CN117420174A - Controllable sample injection high-temperature steam atmosphere experiment system and method - Google Patents
Controllable sample injection high-temperature steam atmosphere experiment system and method Download PDFInfo
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- CN117420174A CN117420174A CN202311383943.2A CN202311383943A CN117420174A CN 117420174 A CN117420174 A CN 117420174A CN 202311383943 A CN202311383943 A CN 202311383943A CN 117420174 A CN117420174 A CN 117420174A
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- 238000002474 experimental method Methods 0.000 title claims abstract description 58
- 238000002347 injection Methods 0.000 title claims abstract description 22
- 239000007924 injection Substances 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 66
- 239000007789 gas Substances 0.000 claims abstract description 54
- 238000006243 chemical reaction Methods 0.000 claims abstract description 36
- 229910052786 argon Inorganic materials 0.000 claims abstract description 33
- 239000000919 ceramic Substances 0.000 claims abstract description 32
- 238000009529 body temperature measurement Methods 0.000 claims abstract description 29
- 238000005259 measurement Methods 0.000 claims abstract description 18
- 239000000523 sample Substances 0.000 claims description 76
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 229910052593 corundum Inorganic materials 0.000 claims description 17
- 239000010431 corundum Substances 0.000 claims description 17
- 238000012544 monitoring process Methods 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 7
- 230000005540 biological transmission Effects 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000005516 engineering process Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 13
- 238000007254 oxidation reaction Methods 0.000 abstract description 7
- 230000003647 oxidation Effects 0.000 abstract description 5
- 239000011261 inert gas Substances 0.000 abstract 1
- 238000005253 cladding Methods 0.000 description 16
- 238000010586 diagram Methods 0.000 description 5
- 230000001276 controlling effect Effects 0.000 description 4
- 229910001093 Zr alloy Inorganic materials 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000013480 data collection Methods 0.000 description 2
- 230000005496 eutectics Effects 0.000 description 2
- PXXKQOPKNFECSZ-UHFFFAOYSA-N platinum rhodium Chemical compound [Rh].[Pt] PXXKQOPKNFECSZ-UHFFFAOYSA-N 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000013401 experimental design Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000013011 mating Effects 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 238000004154 testing of material Methods 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
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01D—MEASURING NOT SPECIALLY ADAPTED FOR A SPECIFIC VARIABLE; ARRANGEMENTS FOR MEASURING TWO OR MORE VARIABLES NOT COVERED IN A SINGLE OTHER SUBCLASS; TARIFF METERING APPARATUS; MEASURING OR TESTING NOT OTHERWISE PROVIDED FOR
- G01D21/00—Measuring or testing not otherwise provided for
- G01D21/02—Measuring two or more variables by means not covered by a single other subclass
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- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
A controllable sample injection high-temperature steam atmosphere experiment system and method, the system includes a gas supply system, an experiment section, an experiment sample moving system, an infrared temperature measuring system; the gas supply system can supply steam and argon with different flow rates to the experimental section, and provides a steam environment or an inert gas environment for the experimental section; the experimental section consists of a horizontal tube furnace and a ceramic reaction tube, wherein the horizontal tube furnace can provide a high-temperature environment of 1750 ℃ for the ceramic reaction tube; the sample moving system can accurately and stably control the speed and the position of the experimental sample entering and exiting the experimental section; the infrared temperature measurement system can accurately measure the temperature of the outer surface of the experimental sample in a non-contact manner; the experiment system also comprises a power distribution system, a numerical control system and a data measurement and acquisition system; the invention also provides an experimental method; the invention provides key data for steam oxidation kinetics, oxidation behavior, high-temperature performance and the like of the material by carrying out high-temperature steam atmosphere experiments of the high-temperature resistant material.
Description
Technical Field
The invention relates to the technical field of high-temperature oxidation resistance testing of materials, in particular to a controllable sample injection high-temperature steam atmosphere experiment system and method.
Background
Under the high-temperature steam environment, the material can undergo various chemical and physical changes such as oxidation, corrosion, volatilization, gas phase reaction and the like, and the mechanical strength, microstructure, fatigue life and other performances of the material can be changed, so that negative effects are generated. Therefore, the application of the high-temperature resistant material in the steam environment needs to be subjected to experimental research in advance, namely, the experimental equipment is used for simulating the high-temperature steam environment under the actual working condition, the high-temperature performance and the behavior of the material in the steam atmosphere are researched, and data or model support is provided for the development and the application of the high-temperature resistant material so as to ensure that the material can maintain the performance and the durability of the material in the high-temperature steam environment.
