A synchrotron radiation source coupled with an online puncture device, its usage and application.

Abstract

A synchrotron radiation source-coupled online puncture device, its usage method, and applications are disclosed, relating to the field of in-situ mechanics technology. This invention addresses the technological gaps in existing technologies regarding the correlation mechanism between macroscopic performance and microscopic mechanisms of puncture behavior, as well as the challenges in combining the synchrotron radiation source with the puncture behavior mechanism. The synchrotron radiation source-coupled online puncture device includes a puncture component, a guide rail component, a motor component, a control system, and an X-ray imaging component. The puncture component comprises a hollow top rod structure, a movable sample clamp, and a fixed sensor. The motor component and guide rail component are connected by a transmission mechanism, driving the movable sample clamp to move upwards to achieve puncture. The control system simultaneously controls the fixed sensor and the X-ray imaging component to collect and export real-time mechanical data and real-time scattering or diffraction intensity data. This invention can be applied to the study of the correlation mechanism between microstructure and macroscopic mechanical properties under puncture load.

Description

Technical Field

[0001] This invention relates to the field of in-situ mechanics technology, specifically to a puncture device used in conjunction with a synchrotron radiation source online, its usage method, and its application. Background Technology

[0002] In the field of materials physics, especially polymer physics, the correlation mechanism between the microstructure evolution and macroscopic mechanical properties of materials under dynamic mechanical action is one of the core research directions. Traditional methods for testing the mechanical properties of materials (such as tension, compression, and puncture) can obtain macroscopic mechanical parameters (such as strength, toughness, and strain rate), but they are difficult to capture the dynamic changes in microstructure (such as crystal orientation, lamellar structure, and phase transitions) in real time, resulting in the long-standing "black box" problem between macroscopic properties and microscopic mechanisms.

[0003] Synchrotron radiation sources, as an advanced detection method with high intensity, high collimation, and high temporal resolution, can achieve real-time characterization of the microstructure of materials under mechanical stress through small-angle X-ray scattering (SAXS), wide-angle X-ray diffraction (WAXS), ultra-small-angle X-ray scattering (USAXS), and grazing-incidence small-angle X-ray scattering (GISAXS), providing key technical support for solving the aforementioned "black box" problem. Currently, researchers have attempted to combine uniaxial tension, biaxial tension, and compression mechanical loading devices with synchrotron radiation sources, achieving the goal of combining some mechanical tests with synchrotron radiation. For example, Chinese invention patent CN112504864A provides a high-temperature mechanical loading device for synchrotron radiation sources. By installing fixtures, actuators, load sensors, and displacement sensors on a fatigue testing machine, it performs mechanical tests such as fatigue tension on samples in a high-temperature environment chamber. However, this device is only suitable for low-speed, quasi-static loading processes such as fatigue tension and isothermal compression. Its loading response speed is slow, the loading path is single, and it is difficult to achieve high strain rate control in the loading area, making it completely unsuitable for puncture-like mechanical behaviors with high-speed suddenness and concentrated local deformation. Furthermore, the high-temperature environment chamber of the device adopts a closed cylindrical structure. Although it is equipped with a high-temperature resistant glass window to meet the needs of synchrotron radiation experiments, it does not systematically consider the requirements of X-ray scattering characterization methods (such as SAXS, WAXS, and GISAXS) on scattering paths, angular degrees of freedom, and device channels. This makes it difficult to achieve multi-angle, wide-range, and instantaneous synchronous acquisition of structural information in actual operation, resulting in the inability to effectively capture microstructural changes during key deformation processes.

