A large sample three-dimensional calorimeter

Abstract

The present invention relates to a large sample three-dimensional calorimeter, belonging to the field of thermal analysis technology, the large sample three-dimensional calorimeter comprises: a measuring chamber, a bracket, a sample cell and a reference cell; the sample cell and the reference cell are suspended inside the measuring chamber through the bracket; the inside of the sample cell is used to load the sample to be measured, and the inside of the reference cell is used to load the reference sample; the sample cell and the reference cell have the same structure, and a target area is set at the same position of the first surface of the sample cell and the first surface of the reference cell; a plurality of first thermocouples are connected in series between the target area of ​​the first surface of the sample cell and the target area of ​​the first surface of the reference cell; the hot ends of the plurality of first thermocouples are located in the target area of ​​the first surface of the sample cell, and the cold ends of the plurality of first thermocouples are located in the target area of ​​the first surface of the reference cell. The method solves the shortcomings of the existing single-point measurement calorimeter, such as low sensitivity and inability to measure heat changes, and can capture the thermal reaction of the sample in the spatial position.

Description

Technical Field

[0001] The invention belongs to the technical field of thermal analysis and relates to a large sample three-dimensional calorimeter. Background Art

[0002] Large sample calorimeter is a scientific instrument used to measure and analyze the thermal effects of large samples. It combines heat measurement technology and thermal field imaging capabilities. It is applied in the fields of material science, chemical engineering, environmental science, etc., especially in the thermal performance testing of high temperature and complex samples.

[0003] Compared with traditional calorimeters, large sample calorimeters have larger sample space and can be used for larger samples.

[0004] In the study of large sample calorimeters, it was found that the number of thermocouples in current large sample calorimeters is only 1 to 2, and their sensitivity is low. In other words, the existing large sample calorimeters can only achieve single-point measurement, which cannot reflect the complete thermal information of the sample, nor can they measure heat flow. Summary of the invention

[0005] In order to solve the above-mentioned problems in the prior art, the present invention provides a large sample three-dimensional calorimeter.

[0006] In order to achieve the above object, the technical solution adopted by the present invention is:

[0007] In a first aspect, an embodiment of the present application provides a large sample three-dimensional calorimeter, comprising: a measuring chamber, a bracket, a sample cell and a reference cell; the sample cell and the reference cell are suspended inside the measuring chamber by the bracket; the interior of the sample cell is used to load the sample to be tested, and the interior of the reference cell is used to load the reference sample; the sample cell and the reference cell are symmetrically arranged inside the measuring chamber; the sample cell and the reference cell have the same structure, and a target area is arranged at the same position on the first surface of the sample cell and the first surface of the reference cell; the first surface of the sample cell faces the reference cell, and the first surface of the reference cell faces the sample cell; a plurality of first thermocouples are connected in series in the target area on the first surface of the sample cell and the reference cell. the target area of ​​the first surface of the sample cell; the hot ends of the multiple first thermocouples are located in the target area of ​​the first surface of the reference cell, and the cold ends of the multiple first thermocouples are located in the target area of ​​the first surface of the reference cell; the target area is also arranged at the same position of the second surface of the sample cell and the second surface of the reference cell; the second surface of the sample cell faces away from the reference cell, and the second surface of the reference cell faces away from the sample cell; multiple second thermocouples are connected in series between the target area of ​​the second surface of the sample cell and the target area of ​​the second surface of the reference cell; the hot ends of the multiple second thermocouples are located in the target area of ​​the second surface of the sample cell, and the cold ends of the multiple second thermocouples are located in the target area of ​​the second surface of the reference cell.

[0008] Optionally, at least two target areas are provided on the first surface of the sample pool and the first surface of the reference pool; and the target areas at the same position on the first surface of the sample pool and the first surface of the reference pool correspond one to one; at least two target areas are provided on the second surface of the sample pool and the second surface of the reference pool; and the target areas at the same position on the second surface of the sample pool and the second surface of the reference pool correspond one to one.

[0009] Optionally, a target area is set at the same position of the third surface of the sample pool and the third surface of the reference pool; a plurality of third thermocouples are connected in series between the target area on the third surface of the sample pool and the target area on the third surface of the reference pool; the hot ends of the plurality of third thermocouples are located in the target area on the third surface of the sample pool, and the cold ends of the plurality of third thermocouples are located in the target area on the third surface of the reference pool.

