Synchrotron radiation light source on-line combined puncturing device and use method and application thereof

Abstract

The invention discloses a synchrotron radiation light source online combined puncturing device and a using method and application thereof, relates to the technical field of in-situ mechanics, and solves the problems that in the prior art, a correlation mechanism between macroscopic performance and a micromechanism of puncturing behaviors has a technical blank, and a combined mechanism of a synchrotron radiation light source and the puncturing behaviors has a combination technical problem. The synchronous radiation light source online combined puncturing device comprises a puncturing assembly, a guide rail assembly, a motor assembly, a control system and an X-ray imaging assembly, the puncturing assembly comprises a hollow ejector rod structure, a movable sample clamp and a fixed sensor, and the motor assembly is in transmission connection with the guide rail assembly to drive the movable sample clamp to move upwards to achieve puncturing; the control system simultaneously controls the fixed sensor and the X-ray imaging assembly to collect and export real-time mechanical data and real-time scattering or diffraction intensity data; the device and the method can be applied to research on a correlation mechanism of a microstructure and macroscopic mechanical properties under the puncture load.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of in-situ mechanics, in particular to a synchrotron radiation light source online combined puncture device, a use method thereof and an application thereof. BACKGROUND

[0002] In the field of material physics, especially in the field of polymer physics, the correlation mechanism between the microstructure evolution and the macroscopic mechanical properties of materials under dynamic mechanical action is one of the core research directions. Although the traditional material mechanical property testing methods (such as tensile, compression, puncture, etc.) can obtain macroscopic mechanical parameters (such as strength, toughness, strain rate, etc.), it is difficult to capture the dynamic change process of the microstructure (such as crystal orientation, lamellar structure, phase transition, etc.) in real time, resulting in the long-term existence of the "black box" problem between the macroscopic performance and the microscopic mechanism.

[0003] As an advanced detection means with high intensity, high collimation and high time resolution, the synchrotron radiation light source can realize the real-time characterization of the microstructure while the material is under mechanical action through small-angle X-ray scattering (SAXS), wide-angle X-ray diffraction (WAXS), ultra-small-angle X-ray scattering (USAXS), grazing incidence small-angle X-ray scattering (GISAXS) and other means, which provides key technical support for solving the above-mentioned "black box" problem. At present, researchers have tried to combine uniaxial tension, biaxial tension, compression and other mechanical loading devices with the synchrotron radiation light source, and have achieved the purpose of combining part of the mechanical test with the synchrotron radiation, such as Chinese invention patent CN112504864A provides a high-temperature mechanical loading device of a synchrotron radiation light source, which installs a fatigue testing machine clamp, an actuator, a load sensor and a displacement sensor to perform mechanical tests such as fatigue tension on the sample in a high-temperature environment chamber. However, the device is only suitable for low-speed, quasi-static loading processes such as fatigue tension and isothermal compression, and its loading response speed is slow, the loading path is single, and the loading area is difficult to realize high strain rate control, so it is completely unsuitable for puncture type mechanical behavior with high-speed burst and local deformation concentration. In addition, the high-temperature environment cabin of the device adopts a closed cylindrical structure, which is equipped with a high-temperature resistant glass window to adapt to the requirements of the synchrotron radiation experiment, but the requirements of X-ray scattering type characterization means (such as SAXS, WAXS, GISAXS) for scattering path, angle freedom and device transmission are not systematically considered, making it difficult to realize multi-angle, wide-range and instantaneous synchronization of structure information acquisition in actual operation, resulting in the inability to effectively capture the microstructure change information in the key deformation process.

[0004] In addition, the prior art generally uses a standard symmetrical rigid clamp to fix the sample, which is suitable for block or long strip samples, and cannot provide stable boundary constraints and control capabilities suitable for local concentrated loading for non-standard sample states such as flexible films, layered composites and porous structures commonly found in polymer materials, so that it is difficult to realize the typical stress concentration and boundary displacement coupling regulation in the piercing behavior, affecting the accuracy and consistency of structure observation and mechanical measurement. In the traditional combined device of uniaxial and biaxial tension, the stress direction of the sample is often perpendicular to the direction of X-ray transmission. This structural arrangement leaves sufficient space for X-ray transmission through the sample, facilitating real-time observation of the microstructure under synchrotron radiation. However, due to the limitations of the experimental form, the stress direction of the sample is consistent with the overall direction of its deformation, and it is difficult to leave space for X-ray transmission as in the former. In addition, according to the national standards and industry specifications, the piercing experiment generally uses a fixed clamp and a moving loading rod, so that the sample is in a dynamic displacement state during the experiment, making it difficult to meet the basic requirements of spatial position stability and variable control in synchrotron radiation testing. At the same time, the structural design of the traditional loading device is not optimized for the detection needs of the synchrotron radiation source. The loading components such as the top rod and the clamp in the device are often directly in the incident path or detection area of X-rays, causing serious obstruction to the passage of X-rays, making it impossible to accurately project X-rays onto the sample, and thus making it impossible to obtain the microstructure information required during the piercing process.

