CN112229752A - In-situ micro-nano indentation testing system and method in ultrahigh-temperature water oxygen environment - Google Patents

In-situ micro-nano indentation testing system and method in ultrahigh-temperature water oxygen environment Download PDF

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CN112229752A
CN112229752A CN202011156254.4A CN202011156254A CN112229752A CN 112229752 A CN112229752 A CN 112229752A CN 202011156254 A CN202011156254 A CN 202011156254A CN 112229752 A CN112229752 A CN 112229752A
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box body
side box
gas
inlet side
pipeline
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曲兆亮
白浩然
吕伯文
王一光
方岱宁
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Beijing Institute of Technology BIT
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
    • G01N3/56—Investigating resistance to wear or abrasion
    • G01N3/567—Investigating resistance to wear or abrasion by submitting the specimen to the action of a fluid or of a fluidised material, e.g. cavitation, jet abrasion
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/02—Details not specific for a particular testing method
    • G01N2203/022—Environment of the test
    • G01N2203/0244—Tests performed "in situ" or after "in situ" use

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Abstract

The invention discloses an in-situ micro-nano indentation testing system and method in an ultrahigh-temperature water oxygen environment. According to the invention, the protection pipeline horizontally placed in the traditional tube furnace is changed into a vertical placement, and the pressure rod and the sample platform respectively enter from two ends of the vertically placed protection pipeline, so that the pipe wall is prevented from being perforated, and the situation that a longer pressure rod is selected by selecting a large-diameter protection pipeline is avoided; the long-range slide rail is selected, the box body is moved to a position far away from the compression bar driver through the slide rail during the water oxygen examination of the sample, and after the water oxygen examination is completed, the box body is moved to the position below the compression bar through the slide rail to complete the indentation test; the in-situ micro-nano indentation testing device adopts an integrated design, can perform in-situ micro-nano indentation testing after performing any water-oxygen ratio assessment on the coating sample in a high-temperature environment of 1600 ℃, realizes in-situ characterization of mechanical properties of the coating sample in an ultrahigh-temperature water-oxygen environment, and has high feasibility and simple operation.

Description

In-situ micro-nano indentation testing system and method in ultrahigh-temperature water oxygen environment
Technical Field
The invention relates to an ultrahigh-temperature mechanical testing technology, in particular to an in-situ micro-nano indentation testing system and a testing method thereof in an ultrahigh-temperature water-oxygen environment.
Background
Increasing the turbine inlet temperature and reducing the structural weight of the engine are key to the development of the next generation of advanced aircraft engines and large bypass ratio civilian engines. As an alternative to superalloys, SiC/SiC composites fabricated into higher temperature resistant thermal structures have been used in commercial engines, with environmental barrier coatings being the key to their successful application. The Environmental Barrier Coating (EBC) is a necessary choice for solving the problem of long-term service of the SiC/SiC hot end component in the engine environment, can effectively prevent the SiC/SiC from being corroded and damaged by the gas environment, and avoids the rapid deterioration of the performance of the SiC/SiC ceramic matrix composite hot end component. In order to solve the core problem of guaranteeing the long service life and the service stability of the SiC/SiC composite material in the complex environment of a combustion chamber, the research of the current domestic and foreign environmental barrier coatings mainly focuses on the characterization and optimization of the corrosion resistance of the coating material. The method is characterized in that the mechanical properties of the SiC/SiC with the environmental barrier coating after the ultrahigh-temperature water-oxygen environment examination are particularly important to represent. The mechanical properties of the coating include hardness, strength, elastic modulus, fracture toughness, and the like. The method has the advantages of representing the mechanical property of the coating, and having important significance in structural design, assessment index determination, health evaluation, service life prediction and the like of the SiC/SiC composite material with the environmental barrier coating. In particular, compared with an off-position mechanical test, the in-situ mechanical test can accurately represent the mechanical property parameters of the coating in an ultrahigh-temperature water-oxygen environment.
Conventionally, the mechanical property characterization of the SiC/SiC composite material sample with the environmental barrier coating after the ultrahigh-temperature water oxygen examination is carried out in two steps: firstly, performing ultrahigh-temperature water oxygen examination on a sample in a tube furnace; and secondly, taking out the examined sample from the tube furnace, transferring the sample into the ultrahigh-temperature micro-nano indentation device and fixing the sample on a sample platform, and representing the mechanical property of the sample by using an ultrahigh-temperature micro-nano indentation testing technology. During the process of transferring the sample from the tube furnace to the high-temperature indentation device, the change of the temperature and the position of the sample can cause the problems of stress release and the like. Therefore, the existing device and the experimental method cannot represent the mechanical property of the sample in the real service environment.