[0010] Optionally, at least two target areas are provided on the third surface of the sample pool and the third surface of the reference pool; and the target areas at the same position on the third surface of the sample pool and the third surface of the reference pool correspond one to one.

[0011] Optionally, the sample pool includes: a receiving bottom plate and a cover plate; the sample to be tested is used to be placed on the receiving bottom plate and fixed by the cover plate.

[0012] Optionally, screw holes are provided at the same positions of the receiving bottom plate and the cover plate; wherein the sample to be tested is fixed between the receiving bottom plate and the cover plate by screwing a spring screw into the screw holes of the receiving bottom plate and the cover plate.

[0013] Optionally, the spacing distance between the receiving bottom plate and the cover plate is adjusted by adjusting the rotation depth of the spring screw, thereby placing different numbers of samples to be tested in the sample pool.

[0014] Optionally, the accommodating bottom plate is further provided with side plates, and the sample to be tested is limited by the side plates; wherein the limiting space for accommodating the sample to be tested is square through the side plates; or, the limiting space for accommodating the sample to be tested is circular through the side plates.

[0015] Optionally, a strip board is provided in the target area of ​​the first surface of the sample pool; the hot ends of the multiple first thermocouples are located on the strip board on the first surface of the sample pool; a strip board is provided in the target area of ​​the first surface of the reference pool; and the cold ends of the multiple first thermocouples are located on the strip board on the first surface of the reference pool.

[0016] Optionally, the measuring chamber includes an insulating cooling layer and a thermostat layer, and the insulating cooling layer is arranged outside the thermostat layer; wherein the insulating cooling layer is used to isolate the external environment and reduce internal heat loss; a heater is arranged on the surface of the thermostat layer to control the internal temperature field.

[0017] The beneficial effects of the embodiments of the present application include:

[0018] First, the existing large sample three-dimensional calorimeter has only 1 to 2 thermocouples and only provides single-point measurement, while in the present application, multiple first thermocouples are connected in series and cover the target area on the first surface of the sample cell and the target area on the first surface of the reference cell, and multiple second thermocouples are connected in series and cover the target area on the second surface of the sample cell and the target area on the second surface of the reference cell, which can cover a wider measurement range (i.e., the distribution of the thermoelectric junctions of the thermocouples wraps the sample cell) and improve sensitivity. It can also better characterize the three-dimensional thermal effect of large samples and realize the analysis of complex thermal behavior inside the sample.

[0019] Second, the single-point measurement of the existing large-sample three-dimensional calorimeter is only a single-point measurement of the sample itself, while the present application also provides a reference cell in the large-sample three-dimensional calorimeter. By connecting multiple first thermocouples in series and covering the target area on the first surface of the sample cell and the target area on the first surface of the reference cell, the temperature difference between the target area on the first surface of the sample cell and the target area on the first surface of the reference cell can be directly obtained, thereby directly and accurately reflecting the heat flow difference between the sample cell and the reference cell, that is, the heat change data can be directly measured.

[0020] In summary, the large sample three-dimensional calorimeter provided in the embodiment of the present application solves the shortcomings of the existing single-point measurement calorimeter, such as low sensitivity and inability to measure heat change, by arranging a reference cell, and by connecting a plurality of first thermocouples in series and covering the target area on the first surface of the sample cell and the target area on the first surface of the reference cell, and connecting a plurality of second thermocouples in series and covering the target area on the second surface of the sample cell and the target area on the second surface of the reference cell. That is, the large sample three-dimensional calorimeter provided in the embodiment of the present application can provide a wider range of measurements, and can directly measure and output heat change data. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 A simplified schematic diagram of a large sample three-dimensional calorimeter provided by an embodiment of the present invention;

[0022] Figure 2 A schematic diagram of the internal structure of a large sample three-dimensional calorimeter provided in an embodiment of the present invention;

[0023] Figure 3 A top view of a sample cell and a reference cell provided in an embodiment of the present invention;

[0024] Figure 4 A schematic diagram of connecting a sample cell and a reference cell via a first thermocouple provided in an embodiment of the present invention;

[0025] Figure 5 A schematic diagram of the structure of a sample pool provided by an embodiment of the present invention;

[0026] Figure 6 A cross-sectional view of a sample cell provided in an embodiment of the present invention;

[0027] Figure 7 A partial structural schematic diagram of a sample pool provided by an embodiment of the present invention;

[0028] Figure 8 A schematic diagram of a structure for connecting a sample cell and a reference cell via a thermocouple provided for the implementation of the present invention;

[0029] Fig. 9A schematic diagram of the structure of a large sample three-dimensional calorimeter provided for the implementation of the present invention;

[0030] Fig.10 A schematic structural diagram of another large sample three-dimensional calorimeter provided for the implementation of the present invention.