[0004] Furthermore, existing technologies generally employ standard symmetrical rigid clamps for sample fixation. This structure is suitable for bulk or elongated samples, but it cannot provide stable boundary constraints or control capabilities suitable for localized concentrated loading for non-standard forms such as flexible films, layered composites, and porous structures commonly found in polymer materials. This makes it difficult to achieve the typical stress concentration and boundary displacement coupling control in puncture behavior, affecting the accuracy and consistency of structural observation and mechanical measurements. In traditional uniaxial and biaxial tensile testing devices, the force direction on the sample is often perpendicular to the direction of X-ray transmission. This structural arrangement provides sufficient space for X-rays to pass through the sample, facilitating real-time observation of the microstructure under synchrotron radiation. However, due to the limitations of the experimental format, the force direction on the sample in puncture experiments is consistent with the overall direction of its deformation, making it impossible to provide space for X-ray penetration as in the former. In addition, according to national standards and industry specifications, puncture experiments generally use a fixed clamp and a moving push rod loading method, causing the sample to be continuously in a dynamic displacement state during the experiment, making it difficult to meet the basic requirements for spatial stability and variable control in synchrotron radiation testing. Meanwhile, the structural design of traditional loading devices has not been optimized for the detection requirements of synchrotron radiation sources. Loading components such as push rods and clamps in the device are often directly located in the incident path or detection area of ​​X-rays, which seriously obstructs the X-ray path, making it impossible to accurately project X-rays onto the sample, and thus making it impossible to obtain the microstructural information required during the puncture process.

[0005] Therefore, existing synchrotron radiation combined with other technologies still suffers from technical shortcomings when facing complex loading conditions with high strain rates, such as lagging loading mechanisms, limited detection paths, poor sample compatibility, and weak data collaboration capabilities. As a result, the study of the microstructure evolution mechanism during the puncture process is still in a technical gap stage, and a stable and widely applicable experimental system has not yet been formed. This is also one of the important technical challenges that urgently need to be overcome in the current research on materials physics, especially the mechanical behavior of polymers. Summary of the Invention

[0006] To address the technological gaps in existing technologies regarding the correlation between the macroscopic performance and microscopic mechanisms of puncture behavior, and the challenges in combining synchrotron radiation sources with puncture behavior, this invention proposes an online puncture device coupled with a synchrotron radiation source, along with its usage and applications. The technical solution of this invention is as follows:

[0007] A synchrotron radiation source-coupled online puncture device includes a puncture component, a guide rail component, a motor component, a control system, and an X-ray imaging component; the synchrotron radiation source-coupled online puncture device also includes a base plate and an instrument handle, the base plate being provided with several screw holes for fixing the various components.

[0008] The puncture assembly includes a movable sample clamp, a push rod, a fixed sensor, a bracket, and an adapter plate. The push rod has a hollow structure, and its non-puncture end is detachably connected to the fixed sensor via an adapter. The movable sample clamp is connected to a guide rail assembly. The X-ray emitted by the X-ray emitter in the X-ray imaging assembly is coaxial with the push rod and the movable sample clamp. The motor assembly is connected to the guide rail assembly to drive the movable sample clamp to move towards the push rod to achieve puncture.

[0009] The control system simultaneously controls the operation of the fixed sensor, motor assembly, and X-ray imaging assembly, enabling the collection and export of real-time mechanical data and real-time scattering or diffraction intensity data while puncturing the object.

[0010] Furthermore, the push rod is any one of a hollow push rod, a window push rod, or a ball-head push rod; the hollow push rod has a circular through hole with a diameter of 4.8 mm along the axial direction; the window push rod has a circular through hole with a diameter of 4.8 mm along the axial direction, and its 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 push rod has a circular through hole with a diameter of 4.8 mm along the axial direction, and its head is assembled with a steel ball with a diameter of 25 mm, the opening diameter of the steel ball being 5 mm, for use in textile bursting tests; it conforms to the national standard GB / T19976 "Determination of Bursting Strength of Textiles - Steel Ball Method", and is close to the standard published by the American Society for Testing and Materials (ASTM) regarding ASTM D6797 "Standard Test Method for Bursting Strength of Fabrics - Constant Rate of Elongation (CRE) Steel Ball Bursting Test" (steel ball diameter is 25.4 mm).