Therefore, how to characterize the in-situ mechanical property of the SiC/SiC composite material with the environmental barrier coating in the ultra-high temperature water oxygen environment and provide the in-situ mechanical property parameters of the coating for the corrosion resistance characterization and optimization research of the environmental barrier coating material becomes an important subject for the research and development of the current domestic ultra-high temperature test instrument.
Disclosure of Invention
In order to solve the technical problem of in-situ measurement, the invention provides an in-situ micro-nano indentation testing system and a testing method thereof in an ultrahigh-temperature water-oxygen environment, and the in-situ characterization of the mechanical property and behavior of the SiC/SiC composite material with the environmental barrier coating in the ultrahigh-temperature water-oxygen environment is completed.
The invention aims to provide an in-situ micro-nano indentation testing system in an ultrahigh-temperature water oxygen environment.
The in-situ micro-nano indentation test system in the ultrahigh-temperature water oxygen environment comprises: the system comprises a gas generation device, an ultrahigh-temperature water oxygen examination and indentation testing device and a tail gas treatment device; wherein, ultra-high temperature water oxygen examination and indentation testing arrangement includes: the device comprises a gas inlet side box body, a gas outlet side box body, a slide rail, a flat plate, a lifting support, a base, a sample platform, a platform fixing seat, a gas inlet side box body water cooling layer, a gas outlet side box body water cooling layer, a gas inlet side box body heat insulation layer, a gas outlet side box body heat insulation layer, a gas inlet side box body protection pipeline, a gas outlet side box body protection pipeline, a temperature sensor, a heating material, a heating device, a sealing gasket, a buckle, a heat preservation sealing device, a pressure rod driver, an extending frame, a pressure rod, a pressure head, an optical observation channel, a; the air inlet side box body is of a semi-shell structure with an opening at one side, the inner surface of the air inlet side box body is covered with an air inlet side box body water cooling layer, the inner surface of the air inlet side water cooling layer is covered with an air inlet side box body heat insulation layer, a semi-cylindrical air inlet side box body protection pipeline is arranged in the air inlet side box body heat insulation layer, and the edge of the air inlet side box body protection pipeline and the edge of the air inlet side box body and the edge of the air inlet side heat insulation layer are positioned; the top end and the bottom end of the gas inlet side box body protection pipeline are abutted against the top end and the bottom end of the inner surface of the gas inlet side box body heat insulation layer; the gas outlet side box body, the gas outlet side box body heat insulation layer, the gas outlet side box body water cooling layer and the gas outlet side box body protection pipeline are arranged in a mode of being opposite to the opening sides of the gas inlet side box body, the gas inlet side box body heat insulation layer, the gas inlet side box body water cooling layer and the gas inlet side box body protection pipeline; the spliced edges of the gas inlet side box body protection pipeline and the gas outlet side box body protection pipeline are respectively provided with a sealing gasket; a buckle is arranged at the joint of the air inlet side box body and the air outlet side box body; the split air inlet side box body and the split air outlet side box body are respectively arranged on a sliding rail and can move along the sliding rail, the sliding rail is arranged on a flat plate, the flat plate is arranged on a lifting support, and the lifting support is arranged on a base; the bottom of the sample platform is fixed at the bottom of the air inlet side box body or the air outlet side box body through the platform fixing seat; the air inlet side box body and the air outlet side box body move towards the center along the slide rail and are combined to form an integrated box body; the gas inlet side box body protection pipeline and the gas outlet side box body protection pipeline are spliced together to form a cylindrical protection pipeline with a hollow inner part and an upper opening and a lower opening, a sealed space is formed in the protection pipeline, a central shaft of the protection pipeline is in the vertical direction, and the sample platform is positioned in the protection pipeline in the box body; the air inlet side box body heat insulation layer and the air port side box body heat insulation layer are spliced into an integral heat insulation layer, so that a closed space is formed between the inner surface of the heat insulation layer and the outer surface of the side wall of the protection pipeline; a temperature sensor and a heating material are arranged in the closed space, and the heating material is connected to a heating device positioned outside the box body; a detachable heat preservation sealing device is arranged at the center of the top wall of the box body, which is opposite to the sample platform; a pressure bar driver is arranged outside the box body and fixed on an overhanging frame, and the overhanging frame is arranged 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 which is arranged on the box body at the gas outlet side and then is introduced into the box body; one end of the gas inlet pipeline is connected with an outlet of the gas generating device, and the other end of the gas inlet pipeline sequentially penetrates through the gas inlet side box body, the gas inlet side box body water cooling layer, the