CN110044753B - High-temperature micro-nano indentation testing device and method with inert gas protection function - Google Patents
High-temperature micro-nano indentation testing device and method with inert gas protection function Download PDFInfo
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- CN110044753B CN110044753B CN201910422275.7A CN201910422275A CN110044753B CN 110044753 B CN110044753 B CN 110044753B CN 201910422275 A CN201910422275 A CN 201910422275A CN 110044753 B CN110044753 B CN 110044753B
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- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/40—Investigating hardness or rebound hardness
- G01N3/54—Performing tests at high or low temperatures
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- 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
- G01N2203/0001—Type of application of the stress
- G01N2203/0003—Steady
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- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0014—Type of force applied
- G01N2203/0016—Tensile or compressive
- G01N2203/0019—Compressive
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- G—PHYSICS
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- G01N2203/0076—Hardness, compressibility or resistance to crushing
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- G01N2203/0082—Indentation characteristics measured during load
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- G01N2203/02—Details not specific for a particular testing method
- G01N2203/022—Environment of the test
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- G01N2203/02—Details not specific for a particular testing method
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- G01N2203/0236—Other environments
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- G01N2203/02—Details not specific for a particular testing method
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Abstract
The invention relates to a high-temperature micro-nano indentation testing device with an inert gas protection function and a method thereof, belonging to the field of mechanical and electrical integration precision instruments. The device comprises a heat insulation unit, an inert atmosphere heating unit, a macro adjustment-precision loading unit, a micro-imaging unit, an XY precision displacement platform, a marble base and the like. And the XY precise displacement platform drives the heat insulation unit, the inert atmosphere heating unit and the test sample to displace in XY directions so as to realize the replacement of press-in points and the adjustment of microscopic imaging positions. The invention can test the micro-nano indentation response and the mechanical property of the material under the environment of room temperature to 800 ℃ and high temperature under the protection of inert gas, and can carry out in-situ observation on the surface morphology and deformation damage of the indentation area of the material test sample under the action of high temperature by combining with a coaxial microscope with a filter lens. The device has the advantages of compact structure, high modularization degree, high testing precision, controllable environment atmosphere, convenience in operation and use and the like.
Description
Technical Field
The invention relates to the field of electromechanical integrated precision instruments, in particular to a high-temperature micro-nano indentation testing device and method with an inert gas protection function, provides an effective technical means for researching the micro-mechanical behavior, the deformation damage mechanism and the performance evolution rule of a material in a high-temperature environment, and has wide application prospects in the fields of aerospace, material science, ferrous metallurgy and the like.
Background
The mechanical property of the obtained material is an important condition for the application of new materials, but with the development of micro-mechanics and micro-electronics technologies and the large application of thin films and coating materials, the characteristic size of the material is smaller and smaller, and the traditional mechanical testing technology cannot meet the requirement of obtaining the mechanical property of the new materials under the micro-scale. The micro-nano indentation test is a novel micro-scale mechanical test technology provided on the basis of the traditional hardness test. The micro-nano indentation test adopts a high-precision load and displacement sensor to measure the indentation load and indentation depth applied to a test sample by a pressure head in real time, and finally obtains a load-indentation depth curve in the indentation process. By analyzing the load-indentation curve, the mechanical performance parameters such as hardness, elastic modulus, fracture toughness and the like of the material can be accurately measured. The micro-nano indentation test has the advantages of convenience in operation, almost no damage, rich test contents, convenience in operation and the like, and is widely applied to mechanical property tests for measuring micro-sized materials such as thin film materials, gradient functional materials, nano materials and the like at present.
As the mechanical properties of materials such as engine turbine blades, rocket nozzles and the like which are in service in a high-temperature environment are greatly influenced by a temperature field, the mechanical properties obtained by conventional tests cannot guide the application of the materials in the service environment, and the development of the mechanical property test under the force-thermal coupling loading condition is very important. Because the oxidation of the material at high temperature can cause great influence to the test result, the high-temperature micro-nano indentation testing device at home and abroad is usually placed in a closed vacuum cavity or an atmosphere cavity at present, which is not beneficial to the operation of operators and greatly increases the cost. Meanwhile, due to the influence of a temperature field and thermal radiation at high temperature, most of the high-temperature micro-nano indentation testing devices at home and abroad at present lack a means for carrying out in-situ observation on the indentation morphology at high temperature, and the original indentation morphology under the action of high temperature is difficult to obtain. For example, chinese patent (CN106404574A), which relates to a high-temperature micro-nano indentation testing device in a vacuum environment, adopts an atmosphere heating furnace to perform synchronous non-contact heating design on a pressure head and a test sample, and minimizes the "temperature drift" in the test; however, the whole device is placed in a closed vacuum cavity, a long-time vacuumizing process is required before testing, and the operation and adjustment of personnel are not facilitated; meanwhile, the surface appearance before and after pressing cannot be observed due to lack of observation means.
Therefore, there is a wide need to develop a high-temperature micro-nano indentation measurement device with inert gas protection and in-situ observation functions without a sealed cavity or a vacuum cavity.
Disclosure of Invention
The invention aims to provide a high-temperature micro-nano indentation testing device with an inert gas protection function and a method thereof, and solves the problems in the prior art. The micro-nano indentation response and mechanical property test under the environment of room temperature to 800 ℃ can be carried out under the protection of inert gas without a vacuum cavity or a sealed cavity, and the in-situ observation of the surface morphology and deformation damage of an indentation area of a test sample under the action of high temperature can be carried out by combining a coaxial microscope with a filter lens; so as to obtain the mechanical performance parameters of the material such as hardness, elastic modulus and the like at different temperatures. Provides an effective technical means for researching the micro-mechanical behavior, the deformation damage mechanism and the performance evolution rule of the material in the high-temperature environment.
