CN110044752B - In-situ high/low temperature indentation testing device for cone beam CT imaging - Google Patents
In-situ high/low temperature indentation testing device for cone beam CT imaging Download PDFInfo
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- CN110044752B CN110044752B CN201910348219.3A CN201910348219A CN110044752B CN 110044752 B CN110044752 B CN 110044752B CN 201910348219 A CN201910348219 A CN 201910348219A CN 110044752 B CN110044752 B CN 110044752B
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- 238000012360 testing method Methods 0.000 title claims abstract description 112
- 238000007373 indentation Methods 0.000 title claims abstract description 74
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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
- G01N3/40—Investigating hardness or rebound hardness
- G01N3/54—Performing tests at high or low temperatures
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- 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
- G01N2203/0001—Type of application of the stress
- G01N2203/0003—Steady
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- 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
- G01N2203/0014—Type of force applied
- G01N2203/0016—Tensile or compressive
- G01N2203/0019—Compressive
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- 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
- G01N2203/003—Generation of the force
- G01N2203/005—Electromagnetic means
- G01N2203/0051—Piezoelectric means
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- 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
- G01N2203/0058—Kind of property studied
- G01N2203/0076—Hardness, compressibility or resistance to crushing
- G01N2203/0078—Hardness, compressibility or resistance to crushing using indentation
- G01N2203/0082—Indentation characteristics measured during load
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- 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
- G01N2203/0222—Temperature
- G01N2203/0226—High temperature; Heating means
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- 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
- G01N2203/0222—Temperature
- G01N2203/0228—Low temperature; Cooling means
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- 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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- 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
- G01N2203/06—Indicating or recording means; Sensing means
- G01N2203/0617—Electrical or magnetic indicating, recording or sensing means
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- 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
- G01N2203/06—Indicating or recording means; Sensing means
- G01N2203/0641—Indicating or recording means; Sensing means using optical, X-ray, ultraviolet, infrared or similar detectors
- G01N2203/0647—Image analysis
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- 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
- G01N2203/06—Indicating or recording means; Sensing means
- G01N2203/067—Parameter measured for estimating the property
- G01N2203/0682—Spatial dimension, e.g. length, area, angle
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Abstract
The invention relates to an in-situ high/low temperature pressure mark testing device for cone beam CT imaging, and belongs to the field of electromechanical integrated precise scientific instruments and material testing. The vibration isolator comprises a cone beam CT imaging unit, a high/low temperature pressure mark testing unit, an electric rotating platform, a vibration isolation platform and a silicone oil temperature control device, wherein the cone beam CT imaging unit, the electric rotating platform and the silicone oil temperature control device are arranged on the vibration isolation platform; the high/low temperature indentation test unit is fixed on the electric rotating platform; the high/low temperature indentation testing unit comprises a high/low temperature loading sub-module, a precision loading and detecting sub-module and a vacuum protection sub-module. The invention can develop in-situ micro-nano indentation test under the high/low temperature environment of-50 ℃ to 120 ℃ under the dynamic monitoring of the cone beam CT imaging unit, and can carry out in-situ observation and three-dimensional imaging on the microscopic deformation and damage process of the material under the action of high stress strain, thereby providing an effective technical means for revealing the mechanical behavior of the material and the constitutive relation of the microscopic structure change under the condition of force thermal coupling loading.
Description
Technical Field
The invention relates to the field of electromechanical integrated precise scientific instruments and the field of material testing, in particular to an in-situ high/low temperature indentation testing device for cone beam CT imaging. The method can realize in-situ micro-nano indentation test at the temperature of-50-120 ℃ under the high/low temperature environment, and provides a new technical means for revealing the mechanical behavior of the material and the constitutive relation of microstructure change of the material under the condition of force thermal coupling loading.
Background
In-situ micro-nano mechanical testing technology refers to testing technology which dynamically monitors the process from microscopic deformation, damage to failure and destruction of a material under the action of a load in real time through imaging instruments such as an electron microscope, an atomic force microscope or an optical microscope in the mechanical property testing process of the tested material under the micro-nano scale. The CT imaging technology is a novel material nondestructive testing technology; CT imaging is a technology which reconstructs a two-dimensional image on a specific layer of a sample by computer processing according to projection data of a certain physical quantity (such as X-ray light intensity) acquired by the periphery of the sample on the premise of not damaging the structure of the object and forms a three-dimensional image according to the obtained two-dimensional image.
With the development of novel thin film materials, micro-mechanical and micro-electronic technologies, and the like, the acquisition of mechanical performance parameters of materials at a microscopic scale becomes more important. However, these tiny components often exhibit mechanical properties that differ from those of macroscopic conditions. Therefore, the micro-nano indentation test technology is provided on the basis of the traditional macro hardness test. The micro-nano indentation test technology synchronously and precisely measures and acquires load and displacement data in the pressing process through a high-precision and high-resolution load and displacement sensor, and the pressing process finally obtains a load-displacement curve. By analyzing the curve by establishing a proper mechanical model, the mechanical performance parameters such as hardness, elastic modulus, creep property, fracture toughness, viscoelastic property and the like of the material can be accurately obtained. The micro-nano indentation test technology has little damage to the surface of the tested material, has the advantages of simple sample preparation, rich test content and the like, and becomes an important technical means for testing the materials at home and abroad.
