A device and method for preventing contamination of a synchronous thermal analysis support

Abstract

The present invention relates to the technical field of thermal analysis instruments and equipment, and in particular to a device and method for preventing contamination of a synchronous thermal analysis support; the device and method comprise a structure of a crucible and a protective support frame; the upper side of the crucible is formed with a flange extending upward, the flange of the crucible is wider than and higher than a main structure of the crucible; the protective support frame comprises a protective support plate of a plate-like structure, a receiving channel is arranged on the protective support plate, and the position of the receiving channel corresponds to the position of the crucible; a liquid overflow prevention groove is arranged on the upper surface of the protective support plate, and the liquid overflow prevention groove does not contact the flange of the crucible.

Description

Technical Field

[0001] The invention relates to the technical field of thermal analysis instruments and equipment, and in particular to a device and method for preventing contamination of a synchronous thermal analysis bracket. Background Art

[0002] At present, the synchronous thermal analyzer is a material property testing instrument that combines thermogravimetric analysis with differential thermal analysis or differential scanning calorimetry. Under the same temperature control measurement conditions, the information of thermogravimetric (the relationship between the change of mass with temperature (or time)) and differential thermal (the functional relationship between the temperature difference between the measured substance and the reference substance and the temperature) can be obtained for the same sample simultaneously. The synchronous thermal analyzer can be used to analyze the dehydration, thermal stability, adsorption and desorption, decomposition and volatilization, oxidation and reduction, crystal transformation, melting point and melting, glass transition temperature, nucleation temperature, crystallization temperature, specific heat, reaction kinetics, etc. of the test material. It is widely used in various organic materials, inorganic materials, metal materials, semiconductor materials, insulation materials, food, biology, medicine, aerospace, geology, building materials and other fields.

[0003] Among them, the most easily damaged part of the synchronous thermal analyzer is the sample holder (sensor holder) that contacts the sample crucible. For materials with known thermophysical properties, equipment operators can basically control the appropriate detection conditions to avoid contamination of the sample holder (sensor holder); however, the breakthrough innovation of science and technology and the development and extension of application fields have promoted the birth of various newly discovered, newly synthesized, and newly modified materials. When these constantly innovative new materials with unknown thermophysical properties are subjected to synchronous thermal analysis, the risk of contamination or even scrapping of the sample holder (sensor holder) is greatly increased; some high-temperature samples will penetrate the alumina crucible, and the volatilized substances of the samples will usually flow around the sample crucible and at the bottom of the crucible. When too much volatile substances flow into the bottom of the crucible, the crucible and the sample platinum holder will stick together, thereby contaminating the holder, and in severe cases, causing the holder to be scrapped; the sample holder (sensor holder) is a key component of synchronous thermal analysis detection, which is precision-made and expensive (taking the STA449 series of synchronous thermal analyzers from Germany's Netzsch as an example, the price of the sensor holder in 2021 is 50,000-110,000), difficult to clean and difficult to repair. Summary of the invention

[0004] The present invention provides a device and method for preventing contamination of a synchronous thermal analysis support, aiming to solve the technical problem of performing thermal analysis on a sample with unknown thermal properties and preventing the sample support from being contaminated when the sample overflows at high temperature.

[0005] The technical solution used in the present invention is as follows: a device for preventing contamination of a synchronous thermal analysis bracket, comprising a structure of a crucible and a protective support frame; a flange extending upward is formed on the upper side of the crucible, and the flange of the crucible is wider than and higher than the main structure of the crucible; the protective support frame comprises a protective support plate of a plate-like structure, on which a receiving channel is arranged, and the position of the receiving channel corresponds to the position of the crucible; a liquid overflow prevention groove is arranged on the upper surface of the protective support plate, and the liquid overflow prevention groove does not contact the flange of the crucible.

[0006] Furthermore, the liquid overflow prevention groove completely surrounds the outside of the flange, and the lowest point of the flange is located in the liquid overflow prevention groove and extends into the liquid overflow prevention groove.

[0007] Furthermore, the flange is either a T-shaped structure or a V-shaped structure.

[0008] Furthermore, the middle part of the liquid overflow prevention groove is connected together through a connecting groove, and the lower side of the connecting groove is fixed to the upper center of the protective support plate through a micro gravity sensor; the lower ends of the left and right sides of the protective support plate are fixed to the card plate through a push rod; the grooves of the two card plates are arranged relatively to each other; the micro gravity sensor and the push rod are connected to the controller respectively; the micro gravity sensor is used to transmit the detected gravity signal to the controller; the controller is used to start the inflation device when it detects that the gravity increases, and increase the input gas flow enhancement; when the gravity signal is detected to reach a preset threshold, the push rod is controlled to extend.