[0011] Furthermore, the movable sample holder includes an upper pressure plate, a lower pressure plate, and fastening screws. The lower pressure plate is detachably connected to the upper pressure plate via the fastening screws, and both have through holes in their centers to form a hollow detection area. The bracket and the fixed sensor are both connected to the top rod with hollow through holes, allowing the X-ray beam to pass through the top rod to the hollow detection area of ​​the movable sample holder.

[0012] Furthermore, the guide rail assembly includes a guide rail housing, two guide rails, bearing I, a lead screw, nut seat I, a bearing sleeve, nut seat II, two sliders, and bearing III. The movable sample holder, nut seat I, and two sliders are connected sequentially from top to bottom. Specifically, the upper pressure plate is fixedly connected to nut seat I via an adapter plate. The two sliders are slidably connected to the two guide rails respectively. The two guide rails are arranged parallel to the lead screw and in the same direction as the puncture. The two ends of the lead screw are rotatably connected to bearing III inside nut seat II and bearing I inside bearing sleeve, respectively. The lead screw is threadedly connected to nut seat I. The bearing sleeve is fixedly connected to the base plate for fixing the guide rail assembly. The fixed sensor is fixedly connected to nut seat II via a bracket. Simultaneously, the guide rail housing has two gaps corresponding to the guide rails for the movable sample holder to move.

[0013] Furthermore, the motor assembly includes a motor, a coupling, a worm gear, a bearing II, a worm wheel, and a bearing housing disposed inside the motor housing; one end of the motor is fixedly connected to the worm gear via the coupling, the other end of the worm gear is rotatably connected to the bearing II in the bearing housing, and the bearing housing is fixedly connected to the base plate for fixing the motor assembly; the worm gear is meshed with the worm wheel for transmission, and the worm wheel is fixedly connected to the end of the lead screw near the fixed sensor.

[0014] Furthermore, the X-ray imaging assembly includes an X-ray emitter and an X-ray detector; the X-ray detector includes a small-angle X-ray scattering detector and a wide-angle X-ray diffraction detector; the small-angle X-ray scattering detector includes a small-angle X-ray scattering detector and an ultra-small-angle X-ray scatterer.

[0015] Furthermore, the control system includes a computer and a PLC controller and an X-ray data acquisition system that are connected in communication with the computer.

[0016] Furthermore, 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 and control the operation of the motor; the data acquisition module is used to acquire the mechanical signals acquired 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 fixture based on the pulse signals and calculates the mechanical data based on the mechanical signals, and transmits the mechanical data and displacement data to the computer; the computer has built-in testing machine measurement and control software to draw mechanical curves in real time.

[0017] 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 to emit X-rays, while the detection module controls the X-ray detector to receive X-ray signals and convert them into electrical signals, which are then transmitted to a computer by the data transmission module. The computer has built-in FIT2D software to draw X-ray scattering or diffraction patterns in real time.

[0018] A method of using the above-mentioned synchrotron radiation source coupled with an online puncture device includes the following steps:

[0019] S1: Adjust the fastening screws to fix the sample to be tested between the upper and lower pressure plates of the movable sample holder;

[0020] S2: The X-ray emission module activates the X-ray emitter, and simultaneously the detection module activates the X-ray detector. The X-rays emitted by the X-ray emitter are adjusted to be coaxial with the push rod, the movable sample clamp, and the small-angle X-ray scattering detector, ensuring that the X-rays sequentially pass through the hollow area of ​​the push rod, the sample to be punctured area, and are received by the X-ray detector. If the X-ray spot size on the sample is greater than 300 × 400 μm... 2 Proceed to step S3; if the X-ray spot size on the sample is less than 300 × 400 μm 2 Then proceed to step S4;

[0021] S3: The control module simultaneously starts the fixed sensor and the motor; the motor drives the worm gear to rotate, which in turn drives the lead screw to rotate, ultimately driving the nut seat I to move the movable sample clamp 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 from the motor in real time, and the data processing module transmits the mechanical data and displacement data to the computer, from which the testing machine's measurement and control software exports the real-time mechanical curve of the puncture process; 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, from which the FIT2D software exports the real-time X-ray scattering or diffraction pattern; until the high-speed or low-speed puncture process of the sample is achieved;