gas inlet side box body heat insulation layer and the gas inlet side box body protection pipeline and is communicated into the protection pipeline; one end of the gas outlet pipeline is connected to an inlet of the tail gas treatment device, and the other end of the gas outlet pipeline sequentially penetrates through the gas outlet side box body, the gas outlet side box body water cooling layer, the gas outlet side box body heat insulation layer and the gas outlet side box body protection pipeline and is communicated into the protection pipeline; placing a sample on a sample platform, respectively moving the air inlet side box body and the air outlet side box body along the slide rail to approach towards the center until the air inlet side box body and the air outlet side box body are spliced into a whole, and tightly fastening the buckles of the air outlet side box body and the air inlet side box body so that the sample is positioned in a sealed space formed by protective pipelines which are connected in a sealing manner through a sealing gasket; integrally moving the combined box body along the slide rail away from the compression bar driver; starting a gas generating device to convey water-oxygen mixed gas with a set water-oxygen ratio into a protective pipeline through a gas inlet pipeline, and simultaneously starting a tail gas treatment device to connect a water cooling layer of a box body on the gas inlet side and a water cooling layer of a box body on the gas outlet side; the heating device is started to heat the heating material, and meanwhile, the temperature outside the protective pipeline is monitored in real time through the temperature sensor, so that the temperature inside the protective pipeline is increased to a preset temperature according to a set temperature increase rate and is kept, high-temperature water oxygen examination of the sample is completed, the heating material is located in a closed space outside the protective pipeline, and is prevented from being contacted with water oxygen in the high-temperature water oxygen examination process, and oxidation is avoided; after the examination of the high-temperature water oxygen is finished, the gas generating device is closed, the interior of the ceramic protection pipeline is pumped to a high vacuum state through the tail gas treatment device, and then the tail gas treatment device is closed; starting the gas generating device to convey inert gas to the gas inlet pipeline; integrally moving the box body along the slide rail to the position under the pressure rod driver, detaching the detachable heat-preservation sealing device, driving the pressure rod through the pressure rod driver to drive the pressure head to slowly penetrate into the protective pipeline until the tip of the pressure head reaches the surface of the sample; meanwhile, the process that the pressure head is pressed into the sample is adjusted through observation of the optical observation channel, so that in-situ micro-nano indentation testing of the sample is realized; and after the in-situ micro-nano indentation test is finished, carrying out post-processing on data to finish the in-situ test.
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, namely materials which can bear certain stress at the temperature of more than 550 ℃ and have oxidation resistance and hot corrosion resistance, high-temperature alloys or high-temperature ceramics, the high-temperature alloys are iron-based, nickel-based, cobalt-based or refractory metal-based, and the like, and the high-temperature ceramics are silicon carbide, aluminum oxide or silicon nitride and the like. The diameter of the protective pipeline is 50-60 mm. .
The heat-preservation sealing device adopts a sealing flange. The sealing gasket is made of alumina fiber or asbestos fiber, and can resist high temperature and realize sealing.
The temperature sensor adopts a temperature control thermocouple, one end of the temperature control thermocouple is positioned in the closed space outside the protective pipeline, and the other end of the temperature control thermocouple is positioned outside the box body.
The heating material adopts a silicon-molybdenum rod or a carbon-silicon rod.
The larger the height dimension of the box body is, the longer the dimension of the pressure rod is, and the measurement error is increased in the measurement process. In order to reduce errors, the height of the box body needs to be reduced so as to reduce the length of the compression bar; the height of the box body is reduced to reduce the heating space, in order to achieve a better heating effect, a silicon-molybdenum rod or a carbon silicon rod with higher heating efficiency is used as a heating element, the heating element is prepared into a bent shape, and the length of the heating element is increased in the same heating space, so that the heating efficiency is improved. The height of the box body is 150 mm-250 mm, if the height of the box body is too high, the compression bar is too long, and if the height of the box body is too low, the function cannot be realized.
The slide rails are a pair of long-range slide rails which are respectively positioned at two ends of the box body, namely, one long-range slide rail is respectively arranged in the direction vertical to the connecting line of the air inlet side box body and the air outlet side box body; and during the water and oxygen examination of the sample, the box body is moved to a position far away from the compression bar driver through the slide rail, and after the water and oxygen examination is completed, the box body is moved to the position below the compression bar through the slide rail, so that the indentation test is completed.
The invention also aims to provide an in-situ micro-nano indentation testing method in an ultrahigh-temperature water oxygen environment.
