CN117147617A - High-temperature eutectic point reproduction method - Google Patents
High-temperature eutectic point reproduction method Download PDFInfo
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- CN117147617A CN117147617A CN202310689235.5A CN202310689235A CN117147617A CN 117147617 A CN117147617 A CN 117147617A CN 202310689235 A CN202310689235 A CN 202310689235A CN 117147617 A CN117147617 A CN 117147617A
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- 230000005496 eutectics Effects 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000010438 heat treatment Methods 0.000 claims abstract description 37
- 238000012360 testing method Methods 0.000 claims abstract description 28
- 238000001816 cooling Methods 0.000 claims abstract description 16
- 238000012937 correction Methods 0.000 claims abstract description 12
- 230000008018 melting Effects 0.000 claims abstract description 12
- 238000002844 melting Methods 0.000 claims abstract description 12
- 238000007711 solidification Methods 0.000 claims abstract description 7
- 230000008023 solidification Effects 0.000 claims abstract description 7
- 230000005855 radiation Effects 0.000 claims description 11
- 230000000087 stabilizing effect Effects 0.000 claims description 7
- 230000007704 transition Effects 0.000 claims description 7
- 238000013459 approach Methods 0.000 claims description 2
- 230000001595 contractor effect Effects 0.000 claims description 2
- 230000010076 replication Effects 0.000 claims description 2
- 238000005336 cracking Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 description 6
- 230000006641 stabilisation Effects 0.000 description 4
- 238000011105 stabilization Methods 0.000 description 4
- 238000009529 body temperature measurement Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000013213 extrapolation Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
- G01N25/12—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering of critical point; of other phase change
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
- G01N25/04—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering of melting point; of freezing point; of softening point
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Pathology (AREA)
- Measuring Temperature Or Quantity Of Heat (AREA)
Abstract
The invention discloses a high-temperature eutectic point reproduction method, and belongs to the technical field of temperature standards. The implementation method of the invention comprises the following steps: the reproduction process is divided into a heating section 1, a heating section 2, a correction section, a reproduction melting section, a reproduction solidifying section and a cooling section 6. The starting temperature, the ending temperature and the heating/cooling rate of each stage are different, the reliability of the reproduction test is improved by adjusting the parameters, the crucible cracking risk is reduced while the high-quality reproduction result is obtained, and the high-temperature eutectic point reproduction parameter adjusting method comprises the steps of adjusting and controlling the parameter range, constructing a parameter correction model, quantitatively adjusting and controlling, and the like. If a single test is needed to be repeated for a plurality of times, repeating the operation of the melting section after the solidification section is repeated according to the test requirement until the number of times of the repeated operation required by the test is completed. The invention can realize the reproduction of the high-temperature eutectic point and is used for carrying out the reproduction test on various high-temperature eutectic points. The invention has the advantages of good reproduction quality and high crucible safety.
Description
Technical Field
The invention relates to a high-temperature eutectic point reproduction method which is used for carrying out reproduction tests on various high-temperature eutectic points and belongs to the technical field of temperature standards.
Background
The high-temperature eutectic point is used as a key technology of a next generation temperature scale, a plurality of high-temperature region reference temperature points are added on the basis of the existing ITS-90 temperature scale, the calibration of a standard radiation thermometer is changed from extrapolation to linear interpolation, and the uncertainty of the high Wen Ouliang transmission is greatly reduced. The high-temperature eutectic point technology is divided into a pouring technology, a repeating technology and the like, wherein the pouring technology mainly comprises the production of a high-temperature eutectic point, and the high-temperature eutectic point crucible meeting the repeating requirement is produced by reasonably designing a crucible structure, a pouring method and the like. The nominal temperature of the eutectic point is accurately realized in the repetition prior art, and the method is used for calibration, calibration and the like of a standard radiation thermometer.
At present, in order to ensure that high-temperature eutectic points manufactured in each country have the capability of performing international comparison, CCT-WG5 (international temperature consultation committee radiation temperature measurement working group) puts forward specific requirements on main structure and key size of a crucible, characteristics of pouring materials and the like, and in the aspect of the reproduction technology, only specific requirements on specific temperature points, such as a lower platform temperature point, an upper platform temperature point and the like, are put forward, but the whole reproduction process has no specific requirements. The reason for this is mainly that the performance of the reproduction devices adopted by the metering mechanisms is different, and the control method, the reproduction parameter setting and the like are different, so that the reproduction method is changed greatly. The good reproduction method has important significance for the reproduction quality of the eutectic point temperature, overcoming the inherent defects of the reproduction device, reducing the risk of crucible breakage and the like.