The above object of the present invention is achieved by the following technical solutions:
the high-temperature micro-nano indentation testing device with the inert gas protection function comprises a heat insulation unit 2, an inert atmosphere heating unit 5, a macro adjustment-precision loading unit 3, a micro-imaging unit 4, an XY precision displacement platform 6 and a marble base 1, wherein the inert atmosphere heating unit 5 is fixed on a water-cooling base 27 of the heat insulation unit 2, the heat insulation unit 2 is installed on the XY precision displacement platform 6, the macro adjustment-precision loading unit 3, the micro-imaging unit 4 and the XY precision displacement platform 6 are respectively fixed on the marble base 1, and the XY precision displacement platform 6 drives the heat insulation unit 2, the inert atmosphere heating unit 5 and a test sample 35 to displace in the XY direction so as to realize the replacement of a pressed point and the adjustment of a micro-imaging position;
the heat insulation unit 2 is: the water-cooling copper pipe 29 is welded on a water-cooling base 27 provided with a cooling water flow channel, the water-cooling furnace body I22 and the water-cooling furnace body II 26 are respectively and fixedly connected with a slide block 30, and a linear guide rail 28 for installing the slide block 30 is fixed on the water-cooling base 27; the locking nut 24 is arranged on the locking stud 23, and the locking stud 23 is arranged on the water-cooled furnace body I22 through pin connection;
the inert atmosphere heating unit 5 is: the heating device base 32 is fixed on the ceramic heat insulation base 31, and the object carrying copper table 40 is fixedly connected with the heating device base 32 through bolts; the object carrying copper table 40 is provided with a U-shaped groove, the U-shaped resistance heater 39 is arranged in the U-shaped groove of the object carrying copper table 40, and the test sample 35 is bonded on the object carrying copper table 40 through high-temperature glue; the nozzle 34 and the inert gas pipeline 37 are welded on the heating device upper cover 33 with a gas flow passage; a heating block support plate 38 is fixed below the heating device base 32 by bolting, and a resistance heating block 36 positioned therebetween is clamped, and the heating device upper cover 33 is fixed above the heating device base 32 by bolting; the inert atmosphere heating unit 5 is fixed to the water-cooled base 27 of the heat insulating unit 2.
The macro adjustment-precision loading unit 3 adopts a piezoelectric ceramic laminated actuator 13 and a flexible hinge 17 as an indentation precision loading power source, and adopts a force sensor 20 and a capacitance displacement sensor 10 to carry out precision detection and feedback control on a load-indentation signal; the Z-axis precision adjusting sliding table 15 is arranged on the marble base 1 and drives the pressure head 7 to displace and adjust the position; a loading device connecting plate 16 is fixed on an objective table of a Z-axis precision adjusting sliding table 15 by bolts, and a piezoelectric ceramic supporting seat 14 and a flexible hinge 17 which are arranged on the loading device connecting plate 16 provide pretightening force to compress a piezoelectric ceramic laminated actuator 13; the connecting rod 19 is fixed below the flexible hinge 17 through threads, the force sensor 20 and the displacement sensor measuring plate 21 are connected between the connecting rod 19 and the water-cooling pressure rod 9 in series, and the pressure head 7 is fixedly bonded at the tail end of the ceramic pressure rod 8; a displacement sensor bracket 11 for clamping the capacitive displacement sensor 10 is arranged on a precise manual displacement table 12, and the precise manual displacement table 12 is fixedly connected on a manual displacement table mounting plate 18 through bolts.
The microscopic imaging unit 4 is: the microscope adjusting sliding table 45 is fixed on the marble base 1 through an L-shaped connecting plate 43, the microscope support 46 is fixed on an object stage of the microscope adjusting sliding table 45, and the coaxial microscope 42 is fixedly connected with the microscope support 46 through a fastening bolt; a CCD image collector 44 is fixed above the coaxial microscope 42.
An inert gas flow channel is formed in the upper cover 33 of the heating device of the inert atmosphere heating unit 5, and inert gas flows into the inert atmosphere heating unit 5; the pressure P1 inside the inert atmosphere heating unit 5 is made to be higher than the outside pressure P2 by continuously flowing inert gas into the narrow space inside the inert atmosphere heating unit 5; the inert gas blows the pressure head 7 and then is sprayed out from the reserved holes above the heat insulation unit 2 and the inert atmosphere heating unit 5 to dilute and drive oxygen in the inert atmosphere heating unit 5; the pressure difference brought by the flowing inert gas and the flow velocity of the ejected inert gas prevent external oxygen from entering the inert atmosphere heating unit 5, and the pressure head 7 and the test sample are prevented from being oxidized under the action of high temperature to influence the indentation test result without a sealed cavity or a vacuum cavity.
The object carrying copper table 40 and the heating device upper cover 33 of the inert atmosphere heating unit 5 are made of oxygen-free copper materials; two resistance heating blocks 36 which are symmetrically arranged front and back are adopted to heat the whole heating device upper cover 33, inert gas is heated when flowing in an inert gas flow channel in the heating device upper cover 33, high-temperature inert gas is sprayed out from a nozzle 34 to blow the pressure head 7, and then the heat radiation of the resistance heating blocks 36 is matched to heat the pressure head 7; the U-shaped resistance heater 39 is arranged in a U-shaped groove in the object carrying copper table 40 and used for heating the test sample 35 on the object carrying copper table 40; two independent thermocouple temperature sensors are respectively adhered to the surfaces of the pressure head 7 and the test sample 35 to measure the surface temperature, the temperature of the pressure head 7 and the temperature of the test sample 35 are accurately controlled to be consistent through the feedback control of the thermocouple temperature sensors, and the influence of temperature drift on the test result is minimized.
