CN116718509A - Low-temperature thermogravimetric analyzer - Google Patents
Low-temperature thermogravimetric analyzer Download PDFInfo
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- CN116718509A CN116718509A CN202310639347.XA CN202310639347A CN116718509A CN 116718509 A CN116718509 A CN 116718509A CN 202310639347 A CN202310639347 A CN 202310639347A CN 116718509 A CN116718509 A CN 116718509A
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- balance
- temperature
- heating system
- furnace body
- thermogravimetric analyzer
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- 238000010438 heat treatment Methods 0.000 claims abstract description 71
- 239000000725 suspension Substances 0.000 claims abstract description 22
- 239000000126 substance Substances 0.000 claims abstract description 11
- 238000005303 weighing Methods 0.000 claims abstract description 7
- 229910052751 metal Inorganic materials 0.000 claims description 28
- 239000002184 metal Substances 0.000 claims description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 239000002826 coolant Substances 0.000 claims description 14
- 238000013016 damping Methods 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 230000000149 penetrating effect Effects 0.000 claims description 3
- 238000002411 thermogravimetry Methods 0.000 abstract description 14
- 238000002844 melting Methods 0.000 abstract description 8
- 230000008018 melting Effects 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 7
- 238000004458 analytical method Methods 0.000 abstract description 4
- 238000005259 measurement Methods 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 230000009467 reduction Effects 0.000 abstract description 3
- 238000011160 research Methods 0.000 abstract description 2
- 238000000197 pyrolysis Methods 0.000 abstract 1
- 238000002474 experimental method Methods 0.000 description 10
- 238000001816 cooling Methods 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- XYQRXRFVKUPBQN-UHFFFAOYSA-L Sodium carbonate decahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.[Na+].[Na+].[O-]C([O-])=O XYQRXRFVKUPBQN-UHFFFAOYSA-L 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 229940018038 sodium carbonate decahydrate Drugs 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000002076 thermal analysis method Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
The invention provides a low-temperature thermogravimetric analyzer, and belongs to the technical field of thermogravimetric analysis. The device comprises a furnace body heating system, a balance weight and a balance, wherein the furnace body heating system comprises a sample tray, a sample holder, a heating system, a temperature control system and a heating furnace, the temperature control system is arranged in the heating furnace, and the heating system is arranged at the inner side of the temperature control system; the two ends of the balance are connected with balance suspension wires, the upper ends of the two balance suspension wires are respectively connected with the sample tray and the balance weighing signal end, and the lower ends of the balance suspension wires are fixedly connected with the balance weights; a temperature sensor and a pressure sensor are arranged in the furnace body heating system; the temperature control system can reduce the internal temperature of the heating furnace, so that the initial temperature of the thermogravimetric analyzer is lower than the room temperature. After a temperature control system is added at the periphery of a heating system of a furnace body of the thermogravimetric analyzer, the measurement can be started from a low-temperature area when the thermogravimetric analysis is performed on special substances such as low melting point, easy volatilization, weathering and the like, and failure analysis can be performed on materials serving under the working condition of the polar end. The application of the device also comprises the research of low-temperature reduction or low-temperature oxidation reaction, low-temperature pyrolysis, thermal stability analysis and the like of the material.
Description
Technical Field
The invention belongs to the technical field of thermogravimetric analysis, and relates to a thermogravimetric analyzer, in particular to a low-temperature thermogravimetric analyzer.
Background
The thermogravimetric analyzer is an instrument for detecting the change relation between the temperature and the mass of a substance by using a thermogravimetric method, and measures the change relation of the mass of the substance along with the temperature or time under the control of a program temperature.
The existing thermogravimetric analysis instrument mainly comprises a balance, a furnace body heating system, a program temperature control system, an atmosphere control system, weighing conversion, amplification, analog/digital conversion, data fact acquisition, recording and the like; the thermogravimetric analyzer acquires damping signals, the computer and thermogravimetric software are used for processing data, then a test curve is displayed on the computer, and the data result can be analyzed through related software.
Through thermogravimetric analysis experiments, the change of crystal properties, such as physical phenomena of melting, evaporation, sublimation, adsorption and the like, can be more conveniently studied; and the method is also helpful for researching chemical phenomena such as thermal stability, decomposition process, dehydration, dissociation, oxidation, reduction, quantitative analysis of components, influence of additives and fillers, moisture and volatile matters, reaction kinetics and the like of substances.
