An in-situ micro-nano indentation testing system and method under ultra-high temperature water-oxygen environment

Abstract

The present invention discloses an in-situ micro-nano indentation testing system and method in an ultra-high temperature water-oxygen environment. The present invention changes the horizontally placed protective pipe in the traditional tube furnace into a vertically placed one, and the pressure rod and the sample platform enter from both ends of the vertically placed protective pipe, respectively, which not only avoids drilling holes on the pipe wall, but also avoids the use of a large-diameter protective pipe so as to use a longer pressure rod; the present invention uses a long-range slide rail, and during the water-oxygen assessment of the sample, the box is moved to a place away from the pressure rod driver through the slide rail. After the water-oxygen assessment is completed, the box is moved to the bottom of the pressure rod through the slide rail to complete the indentation test; the present invention adopts an integrated design, and can carry out in-situ micro-nano indentation testing after any water-oxygen ratio assessment of the coating sample in a high temperature environment of 1600°C, so as to realize the in-situ characterization of the mechanical properties of the coating sample in an ultra-high temperature water-oxygen environment, with high feasibility and simple operation.

Description

Technical Field

[0001] The present invention relates to an ultra-high temperature mechanical testing technology, and in particular to an in-situ micro-nano indentation testing system and a testing method thereof in an ultra-high temperature water-oxygen environment. Background Art

[0002] Increasing the turbine inlet temperature and reducing the structural weight are the key to developing the next generation of advanced aero engines and large bypass ratio civil engines. As a substitute for high temperature alloys, SiC / SiC composites have been used in commercial engines to make hot structural parts resistant to higher temperatures, among which environmental barrier coatings are the key to their successful application. Environmental barrier coatings (EBCs) are the inevitable choice to solve the long-term service of SiC / SiC hot end components in engine environments. They can effectively block the corrosion damage caused by the gas environment to SiC / SiC and avoid the sharp deterioration of the performance of the hot end components of SiC / SiC ceramic matrix composites. In order to solve the core problem of ensuring the long-life service stability of SiC / SiC composites in the complex environment of the combustion chamber, the current research on environmental barrier coatings at home and abroad mainly focuses on the characterization and optimization of the corrosion resistance of coating materials. Among them, it is particularly important to characterize the mechanical properties of SiC / SiC with environmental barrier coatings after ultra-high temperature water and oxygen environment assessment. The mechanical properties of the coating include hardness, strength, elastic modulus, fracture toughness, etc. Characterizing the mechanical properties of the coating is of great significance to the structural design, assessment index determination, health evaluation and life prediction of SiC / SiC composites with environmental barrier coatings. In particular, compared with ex-situ mechanical testing, in-situ mechanical testing can accurately characterize the mechanical performance parameters of the coating in an ultra-high temperature water and oxygen environment.

[0003] Conventionally, the mechanical properties characterization of SiC / SiC composite samples with environmental barrier coatings after ultra-high temperature water and oxygen testing is divided into two steps: the first step is to test the samples in a tube furnace in ultra-high temperature water and oxygen; the second step is to take the tested samples out of the tube furnace, transfer them to an ultra-high temperature micro-nano indentation device and fix them on the sample platform, and then characterize the mechanical properties of the samples by ultra-high temperature micro-nano indentation testing technology. In the process of transferring the samples from the tube furnace to the high temperature indentation device, changes in the temperature and position of the samples will lead to problems such as stress release. Therefore, the existing devices and experimental methods cannot characterize the mechanical properties of the samples in real service environments.

[0004] Therefore, how to characterize the in-situ mechanical properties of SiC / SiC composites with environmental barrier coatings in ultra-high temperature water and oxygen environments and provide in-situ mechanical properties parameters of the coatings for the characterization and optimization of the corrosion resistance of environmental barrier coating materials has become an important topic in the current research and development of ultra-high temperature testing instruments in China. Summary of the invention

[0005] In order to solve the technical problems of in-situ measurement, the present invention proposes an in-situ micro-nano indentation testing system and a testing method in an ultra-high temperature water and oxygen environment to complete the in-situ characterization of the mechanical properties and behaviors of SiC / SiC composite materials with environmental barrier coatings in an ultra-high temperature water and oxygen environment.

[0006] One object of the present invention is to provide an in-situ micro-nano indentation testing system in an ultra-high temperature water-oxygen environment.