At present, a high-temperature steam atmosphere experiment system used at home and abroad mostly adopts an induction heating or infrared heating mode to heat a sample, a thermocouple is used for measuring the temperature of a material, and the material enters and exits a high-temperature experiment section by manual control. However, in a high temperature environment, oxidation reaction or eutectic reaction may occur between the thermocouple and the material, for example, the Cr metal of the Cr coating Zr alloy cladding and the platinum metal in the platinum-rhodium thermocouple may undergo eutectic reaction at about 1550 ℃, which affects the high temperature oxidation reaction process of the Cr coating Zr alloy cladding and may also cause the platinum-rhodium thermocouple to fail. In addition, when a material high-temperature steam experiment is performed, the moving speed of a sample from room temperature to a high-temperature section can influence the heating speed of the sample, further influence the oxidation speed of the sample, and the uncertainty of the high-temperature steam experiment result can be improved by manually controlling the speed of the sample to enter and exit the high-temperature section, particularly in a short-time experiment. Therefore, improvement on the temperature measurement mode and the sample injection system of the current high-temperature steam atmosphere experimental device is needed.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention aims to provide a controllable sample injection high-temperature steam atmosphere experiment system and method, which can perform stable, accurate and long-time high-temperature experiments on experimental samples in a steam environment, accurately control the rate of the experimental samples entering the high temperature from room temperature, and adopt a non-contact measurement method on the temperature of the experimental samples.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the utility model provides a controllable advance kind high temperature steam atmosphere experimental system, includes steam generator 1, and steam generator 1 passes through first valve 101 and links to each other with the steam trunk line, and the steam trunk line has installed first flowmeter 601 and first thermocouple 701, and check valve 201 and corresponding pipeline link to each other with external water source and provide deionized water for steam generator 1, still installs fluviograph 301, relief valve 401 and manometer 501 on the steam generator; the first argon gas bottle 2 is connected with an argon main pipeline through a second valve 102 and a corresponding pipeline, the second argon gas bottle 3 is connected with the argon main pipeline through a second valve 103 and a corresponding pipeline, a second flowmeter 602, a pressure sensor 801 and a second thermocouple 702 are arranged on the argon main pipeline, the steam main pipeline and the argon main pipeline are combined to form a gas main pipeline, a third thermocouple 703 is arranged on the gas main pipeline and used for measuring and monitoring the gas temperature in the gas main pipeline, and a fourth valve 104 is used for controlling the gas flow of the gas main pipeline; the tail end of the main gas pipeline is connected to a ceramic reaction tube 4 of a horizontal tube furnace 7, a base 5 positioned at the constant temperature section of the ceramic reaction tube 4 is used for receiving and supporting an experimental sample 6, the experimental sample 6 is used for simulating an envelope, and the experimental sample 6 is longitudinally placed on the base 5; the movement of the experimental sample 6 and the base 5 in the ceramic reaction tube 4 depends on a corundum rod 8 connected with the base 5, the corundum rod 8 is fixed on a linear sliding table 9, and the direction of a guide rail of the linear sliding table 9 and the axial direction of the corundum rod 8 are parallel to the axial direction of the ceramic reaction tube 4; wherein, the horizontal tube furnace and the ceramic reaction tube form an experimental section; the temperature of the experimental sample 6 is measured by adopting an infrared thermometer 10, and the probe of the infrared thermometer 10 points to the central position of the experimental sample 6; the guide rail of the linear sliding table 9 is automatically controlled by a stepping motor driver 11, a controller 12 and a power supply 13 which are externally connected;
the experimental system also includes a mating power distribution system 14, a numerical control system 15, and a data measurement and acquisition system 16.
The infrared thermometer 10 adopts a bicolor infrared temperature measurement technology.