[0031] Reference numerals:

[0032] 100-large sample three-dimensional calorimeter; 10-measuring chamber; 101-insulating cooling layer; 102-temperature equalizer layer; 103-heater; 20-bracket; 30-sample pool; 301-containing bottom plate; 302-cover plate; 303-spring screw; 304-plug board; 40-reference pool; 50-first thermocouple; 501-thermocouple monomer of first material; 502-thermocouple monomer 501 of second material; 60-second thermocouple. DETAILED DESCRIPTION

[0033] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0034] Compared with traditional calorimeters, large sample calorimeters have larger sample space and can be used for larger samples.

[0035] In the study of large sample calorimeters, it was found that the number of thermocouples in current large sample calorimeters is only 1 to 2, and their sensitivity is low. In other words, the existing large sample calorimeters can only achieve single-point measurement, which cannot reflect the complete thermal information of the sample, nor can they measure heat flow.

[0036] In view of the above problems, the present application provides the following embodiments to solve them:

[0037] See also Figure 1 to Figure 4 The embodiment of the present application provides a large sample three-dimensional calorimeter 100, including: a measurement chamber 10, a bracket 20, a sample cell 30 and a reference cell 40.

[0038] The sample cell 30 and the reference cell 40 are suspended inside the measuring chamber 10 via a bracket 20 .

[0039] It should be noted that the sample cell 30 and the reference cell 40 are each suspended inside the measuring chamber 10 via a bracket 20 .

[0040] Taking the sample pool 30 as an example, in practical applications, the bracket 20 can be fixedly connected to the sample pool 30 , such as by snapping; of course, the bracket 20 can also be integrally formed with the sample pool 30 .

[0041] The interior of the sample cell 30 is used for loading the sample to be tested, and the interior of the reference cell 40 is used for loading the reference sample.

[0042] The type of the sample to be tested may be, but is not limited to, electronic equipment, alloys, building materials, etc. For example, the electronic equipment may specifically be an electronic component such as a battery.

[0043] When the sample to be tested is a battery, thermal performance analysis of the battery may be performed, including but not limited to thermal runaway, reaction heat, and thermal changes during the charge and discharge process of the battery.

[0044] It should be noted that the sample cell 30 and the reference cell 40 have the same structure, and a target area is provided at the same position on the first surface of the sample cell 30 and the first surface of the reference cell 40 .

[0045] In the embodiment of the present application, the sample cell 30 and the reference cell 40 are connected via a thermopile, and the thermopile includes a plurality of first thermocouples 50 .

[0046] It should be noted that the specific number of the first thermocouples 50 can be set according to actual needs. The number of the first thermocouples 50 can be 10 to 20, which is not limited in this application.

[0047] Specifically, multiple first thermocouples 50 are connected in series between the target area on the first surface of the sample pool 30 and the target area on the first surface of the reference pool 40; the hot ends of the multiple first thermocouples 50 are located in the target area on the first surface of the sample pool 30, and the cold ends of the multiple first thermocouples 50 are located in the target area on the first surface of the reference pool 40.

[0048] It should be noted that, since the sample cell 30 and the reference cell 40 have the same structure, the first surface of the sample cell 30 and the first surface of the reference cell 40 are also the same surface.

[0049] The following is a description of the plurality of first thermocouples 50. Figure 4 Each first thermocouple 50 includes a thermocouple monomer 501 made of a first material and a thermocouple monomer 502 made of a second material.

[0050] The first material may be gold, platinum or palladium, and the second material may be gold. Of course, in practical applications, other thermocouple materials may also be used, as long as the first material and the second material are different.