[0005] Therefore, the existing synchrotron radiation combined technology still has technical shortcomings such as lagging loading mechanism, limited detection path, poor sample compatibility and weak data coordination capability when facing piercing type high strain rate complex loading conditions, resulting in that the microstructure evolution mechanism research during the piercing process is still in the technical blank stage, and a stable and widely applicable experimental system has not been formed, which is one of the important technical problems that need to be overcome in the current material physics, especially in the research of high polymer mechanics behavior. SUMMARY

[0006] In order to solve the problems of the existing technology that the correlation mechanism between the macroscopic performance and the microstructure mechanism of the piercing behavior is in a technical blank, and the combination mechanism of the synchrotron radiation source and the piercing behavior is a technical problem. The present application provides a synchrotron radiation source online combined piercing device and its use method and application. The technical scheme of the present application is as follows: A synchrotron radiation source online combined piercing device, comprising a piercing assembly, a guide rail assembly, a motor assembly, a control system, an X-ray imaging assembly; the synchrotron radiation source online combined piercing device further comprises a bottom plate and an instrument handle, the bottom plate is provided with a plurality of screw holes for fixing each component.

[0007] The piercing assembly comprises a movable sample clamp, an ejector rod, a fixed sensor, a bracket and an adapter plate; the ejector rod is a hollow structure, and the non-piercing end of the ejector rod is detachably connected with the fixed sensor through an adapter; the movable sample clamp is connected with a guide rail assembly; the X-ray emitted by the ray emitter in the ray imaging assembly is coaxial with the ejector rod and the movable sample clamp; the motor assembly is drivingly connected with the guide rail assembly to drive the movable sample clamp to move towards the ejector rod to realize piercing. The control system simultaneously controls the operation of the fixed sensor, the motor assembly and the X-ray imaging assembly to realize piercing, real-time mechanical data collection and real-time scattering or diffraction intensity data export.

[0008] Further, the ejector rod is any one of a hollow ejector rod, a windowed ejector rod or a ball head ejector rod; the hollow ejector rod is provided with a circular through hole with a diameter of 4.8 mm in the axial direction; the windowed ejector rod is provided with a circular through hole with a diameter of 4.8 mm in the axial direction, and the head is inlaid with a window with a diameter of 5 mm; the window material is any one of 0.5 mm thick single crystal diamond, polyimide or sapphire glass; the ball head ejector rod is provided with a circular through hole with a diameter of 4.8 mm in the axial direction, and the head is assembled with a steel ball with a diameter of 25 mm, and the steel ball is provided with an opening with a diameter of 5 mm, which is used for textile piercing experiment; the ball head ejector rod meets the provisions of the national standard GB / T19976 “Determination of the bursting strength of textiles-steel ball method” for textile piercing experiment, and is close to the standard (steel ball diameter is 25.4 mm) of ASTM D6797 “Standard Test Method for Standardizing the Bursting Strength of Fabrics-Constant Rate of Extension (CRE) Steel Ball Bursting Test” published by ASTM.

[0009] Further, the movable sample clamp comprises an upper pressing disc, a lower pressing disc and a fastening screw, the lower pressing disc is detachably connected with the upper pressing disc through the fastening screw and is provided with a through hole in the center to form a hollow detection area; the bracket and the fixed sensor are provided with hollow through holes at the connection positions with the ejector rod, so that the X-ray beam can pass through the ejector rod to the hollow detection area of the movable sample clamp.

[0010] Further, the guide rail assembly comprises a guide rail shell, two guide rails, a bearing I, a lead screw, a nut seat I, a bearing sleeve, a nut seat II, two sliders and a bearing III; the movable sample clamp, the nut seat I and the two sliders are sequentially connected from top to bottom, specifically, the upper pressure plate is fixedly connected with the nut seat I through an adapter plate; the two sliders are slidably connected with the two guide rails respectively; the two guide rails are arranged in parallel with the lead screw and in the same piercing direction; the two ends of the lead screw are rotatably connected with the bearing III in the nut seat II and the bearing I in the bearing sleeve respectively, and the lead screw is threadedly connected with the nut seat I; the bearing sleeve is fixedly connected with the bottom plate for fixing the guide rail assembly; the fixed sensor is fixedly connected with the nut seat II through a support. Meanwhile, the guide rail shell is left with two gaps corresponding to the guide rails for the movement of the movable sample clamp.