The power distribution system 14 comprises a power distribution cabinet, a power transmission line and electric equipment which are sequentially connected, and the power supply capacity meets the power consumption requirement of the experiment system; the numerical control system 15 comprises a gas supply system starting control platform, an experimental sample moving control platform, an experimental section starting control platform and an infrared temperature measurement control platform; the data measurement and acquisition system 16 comprises a data acquisition card, a measurement module and a signal conditioner which are connected with an experimental loop sensor, namely a pressure sensor, three thermocouples, an infrared thermometer flowmeter and a water level gauge through junction boxes, and computer driving software and data acquisition software for driving the data acquisition card, the measurement module and the signal conditioner to operate; the numerical control system 15 can control the opening of the valve and the start and stop of the instrument according to the experimental flow and the signal feedback of the data measurement and acquisition system 16, and adjust the power of the instrument.
The guide rail of the linear sliding table 9 adopts an SGK ball screw.
The experimental method of the controllable sample injection high-temperature steam atmosphere experimental system can be used for carrying out high-temperature steam atmosphere experiments; before the experiment starts, all valves are kept normally closed, and the mass of an experimental sample is obtained by adopting a high-precision electronic balance; setting a temperature-raising program of the horizontal tube furnace 7, wherein the program comprises an initial temperature, a temperature-raising time, a target temperature and a heat-preserving time, so that the horizontal tube furnace 7 is slowly heated to the target temperature and then is subjected to long-time heat preservation; when a high-temperature steam atmosphere experiment is carried out, the one-way valve 201 is opened, plasma water is injected into the steam generator 1 from an external water source, the deionized water amount is observed through the water level gauge 301, water injection is stopped after the experiment requirement is met, and the one-way valve 201 is closed; starting the steam generator 1, when the pressure gauge 501 reaches a specified value, starting to generate steam, opening the first valve 101 to lead the steam to the main gas pipe from the main gas pipe, opening the fourth valve 104, leading the steam to the ceramic reaction pipe 4 from the main gas pipe, wherein the temperature of the steam is influenced by the high temperature of the ceramic reaction pipe 4 to rise, measuring and monitoring the temperature of the steam through the first thermocouple 701 and the third thermocouple 703, and respectively monitoring and controlling the steam flow of the main gas pipe through the first flowmeter 601 and the fourth valve 104; after the temperature of the horizontal tube furnace 7 reaches the target temperature, vertically placing a temperature measurement sample on a base 5 connected with a corundum rod 8, and stably pushing the base 5 and the temperature measurement sample onto a constant temperature area of a ceramic reaction tube 4 by using a linear sliding table 9 and the corundum rod 8; the infrared thermometer 10 is opened to aim at a temperature measurement sample for temperature measurement, the temperature difference exists between the measured temperature and the set temperature due to the radial temperature difference of the ceramic reaction tube 4, the set heat preservation temperature of the horizontal tube furnace 7 is adjusted, after the measured temperature reaches the experimental temperature, the temperature measurement sample is replaced by the experimental sample 6, the moving speed and the end position of the linear sliding table 9 on the guide rail are set, and the experimental sample 6 is pushed to the same position as the temperature measurement by the linear sliding table 9; after the appointed time, the second valve 102 and the third valve 103 are immediately opened, the first valve 101 is closed, argon is introduced into the main argon pipeline, so that the experimental sample 6 is isolated from steam, and the experimental sample 6 is moved out by the linear sliding table 9 and cooled at room temperature; after all the samples are tested, all valves are closed, a cooling program of the horizontal tube furnace 7 is set, the temperature of the ceramic reaction tube 4 is reduced to room temperature at a specified rate, all the instruments and equipment are closed in sequence, and the experiment is finished;
and after the experiment is finished, obtaining the mass of the experimental sample again by adopting a high-precision electronic balance, and microcosmically characterizing the outer surface and the cross section of the experimental sample by adopting a scanning electron microscope, a transmission electron microscope and an X-ray diffractometer.
Compared with the prior art, the invention has the following advantages:
1. the linear sliding table and the corundum rod are used for driving the base and the cladding to axially move in the ceramic reaction tube, the linear guide rail is automatically controlled, the moving speed of the sliding table is stable and can be adjusted according to experimental requirements, so that the speed of the cladding entering and exiting the constant temperature section of the horizontal tube furnace is stable and controllable, and the interference of human factors is reduced.
2. The base can be used for receiving fragments or melts generated in the experimental process of the high-temperature steam atmosphere of the cladding, so that the ceramic reaction tube is prevented from being damaged; the cladding is longitudinally placed, so that the reaction area of the cladding can be increased, and the infrared thermometer is convenient for measuring the temperature.