[0051] Taking the first thermocouple 50 of the middle layer as an example, the specific connection relationship is that the first end of the thermocouple monomer of the first material of the first thermocouple 50 is connected to the target area of ​​the first surface of the sample pool 30, and forms a thermoelectric junction with the second end of the thermocouple monomer of the second material of the previous first thermocouple 50. The second end of the thermocouple monomer of the first material of the first thermocouple 50 is connected to the target area of ​​the first surface of the reference pool 40, and forms a thermoelectric junction with the first end of the thermocouple monomer of the second material of the first thermocouple 50. They are connected in series in sequence to form a thermocouple such as Figure 4 A thermopile stacked top-down is shown.

[0052] It should be noted that the large sample three-dimensional calorimeter 100 provided in the embodiment of the present application can directly obtain the temperature difference between the target area on the first surface of the sample pool 30 and the target area on the first surface of the reference pool 40 by differential calculation, that is, the thermocouple connection method provides a temperature difference sensing differential heat flow acquisition method on the left and right sides.

[0053] The sample cell 30 and the reference cell 40 are symmetrically arranged inside the measuring chamber 10 . The first surface of the sample cell 30 faces the reference cell 40 , and the first surface of the reference cell 40 also faces the sample cell 30 .

[0054] In other words, the sample cell 30 and the reference cell 40 are disposed opposite to each other and can be symmetrically arranged with the central axis of the interior of the measuring cell 10 as the axis of symmetry.

[0055] The target area is also arranged at the same position on the second surface of the sample pool 30 and the second surface of the reference pool 40. The first surface and the second surface of the sample pool 30 are opposite surfaces; the first surface and the second surface of the reference pool 40 are opposite surfaces.

[0056] The second surface of the sample cell 30 faces away from the reference cell 40 , and the second surface of the reference cell 40 also faces away from the sample cell 30 .

[0057] In the embodiment of the present application, the sample cell 30 and the reference cell 40 are connected via a thermopile, and the thermopile further includes a plurality of second thermocouples 60 .

[0058] It should be noted that the specific number of the second thermocouples 60 can be set according to actual needs. The number of the second thermocouples 60 can be 10 to 20, which is not limited in this application.

[0059] Specifically, multiple second thermocouples 60 are connected in series between the target area on the second surface of the sample pool 30 and the target area on the second surface of the reference pool 40; the hot ends of the multiple second thermocouples 60 are located in the target area on the second surface of the sample pool 30, and the cold ends of the multiple second thermocouples 60 are located in the target area on the second surface of the reference pool 40.

[0060] Each second thermocouple 60 includes a thermocouple unit made of a first material and a thermocouple unit made of a second material.

[0061] The first material may be gold, platinum or palladium, and the second material may be gold. Of course, in practical applications, other thermocouple materials may also be used, as long as the first material and the second material are different.

[0062] The specific connection relationship is that the first end of the thermocouple monomer of the first material of the second thermocouple 60 is connected to the target area of ​​the second surface of the sample cell 30, and forms a thermoelectric junction with the second end of the thermocouple monomer of the second material of the previous second thermocouple 60. The second end of the thermocouple monomer of the first material of the second thermocouple 60 is connected to the target area of ​​the second surface of the reference cell 40, and forms a thermoelectric junction with the first end of the thermocouple monomer of the second material of the second thermocouple 60. They are connected in series in sequence to form a thermocouple such as Figure 2 A thermopile stacked top-down is shown.

[0063] It should be noted that the large sample three-dimensional calorimeter 100 provided in the embodiment of the present application can directly obtain the temperature difference between the target area on the second surface of the sample cell 30 and the target area on the second surface of the reference cell 40 by differential calculation.

[0064] In summary, the large sample three-dimensional calorimeter 100 provided in the embodiment of the present application has the following beneficial effects:

[0065] First, the existing large sample three-dimensional calorimeter has only 1 to 2 thermocouples and only provides single-point measurement, while in the present application, multiple first thermocouples are connected in series and cover the target area on the first surface of the sample cell and the target area on the first surface of the reference cell, and multiple second thermocouples are connected in series and cover the target area on the second surface of the sample cell and the target area on the second surface of the reference cell, which can cover a wider measurement range (i.e., the distribution of the thermoelectric junctions of the thermocouples wraps the sample cell) and improve sensitivity. It can also better characterize the three-dimensional thermal effect of large samples and realize the analysis of complex thermal behavior inside the sample.