[0022] S4: Several movable sample clamp positions are preset. The control module starts the fixed sensor and motor. The motor drives the worm gear to rotate, the worm wheel to mesh and the lead screw to rotate. Nut seat I moves the movable sample clamp to the first preset position and pauses the movement. The X-ray emission module controls the X-ray emitter to perform X-ray scanning of 4 to 25 points in the center and the upper, lower, left and right directions of the sample area to be punctured. The movable sample clamp is then moved to the next position, and the scanning process is repeated. 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 testing machine control software exports the real-time mechanical curves of the sample under different deformation states during the puncture process. At the same time, the detection module converts the X-ray signals received by the X-ray detector into electrical signals. The data transmission module transmits the electrical signals to the computer. The FIT2D software exports the real-time X-ray scattering or diffraction patterns of the sample under different deformation states. The process continues until the sample is punctured.

[0023] An application of the above-mentioned synchrotron radiation source combined with an online puncture device is used to study the correlation mechanism between the microstructure and macroscopic mechanical properties of polymer films, composite materials and other samples under puncture load.

[0024] Compared with existing technologies, this invention solves the problems of the technical gap in the correlation mechanism between the macroscopic performance and microscopic mechanism of puncture behavior, and the technical difficulties in combining the mechanism of synchrotron radiation source and puncture behavior. Specifically, the beneficial effects are as follows:

[0025] 1. A groundbreaking solution to the challenge of integrating a puncture device with a synchrotron radiation source: This invention employs a hollow, detachable top rod, effectively addressing the X-ray path obstruction problem. Simultaneously, a movable sample holder (with a movement speed of 10~1000 mm / min) provides the device with high-precision displacement control, significantly improving the spatial positioning accuracy and stability of the sample during X-ray detection. This invention, through a control system that regulates the puncture behavior of the device and the synergistic effect of the data acquisition behavior of the sensors and detectors, fundamentally overcomes the technical barrier preventing traditional puncture experiments from being combined with synchrotron radiation detection. It enables real-time observation of the microstructural evolution under complex puncture mechanics, filling the gap in the combined application of synchrotron radiation source technology in high-speed, sudden loading scenarios.

[0026] 2. Replaceable Top Rod Structure Design Enables Multiple Puncture Behaviors and Co-operation with Synchrotron Radiation Sources: The top rod structure provided by this invention includes three replaceable types: hollow top rod, window top rod, and ball-head top rod. Functional optimizations are made for different sample material types, puncture modes, and detection requirements. All types adopt a modular design, allowing for rapid disassembly and interchangeability according to experimental needs, significantly enhancing the adaptability and operational convenience of the loading system. The window material of the window top rod is also replaceable, possessing good versatility and interchangeability, facilitating on-site debugging and rapid switching between multi-task experiments. This structure significantly improves the experimental flexibility and technical scalability of the device, breaking through the limitations of traditional loading systems with single functions and fixed structures, and providing key support for constructing a universal, multi-field coupled, high spatial resolution synchrotron radiation mechanical detection platform.

[0027] 3. Effectively improves instantaneous and transient response during the puncture process: This invention achieves a unified high precision and real-time performance in data acquisition by optimizing the spatial coordination of the loading structure and detection path, combined with the coordinated layout of the hollow top rod, the mobile sample fixing platform, and the multi-angle X-ray detection window. During loading, the control system implements a synchronous triggering mechanism and a high-speed acquisition module, enabling precise matching between mechanical loading and X-ray imaging within a second-level timescale. This ensures that structural response information at critical deformation moments is not missed, thereby significantly improving the temporal resolution and transient response capture capability of the data. Attached Figure Description

[0028] Figure 1 This is a schematic diagram of a puncture device used in conjunction with an online synchrotron radiation source.