The mechanical properties of the material are inevitably influenced by the actual service environment, especially the environment temperature, so that the indentation test technology under the high-temperature environment is researched more and the product is more, but the indentation test technology under the low-temperature environment, especially under the high/low-temperature environment is researched less. Because low temperature has different influence modes on dislocation activity, phase change process, fracture mechanism and the like of the material, cold and hot alternation can couple high temperature and low temperature states, so that the material behavior is more difficult to predict. However, the current indentation testing devices can only realize loading at high temperature or low temperature independently, and most indentation testing devices lack in-situ observation means. For example, chinese patent (CN 106404574 a) relates to a device and a method for testing high-temperature micro-nano indentation in vacuum environment, wherein the testing device placed in the vacuum cavity adopts an atmosphere heating furnace to heat the pressure head and the sample, so as to maximally ensure the consistency of the temperature of the pressure head and the sample, but only realize high-temperature loading, and has no integrated in-situ observation means. For example, chinese patent (CN 104697872A) relates to a continuous temperature-regulating high-vacuum low-temperature micro-nano indentation testing method and device, and a low-temperature thermostat with liquid nitrogen is matched with a temperature-changing object stage with a built-in heater, so that continuous contact temperature change of 77K-500K can be realized, the testing temperature range is greatly expanded, and the microscopic deformation mechanism and mechanical property of the material cannot be unified due to lack of in-situ observation means.
Therefore, the development of an in-situ micro-nano indentation testing device which integrates in-situ observation means and can realize low-temperature and high-temperature continuous temperature loading is not slow.
Disclosure of Invention
The invention aims to provide an in-situ high/low temperature indentation testing device for cone beam CT imaging, which solves the problems in the prior art. The invention is used for realizing microscopic mechanical property test of compression, indentation and the like of materials under high/low temperature loading at-50-120 ℃ in a vacuum environment, and obtaining mechanical property parameters such as hardness, elastic modulus and the like of the materials in the service environment. On the basis of CT imaging technology, the invention can carry out real-time two-dimensional fault imaging on microstructure change and defects of a sample in the indentation or compression test process of the material in a high/low temperature environment through the cone beam CT imaging unit, and can carry out three-dimensional imaging through subsequent three-dimensional reconstruction, thereby being beneficial to researching the real mechanical behavior and deformation damage mechanism of the material and the product in the actual service state of the material by correlating microstructure evolution under the indentation behavior of the material with the mechanical property parameters of the material obtained by the test. The invention researches the mechanical properties of sample materials in a high/low temperature loading environment from a microscopic angle; the method has the advantages that the knowledge of the mechanical behavior and microscopic damage mechanism of the material is enhanced, the technical means is provided, and the method has great application prospect in the field of material science.
The above object of the present invention is achieved by the following technical solutions:
the in-situ high/low temperature indentation testing device for cone beam CT imaging comprises a cone beam CT imaging unit, a high/low temperature indentation testing unit 4, an electric rotating platform 8, a vibration isolation platform 1 and a silicone oil temperature control device 9, wherein the cone beam CT imaging unit, the electric rotating platform 8 and the silicone oil temperature control device 9 are arranged on the vibration isolation platform 1; the high/low temperature indentation test unit 4 is fixed on the electric rotating platform 8 to realize 360-degree rotation of the sample 19;
the high/low temperature indentation test unit 4 comprises a high/low temperature loading sub-module, a precision loading and detecting sub-module and a vacuum protection sub-module, wherein the high/low temperature loading sub-module is as follows: the sample 19 is adhered below the carrying copper platform 20, and the thermocouple 24 is adhered outside the cylindrical surface of the sample 19; the surrounding type silicone oil groove 22 and the heat conduction grease 32 are arranged in the copper carrying platform 20, and the heat insulation layer 21 is surrounded outside the copper carrying platform 20; the silicone oil with target temperature is circularly introduced into the surrounding type silicone oil groove 22 through the silicone oil temperature control device 9 to control the temperature of the sample;
the precise loading and detecting sub-module drives the pressure head 18 and the capacitive displacement sensor 14 to move precisely in the Z direction by taking the Z-axis piezoelectric precise driving platform 11 as a power source, and finally presses the pressure head 18 into the sample 19, and performs real-time precise detection and feedback control on load/displacement signals by the force sensor 27 and the capacitive displacement sensor 14; the pressure head 18 is fixed on the heat insulation compression bar 15 through a clamping screw; the force sensor 27 is connected in series between the heat insulation compression bar 15 and the connecting rod 28 through a threaded connection; the capacitive displacement sensor 14 is fixed at the end of the displacement sensor bracket 26 by a set screw 25; the connecting rod 28 and the displacement sensor bracket 26 are fixed above the XY-axis piezoelectric driving platform 29, and the XY-axis piezoelectric driving platform 29 is fixed on the Z-axis piezoelectric precise driving platform 11; the displacement sensor conducting strip 16 and the conducting strip bracket 17 are adhered to the inner wall of the quartz glass outer wall 13;
the vacuum protection submodule is used for preventing frosting or oxidation of the surface of the sample 19 by creating a vacuum environment, the polyimide flange plate 23 and the quartz glass outer wall 13 are fixed through cementing, the quartz glass outer wall 13 and the vacuum chamber base 10, the polyimide flange plate 23 and the carrying copper table 20 are respectively fixed through threaded connection, and the sealing ring is clamped to achieve a sealing effect; the vacuum chamber is communicated with an electric circuit through gas exchange by a vacuum ball valve 12, an aviation plug 30 and an air inlet valve 31 which are fixed outside the vacuum chamber base 10.