[0066] Second, the single-point measurement of the existing large-sample three-dimensional calorimeter is only a single-point measurement of the sample itself, while the present application also arranges a reference cell 40 in the large-sample three-dimensional calorimeter 100. By connecting multiple first thermocouples 50 in series and covering the target area on the first surface of the sample cell 30 and the target area on the first surface of the reference cell 40, the temperature difference between the target area on the first surface of the sample cell 30 and the target area on the first surface of the reference cell 40 can be directly obtained, and then the heat flow difference between the sample cell 30 and the reference cell 40 can be directly and accurately reflected, that is, the heat change data can be directly measured.

[0067] In summary, the large sample three-dimensional calorimeter provided in the embodiment of the present application solves the shortcomings of the existing single-point measurement calorimeter, such as low sensitivity and inability to measure heat change, by arranging a reference cell, and by connecting a plurality of first thermocouples in series and covering the target area on the first surface of the sample cell and the target area on the first surface of the reference cell, and connecting a plurality of second thermocouples in series and covering the target area on the second surface of the sample cell and the target area on the second surface of the reference cell. That is, the large sample three-dimensional calorimeter provided in the embodiment of the present application can provide a wider range of measurements, and can directly measure and output heat change data.

[0068] In addition, the sample pool 30 and the reference pool 40 are symmetrically arranged inside the measuring chamber 10, providing a symmetrical method that can reduce the error caused by asymmetric heat flow and ensure that the thermal behavior of the samples in the sample pool 30 and the reference pool 40 has a higher consistency. The symmetrical arrangement makes the heat flow distribution more uniform, thereby improving the accuracy of the heat flow measurement.

[0069] At the same time, the configuration of the double-sided thermocouple can enhance the symmetry of the overall temperature field, so that the impact of ambient temperature fluctuations on the sample cell 30 and the reference cell 40 tends to be consistent, reducing the impact of environmental interference and further improving the accuracy of the measurement data.

[0070] Optionally, at least two target areas are set on the first surface of the sample pool 30 and the first surface of the reference pool 40; and the target areas at the same position on the first surface of the sample pool 30 and the first surface of the reference pool 40 correspond one to one; the second surface of the sample pool 30 and the second surface of the reference pool 40 are set on at least two target areas; and the target areas at the same position on the second surface of the sample pool 30 and the second surface of the reference pool 40 correspond one to one.

[0071] like Figure 3 As shown, in the embodiment of the present application, three target areas are provided on the first surface of the sample pool 30 and the first surface of the reference pool 40. A plurality of first thermocouples 50 are connected to each corresponding target area. Two target areas are provided on the second surface of the sample pool 30 and the second surface of the reference pool 40, and a plurality of second thermocouples 60 are connected to each corresponding target area.

[0072] It can be seen that in the embodiment of the present application, at least two target areas are provided on the first surface of the sample pool 30 and the first surface of the reference pool 40, and at least two target areas are provided on the second surface of the sample pool 30 and the second surface of the reference pool 40. A wider measurement range can be provided for the first surface and the second surface, that is, heat flow measurement can be performed at multiple locations on the first surface and the second surface, and more detailed and comprehensive thermal distribution data can be provided. At the same time, it is also more helpful to deeply analyze the thermal behavior of the sample in different thermal effect areas.

[0073] Optionally, a target area is set at the same position of the third surface of the sample pool 30 and the third surface of the reference pool 40; multiple third thermocouples are connected in series between the target area on the third surface of the sample pool 30 and the target area on the third surface of the reference pool 40; the hot ends of the multiple third thermocouples are located in the target area on the third surface of the sample pool 30, and the cold ends of the multiple third thermocouples are located in the target area on the third surface of the reference pool 40.

[0074] It should be noted that for the description of the structure and connection relationship of the third thermocouple, reference may be made to the introduction and description of the first thermocouple 50 and the second thermocouple 60 in the aforementioned embodiment, and the setting of the target area and other contents may also refer to the description in the aforementioned embodiment. The same parts are referenced to each other and will not be repeated.

[0075] The third surface of the sample pool 30 and the third surface of the reference pool 40 are provided with at least two target areas; and the target areas at the same position on the third surface of the sample pool 30 and the third surface of the reference pool 40 correspond one to one.