The heat insulation unit 2 is designed by adopting a slidable split furnace body arranged on a linear guide rail, and alumina fiber heat insulation layers 25 are embedded in the water-cooled furnace body I22 and the water-cooled furnace body II 26 so as to reduce heat loss of the inert atmosphere heating unit 5 and ensure the stability of a temperature field in the heat insulation unit 2; cooling water flow channels are arranged in the water-cooled furnace body I22, the water-cooled furnace body II 26 and the water-cooled base 27 and are used for introducing circulating cooling water.
The indenter 7 is made of diamond or sapphire.
The coaxial microscope 42 is arranged on the microscope adjusting sliding table 45, so that the automatic adjustment of the focal length of the coaxial microscope 42 is realized; a filter lens 41 is arranged on an objective lens of the coaxial microscope 42 to prevent the radiant light under the action of high temperature from influencing the imaging quality.
The invention also aims to provide a high-temperature micro-nano indentation testing method with an inert gas protection function, which comprises the following steps:
a) closing the water-cooled furnace body I22 and the water-cooled furnace body II 26, and locking the furnace body through a locking nut 24 and a locking stud 23; setting a load or displacement loading function and a loading temperature, and continuously filling inert gas into the inert atmosphere heating unit 5 through an external gas cylinder; circulating cooling water is supplied to the water-cooling pressure rod 9, the water-cooling furnace body I22, the water-cooling furnace body II 26 and the water-cooling base 27 through a circulating cooling water tank;
b) respectively outputting control currents to a U-shaped resistance heater 39 and a resistance heating block 36 of the inert atmosphere heating unit 5 by a temperature control unit to realize temperature loading; measuring the actual temperature of the pressure head 7 and the test sample 35 in real time by adopting a thermocouple, and adjusting the output current value by comparing with a preset temperature value to realize feedback control;
c) when the temperature of the pressure head 7 and the temperature of the test sample 35 reach the preset temperature, the Z-axis precision adjustment sliding table 15 is driven to drive the pressure head 7 to move downwards, so that the pressure head 7 approaches the test sample 35;
d) the piezoelectric ceramic laminated actuator 13 drives the pressure head 7 to precisely load and unload according to a set load or displacement loading function, and the force sensor 20 and the capacitive displacement sensor 10 detect the pressing load and the pressing depth of the pressure head 7 pressed into the test sample 35 in real time, so as to finally obtain a load-pressing depth curve of an indentation test at a set temperature;
e) driving the XY precise displacement platform 6 to drive the test sample 35 to perform horizontal displacement so as to replace a pressure point, and repeating the step d), thereby performing a plurality of groups of load-pressure depth curves at set temperature;
f) after the indentation test is finished, driving the Z-axis precision adjustment sliding table 15 to drive the pressure head 7 to move upwards, so that the pressure head 7 is separated from the heat insulation unit 2 and the inert atmosphere heating unit 5; horizontally displacing the indentation area of the test sample 35 to the lower part of the coaxial microscope 42 by utilizing the XY precise displacement platform 6;
g) the CCD image collector 44 sends the image observed by the coaxial microscope 42 to the computer, and the computer drives the microscope to adjust the displacement of the sliding table 45 and adjust the focal length of the coaxial microscope 42 to obtain a clear image; precisely adjusting the position of the test sample by an XY precise displacement platform 6 to finally obtain the surface appearance and deformation damage of the indentation area of the material test sample under the action of high temperature;
h) and (3) processing the load-indentation depth curve Oliver-Pharr method of the test sample by combining the surface morphology and the deformation damage image of the indentation area of the material test sample under the high-temperature effect, so as to obtain the hardness and the elastic modulus of the test sample under the corresponding temperature environment, and completing the test.
In the micro-nano indentation test at high temperature, the high-temperature creep of the material seriously influences the accuracy of the test result, and the measured values of the contact rigidity, the material hardness and the elastic modulus under the high-temperature environment are corrected by the following method:
the contact stiffness S was measured as defined by the Oliver-Pharr method as:
in the formula (1), alpha and n are fitting parameters, hmaxTo the maximum depth of indentation, hfDeepening the unloaded residual pressure;
according to the unloading rate
And displacement rate before unloading
Correcting the measured contact stiffness S to obtain corrected contact stiffness SeComprises the following steps:
correction of contact depth hceComprises the following steps:
where ε is a constant related only to the indenter shape, and for a cone-shaped indenter ε of 0.72, PmaxThe maximum press-in load;
correction of contact area AeComprises the following steps:
the corrected hardness H was obtained as:
defining the modified reduced modulus E of the material and indenterre：
Modified modulus of elasticity E of test sample material under high temperaturee：
Where β is a constant related only to the shape of the indenter, β 1.012 for vickers indenter, v is the poisson's ratio of the test sample material, EiIs the modulus of elasticity, v, of the indentor materialiIs the poisson's ratio of the indenter material.
The invention has the beneficial effects that: the invention can carry out the test of micro-nano indentation response and mechanical property at room temperature to 800 ℃ under the protection of inert gas without a vacuum cavity or a sealed cavity, and can carry out in-situ observation on the surface appearance and deformation damage of the indentation area of the test sample under the action of high temperature by combining with a coaxial microscope with a filter lens. The invention has the advantages of compact structure, high modularization degree, high testing precision, controllable environmental atmosphere, convenient operation and the like, avoids the oxidation of a pressure head and a test sample in a high-temperature environment, does not need to integrate an expensive vacuum cavity or a sealing cavity, and is convenient for operation of operators. The control unit is adopted to independently control the temperature of the pressure head and the test sample, so that the temperature deviation of the pressure head and the test sample can be minimized, and the influence of temperature drift in the pressing-in process on the test result is avoided. The invention provides an effective technical means for researching the micro-mechanical behavior, the deformation damage mechanism and the performance evolution rule of the material in the high-temperature environment, and has wide application prospects in the fields of aerospace, material science, ferrous metallurgy and the like.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the invention without limiting the invention.
Fig. 1 is a schematic view of the overall structure of the present invention.
