CN112834321A - In-situ loading micro CT characterization system in ultralow temperature environment and characterization method thereof - Google Patents
In-situ loading micro CT characterization system in ultralow temperature environment and characterization method thereof Download PDFInfo
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- CN112834321A CN112834321A CN202110018265.4A CN202110018265A CN112834321A CN 112834321 A CN112834321 A CN 112834321A CN 202110018265 A CN202110018265 A CN 202110018265A CN 112834321 A CN112834321 A CN 112834321A
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- 238000012512 characterization method Methods 0.000 title claims abstract description 33
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 31
- 238000010438 heat treatment Methods 0.000 claims abstract description 62
- 238000012360 testing method Methods 0.000 claims abstract description 29
- 238000002591 computed tomography Methods 0.000 claims abstract description 8
- 238000009413 insulation Methods 0.000 claims description 48
- 238000005057 refrigeration Methods 0.000 claims description 32
- 239000000463 material Substances 0.000 claims description 31
- 239000007788 liquid Substances 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 238000010603 microCT Methods 0.000 claims description 14
- 230000004044 response Effects 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- 238000002474 experimental method Methods 0.000 claims description 9
- 230000001105 regulatory effect Effects 0.000 claims description 8
- 239000004964 aerogel Substances 0.000 claims description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 3
- 238000009423 ventilation Methods 0.000 claims description 3
- 239000007769 metal material Substances 0.000 claims description 2
- 230000005540 biological transmission Effects 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 230000007246 mechanism Effects 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
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- 238000006467 substitution reaction Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/02—Details
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
- G01N23/04—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and forming images of the material
- G01N23/046—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and forming images of the material using tomography, e.g. computed tomography [CT]
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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
- G01N3/02—Details
- G01N3/06—Special adaptations of indicating or recording means
-
- 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
- G01N2203/06—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
Abstract
The invention discloses an in-situ loading micro CT characterization system and a characterization method thereof in an ultralow temperature environment. The mechanical testing machine is provided with an experimental environment box body, the tail ends of a pair of clamps are fixed on a beam of the mechanical testing machine, the head ends of the clamps extend into the experimental environment box body to clamp a sample, the environment temperature in the experimental environment box body is controlled by a refrigerating device and a heating device, the real-time feedback is realized by a temperature measuring element, and the transmission of heat in the experimental environment box body is accelerated by matching with a flow guide structure, so that the negative feedback control with rapid and accurate temperature is realized, the mechanical testing machine mechanically loads the sample by the clamps, and meanwhile, a microfocus X-ray source carries out micro CT scanning on the sample through an anti-fog-frost ray window, so that the microstructure and the damage morphology inside the sample when the sample is loaded in situ in an ultralow temperature environment are reconstructed; and through the anti-fog and frost-proof ray window, the phenomena of fogging and frosting of the window sheet at the outer side are avoided.
Description
Technical Field
The invention relates to the field of material microstructure characterization, in particular to an in-situ loading micro CT characterization system in an ultralow temperature environment and a characterization method thereof.
Background
In an ultralow temperature environment, the failure mechanism and damage evolution rule of the material are often obviously different from those of the material in a normal temperature environment. And the study on the failure mechanism and the damage evolution rule of the material needs to observe the internal microstructure and the damage morphology of the material under the condition of in-situ loading in the ultralow temperature environment. Therefore, for better evaluation of the reliability of the material, the reconstruction of the microstructure and the damage morphology of the material in situ under the ultralow temperature environment through the micro CT has great significance.
The existing research on the failure mechanism and the damage evolution law of the material adopts an off-position step-by-step research method, namely, the material is firstly placed in an ultralow temperature environment set by an experiment, after the internal temperature of the material is stable, the material is taken out and clamped on a mechanical testing machine, and the microstructure and the damage morphology inside the material when the material is loaded are reconstructed through X-ray micro CT while the material is loaded in a room temperature environment. Since the micro CT scan takes a long time, one scan lasts more than one hour, so that the temperature of the material changes significantly during the experiment, and even the temperature of the material returns to room temperature before the experiment is finished. The off-site step-by-step research method cannot obtain the internal microstructure and damage morphology of the material at a certain temperature, and the obtained data has larger errors.
Utilize the liquid nitrogen can build the required ultra-low temperature environment of experiment fast to temperature in the box that the temperature measurement element found is adjusted the feed liquor rate according to temperature negative feedback and is come the temperature of accurate regulation experiment environment box, when the box temperature is higher than the settlement temperature, improve feed liquor rate, nevertheless when the box temperature is less than the settlement temperature, need slowly wait for the box in the temperature rise to the settlement temperature, this process greatly increased the response time of control, thereby lead to the temperature great fluctuation to appear.
Disclosure of Invention
The invention provides a characterization system and a characterization method for in-situ loading micro CT in an ultralow temperature environment, aiming at realizing the characterization system for in-situ loading and micro CT scanning in the ultralow temperature environment and stable temperature control.
The invention aims to provide an in-situ loading micro CT characterization system in an ultralow temperature environment.