[0029] Figure 2 This is a schematic diagram of the internal structure of a puncture device used in conjunction with an online synchrotron radiation source.

[0030] Figure 3 This is a schematic diagram of the mandrel structure for a hollow mandrel;

[0031] Figure 4 This is a schematic diagram of the top structure of the window top rod;

[0032] Figure 5 This is a schematic diagram of the top head structure of the ball-end rod;

[0033] Figure 6 This is a schematic diagram of the guide rail assembly and motor assembly.

[0034] Figure 7 This is a diagram of the X-ray propagation path;

[0035] The components include: 1. Movable sample holder; 11. Upper pressure plate; 12. Lower pressure plate; 13. Fastening screw; 14. Adapter plate; 2. Top rod; 21. Adapter; 22. Hollow top rod; 23. Window top rod; 24. Ball head top rod; 3. Fixed sensor; 31. Bracket; 4. Guide rail housing; 41. Guide rail; 42. Bearing I; 43. Lead screw; 44. Nut seat I; 45. Bearing sleeve; 46. Nut seat II; 47. Slider; 5. Motor housing; 51. Motor; 52. Coupling; 53. Worm gear; 54. Bearing II; 55. Worm wheel; 56. Bearing seat; 6. Base plate; 7. Instrument handle; 8. Screw hole; 9. X-ray emitter; 10. X-ray small angle scattering detector; 101. Wide-angle X-ray diffraction detector. Detailed Implementation

[0036] To make the technical solutions of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. It should be noted that the following embodiments are only used to better understand the technical solutions of the present invention and should not be construed as limiting the present invention.

[0037] Example 1.

[0038] This embodiment constructs an online puncture device using a synchrotron radiation source, such as... Figure 1The diagram shows a schematic of the online synchrotron radiation source puncture device. As can be seen from the diagram, the online synchrotron radiation source puncture device includes a puncture component, a guide rail component, a motor component, a control system, and an X-ray imaging component. The online synchrotron radiation source puncture device also includes a base plate 6 and an instrument handle 7. The base plate 6 is provided with several screw holes 8 for fixing the various components.

[0039] like Figure 1-5 As shown, the puncture assembly includes a movable sample holder 1, a push rod 2, a fixed sensor 3, a bracket 31, and an adapter plate 14. The push rod 2 has a hollow structure, and its non-puncture end is detachably connected to the fixed sensor 3 via an adapter 21. The movable sample holder 1 is connected to a guide rail assembly. The X-ray emitted by the X-ray emitter 9 in the X-ray imaging assembly is coaxial with the push rod 2 and the movable sample holder 1. The motor assembly is connected to the guide rail assembly to drive the movable sample holder 1 to move towards 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, so as to collect and export real-time mechanical data and real-time scattering or diffraction intensity data while puncturing.

[0040] Wherein, the push rod 2 is a hollow push rod 22 ( Figure 3 ), Window top bar 23 ( Figure 4 ) or topspin 24 ( Figure 5 The hollow top rod 22 has a circular through hole with a diameter of 4.8 mm along the axial direction; the window top rod 23 has a circular through hole with a diameter of 4.8 mm along 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, and sapphire glass; the ball-head top rod 24 has a circular through hole with a diameter of 4.8 mm along the axial direction, and the head is assembled with a steel ball with a diameter of 25 mm, the opening diameter of the steel ball is 5 mm, for use in textile bursting tests; it conforms to the national standard GB / T19976 "Determination of Bursting Strength of Textiles - Steel Ball Method", and is close to the standard of ASTM D6797 "Standard Test Method for Bursting Strength of Fabrics - Constant Rate of Elongation (CRE) Steel Ball Bursting Test" (steel ball diameter is 25.4 mm) issued by the American Society for Testing and Materials (ASTM).