Fig. 2 is a schematic structural diagram of a macro-adjustment-precision loading unit according to the present invention.
FIG. 3 is a perspective half sectional view of the insulation unit of the present invention.
FIG. 4 is a perspective half sectional view of an inert ambient heating unit of the present invention.
Fig. 5 is a schematic structural diagram of a microscopic imaging unit of the present invention.
FIG. 6 is a schematic view of an inert gas flow channel of the inert atmosphere heating unit of the present invention.
FIG. 7 is a schematic view of the cooling of the thermal insulation unit of the present invention.
FIG. 8 is a force thermal coupling loading schematic of the present invention.
FIG. 9 is a schematic cross-sectional view of an indentation during loading and unloading.
Fig. 10 is a load-indentation curve of a typical indentation test.
In the figure: 1. a marble base; 2. a heat insulation unit; 3. macro-tuning-precision loading unit; 4. a microscopic imaging unit; 5. an inert atmosphere heating unit; 6. an XY precision displacement stage; 7. a pressure head; 8. a ceramic compression bar; 9. water-cooling the compression bar; 10. a capacitive displacement sensor; 11. a displacement sensor support; 12. a precision manual displacement stage; 13. a piezoceramic stack actuator; 14. a piezoelectric ceramic support base; 15. a Z-axis precision adjustment sliding table; 16. a loading device connecting plate; 17. a flexible hinge, 18, a manual displacement table mounting plate; 19. a connecting rod; 20. a force sensor; 21. a displacement sensor measuring plate; 22. a water-cooled furnace body I; 23. locking the stud; 24. locking the nut; 25. an alumina fiber thermal insulation layer; 26. a water-cooled furnace body II; 27. a water-cooled base; 28. a linear guide rail; 29. water-cooling the copper pipe; 30. a slider; 31. a ceramic heat insulating base; 32. a heating device base; 33. an upper cover of the heating device; 34. a nozzle; 35. a test sample; 36. a resistance heating block; 37. an inert gas conduit; 38. a heating block support plate; 39. a U-shaped resistance heater; 40. an object carrying copper table; 41. a filter lens; 42. a coaxial microscope; 43. an L-shaped connecting plate; 44. a CCD image collector; 45. adjusting the sliding table by the microscope; 46. a microscope support.
Detailed Description
The details of the present invention and its embodiments are further described below with reference to the accompanying drawings.
Referring to fig. 1 to 10, the high-temperature micro-nano indentation testing device and method with the inert gas protection function of the invention can test the micro-nano indentation response and mechanical properties of the material under the high-temperature environment of room temperature to 800 ℃ under the protection of the inert gas, and can perform in-situ observation on the surface morphology and deformation damage of the indentation area of the material test sample under the high-temperature action by combining with a coaxial microscope with a filter lens. The invention has the advantages of compact structure, high modularization degree, high testing precision, controllable environment atmosphere, convenient operation and use and the like, and provides an effective technical means for researching the material micro-mechanical behavior, the deformation damage mechanism and the performance evolution rule in a high-temperature environment.
The invention discloses a high-temperature micro-nano indentation testing device with an inert gas protection function, which comprises a heat insulation unit 2, an inert atmosphere heating unit 5, a macro adjustment-precision loading unit 3, a micro imaging unit 4, an XY precision displacement platform 6 and a marble base 1. The macroscopic adjustment-precise loading unit 3 adopts a piezoelectric ceramic-flexible hinge mechanism as a precise loading unit, adopts the force sensor 20 and the capacitance type displacement sensor 10 to carry out real-time detection and feedback control on a load-depth pressing signal, and can adopt two control modes of load control and displacement control to control the pressing speed of a pressing head. The inert atmosphere heating unit 2 adopts a resistance heater as a heat source, the pressure head 7 and the test sample 35 independently control the temperature to ensure the temperature to be consistent, and oxygen is driven by a high-temperature inert gas blowing mode. The microscopic imaging unit 4 adopts a coaxial microscope 42 provided with a filter lens 41 to carry out in-situ observation on the surface indentation morphology of the high-temperature test sample.
Referring to fig. 1, the high-temperature micro-nano indentation testing device with the inert gas protection function comprises a heat insulation unit 2, an inert atmosphere heating unit 5, a macro adjustment-precision loading unit 3, a micro-imaging unit 4, an XY precision displacement platform 6 and a marble base 1, wherein the inert atmosphere heating unit 5 is fixed on a water cooling base 27 of the heat insulation unit 2, the heat insulation unit 2 is installed on the XY precision displacement platform 6, the macro adjustment-precision loading unit 3, the micro-imaging unit 4 and the XY precision displacement platform 6 are respectively fixed on the marble base 1, and the XY precision displacement platform 6 drives the heat insulation unit 2, the inert atmosphere heating unit 5 and a test sample 35 to perform XY direction displacement so as to realize indentation point replacement and micro-imaging position adjustment;
referring to fig. 2, the macro-alignment-precision loading unit 3 is formed by a piezoelectric ceramic stack actuator 13 mounted on a loading device connecting plate 16 and a flexible hinge 17 as a precision loading mechanism, and a driving pressure head 7 is pressed into a test sample 35. The load signal is detected by the force sensor 20, and the displacement signal is detected by the capacitive displacement sensor 10. And the Z-axis precision adjusting sliding table 15 is installed on the marble base 1 through bolts and used for driving the pressure head 7 to adjust the position through macroscopic displacement. The loading device connecting plate 16 is fixed on the objective table of the Z-axis precision adjusting sliding table 15 by bolts; the piezoelectric ceramic laminated actuator 13 is pressed by a pretightening force provided by a piezoelectric ceramic supporting seat 14 and a flexible hinge 17 which are arranged on a connecting plate 16 of a loading device. The connecting rod 19 is fixed below the flexible hinge 17 through threaded connection, the force sensor 20 and the displacement sensor measuring plate 21 are connected between the connecting rod 19 and the water-cooling pressure rod 8 in series, and the pressure head 7 is fixed at the tail end of the ceramic pressure rod 8 through bonding. The precise manual displacement table 12 is fixed on the manual displacement table mounting plate 18, and the displacement sensor bracket 11 for clamping the capacitive displacement sensor 10 is mounted on the precise manual displacement table 12. Fine adjustment of the distance between the capacitive displacement sensor 10 and the displacement sensor measuring plate 21 is realized by the precision manual displacement table 12.