The in-situ loading micro CT characterization system in the ultralow temperature environment comprises: the device comprises a mechanical testing machine, a clamp, an exhaust valve, an experimental environment box body, a flow guide structure, a circulating fan, a refrigerating device, a fixing frame, a control unit, a temperature measuring element, an anti-fog-frost ray window, a heating device, a microfocus X-ray source and a detector; wherein, a fixed mount is arranged on a lower beam of the mechanical testing machine; an experimental environment box body is arranged on the fixed frame; a flow guide structure is arranged in the experimental environment box body, and divides the internal space of the experimental environment box body into two relatively independent spaces which are a sample cavity and a refrigeration cavity respectively; the tail ends of the pair of clamps are respectively fixed on an upper cross beam and a lower cross beam of the mechanical testing machine, the head ends of the pair of clamps respectively penetrate through the top wall and the bottom wall of the experimental environment box body and hermetically extend into a sample cavity in the experimental environment box body, and the pair of clamps are completely identical, are positioned on the same vertical straight line and are vertically symmetrical about a central horizontal plane; a circulating fan is arranged in a refrigerating cavity in the experimental environment box body; a heating device is arranged in a sample cavity of the experimental environment box body; the refrigerating device positioned outside the experimental environment box body conveys the refrigerating liquid to a refrigerating cavity in the experimental environment box body; a temperature measuring element is arranged in the experimental environment box body; an exhaust valve is arranged on the top wall of the experimental environment box body; the method comprises the following steps that anti-fog-frost ray windows are respectively arranged on a pair of opposite side walls of an experimental environment box body; the microfocus X-ray source and the detector respectively face the anti-fog and anti-frost ray window;
the clamp comprises a clamp base, a temperature-relieving waterway, a clamp heat-insulating section, a fixed connecting piece, a clamp connecting section and a clamp head; the tail end of the clamp is provided with a clamp base, a temperature-slow water path is arranged in the clamp base, and the temperature-slow water path is connected to the water pump through a water pipe; a clamp heat insulation section is arranged on the clamp base and is made of a material with a low heat conduction coefficient; a fixture connecting section is arranged on the fixture heat insulation section; the tail end of the clamp connecting section is fixedly connected with the clamp base and the clamp heat insulation section through fixed connecting pieces; arranging a clamp head at the head end of the clamp connecting section; the clamp base, the clamp heat insulation section, the clamp connecting section and the clamp head are coaxial;
the flow guide structure comprises a flow guide plate and a cylindrical duct structure; the guide plate comprises two plane baffles which are vertically symmetrical about a central horizontal plane, and a plurality of ventilation holes which are uniformly distributed are arranged on the plane baffles; each plane baffle plate and the central horizontal plane have an inclination angle, and the inclination angle faces the refrigeration cavity; a through hole is formed in the middle of the guide plate, a cylindrical duct structure is arranged on the through hole, the cylindrical duct structure is a cylindrical shell, and the cylindrical duct structure is positioned in the refrigerating cavity;
the circulating fan comprises fan blades, a long fan shaft and a motor; the motor is positioned on the outer side wall of the experimental environment box body; the fan blade is positioned in a cylindrical duct structure of the flow guide structure in the experimental environment box body, and the outer diameter of the fan blade is smaller than the inner diameter of the cylindrical duct structure; one end of a long shaft of the horizontal fan is connected with the motor, and the other end of the long shaft of the horizontal fan penetrates through the side wall of the experimental environment box body to fan blades in the experimental environment box and located in the cylindrical ducted structure; a liquid outlet of the refrigerating device extends into the cylindrical duct structure and is opposite to the back surface of the fan blade of the fan;
the anti-fog-frost ray window comprises a window flange pipe, an inner side window sheet, a heat insulation ring, a heating ring, an outer side window sheet and a fixed cover plate; coaxial and horizontal through holes are formed in a pair of opposite side walls of the experimental environment box body, and sealed window flange pipes are arranged on the through holes; an inner side window sheet is arranged at one end of the window flange pipe, which is positioned on the inner wall of the experimental environment box body, and a sealed heat insulation ring is arranged at one end of the window flange pipe, which is positioned on the outer wall of the experimental environment box body; a heating ring which is tightly attached is arranged outside the heat insulation ring; an outer window sheet is arranged outside the heating ring; the outer surface of the outer window sheet is provided with a fixed cover plate which is in a circular ring shape, so that the heat insulation ring, the heating ring and the outer window sheet are tightly attached and fixed; the window flange pipe, the inner side window sheet, the heat insulation ring, the heating ring, the outer side window sheet and the fixed cover plate are all coaxial;
the heating device, the refrigerating device, the circulating fan, the temperature measuring element and the heating ring of the anti-fog and frost-ray window are connected to a control unit outside the experimental environment box body through leads;
a sample is placed in a sample cavity in the experimental environment box body and is fixed by a pair of clamps; the liquid outlet rate of the refrigerating device and the power of the heating device are controlled by the control unit, and an adjustable cold source and a heat source are provided for the experiment environment box body; the circulating fan quickly vaporizes refrigerating liquid from a liquid outlet of the refrigerating device and blows refrigerating gas to a sample along the cylindrical duct structure, the refrigerating gas is divided into an upper path and a lower path after being conveyed to the sample cavity, the refrigerating gas returns to the refrigerating cavity through the vent hole in the guide plate and enters the sample cavity through the cylindrical duct structure again through the suction force of the circulating fan, so that circulation is formed, the flow of gas in the experimental environment box body is accelerated, and redundant gas is discharged out of the experimental environment box body through the exhaust valve; the temperature measuring element detects the ambient temperature around the sample in real time and feeds measured data back to the control unit in real time, when the ambient temperature around the sample is lower than a set temperature, the heating device works to improve the ambient temperature around the sample to the set temperature, the heating device shortens the response time of temperature control, and the heating device is matched with the flow guide structure to realize the quick response of temperature control, so that the fluctuation of the ambient temperature around the sample is reduced; the mechanical testing machine mechanically loads a sample through a clamp, meanwhile, a micro-focus X-ray source conducts micro CT scanning on the sample through one anti-fog-frost ray window, a detector collects rays transmitted by the sample through the other anti-fog-frost ray window, and the temperature of a window sheet on the outer side of the anti-fog-frost ray window is regulated and controlled by a heating ring to be always higher than the room temperature, so that the phenomena of fogging and frosting of the window sheet on the outer side are avoided, and the sample can be accurately reconstructed; the water pipe leads to hot water in to slowly warm water route in the experimentation, cooperates the anchor clamps heat insulation section of low thermal conductivity, avoids the ultra-low temperature environment in the experimental environment box to produce the influence through the heat-conduction of anchor clamps to the normal work of mechanical testing machine, and the microstructure and the damage appearance of inside when sample normal position was carried under the reconsitution ultra-low temperature environment.