[0007] The in-situ micro-nano indentation test system under ultra-high temperature water and oxygen environment of the present invention comprises: a gas generating device, an ultra-high temperature water and oxygen assessment and indentation test device and an exhaust gas treatment device; wherein the ultra-high temperature water and oxygen assessment and indentation test device comprises: an air inlet side box, an air outlet side box, a slide rail, a flat plate, a lifting support, a base, a sample platform, a platform fixing seat, an air inlet side box water cooling layer, an air outlet side box water cooling layer, an air inlet side box insulation layer, an air outlet side box insulation layer, an air inlet side box protection pipe, an air outlet side box protection pipe, a temperature sensor, a heating material, a heating device, a sealing pad, a buckle, a heat-insulating sealing device, a pressure rod driver, an outrigger, a pressure rod, a pressure head, an optical observation channel, a gas inlet pipe and a gas outlet pipe; an air inlet The inlet side box is a semi-shell structure with an opening on one side, the inner surface of the inlet side box is covered with the inlet side box water-cooling layer, the inner surface of the inlet side water-cooling layer is covered with the inlet side box insulation layer, a semi-cylindrical inlet side box protection duct is arranged in the inlet side box insulation layer, the edge of the inlet side box protection duct is located in the same plane as the edges of the inlet side box and the inlet side insulation layer; the top and bottom ends of the inlet side box protection duct are against the top and bottom ends of the inner surface of the inlet side box insulation layer; the outlet side box, the outlet side box insulation layer, the outlet side box water-cooling layer and the outlet side box protection duct are opened with the inlet side box, the inlet side box insulation layer, the inlet side box water-cooling layer and the inlet side box protection duct The two sides are arranged opposite to each other; sealing gaskets are respectively arranged on the splicing edges of the air inlet side box protection duct and the air outlet side box protection duct; a buckle is arranged at the connection between the air inlet side box and the air outlet side box; the split air inlet side box and the air outlet side box are respectively placed on the slide rails and can move along the slide rails, the slide rails are placed on the flat plate, the flat plate is placed on the lifting support, and the lifting support is placed on the base; the bottom of the sample platform is fixed to the bottom of the air inlet side box or the air outlet side box through the platform fixing seat; the air inlet side box and the air outlet side box move toward the center along the slide rail and merge to form an integrated box; the air inlet side box protection duct and the air outlet side box protection duct are spliced ​​together to form a cylindrical protection duct with a hollow interior and an upper and lower opening, and the protection duct The inside of the duct is a sealed space, the central axis of the protective duct is along the vertical direction, and the sample platform is located in the protective duct in the box; the heat insulation layer of the box on the air inlet side and the heat insulation layer of the box on the air outlet side are spliced ​​into an integrated heat insulation layer, so as to form a closed space between the inner surface of the heat insulation layer and the outer surface of the side wall of the protective duct; a temperature sensor and a heating material are arranged in the closed space, and the heating material is connected to a heating device located outside the box; a detachable heat preservation sealing device is arranged at the center of the top wall of the box body facing the sample platform; a pressure rod driver is arranged outside the box body, the pressure rod driver is fixed on the outrigger, and the outrigger is placed on the base; a pressure rod is arranged on the pressure rod driver, and a pressure head is arranged at the bottom end of the pressure rod; an optical observation channel leading to the inside of the box body is arranged on the box body on the gas outlet side;One end of the gas inlet pipeline is connected to the outlet of the gas generating device, and the other end passes through the air inlet side box, the air inlet side box water cooling layer, the air inlet side box insulation layer and the air inlet side box protection pipeline in sequence, and is connected to the protection pipeline; one end of the gas outlet pipeline is connected to the inlet of the exhaust gas treatment device, and the other end passes through the air outlet side box, the air outlet side box water cooling layer, the air outlet side box insulation layer and the air outlet side box protection pipeline in sequence, and is connected to the protection pipeline; place the sample on the sample platform, and move it along the slide rail respectively Move the air inlet side box and the air outlet side box toward the center until the two are spliced ​​into an integrated box, fasten the buckles of the air outlet side box and the air inlet side box, so that the sample is in a sealed space formed by the protective pipe connected by the sealing gasket; move the combined box as a whole along the slide rail away from the pressure rod driver; start the gas generating device to transport the water-oxygen mixed gas with a set water-oxygen ratio into the protective pipe through the gas inlet pipe, and at the same time start the exhaust gas treatment device, connect the water cooling layer of the air inlet side box and the water cooling layer of the air outlet side box Cold layer; turn on the heating device to heat the heating material, and monitor the temperature outside the protective pipe in real time through the temperature sensor, so that the inside of the protective pipe is heated to the preset temperature and maintained at the set heating rate to complete the high-temperature water and oxygen test of the sample. The heating material is located in a closed space outside the protective pipe, and is free from contact with water and oxygen during the high-temperature water and oxygen test to avoid oxidation; after the high-temperature water and oxygen test is completed, turn off the gas generation device, and use the tail gas treatment device to pump the inside of the ceramic protective pipe to a high vacuum state and then turn off the tail gas treatment device; start the gas generation device to transport inert gas to the gas inlet pipeline; move the box along the slide rail as a whole to the bottom of the pressure rod driver, remove the detachable heat preservation sealing device, and drive the pressure rod through the pressure rod driver to drive the pressure head to slowly penetrate into the inside of the protective pipe until the tip of the pressure head reaches the surface of the sample; at the same time, adjust the process of the pressure head pressing into the sample from the observation of the optical observation channel to realize the in-situ micro-nano indentation test of the sample; after the in-situ micro-nano indentation test is completed, post-process the data to complete the in-situ test. ;