The high/low temperature loading submodule circularly introduces the silicon oil with stable temperature into a surrounding silicon oil groove 22 arranged in the copper carrying platform 20 through a silicon oil temperature control device 9, heat conduction grease 32 is filled between the copper carrying platform 20 and the surrounding silicon oil groove 22, the heat conduction grease 32 plays a role in heat conduction, and a sample 19 is adhered below the copper carrying platform 20; the silicone oil transfers heat to/from the copper carrying table 20 and the sample 19 in a heat conduction manner in the flowing process, and the liquid flow circulation temperature control manner can continuously and stably control the temperature of the sample 19 between the boiling point and the solidifying point of the liquid flow circulation temperature control manner; the thermocouple 24 is adhered to the surface of the sample 19 to measure the surface temperature of the sample 19 in real time, and the temperature of the sample 19 is accurately controlled at-50-120 ℃.
The sample 19 is inverted above the pressure head 18 so as to place a surrounding silicone oil groove 22 in a carrying copper table 20 which rotates along with the electric rotating platform 8; the copper carrier 20 and the surrounding silicon oil sump 22 are filled with thermal grease 32, but there is no rigid connection between the two; the heat conduction grease 32 plays a role in heat conduction and lubrication, so that the surrounding silicone oil groove 22 does not rotate along with the carrying copper table 20 and is not influenced by the rotating force; the surrounding silicone oil tank 22 and the silicone oil temperature control device 9 are connected through a silicone oil pipe without being interfered by rotation.
The precise loading and detecting sub-module takes a precise piezoelectric platform as a nano indentation loading power source, the Z-axis piezoelectric precise driving platform 11 drives the pressure head 18 and the capacitive displacement sensor 14 to synchronously displace and press in a sample, and the XY-axis piezoelectric driving platform 29 drives the pressure head 18 to precisely displace and replace a pressing-in position in a horizontal plane; the force sensor 27 and the capacitive displacement sensor 14 synchronously perform precise detection and feedback control in the pressing process, and the pressing rate is controlled by adopting two modes of force control and displacement control; different kinds of indentation or compression tests can be performed by changing the indenter.
The vacuum protection submodule is connected with an external vacuum pump through a vacuum ball valve 12 and is used for vacuumizing the high/low temperature indentation test unit 4; closing the vacuum ball valve 12, and keeping high vacuum in the testing device after the testing device is disconnected with the vacuum pump, so that the rotation of the testing device is prevented from being influenced by a vacuum pipeline; after the test is completed, the air inlet valve 31 is opened to restore the pressure in the high/low temperature mark test unit 4 to the atmospheric pressure.
The quartz glass outer wall 13 of the high/low temperature indentation test unit 4 is made of quartz glass materials which do not block X rays, and the polyimide flange plate 23 and the conducting strip bracket 17 are made of polyimide materials which do not block X rays.
The electric circuit in the high/low temperature indentation test unit 4 is connected with an external computer through an aviation plug 30, a beam of electric circuit is integrated outside the high/low temperature indentation test unit 4, the allowance length is reserved, the electric rotating platform 8 rotates at a constant speed for three-dimensional imaging by matching with the cone beam CT imaging unit in the test, and the electric rotating platform slowly rotates to the initial position after the three-dimensional imaging is completed by 360 degrees of rotation.
The cone beam CT imaging unit is as follows: the X-ray microscope 3 is arranged on the three-degree-of-freedom precision displacement platform 2, the X-ray flat panel detector 5 is fixed on the detector Z-axis sliding table 7, and the detector Z-axis sliding table 7 is fixed on the detector X-axis sliding table 6. The X-ray microscope 3 and the X-ray flat panel detector 5 are respectively positioned at two sides of the high/low temperature indentation test unit 4.