[0011] Further, the motor assembly comprises a motor arranged in the motor shell, a shaft coupling, a worm, a bearing II, a worm wheel and a bearing seat; the motor is fixedly connected with one end of the worm through the shaft coupling, the other end of the worm is rotatably connected with the bearing II in the bearing seat, the bearing seat is fixedly connected with the bottom plate for fixing the motor assembly; the worm is in meshing transmission connection with the worm wheel, and the worm wheel is fixedly connected with one end of the lead screw close to the fixed sensor. Further, the X-ray imaging assembly comprises an X-ray emitter and an X-ray detector; the X-ray detector comprises an X-ray small-angle scattering detector and a wide-angle X-ray diffraction detector; the X-ray small-angle scattering detector comprises a small-angle X-ray scattering detector and an ultra-small-angle X-ray scattering detector.

[0012] Further, the control system comprises a computer and a PLC controller and an X-ray data acquisition system which are in communication connection with the computer.

[0013] Further, the PLC controller comprises a control module, a data acquisition module and a data processing module; the control module is used for starting the fixed sensor and controlling the operation of the motor, the data acquisition module is used for acquiring the mechanical signals collected by the fixed sensor and the pulse signals of the motor operation in real time; the data processing module calculates the displacement of the movable sample clamp according to the pulse signals and calculates the mechanical data according to the mechanical signals, and transmits the mechanical data and the displacement data to the computer; the computer is built-in with a test machine measurement and control software, and a mechanical curve is drawn in real time; The X-ray data acquisition system comprises an X-ray emission module, a detection module and a data transmission module; the X-ray emission module drives the X-ray emitter to emit X-rays, the detection module controls the X-ray detector to receive X-ray signals and convert the X-ray signals into electric signals, and the data transmission module transmits the electric signals to the computer; the computer is built-in with a FIT2D software, and an X-ray scattering or diffraction pattern is drawn in real time.

[0014] A method for using the above-mentioned online piercing device of a synchrotron radiation source, comprising the following steps: S1: Adjust the fastening screw to fix the sample to be tested between the upper and lower pressure plates of the movable sample clamp; S2: The X-ray emission module starts the X-ray emitter, and the detection module starts the X-ray detector. The X-rays emitted by the X-ray emitter are coaxial with the top rod, the movable sample clamp, and the X-ray small-angle scattering detector, so that the X-rays can pass through the hollow area of the top rod and the sample piercing area in sequence and be received by the X-ray detector. If the light spot of the X-rays on the sample is greater than 300*400 μm 2 , proceed to step S3; if the light spot of the X-rays on the sample is less than 300*400 μm 2 , proceed to step S4; S3: The control module simultaneously starts the fixed sensor and the motor. The motor drives the worm to rotate, the worm gear engages in transmission, the lead screw rotates, and finally the nut seat I drives the movable sample clamp to move towards the top rod at a speed of 10-1000 mm / min. The data acquisition module collects the mechanical signals output by the fixed sensor and the pulse signals of the motor in real time. The data processing module transmits the mechanical data and displacement data to the computer. The real-time mechanical curve of the piercing process is exported by the test machine control software. At the same time, the detection module converts the X-ray signals received by the X-ray detector into electrical signals, and the data transmission module transmits the electrical signals to the computer. The real-time X-ray scattering or diffraction spectrum is exported by the FIT2D software. Until the high-speed or low-speed piercing process of the sample is realized. S4: A plurality of movable positions of the movable sample clamp are preset. The control module starts the fixed sensor and the motor. The motor drives the worm to rotate, the worm gear engages in transmission, and the lead screw rotates. The nut seat I drives the movable sample clamp to move towards the top rod to the first preset position and pause. The X-ray emission module controls the X-ray emitter to perform X-ray scanning on the center and the up, down, left and right directions of the sample piercing area for 4-25 points. Continue to advance the movable sample clamp to the next position and repeat the scanning process. The data acquisition module collects the mechanical signals output by the fixed sensor and the pulse signals of the motor in real time. The data processing module transmits the mechanical data and displacement data to the computer. The real-time mechanical curve of the piercing process of the sample under different deformation states is exported by the test machine control software. At the same time, the detection module converts the X-ray signals received by the X-ray detector into electrical signals, and the data transmission module transmits the electrical signals to the computer. The real-time X-ray scattering or diffraction spectrum of the sample under different deformation states is exported by the FIT2D software. Until the sample is pierced.