The arrangement modes of the heating furnace and the balance at present mainly comprise: upper dish type, suspension type and parallel type. The existing typical thermogravimetric analysis device, such as microcomputer differential calorimeter, has the temperature measuring range of RT-1000 ℃, and has lower melting point<100 ℃ materials, e.g. sodium carbonate decahydrate (melting point T) m =34 ℃ and easily weathered), if the thermogravimetric curve is measured from room temperature using the existing thermogravimetric analysis device, the water loss amount cannot be accurately determined from the TG curve. Therefore, the existing thermogravimetric analysis device is difficult to measure the sample with the melting point lower than the room temperature, and cannot meet the thermogravimetric analysis of the low-temperature sample.
Disclosure of Invention
The invention aims at solving the problems in the prior art, and provides a low-temperature thermogravimetric analyzer, which aims at solving the technical problems that: how to realize the widening of the thermal analysis temperature range of the thermogravimetric analyzer.
The aim of the invention can be achieved by the following technical scheme:
a low-temperature thermogravimetric analyzer comprises a furnace body heating system, a balance weight and a balance, wherein the furnace body heating system heats substances placed in the furnace body heating system. The furnace body heating system comprises a sample tray, a sample holder, a heating system, a temperature control system and a heating furnace; a temperature control system is arranged in the heating furnace, a heating system is arranged at the inner side of the temperature control system, a sample holder is fixed in the heating system, the sample holder separates the interior of the heating system, a through hole penetrating through the sample holder is formed in the sample holder, and a sample tray is placed at the top of the sample holder; the two ends of the balance are connected with balance suspension wires, the balance is positioned in the middle of the balance suspension wires, the upper ends of the two balance suspension wires are respectively connected with a sample tray and a balance weighing signal end, and the lower ends of the balance suspension wires are fixedly connected with balance weights.
The furnace body heating system is internally provided with a temperature sensor and a pressure sensor, and the temperature sensor and the pressure sensor are connected to the program control and data acquisition system.
The temperature control system can reduce the internal temperature of the heating furnace, so that the initial temperature of the thermogravimetric analyzer is lower than the room temperature.
The furnace body heating system also comprises a strong electric cabinet which is connected with the furnace body heating system.
The temperature control system is used for introducing a cooling medium, and the metal pipe is wound on the periphery of the heating system of the furnace body of the thermogravimetric analyzer, so that the initial temperature of thermogravimetric analysis can be reduced, and the accuracy of experimental results for measuring materials with easy water loss and low melting point is ensured; and can be used as a cooling device to condense and recycle the volatile substances caused by high temperature in the thermogravimetric analysis process, thereby reducing the pollution to the laboratory and the atmosphere.
Further: the temperature control system comprises a metal pipe coiled into a cylindrical structure and a metal shell covered on the periphery of the metal pipe, the metal pipe is sleeved on the periphery of the heating system and is attached to the heating system, cooling medium is introduced into the metal pipe, and the cooling medium is liquid nitrogen.
By adopting the structure, the heating system can directly act on the heating system, the internal temperature is reduced rapidly in time, and the initial temperature of the heating system is conveniently controlled.
Further: the lower port of the metal tube is provided with a medium inlet, the upper port of the metal tube is provided with a medium outlet, cooling medium is introduced into the metal tube from the medium inlet, and the cooling medium flows out from the medium outlet after flowing in the metal tube.
By adopting the structure, the cooling medium flows upwards from the bottom, so that the contact time of the cooling medium inside is ensured, the cooling effect is ensured, and the utilization rate of the cooling medium is improved.
Further: the balance suspension wire at the lower side of the sample tray passes through the through hole to generate vertical downward tension on the sample tray, and the balance weighing signal end is connected with the program control and data acquisition system.
By adopting the structure, the sample tray is ensured to be pulled vertically downwards, and the quality of the test affected by the temperature is more accurately detected.
Further: the two balance suspension wires are respectively connected with a sensor and a damping and balance restorer, and the sensor, the damping and the balance restorer are all connected with a program control and data acquisition system.
By adopting the structure, the balance conditions at two sides of the balance can be monitored, the balance can be adjusted, the two sides of the balance are reset to the horizontal position through the damping effect, and the real and accurate monitoring result is ensured.
Compared with the prior art, the low-temperature thermogravimetric analyzer has the following advantages:
1. after a temperature control system is added to the periphery of a heating system of a furnace body of the thermogravimetric analyzer, refrigerating materials such as liquid nitrogen are introduced, and when the thermogravimetric analysis of special substances such as low melting point, easy volatilization, weathering and the like is performed, the measurement can be started from a low temperature region (liquid nitrogen temperature T=196 ℃), the experimental error of the traditional measurement on an experimental result from room temperature is avoided, the accuracy of the test result is improved, and failure analysis, low-temperature reduction or low-temperature oxidation reaction research, low-temperature thermal decomposition, thermal stability analysis and the like can also be performed on the materials served under the extreme working condition.