[0008] The sample platform, gas inlet pipe, gas outlet pipe, protective pipe, pressure rod and pressure head are all made of high-temperature materials, that is, materials that can withstand certain stress and have oxidation resistance and thermal corrosion resistance under temperature conditions above 550°C, high-temperature alloys or high-temperature ceramics. High-temperature alloys are divided into iron-based, nickel-based, cobalt-based or refractory metal-based, and high-temperature ceramics are silicon carbide, aluminum oxide or silicon nitride. The diameter of the protective pipe is 50-60mm.

[0009] The heat preservation sealing device adopts a sealing flange, and the sealing gasket adopts alumina fiber or asbestos fiber, which can withstand high temperature and achieve sealing.

[0010] The temperature sensor adopts a temperature-controlling thermocouple, one end of which is located in a closed space outside the protective pipe, and the other end of which is located outside the box.

[0011] The heating material is silicon molybdenum rod or carbon silicon rod.

[0012] The larger the height of the box, the longer the pressure rod, which leads to larger measurement errors during the measurement process. In order to reduce the error, it is necessary to reduce the height of the box to reduce the length of the pressure rod; the reduction in the height of the box leads to a smaller heating space. In order to achieve a better heating effect, silicon-molybdenum rods or carbon-silicon rods with higher heating efficiency are used as heating elements, and the heating elements are prepared into a curved shape. In the same heating space, the length of the heating element is increased to improve the heating efficiency. The height of the box is 150mm to 250mm. If the height of the box is too high, the pressure rod will be too long, and if the height is too low, the function cannot be realized.

[0013] The slide rail adopts a pair of long-stroke slide rails, which are respectively located at the two ends of the box, that is, a long-stroke slide rail is set in the direction perpendicular to the connection line of the box on the air inlet side and the box on the air outlet side; during the water and oxygen test of the sample, the box is moved away from the pressure rod driver through the slide rail. After completing the water and oxygen test, the box is moved to the bottom of the pressure rod through the slide rail to complete the indentation test.

[0014] Another object of the present invention is to provide an in-situ micro-nano indentation testing method in an ultra-high temperature water-oxygen environment.

[0015] The in-situ micro-nano indentation testing method under ultra-high temperature water-oxygen environment of the present invention comprises the following steps:

[0016] 1) Place the sample on the sample platform, move the air inlet side box and the air outlet side box along the slide rail to move closer to the sample platform until the two are spliced ​​into an integrated box, and fasten the buckles of the air outlet side box and the air inlet side box so that the sample is in the sealed space formed by the protective pipe sealed by the sealing gasket;

[0017] 2) Move the box along the slide rail as a whole away from the pressure rod driver to avoid the influence of high temperature during the water-oxygen experiment on the indentation drive and the accuracy of the test device;

[0018] 3) Start the gas generating device to deliver the water-oxygen mixed gas with a set water-oxygen ratio into the protective pipe through the gas inlet pipe, and at the same time start the tail gas treatment device to connect the water cooling inlet of the box water cooling layer on the air inlet side and the box water cooling layer on the air outlet side;

[0019] 4) Turn on the heating device to heat the heating material, and monitor the temperature outside the protective pipe in real time through the temperature sensor, so that the inside of the protective pipe is heated to the preset temperature at the set heating rate and maintained to complete the high-temperature water and oxygen assessment of the sample;