Disclosure of Invention
Aiming at a graphite heating-radiation thermometer temperature-control type reproduction device commonly used in high-temperature eutectic point reproduction, the invention mainly aims to provide a high-temperature eutectic point reproduction method which can realize high-temperature eutectic point reproduction and is used for carrying out reproduction tests on various high-temperature eutectic points for radiation temperature measurement. The invention has the advantages of good reproduction quality and high crucible safety.
The aim of the invention is achieved by the following technical scheme.
The invention discloses a high-temperature eutectic point reproduction method, which comprises a reproduction process, wherein the reproduction process comprises 6 stages of a heating stage 1, a heating stage 2, a correction stage, a reproduction melting stage, a reproduction solidification stage and a cooling stage. The starting and ending temperatures and the heating/cooling rates of each stage are different, and by adjusting the parameters, the reliability of the reproduction test can be improved, and the crucible breakage risk is reduced while the high-quality reproduction result is obtained.
The invention discloses a high-temperature eutectic point reproduction method which comprises the following steps:
before the test starts, the high-temperature eutectic point crucible is placed at the center of a furnace tube of the reproduction device, a standard photoelectric pyrometer is used for aiming the high-temperature eutectic point crucible for the first time before heating, and the aiming position of the photoelectric pyrometer is focused to the position of a blackbody cavity opening of the crucible.
Starting the reproduction device, and heating by adjusting the parameter setting of the temperature control instrument. The initial temperature of the heating section 1 is room temperature, the final temperature is 750 ℃ (the display value of the temperature-control radiation thermometer), the heating rate is less than or equal to 15 ℃/min, and after the temperature reaches the final temperature, the standard photoelectric pyrometer is used for aiming the high-temperature eutectic point crucible for the second time, so that aiming deviation caused by the heat expansion and cold contraction effect is reduced.
After aiming, heating is continued, and the mixture enters a heating section 2, wherein the initial temperature is 750 ℃. The ending temperature is 100 ℃ (the display value of the temperature-controlled radiation thermometer) lower than the nominal phase transition temperature of the eutectic point, namely the initial correction temperature, and the heating rate is less than or equal to 25 ℃/min.
After the initial correction temperature is reached, the correction stage is entered. The standard photoelectric pyrometer indication value T needs to be read Photoelectric device And a temperature-controlled radiation thermometer indicating value T Temperature control The two can have larger difference, and the target temperature of the temperature control device is slightly increased for a plurality of times to ensure that T is Photoelectric device Continuously approaches the temperature T of the lower platform (20 ℃ below the nominal phase transition temperature of the eutectic point) Lower platform And finally let T Photoelectric device ＝T Lower platform At the moment, the indication value of the temperature-control radiation thermometer is T Lower platform temperature control 。
When the standard photoelectric pyrometer indication value reaches T Lower platform And stabilizing until the melting stage is repeated, wherein the termination temperature is the upper platform temperature T Upper platform (typically 20 ℃ C. Above the eutectic point name phase transition temperature, according to the test)Requiring adjustment). Adjusting the temperature of the temperature controller of the reproduction device to be T Upper platform temperature control Wherein T is Upper platform temperature control ＝T Lower platform temperature control +(T Upper platform -T Lower platform ). The heating rate is the highest rate of the equipment, namely, the limitation of the heating rate is released, and the fastest heating capacity of the reproduction device is exerted. Standard photoelectric pyrometer indication value reaches T Upper platform Then, the temperature controller of the reproduction device is adjusted to be T Lower platform temperature control And entering a reproduction solidification stage, wherein the cooling rate is the highest rate of the equipment, namely, the limitation of the cooling rate is relieved, and the fastest cooling capacity of the reproduction device is exerted. When the standard photoelectric pyrometer indication number reaches T Lower platform After that, a reproduction test is completed.
When the standard photoelectric pyrometer indication value reaches T Lower platform And stabilizing until the repeated melting stage is entered, preferably, the stabilizing time is in the range of 10min to 15min.