The in-situ micro-nano indentation testing method under the ultrahigh-temperature water oxygen environment comprises the following steps of:
1) placing a sample on a sample platform, moving the air inlet side box body and the air outlet side box body along the slide rail to approach the sample platform until the air inlet side box body and the air outlet side box body are spliced into a whole, and fastening the buckle of the air outlet side box body and the air inlet side box body so that the sample is positioned in a sealed space formed by protective pipelines which are hermetically connected through a sealing gasket;
2) the box body integrally moves along the slide rail and is far away from the compression bar driver, so that the influence of high temperature in the water oxygen experiment process on the accuracy of the indentation driving and testing device is avoided;
3) starting a gas generating device to convey water-oxygen mixed gas with a set water-oxygen ratio into a protective pipeline through a gas inlet pipeline, and simultaneously starting a tail gas treatment device to connect water cooling inlets of a box body water cooling layer at a gas inlet side and a box body water cooling layer at a gas outlet side;
4) opening a heating device to heat the heating material, and simultaneously monitoring the temperature outside the protective pipeline in real time through a temperature sensor, so that the temperature inside the protective pipeline is increased to a preset temperature according to a set temperature increase rate and is kept, and the high-temperature water oxygen examination of the sample is completed;
5) after the examination of the high-temperature water oxygen is finished, the gas generating device is closed, the interior of the ceramic protection pipeline is pumped to a high vacuum state through the tail gas treatment device, and then the tail gas treatment device is closed; starting the gas generating device to convey inert gas to the gas inlet pipeline;
6) the detachable heat-preservation sealing device is detached, and the pressure rod is driven by the pressure rod driver to drive the pressure head to slowly penetrate into the protective pipeline until the tip of the pressure head reaches the surface of the sample; meanwhile, the process that the pressure head is pressed into the sample is adjusted through observation of the optical observation channel, so that in-situ micro-nano indentation testing of the sample is realized;
7) and after the in-situ micro-nano indentation test is finished, carrying out post-processing on data to finish the in-situ test.
In the step 3), the water-oxygen mixed gas is a mixed gas of water vapor and oxygen, wherein the volume of the water vapor accounts for 10-90% of the total volume.
In the step 4), the set heating rate is 1-20 ℃/min; the preset temperature is 1300-1600 ℃; and the temperature inside the protective pipeline is raised to the preset temperature and then is kept for 0-500 hours.
In step 5), the degree of vacuum was 10-1～10-5pa. The inert gas is argon.
The invention has the advantages that:
the method and the structure are innovated, the integrated design is adopted, the defect that the sample subjected to ultra-high temperature water oxygen examination needs to be transferred to the micro-nano indentation tester for dislocation test in the conventional device is overcome, the in-situ test method and the system for the mechanical property of the coating sample in the ultra-high temperature water oxygen environment are provided, the in-situ micro-nano indentation test can be carried out after any water oxygen proportion examination is carried out on the coating sample in the high temperature environment of 1600 ℃, the in-situ characterization of the mechanical property of the coating sample in the ultra-high temperature water oxygen environment is realized, the feasibility is high, and the operation is simple.
The invention is innovative in structure:
1. the protective pipeline of the traditional tube furnace is horizontally arranged, and the examination of a sample under high-temperature water oxygen can be completed. In order to complete the in-situ indentation test, an indentation test system needs to be introduced above the conventional tube furnace, i.e. a through hole is punched in the lower tube wall of the horizontally placed protective tube to serve as an inlet of the sample platform. A sample platform diameter of 60mm leads to two critical problems: holes with the diameter of 60mm need to be drilled on the pipe wall at the lower end of the protection pipeline, so that the service life of the protection pipeline is greatly shortened, and the processing difficulty is improved; the diameter of the protective pipe which is far larger than 60mm needs to be selected, so that a longer pressure rod needs to be selected to press the sample in the protective pipe, but the longer pressure rod brings larger experimental errors. Therefore, the protection pipeline horizontally placed in the traditional tube furnace is changed into vertical placement by the test system, the pressure rod and the sample platform respectively enter from two ends of the vertically placed protection pipeline, through holes with the diameter of 60mm are prevented from being punched on the tube wall, and the situation that the pressure rod is longer in length is prevented from being used for the protection pipeline with the large diameter is avoided.
2. The influence of high temperature on the precision of the pressure rod driver has an accumulative effect, and in order to avoid the influence of heat emitted by the box body on the precision of a sample during long-time water and oxygen examination, the long-range slide rail is selected. And during the water and oxygen examination of the sample, the box body is moved to a position far away from the compression bar driver through the slide rail, and after the water and oxygen examination is completed, the box body is moved to the position below the compression bar through the slide rail, so that the indentation test is completed.