Referring to fig. 3, the thermal insulation unit 2 includes: the water-cooled copper pipe 29 is welded on the water-cooled base 27 with a flow passage. The water-cooled furnace body I22 and the water-cooled furnace body II 26 are respectively and fixedly connected with a slide block 30, and a linear guide rail 28 for installing the slide block 30 is fixed on a water-cooled base 27. An alumina fiber heat-insulating layer 25 is embedded in the water-cooled furnace body I22 and the water-cooled furnace body II 26. The locking stud 23 is installed on the locking stud 23 through threaded connection, and the locking stud 23 is installed on the water-cooled furnace body I22 through pin connection. And locking lugs for locking are arranged on the wall of the water-cooled furnace body II 26, and the locking lugs can be matched with the locking studs 23 and the locking nuts 24 to lock the two split furnace bodies.
Referring to fig. 4, the inert atmosphere heating unit 5 is: the heating device base 32 is fixed on the ceramic heat insulation base 31, and the object carrying copper table 40 is fixedly connected with the heating device base 32 through bolts; the object carrying copper table 40 is provided with a U-shaped groove, the U-shaped resistance heater is placed in the U-shaped groove of the object carrying copper table 40, and the test sample 35 is bonded above the object carrying copper table 40 through high-temperature glue. The nozzle 34 and the inert gas pipe 37 are fixedly connected with the heating device upper cover 33 provided with a gas flow passage through welding. A heating block support plate 38 is secured by bolting below the heating unit base 32 and clamps the resistance heating block 36 therebetween. The heating device upper cover 33 is fixed above the heating device base 32 by bolts. The inert atmosphere heating unit 5 is fixed on a water-cooled base 27.
Referring to fig. 5, the microscopic imaging unit 4 is: the microscope adjustment slide table 45 is fixed to the marble base 1 through an L-shaped connecting plate 43, and the microscope support 46 is fixed to the stage of the microscope adjustment slide table 45. The coaxial microscope 42 is fixedly connected to the microscope stand 46 by a fastening bolt. A CCD image collector 44 is fixed above the coaxial microscope 42. A filter lens 41 is attached to an objective lens of the coaxial microscope 42.
Referring to fig. 4 and 6, the heating device upper cover 33 of the inert atmosphere heating unit 5 is provided with an inert gas flow passage, and the inert gas flows into the inert atmosphere heating unit 5 through the flow passage of the heating device upper cover 33. The pressure P1 inside the inert atmosphere heating unit 5 is made slightly higher than the ambient pressure P2 by the inert gas continuously flowing into the narrow space inside the inert atmosphere heating unit 5. And the inert gas is blown to the pressure head and then is sprayed out from the reserved holes above the heat insulation unit 2 and the inert atmosphere heating unit 5 to dilute and drive oxygen in the inert atmosphere heating unit 5. The pressure difference caused by the flowing inert gas and the flow rate of the ejected inert gas prevent the external oxygen from entering the inert atmosphere heating unit 5. By the method, a sealed cavity or a vacuum cavity is not required to be sealed, and the influence of the oxidation of the pressure head and the test sample on the indentation test result under the action of high temperature can be avoided.
The object carrying copper table 40 and the heating device upper cover 33 of the inert atmosphere heating unit 5 are made of oxygen-free copper materials with good thermal conductivity. Two resistance heating blocks 36 which are symmetrically arranged front and back are adopted to heat the whole heating device upper cover 33, inert gas is preheated when flowing in a flow channel in the heating device upper cover 33, and high-temperature inert gas is sprayed out from a nozzle 34 to blow a pressure head; the ram is heated by hot gas blowing against the ram in conjunction with the thermal radiation from the resistance heating block 36. A U-shaped resistance heater 39 is placed in a U-shaped groove in the copper stage 40 to heat the test specimen 35 on the copper stage 40. The two independent thermocouple temperature sensors are respectively adhered to the surfaces of the pressure head 7 and the test sample 35 to measure the surface temperatures of the pressure head 7 and the test sample 35, the temperature consistency of the pressure head 7 and the test sample 35 is accurately controlled through the feedback control of the thermocouple temperature sensors, and the influence of temperature drift on the test result is minimized.
Referring to fig. 3 and 7, the thermal insulation unit 2 is of a slidable split furnace design mounted on linear guides. An alumina fiber heat-insulating layer 25 is embedded in the water-cooling furnace body I22 and the water-cooling furnace body II 26 to reduce heat loss of the inert atmosphere heating unit 5 and ensure the stability of the temperature field in the heat-insulating unit 2. And cooling water flow channels are formed in the water-cooling furnace body I22, the water-cooling furnace body II 26 and the water-cooling base 27 to introduce circulating cooling water, so that the influence of high temperature on the precision of an external sensor and a precision loading mechanism is avoided. The XY precise displacement platform 6 drives the heat insulation unit 2, the inert atmosphere heating unit 5 and the test sample 35 in the heat insulation unit and the inert atmosphere heating unit to perform displacement in the XY direction so as to realize press-in point replacement and micro-imaging position adjustment and realize press-in point replacement and micro-imaging of indentation morphology.
The indenter 7 is made of diamond or sapphire.