2. The liquid nitrogen circulating cooling system in the temperature control device can cool the experimental instrument in a controllable range rapidly after the experiment is finished, so that the experiment efficiency is improved, the experimental device is protected, and the service life is prolonged.
3. The auxiliary cooling can quickly reduce the temperature of the instrument within the allowable range of the use temperature of the instrument, shorten the waiting time of experiment cooling, and improve the experiment efficiency and the service life of the experiment instrument.
Drawings
Fig. 1 is a schematic structural view of the present invention.
FIG. 2 is a schematic diagram of a furnace heating system according to the present invention.
Fig. 3 is a schematic structural diagram of a temperature control system in the present invention.
In the figure:
111. a furnace body heating system; 112. a strong current cabinet; 113. a sensor; 114. a counterweight; 115. damping and balance reset; 116. and (5) a balance.
101. A sample tray; 102. program control and data acquisition system; 103. a sample holder; 104. a heating system; 105. a temperature control system; 106. a heating furnace; 107. and (5) suspending the balance.
109. A metal tube; 109-a, media inlet; 109-b, medium outlet.
Detailed Description
The following are specific embodiments of the present invention and the technical solutions of the present invention will be further described with reference to the accompanying drawings, but the present invention is not limited to these embodiments.
As shown in fig. 1-3, the embodiment provides a low-temperature thermogravimetric analyzer, which comprises a furnace body heating system 111, a balance 114 and a balance 116, wherein the furnace body heating system 111 heats substances placed in the furnace body heating system, and further comprises a strong electric cabinet 112, and the strong electric cabinet 112 is connected with the furnace body heating system 111 to provide power for equipment.
The furnace body heating system 111 comprises a sample tray 101, a sample holder 103, a heating system 104, a temperature control system 105 and a heating furnace 106: a temperature control system 105 is arranged in the heating furnace 106, and the temperature control system 105 is composed of a metal pipe 109 coiled into a cylindrical structure and a metal shell covered on the periphery of the metal pipe 109; the metal tube 109 is sleeved on the periphery of the heating system 104 and is contacted with the outer wall of the heating system 104, and cooling mediums such as liquid nitrogen and the like are introduced into the metal tube 109 to control the temperature of the heating system 104; the cooling medium flows in the water inlet pipe 109 to absorb the internal heat and reduce the temperature in the heating furnace 106; the lower port of the metal tube 109 is set to 109-a, and the upper port is set to 109-b; the cooling medium is introduced into the metal tube 109 from 109-a, flows out from the medium outlet 109-b after flowing in the metal tube 109, and timely takes away heat, so that the internal temperature is reduced, the applicable environment temperature of the analyzer is lower, and the applicable sample range is wider.
The heating system 104 is arranged on the inner side of the temperature control system 105, heat is generated in the heating system 104, the temperature in the heating system is changed, and the thermal gravimetric experiment requirement is met. A sample holder 103 is fixed in the heating system 104, the sample holder 103 partitions the heating system 104, and a through hole penetrating up and down is formed in the sample holder 103; the sample tray 101 is placed on the top of the sample holder 103, the sample tray 101 is supported by the sample support 103, the bottom of the sample tray 101 is connected with a balance suspension wire 107, and the lower end is fixedly connected with a balance weight 114.
The balance suspension 107 is connected to both ends of the balance 116, and the balance 116 is located in the middle of the balance suspension 107: the upper ends of the two balance suspension wires 107 are respectively connected with the sample tray 101 and the balance weighing signal end, the lower ends of the balance suspension wires 107 are fixedly connected with the balance weights 114, and the balance weights 114 at the two sides keep balance at the two sides of the balance 116. The two balance suspension wires 107 are respectively connected with a sensor 113 and a damping and balance restorer 115, and the sensor 113, the damping and balance restorer 115 are connected with the program control and data acquisition system 102, so that the balance conditions of two sides of a balance 116 can be monitored, and the balance 116 can be adjusted; and the two sides of the balance 116 are reset to the horizontal position under the damping effect, so that the real and accurate monitoring result is ensured.
The furnace body heating system 111 is internally provided with a temperature sensor and a pressure sensor, and is connected to the program control and data acquisition system 102, so as to monitor the temperature and pressure conditions in the heating system 111 and acquire more comprehensive detection data.