[0009] Furthermore, the card board is a C-shaped structure, and the C-shaped grooves of the two card boards are arranged opposite to each other.

[0010] Furthermore, a transmitting device and a receiving device are respectively provided at both ends of the upper side of the protective support plate, which are fixed to the protective support plate through a mounting bracket; a mirror layer is provided in the middle of the connecting groove, and the transmitting device and the receiving device are connected to the controller; the signal of starting the transmitting device and the receiving device is fed back to the controller; when the mirror layer in the connecting groove is blocked by the sample and the receiving device cannot receive the rays; the controller starts the inflation device to increase the input gas flow enhancement.

[0011] According to the device for preventing contamination of a synchronous thermal analysis bracket according to claim 6, it is characterized in that a clamping groove is provided in the middle of the connecting groove, and the U-shaped mirror layer is clamped in the clamping groove.

[0012] Furthermore, a transmitting device and a receiving device are provided on both sides of the protective support plate, and the protective support plate is made of transparent alumina material; the transmitting device is a laser sensor, and the receiving device is used to measure the transmittance and transmit it to the controller; the inflation device is electrically connected to the controller; the controller is used to start the inflation device when it detects that the transmittance change exceeds the limit value.

[0013] The present application also proposes a method for preventing contamination of a synchronous thermal analysis bracket. In the first step, the transmitting device and the receiving device are started without placing any samples, and the transmittance is fed back to the controller; a baseline test is performed to obtain the change in transmittance under the current test conditions.

[0014] In the second step, the sample is placed and tested under the same temperature control conditions as the baseline test to obtain the real-time measured transmittance, which is compared with the transmittance during the baseline measurement.

[0015] In the third step, when the transmittance measured in real time exceeds the transmittance limit value during baseline measurement (for example, a change of 3%), emergency braking measures are initiated through the controller.

[0016] The beneficial effects achieved by the present invention are as follows: the edge protrusion shape of the liquid overflow prevention groove is adapted to the T-shaped structure or V-shaped structure of the crucible, that is, the liquid overflow prevention groove completely surrounds the outside of the flange, and the lowest point of the flange is located in the liquid overflow prevention groove and extends into the liquid overflow prevention groove; if a large amount of sample overflows, the sample solution in the crucible will overflow from the flange into the liquid overflow prevention groove, and the liquid overflow prevention groove plays a secondary protective role for the sample; although a small amount of sample liquid is lost, there is no shutdown braking in the middle, and the measured test data has a certain reference value. The primary protection of the sample by the flange and the secondary protection of the sample in the liquid overflow prevention groove can avoid the problem of sample bracket being contaminated when performing thermal analysis on samples with unknown thermal properties. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 The crucible structure of the present invention is schematically shown in FIG. Figure 1 .

[0018] Figure 2 The crucible structure of the present invention is schematically shown in FIG. Figure 2 .

[0019] Figure 3 It is a schematic diagram of the cross-sectional structure of the protective support plate of the present invention.

[0020] Figure 4 It is a connection diagram of the transmitting device and the receiving device of the present invention.

[0021] Figure 5 It is a schematic diagram of the position of the protective support plate of the present invention.

[0022] Figure 6 It is a schematic diagram of the card board structure of the present invention.

[0023] Figure 7 It is a schematic diagram of the positions of the transmitting device and the receiving device of the present invention.

[0024] Figure 8 It is a schematic diagram of the accommodating channel structure of the present invention.

[0025] In the figure, 1. crucible; 2. protective support plate; 3. flange; 4. receiving channel; 5. liquid overflow prevention groove; 6. connecting groove; 7. card plate; 8. micro gravity sensor; 9. push rod; 10. transmitting device; 11. receiving device 12. controller. DETAILED DESCRIPTION

[0026] To facilitate those skilled in the art to understand the present invention, specific implementations of the present invention are described below with reference to the accompanying drawings.

[0027] In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "installation", "connection" and "connection" 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 mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium, or it can be the internal connection of two elements; for ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood through specific circumstances.