The coaxial microscope 42 is arranged on the microscope adjusting sliding table 45, so that the focal length of the coaxial microscope 42 can be automatically adjusted. A filter lens 41 is arranged on an objective lens of the coaxial microscope 42 to prevent the radiant light under the action of high temperature from influencing the imaging quality.
Referring to fig. 8, the force thermal coupling loading mode of the present invention is as follows: and carrying out high-temperature loading on the test sample on the object carrying copper table through a U-shaped resistance heater. Heating the whole heating device upper cover by adopting two symmetrically arranged resistance heating blocks, and heating inert gas when the inert gas flows in a flow channel inside the heating device upper cover; and the high-temperature gas blows the pressure head to be matched with the heat radiation of the resistance heating block to carry out high-temperature loading on the pressure head. After the high-temperature loading is finished, a piezoelectric ceramic laminated actuator drives a pressure head to press in a test sample, so that the loading of the pressing-in load P is realized.
The invention also aims to provide a high-temperature micro-nano indentation testing method with an inert gas protection function, which comprises the following specific testing steps:
a) the water-cooled furnace body I22 and the water-cooled furnace body II 26 are closed, and the furnace body is locked through a locking nut 24 and a locking stud 23. And setting experimental loading conditions such as a load or displacement loading function, loading temperature and the like through a computer. Continuously filling inert gas into the inert atmosphere heating unit 5 through an external gas cylinder; and circulating cooling water is provided for the water-cooling pressure lever 9, the water-cooling furnace body I22, the water-cooling furnace body II 26 and the water-cooling base 27 through a circulating cooling water tank.
b) The temperature control unit outputs control currents to the U-shaped resistance heater 39 and the resistance heating block 36 of the inert atmosphere heating unit 5, respectively, to realize temperature loading. And measuring the actual temperature of the pressure head 7 and the test sample 35 in real time by adopting a thermocouple, and adjusting the output current value by comparing with a preset temperature value to realize feedback control.
c) When the temperature of the pressure head 7 and the temperature of the test sample 35 reach the preset temperature, the computer drives the Z-axis precision adjustment sliding table 15 to drive the pressure head 7 to move downwards, so that the pressure head 7 approaches the test sample 35.
d) The computer controls the piezoelectric ceramic laminated actuator 13 to drive the pressure head 7 to carry out precise loading and unloading according to a set loading function of load or displacement. The force sensor 20 and the capacitive displacement sensor 10 detect the pressing load and the pressing depth of the indenter 7 into the test specimen 35 in real time. And finally obtaining a load-indentation depth curve of the indentation test at the set temperature.
e) And d, driving the XY precise displacement platform 6 by the computer to drive the test sample 35 to perform horizontal displacement so as to replace the press-in point, and repeating the step d to perform a plurality of groups of load-press depth curves at the set temperature.
f) After the indentation test is finished, the computer drives the Z-axis precision adjustment sliding table 15 to drive the pressure head 7 to move upwards, so that the pressure head 7 is separated from the heat insulation unit 2 and the inert atmosphere heating unit 5. The indentation region of the test specimen 35 is horizontally displaced below the coaxial microscope 42 by the XY precision displacement stage 6.
g) The CCD image collector 44 sends the image observed by the coaxial microscope 42 to the computer, and the computer drives the microscope to adjust the displacement of the slide table 45 to adjust the focal length of the coaxial microscope 42, thereby obtaining a clear image. And precisely adjusting the position of the test sample by an XY precise displacement platform 6 to finally obtain the surface appearance and deformation damage of the indentation area of the material test sample under the action of high temperature.
h) And (3) processing the load-indentation depth curve Oliver-Pharr method of the test sample by combining the surface morphology and the deformation damage image of the indentation area of the material test sample under the high-temperature effect, so as to obtain the parameters of the test sample such as hardness, elastic modulus and the like under the corresponding temperature environment, and completing the test.
The hardness H and the elastic modulus E of the test sample material were determined by the Oliver-Pharr method as follows:
referring to fig. 9 and 10, during the loading phase of the indentation test, the test specimen surface is elastically and plastically deformed to produce indentations having the same geometry as the indenter tip. Defining the contact depth h of the indentation and the indentercAnd contact radius a. When the press-in load reaches the maximum value PmaxThe depth of time-pressing also reaches a maximum value hmax. The test sample is elastically recovered in the unloading section, and the residual pressing depth h is obtained after the unloading is finishedfSlope of the top of the curve with the unloaded section (contact stiffness)
Definition of hardness H:
wherein A is the contact area. In order to accurately obtain the hardness and the elastic modulus of the test sample, the contact rigidity S of the unloading section curve and the contact area A of the pressure head and the surface of the sample must be accurately measured.
The relation between the load and the compression depth of the unloading section of the load-compression depth curve is shown as the formula (2)
P＝α(h-hf)n (2)
Typically, 25% to 50% of the top of the curve of the unloading segment is cut and subjected to least squares fitting to obtain fitting parameters α and n.
The contact stiffness S can be obtained as:
the maximum pressing depth h is due to the elastic deformation in the pressing processmaxIs always greater than the contact depth hcThe method comprises the following steps:
hc＝hmax-hs (4)
press-in deformation hsComprises the following steps:
where ε is a constant related to the indenter tip geometry, and thus the contact depth h can be derivedcComprises the following steps:
for several common indenters, the ideal shape function is: bo's is A ═ 24.56hc 2(ii) a Vickers is A-24.504 hc 2. However, since the indenter tip geometry always deviates from the ideal shape, the ideal area function must be corrected. The contact area function is fitted using the following formula:
the contact area is substituted for the formula (1) to obtain the hardness
Definition of the reduced modulus E of the Material and indenterr：
The modulus of elasticity E of the test sample material is then:
where β is a constant related only to the shape of the indenter, 1.012 for vickers indenter β. v. ofFor the poisson's ratio of the test sample material, the poisson's ratio of the engineering material is generally between 0.15 and 0.35, and v is usually 0.25. EiIs the modulus of elasticity, v, of the indentor materialiIs the poisson's ratio of the indenter material. E of diamond indenteri＝1141Gpa，vi0.007. From this, values of hardness and modulus of elasticity of the test sample material were obtained.
