the differential thermal curve of the sample to be tested are fitted using the reference data and the test data.

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