3. According to the experimental system, a high-temperature steam atmosphere experiment is carried out on an experimental sample by adopting the horizontal tube furnace, the horizontal tube furnace can be used for a long time at the temperature of 1750 ℃, and the large steam flow and the high steam purity can be realized.
4. The non-contact temperature measurement mode is adopted, the infrared thermometer is used for measuring the temperature of the cladding, and compared with the mode of using the thermocouple to measure the temperature on the outer surface of the cladding, the temperature measurement mode has no influence on the reaction of the outer surface of the cladding, and the operation is simple and convenient.
In summary, the invention improves the controllable sample injection high-temperature steam atmosphere experiment system and method, and has reliable design, simple and convenient operation, safety and stability.
Drawings
FIG. 1 is a schematic diagram of a controllable sample injection high temperature steam atmosphere experiment system according to the present invention.
Fig. 2 is a schematic diagram of a power distribution system of the controllable sample injection high-temperature steam atmosphere experiment system of the invention.
FIG. 3 is a schematic diagram of a numerical control system of the controllable sample injection high temperature steam atmosphere experiment system of the invention.
Fig. 4 is a schematic diagram of a data measurement and acquisition system of the controllable sample injection high temperature steam atmosphere experimental system of the invention.
FIG. 5 is a schematic diagram of the operation mode of the numerical control system of the controllable sample injection high-temperature steam atmosphere experiment system and the method of the invention.
Detailed Description
The invention is described in detail below with reference to the attached drawings and detailed description:
as shown in fig. 1, the controllable sample injection high-temperature steam atmosphere experiment system comprises a gas supply system, an experiment section, an experiment sample moving system, an infrared temperature measurement system, a matched power distribution system 14, a numerical control system 15 and a data measurement and acquisition system 16; the gas supply system comprises a steam supply system and an argon gas supply system; in the steam supply system, the steam generator 1 is connected with the steam main pipeline through the first valve 101, a first flowmeter 601 is arranged on the steam main pipeline and used for measuring steam flow in the steam main pipeline, and a first thermocouple 701 is used for measuring and monitoring steam temperature in the steam main pipeline, so that the steam main pipeline and the gas main pipeline are prevented from being damaged due to overhigh steam temperature. The steam generator 1 is connected to an external water source through a check valve 201 to supply deionized water to the steam generator 1, and the water level in the steam generator 1 is observed through a water level gauge 301 connected to the steam generator. Also connected to the steam generator 1 are a pressure gauge 501 and a safety valve 401 for measuring the pressure and overpressure protection, respectively, in the steam generator 1. In the argon gas supply system, a first argon gas cylinder 2 is connected with an argon gas main pipeline through a second valve 102 and a corresponding pipeline, a second argon gas cylinder 3 is connected with the argon gas main pipeline through a third valve 103 and a corresponding pipeline, a second flowmeter 602, a pressure sensor 801 and a second thermocouple 702 are arranged on the argon gas main pipeline and are respectively used for measuring the argon gas flow, the pressure and the temperature of the argon gas main pipeline, and the second argon gas cylinder 3 has the function of timely supplementing argon gas when the argon gas amount in the first argon gas cylinder 2 is insufficient, so that stable experiment performance is ensured; the gas supply system provides steam and argon for the experimental section through a main gas pipe, on which a fourth valve 104 is installed to control the flow rate of the gas supply, and a third thermocouple 703 is installed to measure and monitor the temperature of the main gas pipe. The horizontal tube furnace 7 of the experimental section heats the ceramic reaction tube 4 to a target temperature, and a stable high-temperature steam environment is provided for the experimental sample 6 at the constant-temperature section part of the ceramic reaction tube 4; the experimental sample moving system comprises a base 5, a corundum rod 8 and a linear sliding table 9, wherein the base 5 is connected with the corundum rod 8, the corundum rod 8 is fixed on the linear sliding table 9, and the corundum rod 8 drives the base 5 to axially move in the ceramic reaction tube 4. The linear sliding table 9 adopts automatic control, so that the speed and the position of the cladding moving from the room temperature to the constant temperature section can be accurately controlled, the interference of human factors on the temperature rising speed of the cladding is avoided, and the temperature rising speed of the cladding can influence the reaction speed of the cladding in a high-temperature steam environment. The infrared thermometer 10 of the infrared temperature measuring system is used for performing non-contact temperature measurement on the experimental sample 6, and the central position of the outer surface of the experimental sample 6 is precisely measured by controlling the head-up position, the head-up direction, the head-up focal length and other parameters of the infrared thermometer 10. The guide rail of the linear sliding table 9 adopts an SGK ball screw, and is automatically controlled by a stepping motor driver 11, a controller 12 and a power supply 13 which are externally connected, so that the forward and backward movement rate and the cladding position of the sliding table can be accurately controlled.