[0041] The movable sample holder 1 includes an upper pressure plate 11, a lower pressure plate 12, and fastening screws 13. The lower pressure plate 12 is detachably connected to the upper pressure plate 11 via the fastening screws 13, and both have through holes in their centers to form a hollow detection area. The bracket 31 and the fixed sensor 3 are both connected to the top rod 2 with hollow through holes, allowing the X-ray beam to pass through the top rod 2 to the hollow detection area of ​​the movable sample holder 1.

[0042] like Figure 1 , 2 As shown in Figure 6, the guide rail assembly includes a guide rail housing 4, two guide rails 41, bearing I 42, lead screw 43, nut seat I 44, bearing sleeve 45, nut seat II 46, two sliders 47, and bearing III. The movable sample clamp 1, nut seat I 44, and two sliders 47 are connected sequentially from top to bottom. Specifically, the upper pressure plate 11 is fixedly connected to nut seat I 44 via an adapter plate 14. The two sliders 47 are slidably connected to the two guide rails 41 respectively. The two guide rails 41 are arranged parallel to the lead screw 43 and in the same direction as the puncture. The two ends of the lead screw 43 are rotatably connected to bearing III inside nut seat II 46 and bearing I 42 inside bearing sleeve 45 respectively. The lead screw 43 is threadedly connected to 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 nut seat II 46 via a bracket 31. Meanwhile, the guide rail housing 4 has two gaps corresponding to the guide rail 41, allowing the movable sample clamp 1 to move.

[0043] like Figure 1 , 2 As shown in Figure 6, the motor assembly includes a motor 51, a coupling 52, a worm gear 53, a bearing II 54, a worm wheel 55, and a bearing housing 56 disposed inside the motor housing 5. One end of the motor 51 is fixedly connected to one end of the worm gear 53 via the coupling 52, and the other end of the worm gear 53 is rotatably connected to the bearing II 54 in the bearing housing 56. The bearing housing 56 is fixedly connected to the base plate 6 for fixing the motor assembly. The worm gear 53 is meshed with the worm wheel 55 for transmission, and the worm wheel 55 is fixedly connected to one end of the lead screw 43 near the fixed sensor 3.

[0044] 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 and an X-ray data acquisition system that are connected to the computer in communication. 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 acquire the mechanical signals acquired 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 based on the pulse signals and calculates the mechanical data based on the mechanical signals, and transmits the mechanical data and displacement data to the computer. The computer has built-in testing machine control software to draw mechanical curves 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, 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 the computer by the data transmission module. The computer has built-in FIT2D software to draw X-ray scattering or diffraction patterns in real time.

[0045] Example 2.

[0046] This embodiment is based on embodiment 1, such as... Figure 7 The diagram illustrates a method for using an online puncture device coupled with a synchrotron radiation source, comprising the following steps:

[0047] 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 clamp 1;

[0048] S2: The X-ray emission module activates the X-ray emitter 9, and simultaneously the detection module activates the X-ray detector. The X-rays emitted by the X-ray emitter 9 are adjusted to be coaxial with the top rod 2, the movable sample clamp 1, and the small-angle X-ray scattering detector 10, so that the X-rays can sequentially pass through the hollow area of ​​the top rod 2 and the sample to be punctured, and be received by the X-ray detector. If the X-ray spot size on the sample is greater than 300 × 400 μm... 2 Proceed to step S3; if the X-ray spot size on the sample is less than 300 × 400 μm 2 Then proceed to step S4;

[0049] S3: The control module simultaneously activates the fixed sensor 3 and the motor 51; the motor 51 drives the worm gear 53 to rotate, which in turn drives the worm wheel 55 to mesh and transmit power, thereby driving the lead screw 43 to rotate, and finally driving the nut seat I 44 to drive the movable sample clamp 1 to move towards the push 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, and the data processing module transmits the mechanical data and displacement data to the computer, and the testing machine measurement and control software exports the real-time mechanical curve of the puncture process; at the same time, the detection module converts the X-ray signal received by the X-ray detector into an electrical signal, and the data transmission module transmits the electrical signal to the computer, and the FIT2D software exports the real-time X-ray scattering or diffraction pattern; until the high-speed or low-speed puncture process of the sample is achieved;