[0015] The application of the above-mentioned synchrotron radiation source online combined with a puncture device is applied to the research on the correlation mechanism of the microstructure and macroscopic mechanical properties of polymer films, composite materials and other samples under puncture load.

[0016] Compared with the prior art, the application solves the technical blank of the correlation mechanism between the macroscopic performance and the microstructure of the puncture behavior in the prior art and the combination technical problem of the synchrotron radiation source and the puncture behavior, and has the following specific beneficial effects: 1. The combination difficulty of the puncture device and the synchrotron radiation source is solved for the first time: the hollow detachable ejector rod is adopted, and the problem of X-ray passage obstruction is effectively solved; meanwhile, the movable sample clamp (moving speed: 10-1000 mm / min) is matched, and high-precision displacement regulation and control capability is given to the device, and the spatial positioning accuracy and stability of the sample in the X-ray detection process are significantly improved. The puncture behavior of the puncture device and the data acquisition behavior of the sensor and the detector are regulated and controlled by the control system, which fundamentally breaks through the technical barrier that the traditional puncture experiment cannot be cooperated with the synchrotron radiation detection, realizes real-time observation of the microstructure evolution under complex puncture mechanical behavior, and fills the blank of the combination of the synchrotron radiation source technology in the high-speed and sudden loading behavior.

[0017] 2. The replaceable ejector rod structure design realizes the combination of various puncture behaviors and the synchrotron radiation source: the ejector rod structure provided by the application includes three replaceable types of hollow ejector rod, windowed ejector rod and ball head ejector rod, which are functionally optimized for different sample material categories, puncture modes and detection requirements, and are modularly designed, so that they can be quickly disassembled and interchanged according to experimental requirements, significantly enhancing the adaptability and operation convenience of the loading system. The window material of the windowed ejector rod is also replaceable, and has good universality and interchangeability, facilitating on-site debugging of the device and rapid switching of multi-task experiments. The structure significantly improves the experimental flexibility and technical expandability of the device, breaks through the limitations of the traditional loading system with single function and fixed structure, and provides key support for building a universal, multi-field coupled and high spatial resolution synchrotron radiation mechanical detection platform.

[0018] 3. Instantaneous transient response of the puncture process is effectively improved: the spatial coordination configuration of the loading structure and the detection path is optimized, combined with the linkage layout of the hollow ejector rod, the movable sample fixing platform and the multi-angle X-ray detection window, and the high accuracy and real-time of data acquisition are realized. In the loading process, the control system realizes the synchronous triggering mechanism and the high-speed acquisition module, so that the mechanical loading and the X-ray imaging process are accurately matched within a time scale of seconds, ensuring that the structure response information at the key deformation moment is not missed, thereby greatly improving the time resolution and transient response capture ability of the data. BRIEF DESCRIPTION OF DRAWINGS

[0019] Figure 1 This is a schematic diagram of the structure of the puncture device used online with a synchrotron radiation source; Figure 2 This is a schematic diagram of the internal structure of the puncture device for the online combination of synchrotron radiation source; Figure 3 Schematic diagram of the hollow ejector head structure; Figure 4 Schematic diagram of the top structure of the window ejector rod; Figure 5 Schematic diagram of the jacking head structure of the ball head jack; Figure 6 It is a schematic diagram of the structure of the guide rail assembly and the motor assembly; Figure 7 is the X-ray propagation path diagram; Among them, 1. Mobile sample fixture; 11. Upper pressure plate; 12. Lower pressure plate; 13. Fastening screw; 14. Adapter plate; 2. Push rod; 21. Adapter; 22. Hollow push rod; 23. Window push rod; 24. Ball head push rod; 3. Fixed sensor; 31. Bracket; 4. Guide rail housing; 41. Guide rail; 42. Bearing I; 43. Screw; 44. Nut seat I; 45. Bearing sleeve; 46. Nut seat II; 47. Slider; 5. Motor housing; 51. Motor; 52. Coupling; 53. Worm; 54. Bearing II; 55. Worm gear; 56. Bearing seat; 6. Bottom plate; 7. Instrument grip; 8. Screw hole; 9. X-ray emitter; 10. X-ray small-angle scattering detector; 101. Wide-angle X-ray diffraction detector. DETAILED DESCRIPTION

[0020] In order to make the technical solution of the present invention clearer, the technical solution in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the specification of the present invention. It should be noted that the following embodiments are only used to better understand the technical solution of the present invention and should not be understood as limiting the present invention.