The mechanical testing machine is of a frame structure and comprises a horizontal upper cross beam, a horizontal lower cross beam and a vertical stand column support for supporting the upper cross beam and the lower cross beam, the upper cross beam is a movable cross beam and can move up and down along the vertical direction, and the lower cross beam is a fixed cross beam.
The anchor clamps through-hole has been seted up respectively at the roof and the diapire of experimental environment box, and the head end of a pair of anchor clamps stretches into to the experimental environment box in through-hole of anchor clamps respectively, respectively installs modified polytetrafluoroethylene ultra-low temperature in the anchor clamps through-hole and moves the sealing ring and seal, prevents that gas from revealing along anchor clamps in the experimental process experimental environment box to influence the normal work of mechanics testing machine.
The refrigerating device includes: the refrigeration system comprises a refrigeration tank, a refrigeration pipe and an electromagnetic valve; wherein, be located the refrigeration jar outside the experimental environment box and be connected to the refrigeration chamber in the experimental environment box through the refrigeration pipe, the liquid outlet of refrigeration pipe is located the refrigeration chamber in the experimental environment box, sets up the solenoid valve on the refrigeration pipe, and the solenoid valve is connected to the control unit. The temperature regulating range of the refrigerating device and the heating device in the experimental environment box body is-196 ℃ to-30 ℃, and the fluctuation error after the temperature is stable is 1 ℃.
The front box wall of the experimental environment box body is integrally a box body box door, is fixed on the experimental environment box body through screws and is sealed through a lead ring. The experimental environment box body comprises an inner wall, an outer wall and an aerogel heat insulation layer, wherein the aerogel heat insulation layer is filled between the inner wall and the outer wall which are parallel to each other.
The heating device employs an element that generates heat by energization. The material of the heat insulation section of the clamp adopts an ultralow temperature resistant low-thermal conductivity material.
The heat insulation ring is made of an ultralow temperature resistant low-thermal conductivity material; the heating ring adopts an element which generates heat by electrification; the inner window sheet and the outer window sheet are made of low-density materials; the fixed cover plate is a metal ring.
The tail end of the clamp head is provided with an external thread, the head end of the clamp connecting section is provided with an internal thread, and the clamp head and the clamp connecting section are connected through the thread. The fixed connecting piece adopts a connecting pin; the head end of anchor clamps base is provided with the base recess, and anchor clamps thermal-insulated section is located the base recess, and the head end of anchor clamps thermal-insulated section has thermal-insulated section recess, and the end of anchor clamps linkage segment is located thermal-insulated section recess, and fixed connection spare is with the end and the anchor clamps thermal-insulated section and anchor clamps base fixed connection of anchor clamps linkage segment.
In the flow guide structure, the flow guide plate is made of a metal material with excellent ultralow-temperature mechanical properties; the inner diameter of the cylindrical duct structure is 40 mm-60 mm; the inclination angle of the plane baffle plate which is symmetrical up and down of the guide plate is 60-80 degrees; the inner diameter of the vent hole on the plane baffle plate is 3 mm-10 mm.
The invention also aims to provide an in-situ loading micro CT characterization method in an ultralow temperature environment.