In addition, in the micro-nano indentation test at high temperature, the high-temperature creep of the material seriously influences the accuracy of the test result. The measured values of the contact rigidity, the material hardness and the elastic modulus in a high-temperature environment can be corrected by the following methods aiming at the problem:
the contact stiffness S was measured as defined by the Oliver-Pharr method as:
in the formula (1), alpha and n are fitting parameters, hmaxTo the maximum depth of indentation, hfThe residual stress after unloading is deepened.
According to the unloading rate
And displacement rate before unloading
Obtaining a corrected contact stiffness SeComprises the following steps:
correction of contact depth hceComprises the following steps:
where e is a constant related only to the indenter shape, and 0.72 for a conical indenter.
Correction of contact area AeComprises the following steps:
the corrected hardness H is thus obtained:
defining the modified reduced modulus E of the material and indenterre：
Modified modulus of elasticity E of test sample material under high temperaturee：
Where β is a constant related only to the shape of the indenter, β 1.012 for vickers indenter, v is the poisson's ratio of the test sample material, EiIs the modulus of elasticity, v, of the indentor materialiIs the poisson's ratio of the indenter material. The corrected contact stiffness and the true hardness and elastic modulus of the test sample material at the set temperature are obtained.
The above description is only a preferred example of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like of the present invention shall be included in the protection scope of the present invention.
Claims (7)
1. The utility model provides a micro-nano indentation testing arrangement of high temperature with inert gas protect function which characterized in that: the device comprises a heat insulation unit (2), an inert atmosphere heating unit (5), a macro adjustment-precision loading unit (3), a micro imaging unit (4), an XY precision displacement platform (6) and a marble base (1), wherein the inert atmosphere heating unit (5) is fixed on a water cooling base (27) of the heat insulation unit (2), the heat insulation unit (2) is installed on the XY precision displacement platform (6), the macro adjustment-precision loading unit (3), the micro imaging unit (4) and the XY precision displacement platform (6) are respectively fixed on the marble base (1), and the XY precision displacement platform (6) drives the heat insulation unit (2), the inert atmosphere heating unit (5) and a test sample (35) to displace in the XY direction so as to realize press-in point replacement and micro imaging position adjustment;
the heat insulation unit (2) is: the water-cooling copper pipe (29) is welded on a water-cooling base (27) provided with a cooling water flow channel, the water-cooling furnace body I (22) and the water-cooling furnace body II (26) are respectively and fixedly connected with a sliding block (30), and a linear guide rail (28) for mounting the sliding block (30) is fixed on the water-cooling base (27); the locking nut (24) is arranged on the locking stud (23), and the locking stud (23) is connected and arranged on the water-cooled furnace body I (22) through a pin;
the inert atmosphere heating unit (5) is: the heating device base (32) is fixed on the ceramic heat insulation base (31), and the object carrying copper table (40) is fixedly connected with the heating device base (32) through bolts; the object carrying copper table (40) is provided with a U-shaped groove, the U-shaped resistance heater (39) is arranged in the U-shaped groove of the object carrying copper table (40), and the test sample (35) is bonded on the object carrying copper table (40) through high-temperature glue; the nozzle (34) and the inert gas pipeline (37) are welded on the upper cover (33) of the heating device with the gas flow channel; the heating block supporting plate (38) is fixed below the heating device base (32) through bolt connection, and the resistance heating block (36) positioned between the heating block supporting plate and the heating device base is clamped, and the heating device upper cover (33) is fixed above the heating device base (32) through bolts; the inert atmosphere heating unit (5) is fixed on a water-cooling base (27) of the heat insulation unit (2);
the macroscopic adjustment-precise loading unit (3) adopts a piezoelectric ceramic laminated actuator (13) and a flexible hinge (17) as an indentation precise loading power source, and adopts a force sensor (20) and a capacitance displacement sensor (10) to carry out precise detection and feedback control on a load-indentation signal; the Z-axis precision adjusting sliding table (15) is arranged on the marble base (1) and drives the pressure head (7) to displace and adjust the position; a loading device connecting plate (16) is fixed on an objective table of a Z-axis precision adjusting sliding table (15) by bolts, and a piezoelectric ceramic supporting seat (14) and a flexible hinge (17) which are arranged on the loading device connecting plate (16) provide pretightening force to press a piezoelectric ceramic laminated actuator (13); the connecting rod (19) is fixed below the flexible hinge (17) in a threaded manner, the force sensor (20) and the displacement sensor measuring plate (21) are connected between the connecting rod (19) and the water-cooling pressure rod (9) in series, and the pressure head (7) is fixedly bonded at the tail end of the ceramic pressure rod (8); a displacement sensor bracket (11) for clamping the capacitive displacement sensor (10) is arranged on a precise manual displacement table (12), and the precise manual displacement table (12) is fixedly connected on a manual displacement table mounting plate (18) through a bolt;
the microscopic imaging unit (4) is: the microscope adjusting sliding table (45) is fixed on the marble base (1) through an L-shaped connecting plate (43), the microscope support (46) is fixed on an object stage of the microscope adjusting sliding table (45), and the coaxial microscope (42) is fixedly connected with the microscope support (46) through a fastening bolt; the CCD image collector (44) is fixed above the coaxial microscope (42).