[0028] First, the application scenario of the present application is introduced: the most easily damaged part of the synchronous thermal analyzer is the sensor holder that contacts the sample; for materials with known thermal properties, the equipment operator can basically control the appropriate detection conditions to avoid contamination of the sample holder (sensor holder); however, breakthroughs and innovations in science and technology and the expansion and extension of application fields are driving the birth of various newly discovered, newly synthesized, and newly modified materials. When these constantly innovative new materials with unknown thermal properties are subjected to synchronous thermal analysis, the risk of contamination or even scrapping of the sample holder (sensor holder) is greatly increased; some high-temperature samples will penetrate the alumina crucible 1, and the volatilized substances from the samples will usually flow around the sample crucible 1 and the bottom of the crucible 1. When too much volatile substances flow into the bottom of the crucible 1, the crucible 1 and the sample holder will stick together, thereby contaminating the sample holder and causing the sample holder to be scrapped.

[0029] Embodiment 1

[0030] like Figure 1 As shown, the present invention provides a device for preventing contamination of a synchronous thermal analysis support, comprising a crucible 1 and a protective support frame structure, the material of the crucible 1 is not limited; the crucible 1 structure is a general cylindrical crucible 1, and a T-shaped or V-shaped flange 3 is extended at the upper end ( Figure 1-2(as shown) the flange 3 of the crucible 1 is wider than and higher than the main structure of the crucible 1; when the sample in the crucible 1 overflows, if a small amount of the sample overflows, it will overflow into the flange 3, and the flange 3 plays a primary protection role for the sample, and will not cause the loss of the sample liquid, thereby ensuring the accuracy of the experiment (the sample liquid on both sides is located in the flange 3 and does not separate from the crucible 1); the protective support frame includes a protective support plate 2 of a plate-like structure, and a accommodating channel 4 is arranged on the protective support plate 2. The position of the accommodating channel 4 corresponds to the position of the crucible 1, that is, when the crucible 1 is placed on the sample holder, the two crucibles 1 are located in the accommodating channel 4 and do not contact the crucible 1, so that the measurement data of the crucible 1 will not be affected; a liquid overflow prevention groove 5 is provided on the upper surface of the protective support plate 2, and a support leg is provided on the lower surface thereof, and the protective support plate 2 is placed on the support plate of the thermal analyzer through the support leg; the liquid overflow prevention groove 5 is two annular grooves The structure is as follows: two crucibles 1 are located in the accommodating channel 4, and the liquid overflow prevention groove 5 does not contact the flange 3 of the crucible 1; its shape can be adjusted according to actual conditions, and the edge protrusion shape of the liquid overflow prevention groove 5 is adapted to the T-shaped structure or V-shaped structure of the flange 3 of the crucible 1, that is, the liquid overflow prevention groove 5 completely surrounds the outside of the flange 3, and the lowest point of the flange 3 is located in the liquid overflow prevention groove 5 and extends into the liquid overflow prevention groove 5; if a large amount of sample overflows, the sample solution in the crucible 1 will overflow from the flange 3 into the liquid overflow prevention groove 5, and the liquid overflow prevention groove 5 plays a secondary protection role for the sample; although a small amount of sample liquid is lost; but there is no shutdown braking in the middle, and the measured test data has a certain reference, and the primary protection of the sample by the flange 3 and the secondary protection of the sample in the liquid overflow prevention groove 5 can avoid the problem of sample bracket being contaminated when performing thermal analysis on samples with unknown thermal properties.