[0020] 5) After the high-temperature water-oxygen test is completed, the gas generation device is turned off, the inside of the ceramic protection pipe is evacuated to a high vacuum state through the tail gas treatment device, and then the tail gas treatment device is turned off; the gas generation device is started to transport inert gas to the gas inlet pipeline;

[0021] 6) Remove the detachable heat preservation sealing device, and drive the pressure rod through the pressure rod driver to drive the pressure head to slowly penetrate into the protective pipe until the tip of the pressure head reaches the surface of the sample; at the same time, adjust the process of the pressure head pressing into the sample from the observation of the optical observation channel to realize the in-situ micro-nano indentation test of the sample;

[0022] 7) After the in-situ micro-nano indentation test is completed, the data is post-processed to complete the in-situ test.

[0023] Wherein, in step 3), the water-oxygen mixed gas is a mixed gas of water vapor and oxygen, wherein the volume of water vapor accounts for 10 to 90% of the total volume.

[0024] In step 4), the set heating rate is 1-20°C / min; the preset temperature is 1300°C-1600°C; the temperature inside the protective pipe is raised to the preset temperature and maintained for 0-500 hours.

[0025] In step 5), the vacuum degree is 10 -1 ~10 -5 pa. The inert gas is argon.

[0026] Advantages of the present invention:

[0027] The present invention has made innovations in method and structure, and adopted an integrated design to overcome the shortcoming of conventional devices that samples after ultra-high temperature water and oxygen assessment need to be transferred to a micro-nano indentation tester for off-site testing. An in-situ testing method and system for the mechanical properties of coating samples in an ultra-high temperature water and oxygen environment are proposed. An in-situ micro-nano indentation test can be carried out on the coating samples after any water-oxygen ratio assessment in a high temperature environment of 1600°C, thereby realizing in-situ characterization of the mechanical properties of the coating samples in the ultra-high temperature water and oxygen environment, with high feasibility and simple operation.

[0028] The present invention is innovative in structure:

[0029] 1. The protective pipe of the traditional tube furnace is placed horizontally, which can complete the assessment of the sample under high temperature water and oxygen. In order to complete the indentation test in situ, it is necessary to introduce an indentation test system above the traditional tube furnace, that is, to punch a hole in the lower tube wall of the horizontally placed protective pipe as the entrance of the sample platform. The diameter of the sample platform is 60mm, which will lead to two key problems: it is necessary to punch a hole with a diameter of 60mm in the tube wall at the lower end of the protective pipe, which will greatly reduce the life of the protective pipe and increase the difficulty of processing; it is necessary to use a protective pipe with a diameter much larger than 60mm, which requires the use of a longer pressure rod to press the sample inside the protective pipe, but a longer pressure rod will bring a large experimental error. Therefore, this test system changes the horizontally placed protective pipe in the traditional tube furnace to a vertical one, and the pressure rod and the sample platform enter from both ends of the vertically placed protective pipe, which not only avoids punching a hole with a diameter of 60mm on the tube wall, but also avoids the use of a large diameter protective pipe, which makes the use of a longer pressure rod.

[0030] 2. High temperature will have a cumulative effect on the accuracy of the pressure rod driver. In order to avoid the influence of the heat emitted by the box on the accuracy of the sample during the long-term water and oxygen test, the present invention uses a long-range slide rail. During the water and oxygen test of the sample, the box is moved away from the pressure rod driver through the slide rail. After the water and oxygen test is completed, the box is moved to the bottom of the pressure rod through the slide rail to complete the indentation test. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] Figure 1 It is an overall schematic diagram of an embodiment of an in-situ micro-nano indentation testing system in an ultra-high temperature water-oxygen environment of the present invention;

[0032] Figure 2 It is a full cross-sectional left view of an ultra-high temperature water and oxygen assessment and indentation test device of an embodiment of an in-situ micro-nano indentation test system under an ultra-high temperature water and oxygen environment of the present invention;

[0033] Figure 3 The left schematic diagram of an ultra-high temperature water and oxygen assessment and indentation test device of an embodiment of an in-situ micro-nano indentation test system under an ultra-high temperature water and oxygen environment of the present invention;

[0034] Figure 4 A full cross-sectional front view of an ultra-high temperature water and oxygen assessment and indentation test device of an embodiment of an in-situ micro-nano indentation test system under an ultra-high temperature water and oxygen environment of the present invention;