The in-situ loading micro CT characterization method in the ultralow temperature environment comprises the following steps:
1) placing a sample in a sample cavity in an experimental environment box body, and fixing the sample by a pair of clamps;
2) the liquid outlet rate of the refrigerating device and the power of the heating device are controlled by the control unit, and an adjustable cold source and a heat source are provided for the experiment environment box body; the circulating fan quickly vaporizes refrigerating liquid from a liquid outlet of the refrigerating device and blows refrigerating gas to a sample along the cylindrical duct structure, the refrigerating gas is divided into an upper path and a lower path after being conveyed to the sample cavity, the refrigerating gas returns to the refrigerating cavity through the vent hole in the guide plate and enters the sample cavity through the cylindrical duct structure again through the suction force of the circulating fan, so that circulation is formed, the flow of gas in the experimental environment box body is accelerated, and redundant gas is discharged out of the experimental environment box body through the exhaust valve;
3) the temperature measuring element detects the ambient temperature around the sample in real time and feeds measured data back to the box temperature control unit in real time, when the ambient temperature around the sample is lower than a set temperature, the heating device works to improve the ambient temperature around the sample to the set temperature, the heating device shortens the response time of temperature control, and the heating device is matched with the flow guide structure to realize the quick response of temperature control, so that the fluctuation of the ambient temperature around the sample is reduced;
4) the mechanical testing machine mechanically loads a sample through a clamp, meanwhile, a micro-focus X-ray source conducts micro CT scanning on the sample through one anti-fog-frost ray window, a detector collects rays transmitted by the sample through the other anti-fog-frost ray window, and the temperature of a window sheet on the outer side of the anti-fog-frost ray window is regulated and controlled by a heating ring to be always higher than the room temperature, so that the phenomena of fogging and frosting of the window sheet on the outer side are avoided, and the sample can be accurately reconstructed;
5) the water pipe leads to hot water in to slowly warm water route in the experimentation, cooperates the anchor clamps heat insulation section of low thermal conductivity, can avoid the ultra-low temperature environment in the experimental environment box to pass through the heat conduction of anchor clamps and produce the influence to the normal work of mechanical testing machine, and the microstructure and the damage appearance of inside when sample normal position was carried under the reconsitution ultra-low temperature environment.
The invention has the advantages that:
(1) the method reconstructs the microstructure and the damage morphology of the sample in situ under the ultralow temperature environment, and lays a foundation for the research of the material failure mechanism and the damage evolution rule under the ultralow temperature environment;
(2) according to the invention, the heat conduction between the window sheet at the outer side of the anti-fog and frost ray window and the experimental environment box body is weakened through the heat insulation ring, and the temperature of the window sheet at the outer side is regulated and controlled by the heating ring to be always higher than the room temperature, so that the phenomena of fogging and frosting of the window sheet at the outer side are avoided, and a sample can be accurately reconstructed;
(3) the temperature in the experimental environment box body is regulated and controlled by combining the liquid outlet rate of the refrigerating device and the power of the heating device, the environmental temperature of a sample is fed back in real time by the temperature measuring element, and the heat transfer in the experimental environment box body is accelerated by matching with the flow guide structure, so that the rapid and accurate negative feedback control of the temperature in the experimental environment box body is realized;
(4) the fixture in the invention adopts a sectional type structure, different types of loading on samples can be realized by selecting different types of fixture heads, and the influence of the ultralow temperature environment in the experimental environment box on the normal work of the mechanical testing machine through the heat conduction of the fixture can be avoided through the fixture connecting section with low heat conductivity and the temperature-relieving water path of the fixture base.
Drawings
FIG. 1 is a schematic diagram of an entirety of one embodiment of an in-situ loading micro-CT characterization system in an ultra-low temperature environment of the present invention;
FIG. 2 is a cross-sectional view of a fixture of one embodiment of an in-situ loaded micro CT characterization system in an ultra-low temperature environment of the present invention;
FIG. 3 is a schematic diagram of an experimental environment box of an embodiment of an in-situ loading micro-CT characterization system in an ultra-low temperature environment according to the present invention;
FIG. 4 is a cross-sectional view of an anti-fog-frost radiation window of an embodiment of the in-situ loaded micro-CT characterization system in an ultra-low temperature environment of the present invention.
Detailed Description
The invention will be further elucidated by means of specific embodiments in the following with reference to the drawing.
As shown in fig. 1, the in-situ loading micro CT characterization system in the ultra-low temperature environment of the present embodiment includes: the device comprises a mechanical testing machine 1, a clamp 2, an exhaust valve 3, an experimental environment box 4, a flow guide structure 5, a circulating fan 6, a refrigerating device, a fixing frame 10, a control unit 11, a temperature measuring element 12, an anti-fog and frost ray window 13, a heating device 14, a micro-focus X-ray source and a detector; wherein, a fixed frame 10 is arranged on a lower beam of the mechanical testing machine 1; an experimental environment box body 4 is arranged on the fixed frame 10; a flow guide structure 5 is arranged in the experimental environment box body 4, and the flow guide structure 5 divides the internal space of the experimental environment box body 4 into two relatively independent spaces which are a sample cavity and a refrigeration cavity respectively; the tail ends of the pair of clamps 2 are respectively fixed on an upper cross beam and a