[0031] Embodiment 2

[0032] When the sample overflows the crucible 1, the existing practice is to manually adjust the main control system and issue emergency braking measures, such as increasing the input gas flow rate and starting the exhaust device. This requires manual supervision, and sometimes the test personnel do not notice it. The sample continues to overflow and splash, and it is still possible to contaminate the sample holder. Therefore, the middle parts of the two liquid overflow prevention grooves 5 are connected together through a U-shaped connecting groove 6, and the lower side of the connecting groove 6 is fixed to the upper center of the protective support plate 2 through a micro gravity sensor 8. The lower ends of the left and right sides of the protective support plate 2 are fixed to the clamping plate 7 through a push rod 9. The clamping plate 7 is C The protective support plate 2 has a U-shaped structure, and the C-shaped grooves of the two card boards 7 are arranged opposite to each other, and the card boards 7 are clamped on the support plate of the thermal analyzer; a heat insulation layer is arranged inside the card board 7 to isolate heat (not shown in the figure); a transmitting device 10 and a receiving device 11 (such as a laser sensor) are respectively arranged at both ends of the upper side of the protective support plate 2, which are fixed to the protective support plate 2 through a mounting bracket; a card slot is arranged in the middle of the connecting groove 6, and a U-shaped mirror layer 13 is clamped in the card slot, so as to facilitate the replacement of the mirror layer 13; the transmitting device 10 emits rays, which are reflected by the mirror layer 13 and received by the receiving device 11; the transmitting device 10, the receiving device 11, the micro gravity sensor 8, the push rod 9, and the inflation device (such as a small hair dryer) are respectively connected to the controller; the micro gravity sensor 8 is used to transmit the detected gravity signal to the controller; the controller is used to start the inflation device when it detects that the gravity increases, and increase the input gas flow rate to enhance; when it is detected that the gravity signal reaches a preset threshold , which means that the liquid overflow prevention groove 5 has reached a critical value; the controller controls the push rod 9 to extend so that the liquid overflow prevention groove 5 lifts the flange 3 of the crucible 1, so that the crucible 1 is separated from the sample holder, thereby quickly preventing the crucible 1 from overflowing, thereby avoiding contamination of the sample holder; when a small amount of sample in the crucible 1 overflows into the liquid overflow prevention groove 5, the gravity sensor is not sensitive enough and the mitigation measures cannot be started in time; therefore, a transmitting device 10 and a receiving device 11 are set, the transmitting device 10 and the receiving device 11 are started, and the signal is fed back to the controller; when a small amount of sample in the crucible 1 overflows into the liquid overflow prevention groove 5; the mirror layer 13 in the connecting groove 6 is blocked by the sample, and the rays emitted by the transmitting device 10 are refracted internally after contacting the sample, and the receiving device 11 cannot receive the rays; the inflation device is started to increase the input gas flow rate to enhance; the signals of the transmitting device 10 and the receiving device 11 are in an or logical relationship with the signals emitted by the micro gravity sensor 8, that is, the inflation device is started when one of them is satisfied, thereby mitigating the overflow.

[0033] Embodiment 3

[0034] The transmitting device 10 and the receiving device 11 can be arranged on both sides of the protective support plate, and the protective support plate is made of transparent alumina material (high temperature resistant, insulating, and transparent); the transmitting device 10 is a laser sensor, and the receiving device 11 is used to measure the transmittance and transmit it to the controller. The inflation device for emitting cooling gas is electrically connected to the controller; the controller is used to start the inflation device when it detects that the transmittance change exceeds the limit value.

[0035] A method for preventing contamination of a synchronous thermal analysis bracket: the first step is to start a transmitting device 10 and a receiving device 11 without placing a sample, and feed back the transmittance to a controller; perform a baseline test to obtain a change in transmittance under current test conditions; the second step is to place a sample and perform a test under the same temperature control conditions as the baseline test to obtain a real-time measured transmittance, which is compared with the transmittance during the baseline measurement.

[0036] The purpose of this step is: after the protective support plate is used for many times, its transmittance will change (that is, the transmittance becomes lower and lower). Therefore, each time a new material is tested, a baseline test should be performed first, and then a real-time test should be performed. When the transmittance value of the real-time test is greater than the transmittance value of the baseline test, it means that the sample being tested has fallen into the liquid overflow prevention groove.

[0037] In the third step, when the transmittance measured in real time exceeds the transmittance limit value during baseline measurement (for example, a change of 3%), emergency braking measures are initiated through the controller, such as starting the gas flow of the inflation device to increase, or starting the vacuum pump system or other exhaust device to accelerate the air flow in the chamber.

[0038] If the fixing method is not separately introduced above, the general technical means used by technicians in the industry are used, such as welding, nesting, or threaded fixing.

[0039] In the description of this specification, the description with reference to the terms "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.

[0040] The above-described embodiments of the present invention do not constitute a limitation on the protection scope of the present invention. Any modification, equivalent substitution and improvement made within the spirit and principle of the present invention shall be included in the protection scope of the claims of the present invention.