[0076] In addition, the third surface of the sample pool 30 is any other surface different from the first surface and the second surface of the sample pool 30. Figure 1 or Figure 2 For example, the third surface of the sample pool 30 may be the bottom surface of the sample pool 30 , that is, a surface close to the bottom of the measurement chamber 10 .

[0077] That is, the large sample three-dimensional calorimeter 100 provided in the embodiment of the present application can effectively measure three different surfaces of the sample pool 30, that is, it can effectively improve the measurement capability of the three-dimensional heat flow distribution between the sample pool 30 and the reference pool 40. This method can further improve the comprehensiveness of the measurement data, that is, it can more accurately obtain the thermal response data of different positions (different surfaces) of the sample.

[0078] See also Figure 5-6 Optionally, the sample pool 30 may specifically include: a receiving bottom plate 301 and a cover plate 302 .

[0079] The sample to be tested is placed on the receiving bottom plate 301 and fixed by the cover plate 302 .

[0080] It should be noted that, since the sample cell 30 and the reference cell 40 have the same structure, the reference cell 40 may refer to the description of the sample cell 30 in the embodiment of the present application, and will not be described in detail here.

[0081] The fixing method may be implemented by engaging the cover plate 302 with the receiving bottom plate 301 .

[0082] See also Figure 6-7Optionally, screw holes are provided at the same position of the receiving bottom plate 301 and the cover plate 302. Meanwhile, the sample pool 30 also includes a spring screw 303.

[0083] The sample to be tested is fixed between the receiving bottom plate 301 and the cover plate 302 by screwing the spring screw 303 into the screw holes of the receiving bottom plate 301 and the cover plate 302 .

[0084] It should be noted that in actual research, it is found that the sample may experience a drastic change in temperature during the thermal analysis process, which may cause its volume to expand or contract. For example, the battery may bulge during the heating process. Therefore, in this embodiment, the elastic structure of the spring screw 303 allows the fixing pressure to be automatically adjusted when the sample expands or contracts, thereby avoiding the situation where the fixing is not firm or damaged due to expansion or contraction.

[0085] That is, in this embodiment, by using the spring screw 303, it is possible to adapt to temperature changes, reduce sample fixation problems caused by temperature fluctuations, ensure that the sample is always in a stable fixed state, and thus ensure the reliability and accuracy of the experimental results.

[0086] Optionally, the rotation depth of the spring screw 303 is adjusted to adjust the spacing distance between the receiving bottom plate 301 and the cover plate 302 , thereby placing different numbers of samples to be tested in the sample pool 30 .

[0087] That is, by adjusting the rotation depth of the spring screw 303, different numbers of samples to be tested can be placed in the sample pool 30. Figure 4 and Figure 5 As shown, by adjusting the rotation depth of the spring screw 303 , three battery panels can be placed in the sample pool 30 .

[0088] Of course, in other embodiments, by adjusting the rotation depth of the spring screw 303 , one battery panel, two battery panels, five battery panels, etc. can be placed in the sample pool 30 .

[0089] Optionally, the containing bottom plate 301 is further provided with side plates, and the sample to be tested is limited by the side plates; wherein the limiting space for accommodating the sample to be tested is square by the side plates; or, the limiting space for accommodating the sample to be tested is circular by the side plates.

[0090] That is, the sample pool 30 provided in the embodiment of the present application is not limited to square samples, and various shapes of limiting spaces, such as circle, diamond, etc., can be formed by setting different side panels.

[0091] Specifically, the embodiment of the present application can provide an oversized adjustable sample pool 30, which can adapt to a sample size of 100*75, with adjustable thickness and automatic compression. The maximum expandable sample size can reach 150*100, and larger sizes (set according to demand). The sample pool 30 can accommodate samples of various shapes such as rectangles, squares, trapezoids, discs, and even other special-shaped samples, and has strong versatility and scalability.

[0092] In addition, the sample pool 30 can be completely disassembled and replaced, and the replacement and maintenance are simple, and the overall use cost is low.

[0093] In addition, a temperature sensor may be provided on the receiving bottom plate 301 to achieve temperature measurement, such as a platinum resistor, which is not limited in the present application.

[0094] See also Figure 6 As shown in FIG. 8 , optionally, a plug board 304 is provided in the target area of ​​the first surface of the sample pool 30 ; the hot ends of the plurality of first thermocouples 50 are located on the plug board 304 on the first surface of the sample pool.