lower cross beam of the mechanical testing machine 1, the head ends of the pair of clamps 2 respectively penetrate through the top wall and the bottom wall of the experimental environment box 4 and hermetically extend into a sample cavity in the experimental environment box 4, the pair of clamps 2 are completely identical and are positioned on the same vertical straight line and are vertically symmetrical about a central horizontal plane, and the sample 15 is fixed at the head ends of the pair of clamps 2; a circulating fan 6 is arranged in a refrigeration cavity in the experimental environment box body 4; a heating device 14 is arranged in a sample cavity of the experimental environment box body 4; a refrigerating device positioned outside the mechanical testing machine 1 conveys the refrigerating liquid to a refrigerating cavity in the experimental environment box body 4; a temperature measuring element 12 is arranged in the experimental environment box body 4; an exhaust valve 3 is arranged on the top wall of the experimental environment box body 4; an anti-fog ray window 13 is respectively arranged on a pair of opposite side walls of the experimental environment box body 4;
as shown in fig. 2, the clamp 2 comprises a clamp base 2-1, a temperature-slow waterway 2-2, a clamp heat-insulating section 2-3, a fixed connecting piece 2-4, a clamp connecting section 2-5 and a clamp head 2-6; the tail end of the clamp is provided with a clamp base 2-1, a temperature-slow water path 2-2 is arranged in the clamp base 2-1, and the temperature-slow water path 2-2 is connected to a water pump through a water pipe; a clamp heat insulation section 2-3 is arranged on the clamp base 2-1, and the clamp heat insulation section 2-3 is made of a material with a low heat conduction coefficient; a fixture connecting section 2-5 is arranged on the fixture heat insulation section 2-3; the tail end of the clamp head is provided with an external thread, the head end of the clamp connecting section is provided with an internal thread, the clamp head and the external thread are connected through the thread, and the clamp head extends into the experimental environment box body 4; the head end of the clamp base 2-1 is provided with a base groove, the clamp heat insulation section 2-3 is positioned in the base groove, the head end of the clamp heat insulation section 2-3 is provided with a heat insulation section groove, the tail end of the clamp connecting section 2-5 is positioned in the heat insulation section groove, and the fixed connecting piece adopts a connecting pin to fixedly connect the tail end of the clamp connecting section with the clamp heat insulation section and the clamp base; the clamp base 2-1, the clamp heat insulation section 2-3, the clamp connecting section 2-5 and the clamp head 2-6 are coaxial;
the flow guide structure comprises a flow guide plate and a cylindrical duct structure; the guide plate comprises two plane baffles which are vertically symmetrical about a central horizontal plane, and a plurality of ventilation holes which are uniformly distributed are arranged on the plane baffles; each plane baffle plate and the central horizontal plane have an inclination angle, and the inclination angle faces the refrigeration cavity; a through hole is formed in the middle of the guide plate, a cylindrical duct structure is arranged on the through hole, the cylindrical duct structure is a cylindrical shell, and the cylindrical duct structure is positioned in the refrigerating cavity;
as shown in fig. 3, the circulating fan comprises a fan blade 6-1, a long fan shaft 6-2 and a motor 6-3; the motor 6-3 is positioned on the outer side wall of the experimental environment box body; the fan blades 6-1 are positioned in the cylindrical ducted structure of the flow guide structure in the experimental environment box body, and the outer diameter of the fan blades 6-1 is 2-4 mm smaller than the inner diameter of the cylindrical ducted structure; one end of a horizontal long shaft 6-2 of the fan is connected with a motor 6-3, and the other end of the long shaft penetrates through the side wall of the experimental environment box body to reach fan blades 6-1 in the experimental environment box body and located in the cylindrical ducted structure; a liquid outlet of the refrigerating device extends into the cylindrical duct structure and is opposite to the back surface of the fan blade 6-1;
as shown in fig. 4, the anti-fog-frost ray window includes a window flange tube 12-1, an inner window sheet 12-2, a heat insulating ring 12-3, a heating ring 12-4, an outer window sheet 12-5 and a fixing cover plate 12-6; a pair of opposite side walls of the experimental environment box body are provided with coaxial and horizontal through holes, and window flange pipes 12-1 are welded on the through holes; an inner side window sheet 12-2 is arranged at one end of the window flange pipe 12-1, which is positioned on the inner wall of the experimental environment box body, and two heat insulation rings 12-3 are arranged at one end of the window flange pipe 12-1, which is positioned on the outer wall of the experimental environment box body; a heating ring 12-4 which is tightly attached is arranged outside the heat insulation ring 12-3; an outer window sheet 12-5 is arranged outside the heating ring 12-4; the outer surface of the outer side window sheet 12-5 is provided with a circular fixed cover plate 12-6, so that the heat insulation ring 12-3, the heating ring 12-4 and the outer side window sheet 12-5 are tightly attached and fixed; the inner diameters of the heat insulation ring 12-3, the heating ring 12-4 and the fixed cover plate 12-6 are not less than the inner diameter of the window flange pipe; the diameters of the inner window thin sheet 12-2 and the outer window thin sheet 12-5 are larger than the inner diameter of the window flange pipe 12-1;
the heating device, the refrigerating device, the circulating fan, the temperature measuring element and the heating ring of the anti-fog and frost-ray window are connected to a control unit 11 positioned outside the experimental environment box body through leads;
the microfocus X-ray source and the detector respectively face the anti-fog and anti-frost ray window.
The anchor clamps through-hole has been seted up respectively at the roof and the diapire of experimental environment box, and the head end of a pair of anchor clamps stretches into to the experimental environment box in through-hole of anchor clamps respectively, respectively installs modified polytetrafluoroethylene ultra-low temperature sealing ring in the anchor clamps through-hole and carries out the movive seal, prevents that gas from revealing along anchor clamps in the experimental process experimental environment box to influence the normal work of mechanics testing machine.