2. The high-temperature micro-nano indentation testing device with the inert gas protection function according to claim 1, characterized in that: an inert gas flow channel is formed in the upper cover (33) of the heating device of the inert atmosphere heating unit (5), and inert gas flows into the inert atmosphere heating unit (5); the pressure P1 inside the inert atmosphere heating unit (5) is larger than the external pressure P2 by continuously flowing inert gas into the narrow space inside the inert atmosphere heating unit (5); the inert gas is blown to the pressure head (7) and then is sprayed out from the holes reserved above the heat insulation unit (2) and the inert atmosphere heating unit (5), and oxygen in the inert atmosphere heating unit (5) is diluted and driven; the pressure difference brought by flowing inert gas and the flow velocity of the ejected inert gas prevent external oxygen from entering the inert atmosphere heating unit (5), and the pressure head (7) and the test sample are prevented from being oxidized under the action of high temperature to influence the indentation test result without a sealed cavity or a vacuum cavity.
3. The high-temperature micro-nano indentation testing device with the inert gas protection function according to claim 1, characterized in that: the object carrying copper table (40) of the inert atmosphere heating unit (5) and the upper cover (33) of the heating device are made of oxygen-free copper materials; two resistance heating blocks (36) which are symmetrically arranged in front and back are adopted to heat the whole heating device upper cover (33), inert gas is heated when flowing in an inert gas flow channel in the heating device upper cover (33), high-temperature inert gas is sprayed out from a nozzle (34) to blow a pressure head (7), and the pressure head (7) is heated by matching with heat radiation of the resistance heating blocks (36); the U-shaped resistance heater (39) is arranged in a U-shaped groove in the object carrying copper table (40) and used for heating the test sample (35) on the object carrying copper table (40); two independent thermocouple temperature sensors are respectively adhered to the surfaces of the pressure head (7) and the test sample (35) to measure the surface temperature, the temperature of the pressure head (7) and the temperature of the test sample (35) are accurately controlled to be consistent through the feedback control of the thermocouple temperature sensors, and the influence of 'temperature drift' on the test result is minimized.
4. The high-temperature micro-nano indentation testing device with the inert gas protection function according to claim 1, characterized in that: the heat insulation unit (2) is designed by adopting a slidable split furnace body arranged on a linear guide rail, and alumina fiber heat insulation layers (25) are embedded in the water-cooled furnace body I (22) and the water-cooled furnace body II (26) so as to reduce heat loss of the inert atmosphere heating unit (5) and ensure the stability of the internal temperature field of the heat insulation unit (2); cooling water flow channels are arranged in the water-cooled furnace body I (22), the water-cooled furnace body II (26) and the water-cooled base (27) and are used for introducing circulating cooling water.
5. The high-temperature micro-nano indentation testing device with the inert gas protection function according to claim 2 or 3, characterized in that: the pressure head (7) is made of diamond or sapphire.
6. The high-temperature micro-nano indentation testing device with the inert gas protection function according to claim 1, characterized in that: the coaxial microscope (42) is arranged on the microscope adjusting sliding table (45), so that the automatic adjustment of the focal length of the coaxial microscope (42) is realized; a filter lens (41) is arranged on an objective lens of the coaxial microscope (42) to prevent the radiant light from influencing the imaging quality under the action of high temperature.
7. A high-temperature micro-nano indentation testing method realized by using the high-temperature micro-nano indentation testing device with the inert gas protection function of claim 1 is characterized in that: the method comprises the following steps:
a) closing the water-cooled furnace body I (22) and the water-cooled furnace body II (26), and locking the furnace body through a locking nut (24) and a locking stud (23); setting a load or displacement loading function and a loading temperature, and continuously filling inert gas into the inert atmosphere heating unit (5) through an external gas cylinder; circulating cooling water is provided for the water-cooling pressure rod (9), the water-cooling furnace body I (22), the water-cooling furnace body II (26) and the water-cooling base (27) through a circulating cooling water tank;
b) respectively outputting control currents to a U-shaped resistance heater (39) and a resistance heating block (36) of the inert atmosphere heating unit (5) by a temperature control unit to realize temperature loading; measuring the actual temperature of the pressure head (7) and the test sample (35) in real time by adopting a thermocouple, and adjusting the output current value by comparing with a preset temperature value to realize feedback control;
c) when the temperature of the pressure head (7) and the temperature of the test sample (35) reach the preset temperature, the Z-axis precision adjustment sliding table (15) is driven to drive the pressure head (7) to move downwards, so that the pressure head (7) approaches the test sample (35);
d) the piezoelectric ceramic laminated actuator (13) drives a pressure head (7) to precisely load and unload according to a set load or displacement loading function, a force sensor (20) and a capacitance displacement sensor (10) detect the pressing load and pressing depth of the pressure head (7) pressed into a test sample (35) in real time, and finally a load-pressing depth curve of an indentation test at a set temperature is obtained;
e) driving an XY precise displacement platform (6) to drive a test sample (35) to carry out horizontal displacement so as to replace a pressing point, and repeating the step d) to carry out a plurality of groups of load-pressing depth curves at set temperature;
f) after the indentation test is finished, driving a Z-axis precision adjustment sliding table (15) to drive a pressure head (7) to move upwards, so that the pressure head (7) is separated from the heat insulation unit (2) and the inert atmosphere heating unit (5); horizontally displacing an indentation area of the test sample (35) to the lower part of a coaxial microscope (42) by utilizing an XY precise displacement platform (6);
g) the CCD image collector (44) sends an image observed by the coaxial microscope (42) to the computer, and the computer drives the microscope to adjust the displacement of the sliding table (45) and adjust the focal length of the coaxial microscope (42) to obtain a clear image; precisely adjusting the position of the test sample by an XY precise displacement platform (6) to finally obtain the surface appearance and deformation damage of the indentation area of the material test sample under the action of high temperature;
h) and (3) processing the load-indentation depth curve Oliver-Pharr method of the test sample by combining the surface morphology and the deformation damage image of the indentation area of the material test sample under the high-temperature effect, so as to obtain the hardness and the elastic modulus of the test sample under the corresponding temperature environment, and completing the test.
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