The infrared thermometer 10 adopts a bicolor infrared temperature measurement technology, and utilizes the ratio of infrared radiation energy of two wavebands of adjacent channels to determine the temperature, so that the influences of water vapor, dust, size change of a detection target, partial shielding, emissivity change and the like can be eliminated, and the surface temperature of the experimental sample 6 can be accurately measured.
As shown in fig. 2, as a preferred embodiment of the present invention, the power distribution system 14 mainly includes a power distribution cabinet, a power transmission line and electric equipment which are sequentially connected; the power supply capacity of the power distribution system 14 meets the power consumption requirement of an experiment system, and provides working power for the steam generator 1, the horizontal tube furnace 7, the linear sliding table 9, the infrared thermometer 10, the numerical control system 15, the data measurement and acquisition system 16 and the like.
As shown in fig. 3, as a preferred embodiment of the present invention, the numerical control system 15 mainly includes a gas supply system start control platform, an experiment section start control platform, an experiment sample movement control platform and an infrared temperature measurement control platform, and specific components include a valve controller, a switch controller, a power controller and a function controller; the opening degree of all valves is controlled by a valve controller, all measuring instruments, the steam generator 1, the horizontal tube furnace 7, the linear sliding table 9 and the infrared thermometer 10 are controlled to start and stop by a switch controller, and the power of the steam generator 1 is regulated by a power controller; the position, the moving direction and the speed of the linear sliding table are controlled by the functional controller, and the focal length, the temperature measuring mode and the probe position of the infrared thermometer are controlled.
As shown in fig. 4, as a preferred embodiment of the present invention, the data measurement and collection system 16 mainly includes a data collection card, a measurement module and a signal conditioner connected to the experimental loop sensor, i.e., the pressure sensor, three thermocouples, an infrared thermometer flowmeter and a water level gauge through a junction box, and computer driving software and data collection software for driving the data collection card, the measurement module and the signal conditioner to operate; the thermocouple, the flowmeter, the pressure sensor, the water level gauge and the infrared thermometer convert physical parameters into electric signals, the electric signals are transmitted to the signal conditioner for filtering and setting through the junction box, the electric signals are converted into digital signals by the measuring module and the data acquisition card, the digital signals are provided for driving software and data acquisition software of a computer, and signals of all sensors are processed and displayed by a program compiled by LabView.
As shown in fig. 5, as a preferred embodiment of the present invention, the numerical control system 15 may receive the flow, temperature, pressure, and water level signals of the data measurement and acquisition system 16, compare the signals with experimental design parameters, generate feedback signals, and control the opening of the valve and the start and stop of the equipment according to the experimental procedure, and adjust the power of the equipment.
The experimental method of the system and the method for the controllable sample injection high-temperature steam atmosphere experiment can be used for carrying out the high-temperature steam atmosphere experiment. Before the experiment starts, all valves are kept normally closed, and the mass of the experimental sample is obtained by adopting a high-precision electronic balance. Setting a temperature raising program of the horizontal tube furnace 7, wherein the temperature raising program comprises an initial temperature, a temperature raising time, a target temperature and a heat preservation time, so that the horizontal tube furnace 7 is slowly raised to the target temperature and then keeps a stable temperature in the whole experiment process.