If a single test is needed to be repeated for a plurality of times, repeating the operation of the melting section after the solidification section is repeated according to the test requirement until the number of times of the repeated operation required by the test is completed.
After the reproduction test is completed, the temperature controller of the reproduction device is adjusted to be set at room temperature, and the temperature is reduced to be less than or equal to 15 ℃/min. And (5) after the temperature in the furnace reaches the room temperature, turning off the power supply, and ending the high-temperature eutectic point reproduction test.
The beneficial effects are that:
according to the high-temperature eutectic point reproduction method disclosed by the invention, the characteristics of the high-temperature eutectic point crucible and the high-temperature eutectic point reproduction method are analyzed, the reproduction process is divided into 6 stages of a heating stage 1, a heating stage 2, a correction stage, a reproduction melting stage, a reproduction solidification stage and a cooling stage, the reliability of a reproduction test can be improved by adjusting the starting and ending temperature, the heating/cooling rate and other parameters of each stage and combining time sequence control, and the crucible cracking risk is reduced while the high-quality reproduction result is obtained.
Drawings
Fig. 1 is a stage division flow chart of a high-temperature eutectic point reproduction method disclosed by the invention.
FIG. 2 is a schematic diagram of the high temperature eutectic point replication system.
Detailed Description
In order to facilitate understanding of the invention, embodiments of the invention are described below, and it should be understood by those skilled in the art that the following description is provided for convenience of explanation of the invention and is not intended to limit the scope thereof in any way.
Taking the Co-C high temperature eutectic point as an example (the nominal phase transition temperature is 1324 ℃).
As shown in fig. 1, the implementation method of the high-temperature eutectic point reproduction method disclosed in the embodiment is as follows:
before the test starts, the high-temperature eutectic point crucible is placed at the center of a furnace tube of the reproduction device, a standard photoelectric pyrometer is used for aiming the high-temperature eutectic point crucible for the first time before heating, and the aiming position of the photoelectric pyrometer is focused to the position of a blackbody cavity opening of the crucible. Starting the reproduction device, and heating by adjusting the parameter setting of the temperature control instrument. The initial temperature of the heating section 1 is room temperature, the final temperature is 750 ℃ (the display value of a temperature-control radiation thermometer), the heating rate is less than or equal to 15 ℃/min, the standard photoelectric pyrometer is used for aiming the high-temperature eutectic point crucible for the second time after the final temperature is reached, the temperature-control instrument of the reproduction device is set to 1224 ℃ after the completion, and the heating rate of entering the heating section 2 is less than or equal to 25 ℃/min. And after reaching the set temperature, entering a correction section.
At this time, the measured value of the standard photoelectric pyrometer is 1268 ℃, the temperature controller of the reproduction device is set to 1246 ℃, and the temperature is raised at a rate of less than or equal to 25 ℃/min.
After stabilization, the measured value of the standard photoelectric pyrometer is 1286 ℃, the temperature controller of the reproduction device is 1262 ℃, and the temperature is raised at the speed of less than or equal to 25 ℃/min.
After stabilization, the measured value of the standard photoelectric pyrometer is 1301 ℃, the temperature of the reproduction device is 1265 ℃, and the temperature is raised at the speed of less than or equal to 25 ℃/min.
After stabilization, the measured value of the standard photoelectric pyrometer is 1303 ℃, the temperature of the reproduction device is 1266 ℃, and the temperature is raised at a rate of less than or equal to 25 ℃/min.
After stabilization, the measured value of the standard photoelectric pyrometer is 1304 ℃, namely the lower platform temperature (20 ℃ below the Co-C eutectic point name phase transition temperature), then T is the temperature Lower platform temperature control 1266 ℃, assuming that the upper platform temperature required by the test is 20 ℃ higher than the Co-C eutectic point name phase transition temperature, T is Upper platform temperature control Was 1306 ℃.
After stabilizing for 10min, the temperature rise rate limit of the reproduction device is released, the reproduction device thermometer is set to 1306 ℃, the reproduction melting stage is carried out, and the measurement data are continuously recorded by using a standard photoelectric pyrometer. When the measured value of the photoelectric pyrometer reaches 1344 ℃, the temperature of the reproduction device is set to 1266 ℃, the reproduction solidification stage is carried out, and the standard photoelectric pyrometer is used for continuously recording the measured data. After the photoelectric pyrometer measurement reached 1304 ℃, a repeat test was completed.