The invention has the beneficial effects that: novel conception and compact structure. Aiming at the problem that the existing indentation testing device lacks an in-situ observation means, the in-situ high/low temperature indentation testing device for cone beam CT imaging is provided. The method can realize real-time monitoring and two-dimensional and three-dimensional imaging of the microstructure change of the measured material by CT imaging technology in the process of testing the micromechanics properties such as compression, indentation and the like of the material under the high/low temperature loading condition. The invention researches the physical and mechanical properties of sample materials in a high/low temperature loading environment from a microscopic angle; the technical means is provided for strengthening the knowledge of the mechanical behavior and microscopic damage mechanism of the material. Aiming at the problem that the indentation testing device at home and abroad can only independently realize high-temperature or low-temperature loading, the invention can realize large-range temperature loading from low temperature to high temperature of-50 to 120 ℃, and greatly expands the temperature range of indentation testing. Has important guiding significance for researching the mechanical behavior of the material under the condition of force-heat coupling loading.
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 and explain the invention and together with the description serve to explain the invention.
FIG. 1 is a schematic diagram of the overall structure of the present invention;
FIG. 2 is a schematic cross-sectional view of a high/low temperature indentation test unit according to the present invention;
FIG. 3 is a cross-sectional view of the high/low temperature loading unit of the present invention;
FIG. 4 is a schematic view of a cone beam CT imaging unit according to the present invention;
fig. 5 is a schematic view of an X-ray path of a cone beam CT imaging unit according to the present invention.
In the figure: 1. a vibration isolation table; 2. a three-degree-of-freedom precision displacement platform; 3. an X-ray microscope; 4. a high/low temperature indentation test unit; 5. an X-ray flat panel detector; 6. x-axis sliding table of detector; 7. z-axis sliding table of detector; 8. an electric rotating platform; 9. a silicone oil temperature control device; 10. a vacuum chamber base; 11. a Z-axis piezoelectric precision driving platform; 12. a vacuum ball valve; 13. a quartz glass outer wall; 14. a capacitive displacement sensor; 15. a thermal insulation compression bar; 16. a displacement sensor conductive sheet; 17. a conductive sheet holder; 18. a pressure head; 19. a sample; 20. a copper carrying table; 21. a thermal insulation layer; 22. surrounding type silicon oil groove; 23. polyimide flange plate; 24. a thermocouple; 25. a set screw; 26. a displacement sensor support; 27. a force sensor; 28. a connecting rod; 29. an XY axis piezoelectric driving platform; 30. aviation plug; 31. an intake valve; 32. and (5) heat conducting grease.
Description of the embodiments
The details of the present invention and its specific embodiments are further described below with reference to the accompanying drawings.
Referring to fig. 1 to 5, the in-situ high/low temperature indentation testing apparatus for cone beam CT imaging of the present invention organically combines a CT non-destructive testing technique with an indentation testing technique; in-situ nanoindentation testing in high/low temperature environments can be performed under dynamic monitoring of cone beam CT imaging units. The invention can develop micro-nano indentation test aiming at the mechanical property change of the material in a high/low temperature environment of-50 ℃ to 120 ℃, can also conduct in-situ observation and three-dimensional imaging on the microscopic deformation and damage process of the material under the action of high stress strain, and provides a new technical means for developing the physical and mechanical property research of the sample material in the high/low temperature loading environment from a microscopic angle. The invention relates to an in-situ high/low temperature mark testing device for cone beam CT imaging, which comprises a cone beam CT imaging unit, a high/low temperature mark testing unit 4, an electric rotating platform 8, a vibration isolation platform 1 and a silicone oil temperature control device 9, wherein the cone beam CT imaging unit, the electric rotating platform 8 and the silicone oil temperature control device 9 are arranged on the vibration isolation platform 1; the high/low temperature indentation test unit 4 is fixed on the electric rotating platform 8 to realize 360-degree rotation of the sample 19;
the high/low temperature indentation test unit 4 comprises a high/low temperature loading sub-module, a precision loading and detecting sub-module and a vacuum protection sub-module, wherein the high/low temperature loading sub-module is as follows: the sample 19 is adhered below the carrying copper platform 20, and the thermocouple 24 is adhered outside the cylindrical surface of the sample 19; the surrounding type silicone oil groove 22 and the heat conduction grease 32 are arranged in the copper carrying platform 20, and the heat insulation layer 21 is surrounded outside the copper carrying platform 20; the silicone oil with target temperature is circularly introduced into the surrounding type silicone oil groove 22 through the silicone oil temperature control device 9 to control the temperature of the sample;
the precise loading and detecting sub-module drives the pressure head 18 and the capacitive displacement sensor 14 to move precisely in the Z direction by taking the Z-axis piezoelectric precise driving platform 11 as a power source, and finally presses the pressure head 18 into the sample 19, and performs real-time precise detection and feedback control on load/displacement signals by the force sensor 27 and the capacitive displacement sensor 14; the pressure head 18 is fixed on the heat insulation compression bar 15 through a clamping screw; the force sensor 27 is connected in series between the heat insulation compression bar 15 and the connecting rod 28 through a threaded connection; the capacitive displacement sensor 14 is fixed at the end of the displacement sensor bracket 26 by a set screw 25; the connecting rod 28 and the displacement sensor bracket 26 are fixed above the XY-axis piezoelectric driving platform 29, and the XY-axis piezoelectric driving platform 29 is fixed on the Z-axis piezoelectric precise driving platform 11; the displacement sensor conducting strip 16 and the conducting strip bracket 17 are adhered to the inner wall of the quartz glass outer wall 13;
the vacuum protection submodule is used for preventing frosting or oxidation of the surface of the sample 19 by creating a vacuum environment, the polyimide flange plate 23 and the quartz glass outer wall 13 are fixed through cementing, the quartz glass outer wall 13 and the vacuum chamber base 10, the polyimide flange plate 23 and the carrying copper table 20 are respectively fixed through threaded connection, and the sealing ring is clamped to achieve a sealing effect; the vacuum chamber is communicated with an electric circuit through gas exchange by a vacuum ball valve 12, an aviation plug 30 and an air inlet valve 31 which are fixed outside the vacuum chamber base 10.