[0035] Figure 5 It is a front view of an ultra-high temperature water and oxygen assessment and indentation test device of an embodiment of an in-situ micro-nano indentation test system under an ultra-high temperature water and oxygen environment of the present invention;

[0036] Figure 6A full cross-sectional top view of an ultra-high temperature water and oxygen assessment and indentation test device of an embodiment of an in-situ micro-nano indentation test system under an ultra-high temperature water and oxygen environment of the present invention;

[0037] Figure 7 A top view of an ultra-high temperature water and oxygen assessment and indentation testing device of an embodiment of an in-situ micro-nano indentation testing system in an ultra-high temperature water and oxygen environment of the present invention. DETAILED DESCRIPTION

[0038] The present invention will be further described below through specific embodiments in conjunction with the accompanying drawings.

[0039] The in-situ micro-nano indentation testing system under ultra-high temperature water and oxygen environment of this embodiment comprises: a gas generating device A, an ultra-high temperature water and oxygen assessment and indentation testing device B, and an exhaust gas treatment device C. Figure 1As shown; wherein, the ultra-high temperature water oxygen assessment and indentation test device B comprises: an air inlet side box, an air outlet side box 1, a slide rail 2, a flat plate, a lifting support 3, a base 4, a sample platform 5, a platform fixing seat 6, an air inlet side box water cooling layer, an air outlet side box water cooling layer 7, an air inlet side box insulation layer, an air outlet side box insulation layer 8, an air inlet side box protection pipeline, an air outlet side box protection pipeline 9, a temperature sensor 10, a heating material 11, a heating device, a sealing gasket, a buckle, a heat preservation sealing device 12, a pressure rod driver 13, an outrigger 14, a pressure rod 15, a pressure head, an optical observation channel 16, a gas inlet pipeline 17 and a gas outlet pipeline 18; the air inlet side box and the air outlet side box 1 are respectively a half-shell structure with an opening on one side. The structure is as follows: the opening side is opposite, the inner surface of the air outlet side box 1 is covered with the air outlet side box water cooling layer 7, the inner surface of the air outlet side water cooling layer 7 is covered with the air outlet side box insulation layer 8, a semi-cylindrical air outlet side box protection pipe 9 is arranged in the air outlet side box insulation layer 8, and the edge of the air outlet side box protection pipe 9 is located in the same plane as the edges of the air outlet side box 1 and the air outlet side insulation layer 8; the top and bottom ends of the air outlet side box protection pipe 9 are against the top and bottom ends of the air outlet side box insulation layer 8; the air inlet side box, the air inlet side box insulation layer, the air inlet side box water cooling layer and the air inlet side box protection pipe are in contact with the air outlet side box 1, the air outlet side box insulation layer 8, the air outlet side box water cooling layer 7 and the air outlet side box protection pipe 9 are arranged in a relative manner; sealing pads are respectively arranged on the splicing edges of the air inlet side box protection duct and the air outlet side box protection duct 9; a buckle is arranged at the connection between the air inlet side box and the air outlet side box 1; the split air inlet side box and the air outlet side box 1 are placed on a pair of slide rails 2, which can move along the direction of the slide rails 2, and the pair of slide rails 2 are placed on a flat plate, and the flat plate is placed on a lifting support 3, and the lifting support 3 is placed on a base 4; the bottom of the sample platform 5 is fixed to the bottom of the air inlet side box through a platform fixing seat 6; the air inlet side box and the air outlet side box 1 move toward the center along the slide rails 2 and merge to form an integrated box; the air inlet side box protection duct and the air outlet side box protection duct 9 are spliced ​​together to form a circular hollow inner opening at the top and bottom. A cylindrical protective pipe, the central axis of the protective pipe is along the vertical direction, and the sample platform 5 is located in the protective pipe in the box; the box insulation layer on the air inlet side and the box insulation layer on the air outlet side are spliced ​​into an integrated insulation layer, so that a closed space is formed between the inner surface of the insulation layer and the outer surface of the side wall of the protective pipe; a temperature sensor 10 and a heating material 11 are arranged in the closed space, and the heating material 11 is connected to a heating device located outside the box; a detachable heat-insulating sealing device 12 is arranged at the center of the top wall of the box body facing the sample platform 5; a pressure rod driver 13 is arranged outside the box body, and the pressure rod driver 13 is fixed on an outrigger 14, and the outrigger 14 is placed on a base 4; a pressure rod 15 is arranged on the pressure rod driver 13, and a pressure head is arranged at the bottom end of the pressure rod 15;An optical observation channel 16 leading to the inside of the box body is arranged on the gas outlet side box body; one end of the gas inlet pipe 17 is connected to the outlet of the gas generating device, and the other end passes through the air inlet side box body, the air inlet side box body water cooling layer, the air inlet side box body insulation layer and the air inlet side box body protection pipe in sequence, and is connected to the protection pipe; one end of the gas outlet pipe 18 is connected to the inlet of the tail gas treatment device, and the other end passes through the air outlet side box body 1, the air outlet side box body water cooling layer 7, the air outlet side box body insulation layer 8 and the air outlet side box body protection pipe 9 in sequence, and is connected to the protection pipe. ;