The test needs to be continuously repeated for 4 times, and the operation is repeated for 3 times, so that 4 groups of reproduction curves can be obtained, and the crucible cracking risk can be reduced while the high-quality reproduction result can be obtained.
Setting the temperature meter of the reproduction device to 25 ℃ (room temperature) after the test is finished, wherein the cooling rate is less than or equal to 15 ℃/min, and turning off the power supply and other auxiliary equipment after the furnace temperature is reduced to the room temperature, so that the test is finished.
While the foregoing is directed to embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.
Claims (2)
1. A high-temperature eutectic point reproduction method is characterized in that: dividing the reproduction process into 6 stages of a heating stage 1, a heating stage 2, a correction stage, a reproduction melting stage, a reproduction solidifying stage and a cooling stage;
before the test starts, the high-temperature eutectic point crucible is placed at the center of a furnace tube of the reproduction device, a standard photoelectric pyrometer is used for aiming the high-temperature eutectic point crucible for the first time before heating, and the aiming position of the photoelectric pyrometer is focused to the position of a blackbody cavity opening of the crucible;
starting the reproduction device, and heating by adjusting the parameter setting of the temperature control instrument; the initial temperature of the heating section 1 is room temperature, the final temperature is 750 ℃, the heating rate is less than or equal to 15 ℃/min, and after the final temperature is reached, a standard photoelectric pyrometer is used for aiming the high-temperature eutectic point crucible for the second time, so that aiming deviation caused by the thermal expansion and contraction effect is reduced;
after aiming, continuing heating, and entering a heating section 2, wherein the initial temperature is 750 ℃; the termination temperature is 100 ℃ lower than the nominal phase transition temperature of the eutectic point, namely the initial correction temperature, and the heating rate is less than or equal to 25 ℃/min;
after the initial correction temperature is reached, a correction stage is entered; the standard photoelectric pyrometer indication value T needs to be read Photoelectric device And a temperature-controlled radiation thermometer indicating value T Temperature control The two can have larger difference, and the target temperature of the temperature control device is slightly increased for a plurality of times to ensure that T is Photoelectric device Continuously approaches the lower platform temperature T Lower platform And finally let T Photoelectric device ＝T Lower platform At the moment, the indication value of the temperature-control radiation thermometer is T Lower platform temperature control ；
When the standard photoelectric pyrometer indication value reaches T Lower platform And stabilizing until the melting stage is repeated, wherein the termination temperature is the upper platform temperature T Upper platform The method comprises the steps of carrying out a first treatment on the surface of the Adjusting the temperature of the temperature controller of the reproduction device to be T Upper platform temperature control Wherein T is Upper platform temperature control ＝T Lower platform temperature control +(T Upper platform -T Lower platform ) The method comprises the steps of carrying out a first treatment on the surface of the The heating rate is the highest rate of the equipment, namely the limitation of the heating rate is released, and the fastest heating capacity of the reproduction device is exerted; standard photoelectric pyrometer indication value reaches T Upper platform Then, the temperature controller of the reproduction device is adjusted to be T Lower platform temperature control Entering a reproduction solidification stage, wherein the cooling rate is the highest rate of the equipment, namely, the limitation of the cooling rate is relieved, and the fastest cooling capacity of the reproduction device is exerted; when the standard photoelectric pyrometer indication number reaches T Lower platform After that, a reproduction test is completed;
if the test needs to be repeated continuously for a plurality of times, repeating the operation after completing one repetition, re-entering the repeated melting stage, and starting the next repetition;
after the reproduction test is finished, adjusting a temperature controller of the reproduction device to be at room temperature, and entering a cooling stage, wherein the cooling rate is less than or equal to 15 ℃/min; and (5) after the temperature in the furnace reaches the room temperature, turning off the power supply, and ending the high-temperature eutectic point reproduction test.
2. A method of high temperature eutectic point replication as claimed in claim 1, wherein: when the standard photoelectric pyrometer indication value reaches T Lower platform Stabilizing until the melting stage is repeated, wherein the stabilizing time range is 10-15 min; .
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| CN202310689235.5A CN117147617A (en) | 2023-06-12 | 2023-06-12 | High-temperature eutectic point reproduction method |
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| CN202310689235.5A CN117147617A (en) | 2023-06-12 | 2023-06-12 | High-temperature eutectic point reproduction method |
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