[0021] Example 1. This embodiment constructs a synchrotron radiation light source online combined with a puncture device, such as Figure 1 The figure shows a structural schematic diagram of the online puncture device for a synchrotron radiation light source. As can be seen from the figure, the online puncture device for a synchrotron radiation light source includes a puncture component, a guide rail component, a motor component, a control system, and an X-ray imaging component; the online puncture device for a synchrotron radiation light source also includes a base plate 6 and an instrument handle 7, and the base plate 6 is provided with a plurality of screw holes 8 for fixing the various components.

[0022] like Figures 1-5As shown, the piercing assembly includes a movable sample clamp 1, a top rod 2, a fixed sensor 3, a bracket 31 and an adapter plate 14; the top rod 2 is a hollow structure, and the non-piercing end of the top rod 2 is detachably connected with the fixed sensor 3 through an adapter 21; the movable sample clamp 1 is connected with a guide rail assembly; the X-ray emitted by the X-ray emitter 9 in the X-ray imaging assembly is coaxial with the top rod 2 and the movable sample clamp 1; the motor assembly is drivingly connected with the guide rail assembly to drive the movable sample clamp 1 to move towards the top rod 2 to realize piercing; the control system simultaneously controls the operation of the fixed sensor 3, the motor assembly and the X-ray imaging assembly to realize piercing while collecting and exporting real-time mechanical data and real-time scattering or diffraction intensity data.

[0023] The top rod 2 is any one of a hollow top rod 22, Figure 3 a windowed top rod 23, Figure 4 or a ball head top rod 24. Figure 5 The hollow top rod 22 is provided with a circular through hole with a diameter of 4.8 mm in the axial direction; the windowed top rod 23 is provided with a circular through hole with a diameter of 4.8 mm in the axial direction, and the head is inlaid with a window with a diameter of 5 mm; the window material is any one of 0.5 mm thick single crystal diamond, polyimide or sapphire glass; the ball head top rod 24 is provided with a circular through hole with a diameter of 4.8 mm in the axial direction, and the head is assembled with a steel ball with a diameter of 25 mm, and the steel ball is provided with an opening with a diameter of 5 mm for textile piercing experiment; it meets the provisions of the national standard GB / T19976 “Determination of the bursting strength of textiles-steel ball method” for textile piercing experiment, and is close to the standard (steel ball diameter is 25.4 mm) of ASTM D6797 “Standard Test Method for Standardizing the Bursting Strength of Fabrics-Constant Rate of Extension (CRE) Steel Ball Bursting Test” published by American Society for Testing and Materials (ASTM).

[0024] The movable sample clamp 1 includes an upper pressing disc 11, a lower pressing disc 12 and a fastening screw 13, the lower pressing disc 12 is detachably connected with the upper pressing disc 11 through the fastening screw 13 and is provided with a through hole in the center to form a hollow detection area; the bracket 31 and the fixed sensor 3 are provided with a hollow through hole at the connection with the top rod 2, so that the X-ray beam can pass through the top rod 2 to the hollow detection area of the movable sample clamp 1.