Drawings
FIG. 1 is an overall schematic view of an embodiment of an in-situ micro-nano indentation testing system in an ultrahigh-temperature water oxygen environment according to the invention;
FIG. 2 is a left side view of a full section of an in-situ micro-nano indentation testing system in an ultrahigh-temperature water oxygen environment according to an embodiment of the invention;
FIG. 3 is a left schematic view of an in-situ micro-nano indentation testing system under an ultrahigh-temperature water oxygen environment according to an embodiment of the invention;
FIG. 4 is a front view of a full section of an in-situ micro-nano indentation testing system under an ultrahigh-temperature water oxygen environment according to an embodiment of the invention;
FIG. 5 is a front view of an in-situ micro-nano indentation testing system under an ultrahigh-temperature water oxygen environment according to an embodiment of the invention;
FIG. 6 is a top view of a full section of an in-situ micro-nano indentation testing system under an ultrahigh-temperature water oxygen environment according to an embodiment of the invention;
fig. 7 is a top view of an ultrahigh-temperature water oxygen assessment and indentation testing device of an in-situ micro-nano indentation testing system in an ultrahigh-temperature water oxygen environment according to an embodiment of the invention.
Detailed Description
The invention will be further elucidated by means of specific embodiments in the following with reference to the drawing.
The micro-nano indentation test system of normal position under ultra-temperature water oxygen environment of this embodiment includes: a gas generating device A, an ultrahigh-temperature water oxygen assessment and indentation testing device B and a tail gas treatment device C, which are shown in figure 1; wherein, ultra-high temperature water oxygen examination and indentation testing arrangement B includes: the device comprises an air inlet side box body, an air outlet side box body 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 body water cooling layer, an air outlet side box body water cooling layer 7, an air inlet side box body heat insulation layer, an air outlet side box body heat insulation layer 8, an air inlet side box body protection pipeline, an air outlet side box body 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, an air inlet pipeline; the gas inlet side box body and the gas outlet side box body 1 are respectively of a semi-shell structure with an opening at one side, the opening sides are opposite, the inner surface of the gas outlet side box body 1 is covered with a gas outlet side box body water cooling layer 7, the inner surface of the gas outlet side water cooling layer 7 is covered with a gas outlet side box body heat insulation layer 8, a semi-cylindrical gas outlet side box body protection pipeline 9 is arranged in the gas outlet side box body heat insulation layer 8, and the edge of the gas outlet side box body protection pipeline 9 and the edge of the gas outlet side box body 1 and the edge of the gas outlet side; the top end and the bottom end of the gas outlet side box body protection pipeline 9 are propped against the top end and the bottom end of the gas outlet side box body heat insulation layer 8; the air inlet side box body, the air inlet side box body heat insulation layer, the air inlet side box body water cooling layer and the air inlet side box body protection pipeline are arranged in a mode of being opposite to the air outlet side box body 1, the air outlet side box body heat insulation layer 8, the air outlet side box body water cooling layer 7 and the air outlet side box body protection pipeline 9; the splicing edges of the gas port side box body protection pipeline and the gas outlet side box body protection pipeline 9 are respectively provided with a sealing gasket; a buckle is arranged at the joint of the air inlet side box body and the air outlet side box body 1; the split air inlet side box body and the split air outlet side box body 1 are arranged on a pair of slide rails 2 and can move along the direction of the slide rails 2, the pair of slide rails 2 are arranged on a flat plate, the flat plate is arranged on a lifting support 3, and the lifting support 3 is arranged on a base 4; the bottom of the sample platform 5 is fixed at the bottom of the box body at the air inlet side through a platform fixing seat 6; the air inlet side box body and the air outlet side box body 1 move towards the center along the slide rail 2 and are combined to form an integrated box body; the gas inlet side box body protection pipeline and the gas outlet side box body protection pipeline 9 are spliced together to form a cylindrical protection pipeline with a hollow inner part and an upper opening and a lower opening, the central axis of the protection pipeline is along the vertical direction, and the sample platform 5 is positioned in the protection pipeline in the box body; the air inlet side box body heat insulation layer and the air port side box body heat insulation layer are spliced into an integral heat insulation layer, so that a closed space is formed between the inner surface of the heat insulation layer and the outer surface of the side wall of the protection pipeline; 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 positioned outside the box body; a detachable heat preservation sealing device 12 is arranged at the center of the top wall of the box body, which is opposite to the sample platform 5; a pressure lever driver 13 is arranged outside the box body, the pressure lever driver 13 is fixed on an outer extending frame 14, and the outer extending frame 14 is arranged on the 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 which is arranged on the box body at the gas outlet side and then is introduced into the box body; one end of the gas inlet pipeline 17 is connected with an outlet of the gas generating device, and the other end of the gas inlet pipeline passes through the gas inlet side box body, the gas inlet side box body water cooling layer, the gas inlet side box body heat insulation layer and the gas inlet side box body protection pipeline in sequence and is communicated into the protection pipeline; one end of the gas outlet pipeline 18 is connected to an inlet of the tail gas treatment device, and the other end of the gas outlet pipeline passes through the gas outlet side box body 1, the gas outlet side box body water cooling layer 7, the gas outlet side box body heat insulation layer 8 and the gas outlet side box body protection pipeline 9 in sequence and is communicated into the protection pipeline.