[0095] It should be noted that the socket board 304 has a plurality of sockets to facilitate the fixing and convenient fixing of the thermoelectric junction, and can provide stable installation and convenient replacement.

[0096] In addition, a plug-in board may also be provided in the target area of ​​the first surface of the reference cell 40 ; the cold ends of the plurality of first thermocouples 50 are located on the plug-in board on the first surface of the reference cell 40 .

[0097] Of course, other target areas may also be provided with power strips, and this application does not limit this.

[0098] Please combine Figure 1 , Figure 2 , Fig. 9 as well as Fig.10 Optionally, the measurement chamber 10 may include a heat insulation cooling layer 101 , a temperature equalizer layer 102 and a heater 103 .

[0099] The thermal insulation cooling layer 101 is disposed outside the thermostat layer 102 .

[0100] The heat-insulating cooling layer 101 is used to isolate the external environment and reduce internal heat loss. A cooler can be set on its outer layer to connect to the circulating coolant to achieve cooling. The cooler is used to prevent the outer wall of the instrument from being heated when the instrument is used at high temperatures, reduce environmental impact, and also play a safety protection role.

[0101] A heater 103 is provided on the surface of the temperature equalizer layer 102 to control the internal temperature field.

[0102] The temperature equalizer layer 102 is cylindrical as a whole, and heaters capable of independent computer automatic temperature control are arranged on the upper surface, lower surface and cylindrical surface of the temperature equalizer layer 102 to achieve precise control of the temperature field inside the calorimeter and rapid heating at the same time.

[0103] In summary, the large sample three-dimensional calorimeter 100 provided in the embodiment of the present application mainly utilizes the basic principle of three-dimensional microcalorimetry, adopts differential heat flow calorimetry, and is combined with an adjustable large sample pool structure, which can be applied to the heat flow measurement of similar large-sized and special-shaped samples such as blade batteries. It has a wide temperature range and can meet the test conditions of temperature sweeping and constant temperature in any temperature range from room temperature to 700°C, while also taking into account the synchronous tests of external charging and discharging, high voltage, chromatography, etc.

[0104] In addition, in the description of the present application specification and the appended claims, the terms "first", "second", "third", etc. are only used to distinguish the descriptions and cannot be understood as indicating or implying relative importance.

[0105] References to "one embodiment" or "some embodiments" etc. described in the specification of this application mean that one or more embodiments of the present application include specific features, structures or characteristics described in conjunction with the embodiment. Therefore, the statements "in one embodiment", "in some embodiments", "in some other embodiments", "in some other embodiments", etc. that appear in different places in this specification do not necessarily refer to the same embodiment, but mean "one or more but not all embodiments", unless otherwise specifically emphasized in other ways. The terms "including", "comprising", "having" and their variations all mean "including but not limited to", unless otherwise specifically emphasized in other ways.

[0106] In the description of the embodiments of the present invention, it needs to be understood that terms such as “up”, “down”, “front”, “back”, “left”, “right”, “vertical”, “horizontal”, “center”, “top”, “bottom”, “top”, “bottom”, “inside”, “outside”, “inside”, and “outside” indicate orientation or positional relationships.

[0107] In the description of the embodiments of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "install", "connect", "connect", and "assemble" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a direct connection, or an indirect connection through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0108] In the description of the embodiments of the present invention, specific features, structures, materials or characteristics may be combined in a suitable manner in any one or more embodiments or examples.

[0109] In the description of the embodiments of the present invention, it should be understood that "-" and "~" represent a range between two values, and the range includes the endpoints. For example: "AB" represents a range greater than or equal to A, and less than or equal to B. "A~B" represents a range greater than or equal to A, and less than or equal to B.

[0110] In the description of the embodiments of the present invention, the term "and / or" herein is merely a description of the association relationship of associated objects, indicating that three relationships may exist. For example, A and / or B may represent: A exists alone, A and B exist at the same time, and B exists alone. In addition, the character " / " herein generally indicates that the associated objects before and after are in an "or" relationship.