[0040] In this embodiment, the gas inlet pipe, gas outlet pipe, pressure rod and pressure head are made of nickel-based high-temperature alloy or refractory metal-based alloy, and the sample platform and protection pipe are made of alumina ceramics; the diameter of the protection pipe is 55 mm; and the height of the box is 190 mm.

[0041] The in-situ micro-nano indentation testing method in an ultra-high temperature water-oxygen environment of this embodiment comprises the following steps:

[0042] 1) Place the sample on the sample platform 5, move the air inlet side box and the air outlet side box 1 along the slide rail 2 toward the sample platform 5 until the two are spliced ​​into an integrated box, and fasten the buckles of the air outlet side box 1 and the air inlet side box so that the sample is in the sealed space formed by the protective pipe sealed by the sealing gasket;

[0043] 2) Move the box along the slide rail 2 away from the pressure rod driver 13 to avoid the influence of high temperature during the water-oxygen experiment on the indentation drive and the accuracy of the test device;

[0044] 3) Start the gas generating device to deliver a water-oxygen mixed gas, a mixed gas of water vapor and oxygen with a set water-oxygen ratio into the protective pipe through the gas inlet pipe 17, wherein the volume of water vapor accounts for 90% of the total volume, and at the same time start the tail gas treatment device to connect the water cooling inlet of the box water cooling layer on the air inlet side and the water cooling inlet 7 of the box water cooling layer on the air outlet side;

[0045] 4) Turn on the heating device to heat the heating material 11, and monitor the temperature outside the protective pipe in real time through the temperature sensor 10, so that the temperature inside the protective pipe is raised to 1400° C. at a heating rate of 10° C. / min and maintained for 150 hours to complete the high-temperature water and oxygen assessment of the sample;

[0046] 5) After the high-temperature water and oxygen test is completed, turn off the gas generation device and use the tail gas treatment device to pump the inside of the ceramic protection pipe to 10 -5 After pa, the tail gas treatment device is turned off; the gas generation device is started to deliver argon gas to the gas inlet pipeline 17;

[0047] 6) Remove the detachable heat-insulating sealing device 12, and drive the pressure rod 15 through the pressure rod driver 13 to drive the pressure head to slowly penetrate into the protective pipe until the tip of the pressure head approaches the surface of the sample; at the same time, adjust the process of the pressure head pressing into the sample from the observation of the optical observation channel 16 to realize the in-situ micro-nano indentation test of the sample;

[0048] 7) After the in-situ micro-nano indentation test is completed, the data is post-processed to complete the in-situ test.

[0049] Finally, it should be noted that the purpose of publishing the embodiments is to help further understand the present invention, but those skilled in the art can understand that various substitutions and modifications are possible without departing from the spirit and scope of the present invention and the appended claims. Therefore, the present invention should not be limited to the contents disclosed in the embodiments, and the scope of protection claimed by the present invention shall be subject to the scope defined in the claims.