In the embodiment, the gas inlet pipeline, the gas outlet pipeline, the pressure rod and the pressure head are made of nickel-based high-temperature alloy or refractory metal-based alloy, and the sample platform and the protective pipeline are made of alumina ceramic; the diameter of the protective pipeline is 55 mm; the height of the box body is 190 mm.
The in-situ micro-nano indentation testing method in the ultrahigh-temperature water oxygen environment comprises the following steps:
1) placing a sample on a sample platform 5, moving an air inlet side box body and an air outlet side box body 1 along a slide rail 2 to approach the sample platform 5 until the air inlet side box body and the air outlet side box body are spliced into a whole, and fastening a buckle of the air outlet side box body 1 and the air inlet side box body so that the sample is positioned in a sealed space formed by protective pipelines which are hermetically connected through a sealing gasket;
2) the box body is moved to a position far away from the compression bar driver 13 along the slide rail 2, so that the influence of high temperature in the water oxygen experiment process on the accuracy of the indentation driving and testing device is avoided;
3) starting a gas generating device to convey a water-oxygen mixed gas with a set water-oxygen ratio, a mixed gas of water vapor and oxygen into the protective pipeline through a gas inlet pipeline 17, wherein the volume of the water vapor accounts for 90% of the total volume, and simultaneously starting a tail gas treatment device to connect a water cooling inlet of a water cooling layer of a box body on the gas inlet side and a water cooling inlet of a water cooling layer 7 of a box body on the gas outlet side;
4) opening a heating device to heat the heating material 11, and simultaneously monitoring the temperature outside the protective pipeline in real time through a temperature sensor 10, so that the temperature inside the protective pipeline is increased to 1400 ℃ at the heating rate of 10 ℃/min and is kept for 150 hours, thereby completing the high-temperature water-oxygen examination of the sample;
5) after the examination of the high-temperature water oxygen is finished, the gas generating device is closed, and the interior of the ceramic protection pipeline is pumped to 10 degrees by the tail gas treatment device-5Closing the tail gas treatment device after pa; starting the gas generating device to deliver argon to the gas inlet pipe 17;
6) the detachable heat preservation sealing device 12 is disassembled, the pressure rod 15 is driven by the pressure rod driver 13 to drive the pressure head to slowly penetrate into the protection pipeline until the tip of the pressure head is close to the surface of the sample; meanwhile, the process that the pressure head is pressed into the sample is adjusted through the observation of the optical observation channel 16, so that the in-situ micro-nano indentation test of the sample is realized;
7) and after the in-situ micro-nano indentation test is finished, carrying out post-processing on data to finish the in-situ test.
Finally, it is noted that the disclosed embodiments are intended to aid in further understanding of the invention, but those skilled in the art will appreciate that: various substitutions and modifications are possible without departing from the spirit and scope of the invention and the appended claims. Therefore, the invention should not be limited to the embodiments disclosed, but the scope of the invention is defined by the appended claims.