The high/low temperature loading submodule circularly introduces the silicon oil with stable temperature into a surrounding silicon oil groove 22 arranged in the copper carrying platform 20 through a silicon oil temperature control device 9, heat conduction grease 32 is filled between the copper carrying platform 20 and the surrounding silicon oil groove 22, the heat conduction grease 32 plays a role in heat conduction, and a sample 19 is adhered below the copper carrying platform 20; the silicone oil transfers heat to/from the copper carrying table 20 and the sample 19 in a heat conduction manner in the flowing process, and the liquid flow circulation temperature control manner can continuously and stably control the temperature of the sample 19 between the boiling point and the solidifying point of the liquid flow circulation temperature control manner; the thermocouple 24 is adhered to the surface of the sample 19 to measure the surface temperature of the sample 19 in real time for feedback control, and the adhesion mode can directly and accurately measure the surface temperature of the sample 19; the invention can accurately control the temperature of the sample 19 at-50-120 ℃.
Unlike the conventional indentation test device, which arranges the indenter and the driving unit above the sample, the present invention adopts an arrangement in which the sample 19 is inverted above the indenter 18, and in this arrangement, the surrounding silicone oil tank 22 can be conveniently placed in the copper carrying table 20 rotating with the electric rotating platform 8; the copper carrier 20 and the surrounding silicon oil sump 22 are filled with thermal grease 32, but there is no rigid connection between the two; the heat conduction grease 32 plays a role in heat conduction and lubrication, so that the surrounding silicone oil groove 22 does not rotate along with the carrying copper table 20 and is not influenced by the rotating force; the surrounding silicone oil tank 22 and the silicone oil temperature control device 9 are connected through a silicone oil pipe without being interfered by rotation.
The precise loading and detecting sub-module takes a precise piezoelectric platform as a nano indentation loading power source, the Z-axis piezoelectric precise driving platform 11 drives the pressure head 18 and the capacitive displacement sensor 14 to synchronously displace and press in a sample, and the XY-axis piezoelectric driving platform 29 drives the pressure head 18 to precisely displace and replace a pressing-in position in a horizontal plane; the force sensor 27 and the capacitive displacement sensor 14 synchronously perform precise detection and feedback control in the pressing process, and the pressing rate is controlled by adopting two modes of force control and displacement control; different kinds of indentation or compression tests can be performed by changing the indenter.
The vacuum protection submodule is connected with an external vacuum pump through a vacuum ball valve 12 and is used for vacuumizing the high/low temperature indentation test unit 4; the vacuum environment avoids the influence of frosting on the surface of the material at low temperature and accelerated oxidation of the material at high temperature on the test result. Closing the vacuum ball valve 12, and keeping high vacuum in the testing device after the testing device is disconnected with the vacuum pump, so that the rotation of the testing device is prevented from being influenced by a vacuum pipeline; after the test is completed, the air inlet valve 31 is opened, so that the pressure in the high/low temperature pressure mark test unit 4 is recovered to the atmospheric pressure, and the sample is convenient to replace for subsequent test.
The quartz glass outer wall 13, the polyimide flange plate 23 and the conductive sheet support 17 of the high/low temperature indentation test unit 4 are made of quartz glass and polyimide materials which do not block X rays, and the imaging quality of the cone beam CT imaging unit on the sample 19 is not affected. Meanwhile, the low heat conductivity of the polyimide flange plate 23 can reduce the temperature of the carrying copper table 20 to be transmitted to other sealing parts, so that the sealing effect is prevented from being influenced by temperature change.