[0025] As Figure 1 , 2As shown in Figure 6, the guide rail assembly includes a guide rail housing 4, two guide rails 41, bearing I 42, a screw 43, a nut seat I 44, a bearing sleeve 45, a nut seat II 46, two sliders 47 and a bearing III; the movable sample fixture 1, the nut seat I 44 and the two sliders 47 are connected in sequence from top to bottom, specifically the upper pressure plate 11 is fixedly connected to the nut seat I 44 through the adapter plate 14; the two sliders 47 are respectively slidably connected to the two guide rails 41; the two guide rails 41 are arranged parallel to the screw 43, in the same direction as the puncture; the two ends of the screw 43 are rotatably connected to the bearing III inside the nut seat II 46 and the bearing I 42 inside the bearing sleeve 45, and the screw 43 is threadedly connected to the nut seat I 44; the bearing sleeve 45 is fixedly connected to the base plate 6 for fixing the guide rail assembly; the fixed sensor 3 is fixedly connected to the nut seat II 46 through the bracket 31. At the same time, the guide rail housing 4 leaves two gaps corresponding to the guide rails 41 for the movable sample fixture 1 to move. like Figure 1 、 2 As shown in Figure 6, the motor assembly includes a motor 51, a coupling 52, a worm 53, a bearing II 54, a worm wheel 55 and a bearing seat 56 arranged inside the motor housing 5; the motor 51 is fixedly connected to one end of the worm 53 through the coupling 52, and the other end of the worm 53 is rotationally connected to the bearing II 54 in the bearing seat 56. The bearing seat 56 is fixedly connected to the base plate 6 for fixing the motor assembly; the worm 53 is meshingly connected to the worm wheel 55, and the worm wheel 55 is fixedly connected to the end of the screw 43 near the fixed sensor 3. like Figure 7As shown, the X-ray imaging assembly includes an X-ray emitter 9 and an X-ray detector; the X-ray detector includes a small-angle X-ray scattering detector 10 and a wide-angle X-ray diffraction detector 101; the small-angle X-ray scattering detector 10 includes a small-angle X-ray scattering detector and an ultra-small-angle X-ray scatterer; the control system includes a computer and a PLC controller connected to the computer for communication, and an X-ray data acquisition system. The PLC controller includes a control module, a data acquisition module and a data processing module; the control module is used to start the fixed sensor 3 and control the operation of the motor 51, and the data acquisition module is used to collect the mechanical signals collected by the fixed sensor 3 and the pulse signals of the motor 51 in real time; the data processing module calculates the displacement of the movable sample fixture 1 and the mechanical data according to the pulse signal and the mechanical signal, and transmits the mechanical data and displacement data to the computer, which has built-in testing machine measurement and control software to draw the mechanical curve in real time; the X-ray data acquisition system includes an X-ray emission module, a detection module and a data transmission module, the X-ray emission module drives the X-ray emitter 9 to emit X-rays, and the detection module controls the X-ray detector to receive the X-ray signal and convert the X-ray signal into an electrical signal, which is transmitted to the computer by the data transmission module, and the computer has built-in FIT2D software to draw the X-ray scattering or diffraction spectrum in real time.

[0026] Example 2. This embodiment is based on embodiment 1. Figure 7 A method for using a puncture device coupled with a synchrotron radiation light source online is provided, comprising the following steps: S1: Adjust the fastening screw 13 to fix the sample to be tested between the upper pressure plate 11 and the lower pressure plate 12 of the movable sample fixture 1; S2: The X-ray emission module starts the X-ray emitter 9, and the detection module starts the X-ray detector at the same time, and adjusts the X-ray emitted by the X-ray emitter 9 to be coaxial with the ejector 2, the movable sample holder 1 and the X-ray small-angle scattering detector 10, so that the X-ray can pass through the hollow area of ​​the ejector 2 and the sample to be punctured in sequence and be received by the X-ray detector; if the X-ray light source spot on the sample is larger than 300×400 μm 2 , enter step S3; if the X-ray light source spot on the sample is less than 300×400 μm 2 , then go to step S4; S3: the control module simultaneously starts the fixed sensor 3 and the motor 51; the motor 51 drives the worm 53 to rotate to drive the worm gear 55 to mesh transmission, and then drives the lead screw 43 to rotate, and finally drives the nut seat I 44 to drive the movable sample clamp 1 to move to the ejector rod 2 at a speed of 10~1000 mm / min; the data acquisition module collects the mechanical signals output by the fixed sensor 3 and the pulse signals of the motor 51 in real time, the data processing module transmits the mechanical data and displacement data to the computer, and the real-time mechanical curve of the piercing process is exported by the test machine control software; at the same time, the detection module converts the X-ray signals received by the X-ray detector into electrical signals, and the data transmission module transmits the electrical signals to the computer, and the real-time X-ray scattering or diffraction spectrum is exported by the FIT2D software; until the high-speed or low-speed piercing process of the sample is realized; S4: a plurality of movable positions of the movable sample clamp 1 are preset, the control module starts the fixed sensor 3 and the motor 51, the motor 51 drives the worm 53 to rotate, the worm gear 55 to mesh transmission, and the lead screw 43 to rotate, and the nut seat I 44 drives the movable sample clamp 1 to move to the first preset position and pause movement; the X-ray emission module controls the X-ray emitter 9 to perform X-ray scanning on 4~25 points respectively in the center and up, down, left and right directions of the sample piercing area; continue to advance the movable sample clamp 1 to the next position, repeat the scanning process; the data acquisition module collects the mechanical signals output by the fixed sensor 3 and the pulse signals of the motor 51 in real time, the data processing module transmits the mechanical data and displacement data to the computer, and the real-time mechanical curve of the piercing process of the sample under different deformation states is exported by the test machine control software; at the same time, the detection module converts the X-ray signals received by the X-ray detector into electrical signals, and the data transmission module transmits the electrical signals to the computer, and the real-time X-ray scattering or diffraction spectrum of the sample under different deformation states is exported by the FIT2D software; until the sample is pierced.