[0111] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A large sample three-dimensional calorimeter, characterized in that: include: Measuring chamber, bracket, sample cell and reference cell; The sample pool and the reference pool are suspended inside the measuring chamber through the bracket; the inside of the sample pool is used to load the sample to be tested, and the inside of the reference pool is used to load the reference sample; the sample pool and the reference pool are symmetrically arranged inside the measuring chamber; The sample pool and the reference pool have the same structure, and a target area is arranged at the same position on the first surface of the sample pool and the first surface of the reference pool; the first surface of the sample pool faces the reference pool, and the first surface of the reference pool faces the sample pool; A plurality of first thermocouples are connected in series between a target area on the first surface of the sample cell and a target area on the first surface of the reference cell; The hot ends of the plurality of first thermocouples are located at the target area of ​​the first surface of the sample cell, and the cold ends of the plurality of first thermocouples are located at the target area of ​​the first surface of the reference cell. The target area is also arranged at the same position of the second surface of the sample cell and the second surface of the reference cell; the second surface of the sample cell faces away from the reference cell, and the second surface of the reference cell faces away from the sample cell; A plurality of second thermocouples are connected in series between the target area on the second surface of the sample cell and the target area on the second surface of the reference cell; The hot ends of the plurality of second thermocouples are located at the target area of ​​the second surface of the sample cell, and the cold ends of the plurality of second thermocouples are located at the target area of ​​the second surface of the reference cell.

2. The large sample three-dimensional calorimeter according to claim 1, characterized in that: The first surface of the sample pool and the first surface of the reference pool are provided with at least two target areas; and the target areas at the same position on the first surface of the sample pool and the first surface of the reference pool correspond one to one; The second surface of the sample cell and the second surface of the reference cell are provided with at least two target areas; Furthermore, the target areas at the same position on the second surface of the sample cell and the second surface of the reference cell correspond one to one.

3. The large sample three-dimensional calorimeter according to claim 1, characterized in that: A target area is provided at the same position of the third surface of the sample cell and the third surface of the reference cell; A plurality of third thermocouples are connected in series between a target area on the third surface of the sample pool and a target area on the third surface of the reference pool; hot ends of the plurality of third thermocouples are located in the target area on the third surface of the sample pool, and cold ends of the plurality of third thermocouples are located in the target area on the third surface of the reference pool.

4. The large sample three-dimensional calorimeter according to claim 3, characterized in that: The third surface of the sample pool and the third surface of the reference pool are provided with at least two target areas; and the target areas at the same position on the third surface of the sample pool and the third surface of the reference pool correspond one to one.

5. The large sample three-dimensional calorimeter according to claim 1, characterized in that: The sample pool comprises: a receiving bottom plate and a cover plate; The sample to be tested is used to be placed on the receiving bottom plate and is fixed by the cover plate.

6. The large sample three-dimensional calorimeter according to claim 5, characterized in that: The same position of the receiving bottom plate and the cover plate is provided with screw holes; The sample to be tested is fixed between the containing bottom plate and the cover plate by screwing the spring screw into the screw holes of the containing bottom plate and the cover plate.

7. The large sample three-dimensional calorimeter according to claim 6, characterized in that: The rotation depth of the spring screw is adjusted to adjust the spacing distance between the receiving bottom plate and the cover plate, thereby placing different quantities of samples to be tested in the sample pool.

8. The large sample three-dimensional calorimeter according to claim 5, characterized in that: The receiving bottom plate is also provided with a side plate, through which the position of the sample to be tested is limited; Wherein, the limiting space for accommodating the sample to be tested is made square by the side plate; or, the limiting space for accommodating the sample to be tested is made circular by the side plate.

9. The large sample three-dimensional calorimeter according to claim 1, characterized in that: A plug-in board is provided in the target area of ​​the first surface of the sample pool; the hot ends of the plurality of first thermocouples are located on the plug-in board on the first surface of the sample pool; A plug-in board is provided in the target area of ​​the first surface of the reference cell; and the cold ends of the plurality of first thermocouples are located on the plug-in board on the first surface of the reference cell.

10. The large sample three-dimensional calorimeter according to claim 1, characterized in that: The measuring chamber comprises a heat-insulating cooling layer and a thermostatic layer, wherein the heat-insulating cooling layer is arranged outside the thermostatic layer; Wherein, the heat insulation and cooling layer is used to isolate the external environment and reduce internal heat loss; A heater is arranged on the surface of the temperature equalizer layer to control the internal temperature field.

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