The refrigerating device includes: the refrigeration system comprises a refrigeration tank, a refrigeration pipe and an electromagnetic valve; wherein, be located the refrigeration jar outside the experimental environment box and be connected to the refrigeration chamber in the experimental environment box through the refrigeration pipe, set up the solenoid valve on the refrigeration pipe, the solenoid valve is connected to the control unit.
The front box wall of the experimental environment box body is integrally a box body box door, is fixed on the experimental environment box body through screws and is sealed through a lead ring. The experimental environment box body comprises an inner wall 4-1, an outer wall 4-2 and an aerogel heat insulation layer 4-3, and the aerogel heat insulation layer 4-3 is filled between the inner wall 4-1 and the outer wall 4-2 which are parallel to each other.
In the embodiment, the heat insulation section of the clamp is made of polytetrafluoroethylene, and the heating device is made of a resistance wire; the outer side window sheet and the inner side window sheet are made of quartz glass; the material of the heat insulation ring adopts polytetrafluoroethylene; the heating ring adopts a resistance wire; the inner window sheet and the outer window sheet are made of low-density materials; the fixed cover plate is a metal ring; liquid in the refrigerating device adopts liquid nitrogen; the temperature measuring element adopts PT 100; the refrigerating liquid is liquid nitrogen.
The in-situ loading micro CT characterization method in the ultralow temperature environment comprises the following steps:
1) placing a sample in a sample cavity in an experimental environment box body, and fixing the sample by a pair of clamps;
2) the control unit controls the liquid outlet rate of the refrigerating device and the power of the heating device through the electromagnetic valve and provides an adjustable cold source and a heat source for the experimental environment box body; the circulating fan quickly vaporizes liquid nitrogen from a liquid outlet of the refrigerating device, blows the nitrogen to a sample along a cylindrical duct structure, the nitrogen is divided into an upper path and a lower path after being conveyed to the sample cavity, and returns to the refrigerating cavity through a vent hole in the guide plate, so that circulation is formed, the flow of gas in the experimental environment box body is accelerated, and redundant gas is discharged out of the experimental environment box body through a vent valve;
3) the temperature measuring element detects the ambient temperature around the sample in real time and feeds measured data back to the box temperature control unit in real time, when the ambient temperature around the sample is lower than a set temperature, the heating device works to improve the ambient temperature around the sample to the set temperature, the heating device shortens the response time of temperature control, and the heating device is matched with the flow guide structure to realize the quick response of temperature control, so that the fluctuation of the ambient temperature around the sample is reduced;
4) the mechanical testing machine mechanically loads a sample through a clamp, meanwhile, a micro-focus X-ray source conducts micro CT scanning on the sample through one anti-fog-frost ray window, a detector collects rays transmitted by the sample through the other anti-fog-frost ray window, and the temperature of a window sheet on the outer side of the anti-fog-frost ray window is regulated and controlled by a heating ring to be always higher than the room temperature, so that the phenomena of fogging and frosting of the window sheet on the outer side are avoided, and the sample can be accurately reconstructed;
5) the water pipe leads to hot water in to slowly warm water route in the experimentation, cooperates the anchor clamps heat insulation section of low thermal conductivity, can avoid the ultra-low temperature environment in the experimental environment box to pass through the heat conduction of anchor clamps and produce the influence to the normal work of mechanical testing machine, and the microstructure and the damage appearance of inside when sample normal position was carried under the reconsitution ultra-low temperature environment.
Finally, it is noted that the disclosed embodiments are intended to aid in further understanding of the invention, but those skilled in the art will appreciate that: various substitutions and modifications are possible without departing from the spirit and scope of the invention and the appended claims. Therefore, the invention should not be limited to the embodiments disclosed, but the scope of the invention is defined by the appended claims.
Claims (10)
1. An in-situ loading micro-CT characterization system in an ultra-low temperature environment, the in-situ loading micro-CT characterization system in the ultra-low temperature environment comprising: the device comprises a mechanical testing machine, a clamp, an exhaust valve, an experimental environment box body, a flow guide structure, a circulating fan, a refrigerating device, a fixing frame, a control unit, a temperature measuring element, an anti-fog-frost ray window, a heating device, a microfocus X-ray source and a detector; wherein, a fixed mount is arranged on a lower beam of the mechanical testing machine; an experimental environment box body is arranged on the fixed frame; a flow guide structure is arranged in the experimental environment box body, and divides the internal space of the experimental environment box body into two relatively independent spaces which are a sample cavity and a refrigeration cavity respectively; the tail ends of the pair of clamps are respectively fixed on an upper cross beam and a lower cross beam of the mechanical testing machine, the head ends of the pair of clamps respectively penetrate through the top wall and the bottom wall of the experimental environment box body and hermetically extend into a sample cavity in the experimental environment box body, and the pair of clamps are completely identical, are positioned on the same vertical straight line and are vertically symmetrical about a central horizontal plane; a circulating fan is arranged in a refrigerating cavity in the experimental environment box body; a heating device is arranged in a sample cavity of the experimental environment box body; the refrigerating device positioned outside the experimental environment box body conveys the refrigerating liquid to a refrigerating cavity in the experimental environment box body; a temperature measuring element is arranged in the experimental environment box body; an exhaust valve is arranged on the top wall of the experimental environment box body; the method comprises the following steps that anti-fog-frost ray windows are respectively arranged on a pair of opposite side walls of an experimental environment box body; the microfocus X-ray source and the detector respectively face the anti-fog and anti-frost ray window;