When a high-temperature steam atmosphere experiment is carried out, the one-way valve 201 is opened, plasma water is injected into the steam generator 1 from an external water source, the deionized water amount is observed through the water level gauge 301, water injection is stopped after the experiment requirement is met, and the one-way valve 201 is closed; after the pressure gauge 501 reaches a specified value, the steam generator 1 is started, steam starts to be generated, the first valve 101 is opened to enable the steam to be led to the gas main pipeline from the gas main pipeline, the fourth valve 104 is opened, the gas main pipeline is led to the ceramic reaction pipe 4, the temperature of the steam is influenced by the high temperature of the ceramic reaction pipe 4 to rise, the temperature of the steam is measured and monitored through the first thermocouple 701 and the third thermocouple 703, and the steam flow of the main pipeline is monitored and controlled through the first flowmeter 601 and the fourth valve 104 respectively. After the temperature of the horizontal tube furnace 7 reaches the target temperature, vertically placing a temperature measurement sample on a base 5 connected with a corundum rod 8, and stably pushing the base 5 and the temperature measurement sample onto a constant temperature area of a ceramic reaction tube 4 by using a linear sliding table 9 and the corundum rod 8; the infrared thermometer 10 is opened to aim at a temperature measurement sample for temperature measurement, and the temperature difference exists between the measured temperature and the set temperature due to the radial temperature difference of the ceramic reaction tube 4, the set heat preservation temperature of the horizontal tube furnace 7 is adjusted, after the measured temperature reaches the experimental temperature, the temperature measurement sample is replaced by the experimental sample 6, the moving speed and the end position of the linear sliding table 9 on the guide rail are set, and the experimental sample 6 is pushed to the same position as the temperature measurement by the linear sliding table 9. After the experimental sample 6 is subjected to isothermal standing for a designated time, the second valve 102 and the third valve 103 are immediately opened, the first valve 101 is closed, argon is introduced into the main argon pipeline, so that the experimental sample 6 is isolated from steam, and the experimental sample 6 is removed by the linear sliding table 9 and cooled at room temperature. After all the samples are tested, all valves are closed, the temperature reducing program of the horizontal tube furnace 7 is set, the temperature of the ceramic reaction tube 4 is reduced to room temperature at a specified rate, all the instruments and equipment are closed in sequence, and the experiment is finished.
And after the experiment is finished, the mass of the experimental part is obtained again by adopting a high-precision electronic balance, and microscopic characterization is carried out on the outer surface and the cross section of the cladding by adopting a scanning electron microscope, a transmission electron microscope and an X-ray diffractometer.
The foregoing is a further elaboration of the present invention in connection with the specific principles, and it is not intended that the invention be limited to the specific embodiments shown, but is to be accorded the scope of the claims without departing from the true spirit and scope of the invention.
Claims (5)
1. A controllable advance kind high temperature steam atmosphere experimental system, its characterized in that: the steam generator (1) is connected with a main steam pipeline through a first valve (101), the main steam pipeline is provided with a first flowmeter (601) and a first thermocouple (701), a one-way valve (201) and corresponding pipelines are connected with an external water source to provide deionized water for the steam generator (1), and the steam generator is also provided with a water level gauge (301), a safety valve (401) and a pressure gauge (501); the first argon gas cylinder (2) is connected with an argon main pipeline through a second valve (102) and a corresponding pipeline, the second argon gas cylinder (3) is connected with the argon main pipeline through a second valve (103) and a corresponding pipeline, a second flowmeter (602), a pressure sensor (801) and a second thermocouple (702) are arranged on the argon main pipeline, the steam main pipeline and the argon main pipeline are combined to form a gas main pipeline, a third thermocouple (703) is arranged on the gas main pipeline and used for measuring and monitoring the gas temperature in the gas main pipeline, and a fourth valve (104) is used for controlling the gas flow of the gas main pipeline; the tail end of the main gas pipeline is connected to a ceramic reaction tube (4) of a horizontal tube furnace (7), a base (5) positioned at the constant temperature section of the ceramic reaction tube (4) is used for receiving and supporting an experimental sample (6), the experimental sample (6) is used for simulating an envelope, and the experimental sample is longitudinally placed on the base (5); the movement of the experimental sample (6) and the base (5) in the ceramic reaction tube (4) depends on a corundum rod (8) connected with the base (5), the corundum rod (8) is fixed on a linear sliding table (9), and the direction of a guide rail of the linear sliding table (9) and the axial direction of the corundum rod (8) are parallel to the axial direction of the ceramic reaction tube (4); wherein, the horizontal tube furnace and the ceramic reaction tube form an experimental section; the method comprises the steps of carrying out a first treatment on the surface of the The temperature of the experimental sample (6) is measured by an infrared thermometer (10), and the probe of the infrared thermometer (10) points to the central position of the experimental sample (6); the guide rail of the linear sliding table (9) is automatically controlled by a stepping motor driver (11), a controller (12) and a power supply (13) which are externally connected;
the experimental system also comprises a matched power distribution system (14), a numerical control system (15) and a data measurement and acquisition system (16).