[0027] In actual operation, as Figure 7The shown synchrotron radiation source is connected online with the puncture device, the polymer sample (such as a polyethylene film) is fixed through the movable sample clamp 1, the window top rod 23 is selected for the top rod 2, the window top rod 23 is provided with a circular through hole with a diameter of 4.8 mm in the axial direction, and the head is inlaid with a single crystal diamond with a diameter of 5 mm and a thickness of 0.5 mm. The X-ray small-angle scattering detector 10 is selected as a small-angle X-ray scattering detector, and is matched with a wide-angle X-ray diffraction detector 101; the X-ray emission module drives the X-ray emitter 9, and the detection module starts the X-ray detector, adjusts the coaxiality of the X-ray, the top rod 2, the sample to be punctured and the small-angle X-ray scattering detector, and the wide-angle X-ray diffraction detector 101 is located at a distance of 45~1800 mm above the light path; whether X-ray scanning is needed is determined according to the light spot size of the X-ray on the sample. The fixed sensor 3 and the motor 51 are started at the same time under the control of the module, the movable sample clamp 1 is driven by the nut seat I 44 to move towards the top rod 2, and the puncture process is realized; the real-time X-ray scattering and diffraction spectrum of the puncture process is exported by the FIT2D software; the real-time mechanical curve of the puncture process is exported by the tester control software. Combined with the macro mechanical data and microstructure evolution data of the polymer sample puncture process, the correlation mechanism of the microstructure and macro mechanical properties of the polymer film, composite material and other samples under the puncture load can be studied. The time resolution of the synchrotron radiation source of the synchrotron radiation source online connection puncture device provided by the application can reach seconds.

[0028] In summary, the detachable top rod 2 with a hollow structure is adopted in the application, the movable sample clamp 1 is matched, the puncture behavior of the puncture device and the data acquisition behavior of the sensor and the detector are cooperated through the control system, and the organic unity of high precision and real-time of data acquisition is realized. The technical barrier that the traditional puncture experiment cannot be cooperated with the synchrotron radiation detection is fundamentally broken, the real-time observation of the microstructure evolution under the complex puncture mechanical behavior is realized, and the blank of the synchrotron radiation source technology in the connection of high-speed and sudden loading behavior is filled.

[0029] The above examples are only used to help understand the method of the application and its core idea. It should be noted that those skilled in the art can make some improvements and modifications to the application without departing from the principles of the application, and these improvements and modifications also fall within the protection scope of the claims of the application.

[0030] The foregoing description of the embodiments disclosed enables a person skilled in the art to make or use the application. Numerous modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein can be applied to other embodiments without the use of the inventive faculty. Therefore, the present application is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A puncture device for an online synchrotron radiation source, characterized in that: Including puncture assembly, guide rail assembly, motor assembly, control system and X-ray imaging assembly; The puncture assembly comprises a movable sample fixture (1), a push rod (2) and a fixed sensor (3); the push rod (2) is a hollow structure; the non-puncture end of the push rod (2) is detachably connected to the fixed sensor (3); the movable sample fixture (1) is connected to the guide rail assembly; the X-rays emitted by the X-ray emitter (9) in the X-ray imaging assembly are coaxial with the push rod (2) and the movable sample fixture (1); the motor assembly is in transmission connection with the guide rail assembly to drive the movable sample fixture (1) to move toward the push rod (2) to achieve puncture; The control system simultaneously controls the operation of the fixed sensor (3), the motor assembly, and the X-ray imaging assembly, thereby collecting and exporting real-time mechanical data and real-time scattering or diffraction intensity data while puncturing.

2. The synchrotron radiation light source online puncture device according to claim 1, characterized in that: The movable sample fixture (1) comprises an upper pressing plate (11) and a lower pressing plate (12), wherein the lower pressing plate (12) is detachably connected to the upper pressing plate (11) and has a through hole at its center; The push rod (2) is any one of a hollow push rod (22), a window push rod (23) or a ball push rod (24); the hollow push rod (22) has a circular through hole in the axial direction; the window push rod (23) has a circular through hole in the axial direction, and a window is embedded in the head; the ball push rod (24) has a circular through hole in the axial direction, and a steel ball with a circular through hole in the axial direction is assembled in the head.