The electric circuit in the high/low temperature indentation test unit 4 is connected with an external computer through an aviation plug 30, a bundle of electric circuits is integrated outside the high/low temperature indentation test unit 4, and a certain allowance length is reserved to prevent the electric circuit from being broken when the high/low temperature indentation test unit 4 rotates for 360 degrees. In the test, the electric rotating platform 8 rotates at a constant speed for 360 degrees to be matched with the cone beam CT imaging unit for three-dimensional imaging, and the electric rotating platform slowly rotates to an initial position after the three-dimensional imaging is completed by 360 degrees. The invention can complete three-dimensional imaging by matching with the cone beam CT imaging unit under the premise of not damaging an electric circuit by adopting the rotation mode.
Referring to fig. 4, the cone beam CT imaging unit is that an X-ray microscope 3 is mounted on a three-degree-of-freedom precision displacement platform 2, an X-ray flat panel detector 5 is fixed on a detector Z-axis sliding table 7, and the detector Z-axis sliding table 7 is fixed on a detector X-axis sliding table 6. The X-ray microscope 3 and the X-ray flat panel detector 5 are respectively positioned at two sides of the high/low temperature indentation test unit 4.
Referring to fig. 1 to 5, the in-situ high/low temperature indentation testing device for cone beam CT imaging of the present invention can perform indentation and compression mechanical property testing on a tested material under high/low temperature loading at-50 ℃ to 120 ℃ in a vacuum environment, and simultaneously perform real-time in-situ monitoring on a sample by adopting an X-ray microscope. The invention is used for researching constitutive relation between microstructure change of the material and mechanical property parameters thereof under the condition of force thermal coupling loading. The related components and specific models are as follows: the Z-axis piezoelectric driving platform 11 is ECSZ5050, the XY-axis piezoelectric driving point changing platform 29 is ECSxy5050/AL/RT, the capacitive displacement sensor 14 is capaNCDT CS02, the force sensor 27 is Model31 Mid-1000g, and the electric rotating platform 8 is RAK100. The Z-axis piezoelectric precise driving platform 11 drives the capacitive displacement sensor 14 and the pressure head 18 to synchronously displace to load the sample 19, and the XY-axis piezoelectric driving platform drives the pressure head 18 to precisely displace in the horizontal plane to change the pressing-in position. The force sensor 27 performs precision detection and feedback control in synchronization with the capacitive displacement sensor 14 during the press-in process. The pressing rate can be controlled by adopting two modes of force control and displacement control. The electric rotating platform 8 drives the high/low temperature indentation testing unit 4 and the sample 19 to rotate at a constant speed of 360 degrees, and the cone beam CT imaging unit monitors the microstructure change in the sample 19 in real time and performs two-dimensional tomography. And carrying out three-dimensional reconstruction on the two-dimensional tomographic image obtained in the rotation process of the sample 19 at a later stage to finally obtain a three-dimensional stereo image of the internal microstructure of the sample 19 and three-dimensional size information of the internal defect.
In the specific test process, firstly, a tested sample is processed into a cylindrical test piece with a fixed size by adopting a linear cutting mode. The surface of sample 19 was sanded with sandpaper to give it a better finish for in situ visualization. Sample 19 was electropolished pressed into the surface to reduce the effect of surface roughness on the test results. Sample 19 was adhered under copper carrier 20 and thermocouple 24 was adhered to the cylindrical surface of sample 19. The pressure head 18 is selected according to the type of test, and the clamping screw is tightened to fix the pressure head 18 above the heat insulation compression bar 15. The external thread of the force sensor 27 is fixedly connected with the internal thread of the heat insulation compression bar 15. The force sensor 28 is fixed above the XY axis piezoelectric driving stage 29 by a connecting rod 28. Then the quartz glass outer wall 13 and the vacuum chamber base 10, the polyimide flange plate 23 and the copper carrying table 20 are fixed by bolts, and the sealing ring is pressed tightly to achieve a sealing effect. Vacuum is pumped by an external vacuum pump, and after the vacuum pumping is finished, the vacuum ball valve 12 is closed and the vacuum pipeline is disconnected. The surrounding type silicon oil groove 22 is placed above the carrying copper platform 20, and the heat insulation layer 21 is sleeved outside the carrying copper platform. And starting the silicone oil temperature control device 9 to circularly introduce the silicone oil with the target temperature into the surrounding type silicone oil groove 22 to heat/refrigerate the sample 19, and detecting and feedback-controlling the temperature of the sample 19 through the thermocouple 24.
In the pressing process, an external computer controls the Z-axis piezoelectric precision driving platform 11 to serve as a loading driver to drive the pressure head 18 and the capacitive displacement sensor 14 to move precisely for testing. After the point test is completed, the XY axis piezoelectric driving platform 29 fixed above the Z axis piezoelectric precision driving platform 11 drives the pressing head 18 to horizontally displace to replace the next pressing point. The capacitive displacement sensor 14 is fixed inside the displacement sensor bracket 26 by a set screw 25. The displacement sensor conductive sheet 16 is fixed below the conductive sheet support 17, and the conductive sheet support 17 is adhered inside the quartz glass outer wall 13. The force sensor 27 and the capacitive displacement sensor 14 precisely detect the pressing load and the pressing displacement in real time and send data to an external computer in the process that the Z-axis piezoelectric precise driving platform drives the pressing head 18 to press the sample.