2. The controlled-injection high-temperature steam atmosphere experiment system according to claim 1, wherein: the infrared thermometer (10) adopts a bicolor infrared temperature measurement technology.
3. The controlled-injection high-temperature steam atmosphere experiment system according to claim 1, wherein: the power distribution system (14) comprises a power distribution cabinet, a power transmission line and electric equipment which are sequentially connected, and the power supply capacity meets the power consumption requirement of the experiment system; the numerical control system (15) comprises a gas supply system starting control platform, an experimental sample moving control platform, an experimental section starting control platform and an infrared temperature measurement control platform; the data measurement and acquisition system (16) comprises a data acquisition card, a measurement module and a signal conditioner which are connected with an experimental loop sensor, namely a pressure sensor, three thermocouples, an infrared thermometer flowmeter and a water level gauge through junction boxes, and computer driving software and data acquisition software which drive the data acquisition card, the measurement module and the signal conditioner to operate; the numerical control system (15) can control the opening of the valve and the start and stop of the instrument according to the experimental flow and the signal feedback of the data measurement and acquisition system (16), and regulate the power of the instrument.
4. The controlled-injection high-temperature steam atmosphere experiment system according to claim 1, wherein: the guide rail of the linear sliding table (9) adopts an SGK ball screw.
5. The experimental method of the controllable sample injection high-temperature steam atmosphere experimental system according to any one of claims 1 to 4, which is characterized in that: the experimental system can be used for carrying out high-temperature steam atmosphere experiments; before the experiment starts, all valves are kept normally closed, and the mass of an experimental sample is obtained by adopting a high-precision electronic balance; setting a heating program of the horizontal tube furnace (7), wherein the heating program comprises an initial temperature, heating time, a target temperature and heat preservation time, so that the horizontal tube furnace (7) is slowly heated to the target temperature and then is subjected to long-time heat preservation; when a high-temperature steam atmosphere experiment is carried out, a one-way valve (201) is opened, plasma water is injected into the steam generator (1) from an external water source, the deionized water quantity is observed through a water level gauge (301), water injection is stopped after the experiment requirement is met, and the one-way valve (201) is closed; starting a steam generator (1), when a pressure gauge (501) reaches a specified value, starting to generate steam, opening a first valve (101) to enable the steam to be led into a main gas pipeline from the main gas pipeline, opening a fourth valve (104), enabling the main gas pipeline to lead steam into a ceramic reaction pipe (4), enabling the temperature of the steam to rise under the influence of the high temperature of the ceramic reaction pipe (4), measuring and monitoring the temperature of the steam through a first thermocouple (701) and a third thermocouple (703), and respectively monitoring and controlling the steam flow of the main gas pipeline through a first flowmeter (601) and the fourth valve (104); after the temperature of the horizontal tube furnace (7) reaches the target temperature, vertically placing a temperature measurement sample on a base (5) connected with a corundum rod (8), and stably pushing the base (5) and the temperature measurement sample onto a constant temperature area of a ceramic reaction tube (4) by using a linear sliding table (9) and the corundum rod (8); the infrared thermometer (10) is opened to aim at a temperature measurement sample for measuring temperature, the temperature difference exists between the measured temperature and the set temperature due to the radial temperature difference of the ceramic reaction tube (4), the set heat preservation temperature of the horizontal tube furnace (7) is adjusted, after the measured temperature reaches the experimental temperature, the temperature measurement sample is replaced by the experimental sample (6), the moving speed and the end position of the linear sliding table (9) on the guide rail are set, and the experimental sample (6) is pushed to the same position as the temperature measurement by the linear sliding table (9); after the appointed time, the second valve (102) and the third valve (103) are immediately opened, the first valve (101) is closed, argon is introduced into the main argon pipeline, so that the experimental sample (6) is isolated from steam, and the experimental sample (6) is moved out by the linear sliding table (9) and cooled at room temperature; after all samples are tested, all valves are closed, a cooling program of a horizontal tube furnace (7) is set, the temperature of a ceramic reaction tube (4) is reduced to room temperature at a specified rate, all instruments and equipment are closed in sequence, and the experiment is ended;
and after the experiment is finished, obtaining the mass of the experimental sample again by adopting a high-precision electronic balance, and microcosmically characterizing the outer surface and the cross section of the experimental sample by adopting a scanning electron microscope, a transmission electron microscope and an X-ray diffractometer.
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