Claims

1. A device for preventing contamination of a synchronous thermal analysis support, characterized in that: The structure comprises a crucible (1) and a protective support frame; the upper side of the crucible (1) is formed with a flange (3) extending upward, the flange (3) of the crucible (1) being wider than and higher than the main structure of the crucible (1); the protective support frame comprises a protective support plate (2) of a plate-like structure, a receiving channel (4) is arranged on the protective support plate (2), the position of the receiving channel (4) corresponds to the position of the crucible (1); a liquid overflow prevention groove (5) is arranged on the upper surface of the protective support plate (2), the liquid overflow prevention groove (5) does not contact the flange (3) of the crucible (1); the liquid overflow prevention groove (5) completely surrounds the outside of the flange (3), the lowest point of the flange (3) is located in the liquid overflow prevention groove (5) and extends into the liquid overflow prevention groove (5); The middle parts of the two liquid overflow prevention grooves (5) are connected together through a connecting groove (6), and the lower side of the connecting groove (6) is fixed to the upper center of the protective support plate (2) through a micro gravity sensor; the lower ends of the left and right sides of the protective support plate (2) are fixed to the card plate (7) through a push rod (9); the grooves of the two card plates (7) are arranged opposite to each other; the micro gravity sensor and the push rod (9) are respectively connected to the controller; the micro gravity sensor is used to transmit the detected gravity signal to the controller; the controller is used to start the inflation device and increase the input gas flow when it detects that the gravity increases; when it detects that the gravity signal reaches a preset threshold, the push rod (9) is controlled to extend, so that the liquid overflow prevention groove (5) lifts up the flange (3) of the crucible (1), so that the crucible (1) is separated from the sample holder.

2. The device for preventing contamination of a synchronous thermal analysis support according to claim 1, characterized in that: The flange (3) is either a T-shaped structure or a V-shaped structure.

3. The device for preventing contamination of a synchronous thermal analysis support according to claim 1, characterized in that: The clamping plate (7) is a C-shaped structure, and the C-shaped grooves of the two clamping plates (7) are arranged opposite to each other.

4. The device for preventing contamination of a synchronous thermal analysis support according to claim 1, characterized in that: An emitting device (10) and a receiving device (11) are respectively provided at both ends of the upper side of the protective support plate (2), and the emitting device (10) and the receiving device (11) are fixed to the protective support plate (2) via a mounting bracket; a mirror layer (13) is provided in the middle of the connecting groove (6), and the emitting device (10), the receiving device (11), and the inflation device are respectively connected to a controller; signals for starting the emitting device (10) and the receiving device (11) are fed back to the controller; when the mirror layer (13) in the connecting groove (6) is blocked by the sample and the receiving device (11) cannot receive radiation, the controller starts the inflation device to increase the input gas flow rate.

5. The device for preventing contamination of a synchronous thermal analysis support according to claim 4, characterized in that: A clamping groove is provided in the middle of the connecting groove (6), and the U-shaped mirror layer (13) is clamped in the clamping groove.

6. A device for preventing contamination of a synchronous thermal analysis support, characterized in that: The structure comprises a crucible (1) and a protective support frame; the upper side of the crucible (1) is formed with a flange (3) extending upward, the flange (3) of the crucible (1) being wider than and higher than the main structure of the crucible (1); the protective support frame comprises a protective support plate (2) of a plate-like structure, a receiving channel (4) is arranged on the protective support plate (2), the position of the receiving channel (4) corresponds to the position of the crucible (1); a liquid overflow prevention groove (5) is arranged on the upper surface of the protective support plate (2), the liquid overflow prevention groove (5) does not contact the flange (3) of the crucible (1); The liquid overflow prevention groove (5) completely surrounds the outside of the flange (3); the lowest point of the flange (3) is located in the liquid overflow prevention groove (5) and extends into the liquid overflow prevention groove (5); a transmitting device (10) and a receiving device (11) are provided on both sides of the protective support plate; the protective support plate is made of transparent aluminum oxide material; the transmitting device (10) is a laser sensor, and the receiving device (11) is used to measure the transmittance and transmit it to the controller; the inflation device is electrically connected to the controller; and the controller is used to start the inflation device when it detects that the transmittance changes beyond a limit value.

7. A method for preventing contamination of a synchronous thermal analysis support, using the device for preventing contamination of a synchronous thermal analysis support as claimed in claim 6, comprising: first, without placing a sample, starting a transmitting device (10) and a receiving device (11), and feeding back the transmittance to a controller; performing a baseline test to obtain the transmittance under current test conditions; The second step is to place the sample and test it under the same temperature control conditions as the baseline test to obtain the real-time measured transmittance, which is compared with the transmittance during the baseline measurement; In the third step, when the transmittance measured in real time exceeds the transmittance limit value during the baseline measurement, emergency braking measures are initiated through the controller.

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