the clamp comprises a clamp base, a temperature-relieving waterway, a clamp heat-insulating section, a fixed connecting piece, a clamp connecting section and a clamp head; the tail end of the clamp is provided with a clamp base, a temperature-slow water path is arranged in the clamp base, and the temperature-slow water path is connected to the water pump through a water pipe; a clamp heat insulation section is arranged on the clamp base and is made of a material with a low heat conduction coefficient; a fixture connecting section is arranged on the fixture heat insulation section; the tail end of the clamp connecting section is fixedly connected with the clamp base and the clamp heat insulation section through fixed connecting pieces; arranging a clamp head at the head end of the clamp connecting section; the clamp base, the clamp heat insulation section, the clamp connecting section and the clamp head are coaxial;
the flow guide structure comprises a flow guide plate and a cylindrical duct structure; the guide plate comprises two plane baffles which are vertically symmetrical about a central horizontal plane, and a plurality of ventilation holes which are uniformly distributed are arranged on the plane baffles; each plane baffle plate and the central horizontal plane have an inclination angle, and the inclination angle faces the refrigeration cavity; a through hole is formed in the middle of the guide plate, a cylindrical duct structure is arranged on the through hole, the cylindrical duct structure is a cylindrical shell, and the cylindrical duct structure is positioned in the refrigerating cavity;
the circulating fan comprises fan blades, a long fan shaft and a motor; the motor is positioned on the outer side wall of the experimental environment box body; the fan blade is positioned in a cylindrical duct structure of the flow guide structure in the experimental environment box body, and the outer diameter of the fan blade is smaller than the inner diameter of the cylindrical duct structure; one end of a long shaft of the horizontal fan is connected with the motor, and the other end of the long shaft of the horizontal fan penetrates through the side wall of the experimental environment box body to fan blades in the experimental environment box and located in the cylindrical ducted structure; a liquid outlet of the refrigerating device extends into the cylindrical duct structure and is opposite to the back surface of the fan blade of the fan;
the anti-fog-frost ray window comprises a window flange pipe, an inner side window sheet, a heat insulation ring, a heating ring, an outer side window sheet and a fixed cover plate; coaxial and horizontal through holes are formed in a pair of opposite side walls of the experimental environment box body, and sealed window flange pipes are arranged on the through holes; an inner side window sheet is arranged at one end of the window flange pipe, which is positioned on the inner wall of the experimental environment box body, and a sealed heat insulation ring is arranged at one end of the window flange pipe, which is positioned on the outer wall of the experimental environment box body; a heating ring which is tightly attached is arranged outside the heat insulation ring; an outer window sheet is arranged outside the heating ring; the outer surface of the outer window sheet is provided with a fixed cover plate which is in a circular ring shape, so that the heat insulation ring, the heating ring and the outer window sheet are tightly attached and fixed; the window flange pipe, the inner side window sheet, the heat insulation ring, the heating ring, the outer side window sheet and the fixed cover plate are all coaxial;
the heating device, the refrigerating device, the circulating fan, the temperature measuring element and the heating ring of the anti-fog and frost-ray window are connected to a control unit outside the experimental environment box body through leads;
a sample is placed in a sample cavity in the experimental environment box body and is fixed by a pair of clamps; the liquid outlet rate of the refrigerating device and the power of the heating device are controlled by the control unit, and an adjustable cold source and a heat source are provided for the experiment environment box body; the circulating fan quickly vaporizes refrigerating liquid from a liquid outlet of the refrigerating device and blows refrigerating gas to a sample along the cylindrical duct structure, the refrigerating gas is divided into an upper path and a lower path after being conveyed to the sample cavity, the refrigerating gas returns to the refrigerating cavity through the vent hole in the guide plate and enters the sample cavity through the cylindrical duct structure again through the suction force of the circulating fan, so that circulation is formed, the flow of gas in the experimental environment box body is accelerated, and redundant gas is discharged out of the experimental environment box body through the exhaust valve; the temperature measuring element detects the ambient temperature around the sample in real time and feeds measured data back to the control unit in real time, when the ambient temperature around the sample is lower than a set temperature, the heating device works to improve the ambient temperature around the sample to the set temperature, the heating device shortens the response time of temperature control, and the heating device is matched with the flow guide structure to realize the quick response of temperature control, so that the fluctuation of the ambient temperature around the sample is reduced; the mechanical testing machine mechanically loads a sample through a clamp, meanwhile, a micro-focus X-ray source conducts micro CT scanning on the sample through one anti-fog-frost ray window, a detector collects rays transmitted by the sample through the other anti-fog-frost ray window, and the temperature of a window sheet on the outer side of the anti-fog-frost ray window is regulated and controlled by a heating ring to be always higher than the room temperature, so that the phenomena of fogging and frosting of the window sheet on the outer side are avoided, and the sample can be accurately reconstructed; the water pipe leads to hot water in to slowly warm water route in the experimentation, cooperates the anchor clamps heat insulation section of low thermal conductivity, avoids the ultra-low temperature environment in the experimental environment box to produce the influence through the heat-conduction of anchor clamps to the normal work of mechanical testing machine, and the microstructure and the damage appearance of inside when sample normal position was carried under the reconsitution ultra-low temperature environment.