Claims

1. An in-situ micro-nano indentation testing system in an ultra-high temperature water-oxygen environment, characterized in that: The in-situ micro-nano indentation test system under the ultra-high temperature water-oxygen environment comprises: a gas generating device, an ultra-high temperature water-oxygen assessment and indentation test device and an exhaust gas treatment device; wherein the ultra-high temperature water-oxygen assessment and indentation test device comprises: an air inlet side box, an air outlet side box, a slide rail, a flat plate, a lifting support, a base, a sample platform, a platform fixing seat, an air inlet side box water cooling layer, an air outlet side box water cooling layer, an air inlet side box insulation layer, an air outlet side box insulation layer, an air inlet side box protection pipe, an air outlet side box protection pipe, a temperature sensor, a heating material, a heating device, a sealing pad, a buckle, a heat-insulating sealing device, a pressure rod driver, an outrigger, a pressure rod, a pressure head, an optical observation channel, a gas inlet pipe and a gas outlet pipe; the air inlet The side box is a semi-shell structure with an opening on one side, the inner surface of the air inlet side box is covered with an air inlet side box water-cooling layer, the inner surface of the air inlet side water-cooling layer is covered with an air inlet side box insulation layer, a semi-cylindrical air inlet side box protection duct is arranged in the air inlet side box insulation layer, the edge of the air inlet side box protection duct is located in the same plane as the edges of the air inlet side box and the air inlet side insulation layer; the top and bottom ends of the air inlet side box protection duct are against the top and bottom ends of the inner surface of the air inlet side box insulation layer; the air outlet side box, the air outlet side box insulation layer, the air outlet side box water-cooling layer and the air outlet side box protection duct are so as to be in contact with the air inlet side box, the air inlet side box insulation layer, the air inlet side box water-cooling layer and the air inlet side box protection duct on the opening side. The air inlet side box and the air outlet side box are arranged in a relative manner; sealing gaskets are respectively arranged on the splicing edges of the air inlet side box protection duct and the air outlet side box protection duct; a buckle is arranged at the connection between the air inlet side box and the air outlet side box; the split air inlet side box and the air outlet side box are respectively placed on the slide rails and can move along the slide rails, the slide rails are placed on the flat plate, the flat plate is placed on the lifting support, and the lifting support is placed on the base; the bottom of the sample platform is fixed to the bottom of the air inlet side box or the air outlet side box through the platform fixing seat; the air inlet side box and the air outlet side box move toward the center along the slide rail and merge to form an integrated box; the air inlet side box protection duct and the air outlet side box protection duct are spliced ​​together to form a cylindrical protection duct with a hollow interior and upper and lower openings, and the protection duct The interior is a sealed space, the central axis of the protective pipe is along the vertical direction, and the sample platform is located in the protective pipe inside the box; the box insulation layer on the air inlet side and the box insulation layer on the air outlet side are spliced ​​into an integrated insulation layer, so as to form a closed space between the inner surface of the insulation layer and the outer surface of the side wall of the protective pipe; a temperature sensor and a heating material are arranged in the closed space, and the heating material is connected to a heating device located outside the box; a detachable heat-insulating sealing device is arranged at the center of the top wall of the box facing the sample platform; a pressure rod driver is arranged outside the box, the pressure rod driver is fixed on an outrigger, and the outrigger is placed on a base; a pressure rod is arranged on the pressure rod driver, and a pressure head is arranged at the bottom end of the pressure rod; an optical observation channel leading to the inside of the box is arranged on the box on the gas outlet side;One end of the gas inlet pipeline is connected to the outlet of the gas generating device, and the other end passes through the air inlet side box, the air inlet side box water cooling layer, the air inlet side box insulation layer and the air inlet side box protection pipeline in sequence, and is connected to the protection pipeline; one end of the gas outlet pipeline is connected to the inlet of the exhaust gas treatment device, and the other end passes through the air outlet side box, the air outlet side box water cooling layer, the air outlet side box insulation layer and the air outlet side box protection pipeline in sequence, and is connected to the protection pipeline; place the sample on the sample platform, and move it along the slide rail respectively Move the air inlet side box and the air outlet side box toward the center until the two are spliced ​​into an integrated box, fasten the buckles of the air outlet side box and the air inlet side box, so that the sample is in a sealed space formed by the protective pipe connected by the sealing gasket; move the combined box as a whole along the slide rail away from the pressure rod driver; start the gas generating device to transport the water-oxygen mixed gas with a set water-oxygen ratio into the protective pipe through the gas inlet pipe, and at the same time start the exhaust gas treatment device, connect the water cooling layer of the air inlet side box and the air outlet side box Water cooling layer; turn on the heating device to heat the heating material, and monitor the temperature outside the protective pipe in real time through the temperature sensor, so that the inside of the protective pipe is heated to the preset temperature at the set heating rate and maintained to complete the high-temperature water and oxygen test of the sample. The heating material is located in a closed space outside the protective pipe, and is free from contact with water and oxygen during the high-temperature water and oxygen test to avoid oxidation; after the high-temperature water and oxygen test is completed, turn off the gas generation device, and use the tail gas treatment device to evacuate the inside of the protective pipe to a high vacuum state, and then turn off the tail gas treatment device; start the gas generation device to transport inert gas to the gas inlet pipeline; move the box along the slide rail as a whole to the bottom of the pressure rod driver, remove the detachable heat preservation sealing device, and drive the pressure rod through the pressure rod driver to drive the pressure head to slowly penetrate into the inside of the protective pipe until the tip of the pressure head reaches the surface of the sample; at the same time, adjust the process of the pressure head pressing into the sample from the observation of the optical observation channel to realize the in-situ micro-nano indentation test of the sample; after the in-situ micro-nano indentation test is completed, post-process the data to complete the in-situ test. ; 2. The in-situ micro-nano indentation testing system in an ultra-high temperature water-oxygen environment as claimed in claim 1, characterized in that: The sample platform, the gas inlet pipeline, the gas outlet pipeline, the protective pipeline, the pressure rod and the pressure head are all made of high-temperature materials.