The temperature control system 105 is arranged in the equipment, so that the initial temperature of thermogravimetric analysis can be reduced, and the accuracy of experimental results for measuring materials with easy water loss and low melting point is ensured; and can be used as a cooling device to condense and recycle the volatile substances caused by high temperature in the thermogravimetric analysis process, thereby reducing the pollution to the laboratory and the atmosphere. Auxiliary cooling can be used at instrument use temperatureThe temperature of the instrument is quickly reduced within the allowable range, the experiment cooling waiting time is shortened, and the experiment efficiency and the service life of the experiment instrument are improved. Meanwhile, the gas-carrying atmosphere in the heating furnace is not limited to inert atmospheres such as nitrogen or helium, and also comprises CO and H 2 Such as reducing atmosphere, oxidizing atmosphere such as air and oxygen, and other carrier gases.
The specific embodiments described herein are offered by way of example only to illustrate the spirit of the invention. Those skilled in the art may make various modifications or additions to the described embodiments or substitutions thereof without departing from the spirit of the invention or exceeding the scope of the invention as defined in the accompanying claims.
Claims (7)
1. The low-temperature thermogravimetric analyzer comprises a furnace body heating system (111), a balance weight (114) and a balance (116), wherein the furnace body heating system (111) heats substances put in the furnace body heating system; the method is characterized in that: the furnace body heating system (111) comprises a sample tray (101), a sample holder (103), a heating system (104), a temperature control system (105) and a heating furnace (106), wherein the temperature control system (105) is arranged in the heating furnace (106); a heating system (104) is arranged on the inner side of the temperature control system (105), a sample holder (103) is fixed in the heating system (104), and the sample holder (103) divides the inside of the heating system (104); the sample holder (103) is provided with a through hole penetrating through the upper part and the lower part, and the sample tray (101) is placed on the top of the sample holder (103); two ends of the balance (116) are connected with a balance suspension wire (107), the balance (116) is positioned in the middle of the balance suspension wire (107), the upper ends of the two balance suspension wires (107) are respectively connected with the sample tray (101) and the balance weighing signal end, and the lower ends of the balance suspension wires (107) are fixedly connected with a balance weight (114);
a temperature sensor and a pressure sensor are arranged in the furnace body heating system (111) and are connected to the program control and data acquisition system (102);
the temperature control system (105) can reduce the internal temperature of the heating furnace (106) so that the initial temperature of the thermogravimetric analyzer is lower than the room temperature.
2. The cryogenic thermogravimetric analyzer of claim 1, wherein the temperature control system (105) comprises a metal tube (109) coiled into a cylindrical structure and a metal housing covering the periphery thereof; the metal tube (109) is sleeved on the periphery of the heating system (104) and is attached to the heating system (104), and cooling medium is introduced into the metal tube (109).
3. The low temperature thermogravimetric analyzer of claim 1, wherein: the cooling medium introduced into the metal pipe (109) is liquid nitrogen.
4. A cryogenic thermogravimetric analyzer according to claim 2 or 3, wherein: the lower port of the metal tube (109) is provided with a medium inlet (109-a), the upper port of the metal tube is provided with a medium outlet (109-b), cooling medium is introduced into the metal tube (109) from the medium inlet (109-a), and the cooling medium flows out from the medium outlet (109-b) after flowing in the metal tube (109).
5. The low temperature thermogravimetric analyzer of claim 1, wherein: a balance suspension line (107) at the lower side of the sample tray (101) passes through the through hole to generate vertical downward tension on the sample tray (101), and a balance weighing signal end is connected with a program control and data acquisition system (102).
6. The low temperature thermogravimetric analyzer of claim 1, wherein: the two balance suspension wires (107) are respectively connected with a sensor (113) and a damping and balance restorer (115), and the sensor (113) and the damping and balance restorer (115) are connected with a program control and data acquisition system (102).
7. The low-temperature thermogravimetric analyzer of claim 1, further comprising a strong electric cabinet (112), wherein the strong electric cabinet (112) is connected to the furnace body heating system (111).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310639347.XA CN116718509A (en) | 2023-06-01 | 2023-06-01 | Low-temperature thermogravimetric analyzer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310639347.XA CN116718509A (en) | 2023-06-01 | 2023-06-01 | Low-temperature thermogravimetric analyzer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116718509A true CN116718509A (en) | 2023-09-08 |
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ID=87865299
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310639347.XA Pending CN116718509A (en) | 2023-06-01 | 2023-06-01 | Low-temperature thermogravimetric analyzer |
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| Country | Link |
|---|---|
| CN (1) | CN116718509A (en) |
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2023
- 2023-06-01 CN CN202310639347.XA patent/CN116718509A/en active Pending
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