2. The in-situ loading micro-CT characterization system under the ultra-low temperature environment as claimed in claim 1, wherein the top wall and the bottom wall of the experimental environment box are respectively provided with a clamp through hole, the head ends of the pair of clamps respectively extend into the experimental environment box through the clamp through holes, and the clamp through holes are respectively provided with a modified polytetrafluoroethylene ultra-low temperature dynamic sealing ring for sealing.
3. The in-situ loading micro-CT characterization system according to claim 1, wherein the refrigeration device comprises: the refrigeration system comprises a refrigeration tank, a refrigeration pipe and an electromagnetic valve; the refrigeration tank located outside the mechanical test machine is connected to the refrigeration cavity in the experimental environment box body through the refrigeration pipe, the electromagnetic valve is arranged on the refrigeration pipe, and the electromagnetic valve is connected to the control unit.
4. The in-situ loading micro-CT characterization system under the ultra-low temperature environment as claimed in claim 1, wherein the temperature regulation interval of the refrigeration device and the heating device to the experimental environment box body is-196 ℃ to-30 ℃.
5. The in-situ loading micro-CT characterization system under the ultralow temperature environment of claim 1, wherein the experimental environment box body comprises an inner wall, an outer wall and an aerogel thermal insulation layer, and the aerogel thermal insulation layer is filled between the inner wall and the outer wall which are parallel to each other.
6. The in-situ loading micro-CT characterization system under the ultra-low temperature environment as claimed in claim 1, wherein in the flow guide structure, the material of the flow guide plate is a metal material with excellent ultra-low temperature mechanical properties; the inner diameter of the cylindrical duct structure is 40 mm-60 mm; the inclination angle of the plane baffle plate which is symmetrical up and down of the guide plate is 60-80 degrees; the inner diameter of the vent hole on the plane baffle plate is 3 mm-10 mm.
7. The in-situ loading micro-CT characterization system under the ultra-low temperature environment as claimed in claim 1, wherein the material of the heat insulation ring of the anti-fog-frost ray window is ultra-low temperature resistant low thermal conductivity material; the heating ring adopts an element which generates heat by electrification; the inner window sheet and the outer window sheet are made of low-density materials; the fixed cover plate is a metal ring.
8. The in-situ loading micro-CT characterization system under ultra-low temperature environment of claim 1, wherein the fixed connection member employs a connection pin; the head end of anchor clamps base is provided with the base recess, and anchor clamps thermal-insulated section is located the base recess, and the head end of anchor clamps thermal-insulated section has thermal-insulated section recess, and the end of anchor clamps linkage segment is located thermal-insulated section recess, and fixed connection spare is with the end and the anchor clamps thermal-insulated section and anchor clamps base fixed connection of anchor clamps linkage segment.
9. The in-situ loading micro-CT characterization system according to claim 1, wherein the fixture head has an external thread at a distal end thereof, and an internal thread at a head end thereof, and wherein the fixture connection section is connected to the fixture head by a screw.
10. A method for characterizing an in-situ loaded micro-CT characterization system in an ultra-low temperature environment according to claim 1, wherein the method comprises the steps of:
1) placing a sample in a sample cavity in an experimental environment box body, and fixing the sample by a pair of clamps;
2) the liquid outlet rate of the refrigerating device and the power of the heating device are controlled by the control unit, and an adjustable cold source and a heat source are provided for the experiment environment box body; the circulating fan quickly vaporizes refrigerating liquid from a liquid outlet of the refrigerating device and blows refrigerating gas to a sample along the cylindrical duct structure, the refrigerating gas is divided into an upper path and a lower path after being conveyed to the sample cavity, the refrigerating gas returns to the refrigerating cavity through the vent hole in the guide plate and enters the sample cavity through the cylindrical duct structure again through the suction force of the circulating fan, so that circulation is formed, the flow of gas in the experimental environment box body is accelerated, and redundant gas is discharged out of the experimental environment box body through the exhaust valve;
3) the temperature measuring element detects the ambient temperature around the sample in real time and feeds measured data back to the box temperature control unit in real time, when the ambient temperature around the sample is lower than a set temperature, the heating device works to improve the ambient temperature around the sample to the set temperature, the heating device shortens the response time of temperature control, and the heating device is matched with the flow guide structure to realize the quick response of temperature control, so that the fluctuation of the ambient temperature around the sample is reduced;
4) the mechanical testing machine mechanically loads a sample through a clamp, meanwhile, a micro-focus X-ray source conducts micro CT scanning on the sample through one anti-fog-frost ray window, a detector collects rays transmitted by the sample through the other anti-fog-frost ray window, and the temperature of a window sheet on the outer side of the anti-fog-frost ray window is regulated and controlled by a heating ring to be always higher than the room temperature, so that the phenomena of fogging and frosting of the window sheet on the outer side are avoided, and the sample can be accurately reconstructed;
5) the water pipe leads to hot water in to slowly warm water route in the experimentation, cooperates the anchor clamps heat insulation section of low thermal conductivity, can avoid the ultra-low temperature environment in the experimental environment box to pass through the heat conduction of anchor clamps and produce the influence to the normal work of mechanical testing machine, and the microstructure and the damage appearance of inside when sample normal position was carried under the reconsitution ultra-low temperature environment.
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