3. The in-situ micro-nano indentation testing system under ultra-high temperature water and oxygen environment as claimed in claim 1, characterized in that: The heat-insulating sealing device adopts a sealing flange.

4. The in-situ micro-nano indentation testing system in an ultra-high temperature water-oxygen environment as claimed in claim 1, characterized in that: The sealing gasket is made of alumina fiber or asbestos fiber.

5. The in-situ micro-nano indentation testing system in an ultra-high temperature water-oxygen environment as claimed in claim 1, characterized in that: The temperature sensor is a temperature-controlling thermocouple, one end of which is located in a closed space outside the protection pipe, and the other end of which is located outside the box.

6. The in-situ micro-nano indentation testing system in an ultra-high temperature water-oxygen environment as claimed in claim 1, characterized in that: The heating material is a silicon-molybdenum rod or a carbon-silicon rod.

7. The in-situ micro-nano indentation testing system in an ultra-high temperature water-oxygen environment as claimed in claim 1, characterized in that: The slide rails are a pair of long-distance slide rails, which are respectively located at two ends of the box body.

8. A testing method for an in-situ micro-nano indentation testing system in an ultra-high temperature water-oxygen environment as claimed in claim 1, characterized in that: The test method comprises the following steps: 1) Place the sample on the sample platform, move the air inlet side box and the air outlet side box along the slide rail to move closer to the sample platform until the two are spliced ​​into an integrated box, and fasten the buckles of the air outlet side box and the air inlet side box so that the sample is in the sealed space formed by the protective pipe sealed by the sealing gasket; 2) Move the box along the slide rail as a whole away from the pressure rod driver to avoid the influence of high temperature during the water-oxygen experiment on the indentation drive and the accuracy of the test device; 3) Start the gas generating device to deliver the water-oxygen mixed gas with a set water-oxygen ratio into the protective pipe through the gas inlet pipe, and at the same time start the tail gas treatment device to connect the water cooling inlet of the box water cooling layer on the air inlet side and the box water cooling layer on the air outlet side; 4) Turn on the heating device to heat the heating material, and monitor the temperature outside the protective pipe in real time through the temperature sensor, so that the inside of the protective pipe is heated to the preset temperature at the set heating rate and maintained to complete the high-temperature water and oxygen assessment of the sample; 5) After the high-temperature water-oxygen test is completed, the gas generating device is turned off, the inside of the protective pipe is evacuated to a high vacuum state through the tail gas treatment device, and then the tail gas treatment device is turned off; the gas generating device is started to deliver inert gas to the gas inlet pipeline; 6) Remove the detachable heat preservation sealing device, and drive the pressure rod through the pressure rod driver to drive the pressure head to slowly penetrate into the protective pipe until the tip of the pressure head reaches the surface of the sample; at the same time, adjust the process of the pressure head pressing into the sample from the observation of the optical observation channel to realize the in-situ micro-nano indentation test of the sample; 7) After the in-situ micro-nano indentation test is completed, the data is post-processed to complete the in-situ test.

9. The testing method according to claim 8, characterized in that: In step 3), the water-oxygen mixed gas is a mixed gas of water vapor and oxygen, wherein the volume of water vapor accounts for 10-90% of the total volume.

10. The testing method according to claim 8, characterized in that: In step 4), the set heating rate is 1-20°C / min; the preset temperature is 1300°C-1600°C; the temperature inside the protective pipe is raised to the preset temperature and maintained for 0-500 hours.

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