Claims (10)

1. The utility model provides a little nanometer indentation test system of normal position under ultra-temperature water oxygen environment, its characterized in that, little nanometer indentation test system of normal position under ultra-temperature water oxygen environment includes: the system comprises a gas generation device, an ultrahigh-temperature water oxygen examination and indentation testing device and a tail gas treatment device; wherein, ultra-high temperature water oxygen examination and indentation testing arrangement includes: the device comprises a gas inlet side box body, a gas outlet side box body, a slide rail, a flat plate, a lifting support, a base, a sample platform, a platform fixing seat, a gas inlet side box body water cooling layer, a gas outlet side box body water cooling layer, a gas inlet side box body heat insulation layer, a gas outlet side box body heat insulation layer, a gas inlet side box body protection pipeline, a gas outlet side box body protection pipeline, a temperature sensor, a heating material, a heating device, a sealing gasket, a buckle, a heat preservation sealing device, a pressure rod driver, an extending frame, a pressure rod, a pressure head, an optical observation channel, a; the air inlet side box body is of a semi-shell structure with an opening at one side, the inner surface of the air inlet side box body is covered with an air inlet side box body water cooling layer, the inner surface of the air inlet side water cooling layer is covered with an air inlet side box body heat insulation layer, a semi-cylindrical air inlet side box body protection pipeline is arranged in the air inlet side box body heat insulation layer, and the edge of the air inlet side box body protection pipeline and the edge of the air inlet side box body and the edge of the air inlet side heat insulation layer are positioned; the top end and the bottom end of the gas inlet side box body protection pipeline are abutted against the top end and the bottom end of the inner surface of the gas inlet side box body heat insulation layer; the gas outlet side box body, the gas outlet side box body heat insulation layer, the gas outlet side box body water cooling layer and the gas outlet side box body protection pipeline are arranged in a mode of being opposite to the opening sides of the gas inlet side box body, the gas inlet side box body heat insulation layer, the gas inlet side box body water cooling layer and the gas inlet side box body protection pipeline; the spliced edges of the gas inlet side box body protection pipeline and the gas outlet side box body protection pipeline are respectively provided with a sealing gasket; a buckle is arranged at the joint of the air inlet side box body and the air outlet side box body; the split air inlet side box body and the split air outlet side box body are respectively arranged on a sliding rail and can move along the sliding rail, the sliding rail is arranged on a flat plate, the flat plate is arranged on a lifting support, and the lifting support is arranged on a base; the bottom of the sample platform is fixed at the bottom of the air inlet side box body or the air outlet side box body through the platform fixing seat; the air inlet side box body and the air outlet side box body move towards the center along the slide rail and are combined to form an integrated box body; the gas inlet side box body protection pipeline and the gas outlet side box body protection pipeline are spliced together to form a cylindrical protection pipeline with a hollow inner part and an upper opening and a lower opening, a sealed space is formed in the protection pipeline, a central shaft of the protection pipeline is in the vertical direction, and the sample platform is positioned in the protection pipeline in the box body; the air inlet side box body heat insulation layer and the air port side box body heat insulation layer are spliced into an integral heat insulation layer, so that a closed space is formed between the inner surface of the heat insulation layer and the outer surface of the side wall of the protection pipeline; a temperature sensor and a heating material are arranged in the closed space, and the heating material is connected to a heating device positioned outside the box body; a detachable heat preservation sealing device is arranged at the center of the top wall of the box body, which is opposite to the sample platform; a pressure bar driver is arranged outside the box body and fixed on an overhanging frame, and the overhanging frame is arranged 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 which is arranged on the box body at the gas outlet side and then is introduced into the box body; one end of the gas inlet pipeline is connected with an outlet of the gas generating device, and the other end of the gas inlet pipeline sequentially penetrates through the gas inlet side box body, the gas inlet side box body water cooling layer, the gas inlet side box body heat insulation layer and the gas inlet side box body protection pipeline and is communicated into the protection pipeline; one end of the gas outlet pipeline is connected to an inlet of the tail gas treatment device, and the other end of the gas outlet pipeline sequentially penetrates through the gas outlet side box body, the gas outlet side box body water cooling layer, the gas outlet side box body heat insulation layer and the gas outlet side box body protection pipeline and is communicated into the protection pipeline; placing a sample on a sample platform, respectively moving the air inlet side box body and the air outlet side box body along the slide rail to approach towards the center until the air inlet side box body and the air outlet side box body are spliced into a whole, and tightly fastening the buckles of the air outlet side box body and the air inlet side box body so that the sample is positioned in a sealed space formed by protective pipelines which are connected in a sealing manner through a sealing gasket; integrally moving the combined box body along the slide rail away from the compression bar driver; starting a gas generating device to convey water-oxygen mixed gas with a set water-oxygen ratio into a protective pipeline through a gas inlet pipeline, and simultaneously starting a tail gas treatment device to connect a water cooling layer of a box body on the gas inlet side and a water cooling layer of a box body on the gas outlet side; the heating device is started to heat the heating material, and meanwhile, the temperature outside the protective pipeline is monitored in real time through the temperature sensor, so that the temperature inside the protective pipeline is increased to a preset temperature according to a set temperature increase rate and is kept, high-temperature water oxygen examination of the sample is completed, the heating material is located in a closed space outside the protective pipeline, and is prevented from being contacted with water oxygen in the high-temperature water oxygen examination process, and oxidation is avoided; after the examination of the high-temperature water oxygen is finished, the gas generating device is closed, the interior of the ceramic protection pipeline is pumped to a high vacuum state through the tail gas treatment device, and then the tail gas treatment device is closed; starting the gas generating device to convey inert gas to the gas inlet pipeline; integrally moving the box body along the slide rail to the position under the pressure rod driver, detaching the detachable heat-preservation sealing device, driving the pressure rod through the pressure rod driver to drive the pressure head to slowly penetrate into the protective pipeline until the tip of the pressure head reaches the surface of the sample; meanwhile, the process that the pressure head is pressed into the sample is adjusted through observation of the optical observation channel, so that in-situ micro-nano indentation testing of the sample is realized; and after the in-situ micro-nano indentation test is finished, carrying out post-processing on data to finish the in-situ test.