3. The synchrotron radiation light source online puncture device according to claim 2, characterized in that: The guide rail assembly includes a guide rail (41), a lead screw (43), a nut seat I (44), a bearing sleeve (45), a nut seat II (46) and a slider (47); the movable sample fixture (1), the nut seat I (44) and the slider (47) are connected in sequence from top to bottom; the slider (47) is slidably connected to the guide rail (41); the guide rail (41) and the lead screw (43) are arranged in parallel and in the same direction as the puncture direction; the two ends of the lead screw (43) are rotatably connected to the nut seat II (46) and the bearing sleeve (45) respectively; the lead screw (43) is threadedly connected to the nut seat I (44); and the fixed sensor (3) is connected to the nut seat II (46).

4. The synchrotron radiation light source online puncture device according to claim 3, characterized in that: The motor assembly comprises a motor (51), a worm (53) and a worm wheel (55); the motor (51) is fixedly connected to the worm (53); the worm (53) and the worm wheel (55) are meshingly connected, and the worm wheel (55) is fixedly connected to an end of the lead screw (43) close to the fixed sensor (3).

5. The synchrotron radiation light source online puncture device according to claim 4, characterized in that: The X-ray imaging assembly comprises an X-ray emitter (9) and an X-ray detector; the X-ray detector comprises an X-ray small-angle scattering detector (10) and a wide-angle X-ray diffraction detector (101); the X-ray small-angle scattering detector (10) comprises a small-angle X-ray scattering detector and an ultra-small-angle X-ray scatterer.

6. The synchrotron radiation light source online puncture device according to claim 5, characterized in that: The control system includes a computer, a PLC controller and an X-ray data acquisition system which are communicatively connected to the computer.

7. The synchrotron radiation light source online puncture device according to claim 6, characterized in that: The PLC controller includes a control module, a data acquisition module and a data processing module; the control module is used to start the fixed sensor (3) and control the operation of the motor (51); the data acquisition module is used to collect the mechanical signal collected by the fixed sensor (3) and the pulse signal of the motor (51) in real time; the data processing module calculates the displacement of the movable sample fixture (1) and the mechanical signal according to the pulse signal and calculates the mechanical data, and transmits the mechanical data and the displacement data to the computer, and the computer draws the mechanical curve in real time; The X-ray data acquisition system comprises an X-ray emission module, a detection module and a data transmission module. The X-ray emission module drives the X-ray emitter (9) to emit X-rays, while the detection module controls the X-ray detector to receive X-ray signals and convert the X-ray signals into electrical signals, which are then transmitted to a computer by the data transmission module. The computer then draws an X-ray scattering or diffraction pattern in real time.

8. A method for using the synchrotron radiation light source online puncture device as claimed in claim 7, characterized in that: The following steps are involved: S1: Fix the sample to be tested between the upper pressing plate (11) and the lower pressing plate (12) of the movable sample fixture (1); S2: The X-ray emission module drives the X-ray emitter (9), and the detection module starts the X-ray detector at the same time, and adjusts the X-ray emitted by the X-ray emitter (9) to be coaxial with the top rod (2), the movable sample holder (1) and the X-ray small-angle scattering detector (10), so that the X-ray can pass through the hollow area of ​​the top rod (2) and the area to be punctured of the sample in sequence and be received by the X-ray detector; if the light source spot of the X-ray on the sample is larger than 300×400 μm 2 , enter step S3; If the X-ray source spot on the sample is smaller than 300×400 μm 2 , then enter step S4; S3: The control module starts the fixed sensor (3) and the motor (51) at the same time, and the nut seat I (44) drives the movable sample holder (1) to move toward the ejector rod (2); the computer derives the real-time mechanical curve and real-time X-ray scattering or diffraction pattern of the puncture process; until the sample is punctured; S4: Preset several movable positions of the movable sample fixture (1), the control module starts the fixed sensor (3) and the motor (51), the nut seat I (44) drives the movable sample fixture (1) to move to the first preset position toward the push rod (2) and pauses the movement; the X-ray emission module controls the X-ray emitter (9) to perform X-ray scanning of 4 to 25 points in the center and the upper, lower, left and right directions of the area to be punctured of the sample; continue to advance the movable sample fixture (1) to the next position and repeat the scanning process; the computer derives the real-time mechanical curves and real-time X-ray scattering or diffraction patterns of the sample under different deformation states during the puncture process; until the sample is punctured.

9. The method for using the synchrotron radiation light source online puncture device according to claim 8, characterized in that: The speed of driving the movable sample holder (1) in S3 is 10~1000 mm / min.

10. An application of the synchrotron radiation light source online puncture device according to any one of claims 1 to 7, characterized in that: It is used to study the correlation mechanism between the microstructure and macroscopic mechanical properties of samples such as polymer films and composite materials under puncture load.

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