The positions of the X-ray microscope 3 and the X-ray flat panel detector 5 are precisely adjusted by matching the three-degree-of-freedom precise displacement platform 2 with the detector X-axis sliding table 6 and the detector Z-axis sliding table 7; the sample is ensured to be positioned in an imaging center, and the X-ray microscope 3 and the X-ray flat panel detector 5 are used for carrying out real-time two-dimensional tomographic imaging observation on the sample 19 in the test process. If three-dimensional imaging of the sample 19 is desired, the electric rotating platform 8 is started in the testing process to drive the high/low temperature indentation testing unit 4 and the sample 19360 degrees to rotate, and three-dimensional reconstruction is performed on the two-dimensional tomographic image obtained in the rotating process after the testing is completed to obtain three-dimensional size information and a three-dimensional image. The electric circuit inside the high/low temperature indentation test unit 4 is connected with an external computer through an aviation plug 30 fixed outside the vacuum base 10, the silicone oil temperature control device 9 is closed after the test is completed, the air inlet valve 31 is opened, and the electric rotating platform 8 rotates to an initial position.
And combining the two-dimensional tomographic image and the three-dimensional image obtained in the testing process, and analyzing the load-displacement curve obtained by the test through a proper mechanical model to accurately obtain the mechanical performance parameters such as hardness, elastic modulus, fracture toughness and the like for representing the mechanical properties of the material.
The above description is only a preferred example of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. An in-situ high/low temperature indentation testing device for cone beam CT imaging, which is characterized in that: the vibration isolator comprises a cone beam CT imaging unit, a high/low temperature indentation testing unit (4), an electric rotating platform (8), a vibration isolation platform (1) and a silicone oil temperature control device (9), wherein the cone beam CT imaging unit, the electric rotating platform (8) and the silicone oil temperature control device (9) are arranged on the vibration isolation platform (1); the high/low temperature indentation test unit (4) is fixed on the electric rotating platform (8);
the high/low temperature indentation test unit (4) comprises a high/low temperature loading sub-module, a precision loading and detecting sub-module and a vacuum protection sub-module, wherein the high/low temperature loading sub-module is as follows: the sample (19) is adhered below the carrying copper table (20), and the thermocouple (24) is adhered outside the cylindrical surface of the sample (19); the inside of the carrying copper table (20) is provided with a surrounding type silicon oil groove (22) and heat conduction grease (32), and the outside of the carrying copper table (20) is surrounded by a heat insulation layer (21); the silicon oil with target temperature is circularly led into a surrounding silicon oil groove (22) through a silicon oil temperature control device (9) to control the temperature of the sample;
the precise loading and detecting sub-module drives the pressure head (18) and the capacitive displacement sensor (14) to move in the Z direction precisely by taking the Z-axis piezoelectric precise driving platform (11) as a power source, and finally presses the pressure head (18) into the sample (19), and the load/displacement signal is precisely detected and feedback controlled in real time by the force sensor (27) and the capacitive displacement sensor (14); the pressure head (18) is fixed on the heat insulation compression bar (15) through a clamping screw; the force sensor (27) is connected in series between the heat insulation compression bar (15) and the connecting rod (28) through screw threads; the capacitive displacement sensor (14) is fixed at the tail end of the displacement sensor bracket (26) through a set screw (25); the connecting rod (28) and the displacement sensor bracket (26) are fixed above the XY-axis piezoelectric driving platform (29), and the XY-axis piezoelectric driving platform (29) is fixed on the Z-axis piezoelectric precise driving platform (11); the displacement sensor conducting strip (16) and the conducting strip bracket (17) are adhered to the inner wall of the quartz glass outer wall (13);
the vacuum protection submodule is used for preventing frosting or oxidation on the surface of a sample (19) by creating a vacuum environment, the polyimide flange plate (23) is fixed with the quartz glass outer wall (13) through cementing, and the polyimide flange plate (23) is respectively fixed with the vacuum chamber base (10) and the copper carrying platform (20) through threaded connection, and the sealing ring is clamped to achieve a sealing effect; the vacuum chamber is communicated with an electric circuit through gas exchange by a vacuum ball valve (12), an aviation plug (30) and an air inlet valve (31) which are fixed outside a vacuum chamber base (10);
the high/low temperature loading submodule circularly introduces the silicon oil with stable temperature into a surrounding type silicon oil groove (22) arranged in the copper carrying platform (20) through a silicon oil temperature control device (9), heat conduction grease (32) is filled between the copper carrying platform (20) and the surrounding type silicon oil groove (22), the heat conduction grease (32) plays a role in heat conduction, and a sample (19) is adhered below the copper carrying platform (20); the silicone oil transfers heat into/out of the copper carrying table (20) and the sample (19) in the flowing process in a heat conduction mode, and the liquid flow circulation temperature control mode can continuously and stably control the temperature of the sample (19) between the boiling point and the solidifying point of the liquid flow circulation temperature control mode; the thermocouple (24) is adhered to the surface of the sample (19), the surface temperature of the sample (19) is measured in real time, and the sample (19) is precisely controlled at-50-120 ℃;
the precise loading and detecting sub-module takes a precise piezoelectric platform as a nano indentation loading power source, a Z-axis piezoelectric precise driving platform (11) drives a pressing head (18) to synchronously displace with a capacitive displacement sensor (14) to press in a sample, and an XY-axis piezoelectric driving platform (29) drives the pressing head (18) to precisely displace in a horizontal plane to change the pressing position; in the pressing-in process, a force sensor (27) and a capacitive displacement sensor (14) synchronously perform precise detection and feedback control, and the pressing-in rate is controlled by adopting two modes of force control and displacement control; different kinds of indentation or compression tests were performed by changing the indenter.