2. The in-situ micro-nano indentation testing system in the ultrahigh-temperature water oxygen environment of claim 1, wherein the sample platform, the gas inlet pipeline, the gas outlet pipeline, the protective pipeline, the pressure rod and the pressure head are made of high-temperature materials.
3. The in-situ micro-nano indentation testing system in the ultrahigh-temperature water oxygen environment of claim 1, wherein the heat-preservation sealing device adopts a sealing flange.
4. The in-situ micro-nano indentation testing system in the ultrahigh-temperature water oxygen environment of claim 1, wherein the sealing gasket is made of alumina fibers or asbestos fibers.
5. The in-situ micro-nano indentation testing system in the ultrahigh-temperature water oxygen environment of claim 1, wherein the temperature sensor is a temperature control thermocouple, one end of the temperature control thermocouple is located in a closed space outside the protective pipeline, and the other end of the temperature control thermocouple is located outside the box body.
6. The in-situ micro-nano indentation testing system in the ultrahigh-temperature water oxygen environment of claim 1, wherein the heating material is a silicon-molybdenum rod or a carbon-silicon rod.
7. The in-situ micro-nano indentation testing system in the ultrahigh-temperature water oxygen environment of claim 1, wherein the slide rails are a pair of long-range slide rails and are respectively located at two ends of the box body.
8. The testing method of the in-situ micro-nano indentation testing system in the ultrahigh-temperature water oxygen environment according to claim 1 is characterized by comprising the following steps:
1) placing a sample on a sample platform, moving the air inlet side box body and the air outlet side box body along the slide rail to approach the sample platform until the air inlet side box body and the air outlet side box body are spliced into a whole, and fastening the buckle of the air outlet side box body and the air inlet side box body so that the sample is positioned in a sealed space formed by protective pipelines which are hermetically connected through a sealing gasket;
2) the box body integrally moves along the slide rail and is far away from the compression bar driver, so that the influence of high temperature in the water oxygen experiment process on the accuracy of the indentation driving and testing device is avoided;
3) starting a gas generating device to convey water-oxygen mixed gas with a set water-oxygen ratio into a protective pipeline through a gas inlet pipeline, and simultaneously starting a tail gas treatment device to connect water cooling inlets of a box body water cooling layer at a gas inlet side and a box body water cooling layer at a gas outlet side;
4) opening a heating device to heat the heating material, and simultaneously monitoring the temperature outside the protective pipeline in real time through a temperature sensor, so that the temperature inside the protective pipeline is increased to a preset temperature according to a set temperature increase rate and is kept, and the high-temperature water oxygen examination of the sample is completed;
5) after the examination of the high-temperature water oxygen is finished, the gas generating device is closed, the interior of the ceramic protection pipeline is pumped to a high vacuum state through the tail gas treatment device, and then the tail gas treatment device is closed; starting the gas generating device to convey inert gas to the gas inlet pipeline;
6) the detachable heat-preservation sealing device is detached, and the pressure rod is driven by the pressure rod driver to drive the pressure head to slowly penetrate into the protective pipeline until the tip of the pressure head reaches the surface of the sample; meanwhile, the process that the pressure head is pressed into the sample is adjusted through observation of the optical observation channel, so that in-situ micro-nano indentation testing of the sample is realized;
7) and after the in-situ micro-nano indentation test is finished, carrying out post-processing on data to finish the in-situ test.
9. The test method according to claim 8, wherein in the step 3), the water-oxygen mixed gas is a mixed gas of water vapor and oxygen, wherein the volume of the water vapor is 10-90% of the total volume.
10. The test method according to claim 8, wherein in the step 4), the set temperature rise rate is 1-20 ℃/min; the preset temperature is 1300-1600 ℃; and the temperature inside the protective pipeline is raised to the preset temperature and then is kept for 0-500 hours.
CN202011156254.4A 2020-10-26 2020-10-26 In-situ micro-nano indentation testing system and method in ultrahigh-temperature water oxygen environment Pending CN112229752A (en)

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