2. The in situ high/low temperature indentation testing device for cone beam CT imaging as claimed in claim 1, wherein: the sample (19) is inverted above the pressure head (18) so as to conveniently place a surrounding silicon oil groove (22) in a carrying copper table (20) rotating along with the electric rotating platform (8); the copper carrying platform (20) and the surrounding silicon oil groove (22) are filled with heat conduction grease (32), but no rigid connection exists between the copper carrying platform and the surrounding silicon oil groove; the heat conduction grease (32) has the heat conduction function and the lubrication function, so that the surrounding silicone oil groove (22) does not rotate along with the carrying copper table (20) and is not influenced by the rotation force; the surrounding type silicone oil tank (22) and the silicone oil temperature control device (9) are connected through a silicone oil pipe without being interfered by rotation.
3. The in situ high/low temperature indentation testing device for cone beam CT imaging as claimed in claim 1, wherein: the vacuum protection submodule is connected with an external vacuum pump through a vacuum ball valve (12) and is used for vacuumizing the high/low temperature indentation test unit (4); closing a vacuum ball valve (12), and keeping high vacuum in the test device after the test device is disconnected with the vacuum pump, so that the rotation of the test device is prevented from being influenced by a vacuum pipeline; after the test is completed, the air inlet valve (31) is opened, so that the pressure in the high/low temperature pressure mark test unit (4) is recovered to the atmospheric pressure.
4. The in situ high/low temperature indentation testing device for cone beam CT imaging as claimed in claim 1, wherein: the quartz glass outer wall (13) of the high/low temperature indentation test unit (4) is made of quartz glass materials which do not block X rays, and the polyimide flange plate (23) and the conducting plate bracket (17) are made of polyimide materials which do not block X rays.
5. The in situ high/low temperature indentation testing device for cone beam CT imaging as claimed in claim 1, wherein: the electric circuit in the high/low temperature indentation test unit (4) is connected with an external computer through an aviation plug (30), the electric circuit is integrated with one beam outside the high/low temperature indentation test unit (4) and is provided with a residual length, the electric rotating platform (8) rotates at a constant speed for three-dimensional imaging by matching with the cone beam CT imaging unit in the test, and the electric rotating platform slowly rotates to an initial position after the three-dimensional imaging is completed by 360 degrees of rotation.
6. The in situ high/low temperature indentation testing device for cone beam CT imaging as claimed in claim 1, wherein: the cone beam CT imaging unit is as follows: the X-ray microscope (3) is arranged on the three-degree-of-freedom precision displacement platform (2), the X-ray flat panel detector (5) is fixed on the detector Z-axis sliding table (7), and the detector Z-axis sliding table (7) is fixed on the detector X-axis sliding table (6); the X-ray microscope (3) and the X-ray flat panel detector (5) are respectively positioned at two sides of the high/low temperature indentation test unit (4).
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| CN111289357B (en) * | 2020-04-01 | 2022-03-29 | 南京工业大学 | Clamp device for vacuum high-temperature indentation creep test |
| CN111855457B (en) * | 2020-07-14 | 2024-07-09 | 吉林大学 | Traceable in-situ micro-nano indentation test instrument and method under variable temperature working condition |
| CN112255111B (en) * | 2020-09-14 | 2023-04-14 | 中国航发北京航空材料研究院 | Miniature loading device for DVC method test under ultralow temperature condition |
| WO2023150755A1 (en) * | 2022-02-07 | 2023-08-10 | West Pharmaceutical Services, Inc. | Scanning parts at target temperatures |
| CN117030430B (en) * | 2023-08-04 | 2024-02-06 | 青岛海洋地质研究所 | Hydrate nanometer indentation device |
| CN117129355B (en) * | 2023-10-23 | 2024-02-13 | 北京大学 | High-temperature visual micrometer indentation test device and method |
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