[0050] S4: Several movable positions of the movable sample clamp 1 are preset. The control module starts the fixed sensor 3 and motor 51. The motor 51 drives the worm gear 53 to rotate, the worm wheel 55 engages and drives the lead screw 43 to rotate. The nut seat I 44 drives the movable sample clamp 1 to move towards the top rod 2 to the first preset position 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 sample to be punctured area. The movable sample clamp 1 is then moved to the next position, and the scanning process is repeated. 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. The testing machine control software exports the real-time mechanical curves of the sample under different deformation states during the puncture process. At the same time, the detection module converts the X-ray signals received by the X-ray detector into electrical signals. The data transmission module transmits the electrical signals to the computer. The FIT2D software exports the real-time X-ray scattering or diffraction patterns of the sample under different deformation states. The process continues until the sample is punctured.

[0051] In practice, the following methods are adopted: Figure 7The synchrotron radiation source-coupled online puncture device shown uses a movable sample holder 1 to fix a polymer sample (such as a polyethylene film). The push rod 2 is a window push rod 23, with a circular through-hole of 4.8 mm in diameter along the axial direction and a single-crystal diamond of 5 mm in diameter and 0.5 mm in thickness embedded at its head. The small-angle X-ray scattering detector 10 is a small-angle X-ray scattering detector, paired with a wide-angle X-ray diffraction detector 101. The X-ray emission module drives the X-ray emitter 9, while the detection module activates the X-ray detector. The X-ray beam is adjusted to be coaxial with the push rod 2, the sample to be punctured area, and the small-angle X-ray scattering detector. The wide-angle X-ray diffraction detector 101 is located 45–1800 mm above the optical path. Whether X-ray scanning is needed is determined based on the size of the X-ray spot on the sample. Simultaneously, the control module activates the fixed sensor 3 and motor 51, and the nut seat I 44 drives the movable sample clamp 1 to move towards the top rod 2, realizing the puncture process. The FIT2D software exports real-time X-ray scattering and diffraction patterns of the puncture process; the testing machine's measurement and control software exports real-time mechanical curves of the puncture process. By combining the macroscopic mechanical data and microstructure evolution data of the polymer sample puncture process, the correlation mechanism between the microstructure and macroscopic mechanical properties of polymer films, composite materials, and other samples under puncture loads can be studied. The synchrotron radiation source time resolution of the puncture device coupled with the synchrotron radiation source provided by this invention can reach the second level.

[0052] In summary, this invention employs a hollow, detachable top rod 2, in conjunction with a movable sample holder 1. Through a control system, it regulates the piercing behavior of the piercing device and the synergistic effect of the data acquisition behavior of the sensors and detectors, achieving a unified high precision and real-time performance in data acquisition. This fundamentally overcomes the technical barrier of traditional piercing experiments being unable to be conducted in conjunction with synchrotron radiation detection, enabling real-time observation of the microstructural evolution under complex piercing mechanics, and filling the gap in the combined application of synchrotron radiation source technology in high-speed, sudden loading behaviors.

[0053] The above description of the embodiments is only for the purpose of helping to understand the method and core ideas of the present invention. It should be noted that those skilled in the art can make several improvements and modifications to the present invention without departing from the principles of the present invention, and these improvements and modifications also fall within the protection scope of the claims of the present invention.

[0054] The above description of the disclosed embodiments enables those skilled in the art to make or use the invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Therefore, the invention is not 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 online use with a synchrotron radiation source, characterized in that, It includes a puncture assembly, a guide rail assembly, a motor assembly, a control system, and an X-ray imaging assembly; The puncture assembly includes a movable sample clamp (1), a push rod (2), and a fixed sensor (3); the push rod (2) has a hollow structure; the non-puncture end of the push rod (2) is detachably connected to the fixed sensor (3); the movable sample clamp (1) is connected to the guide rail assembly; the X-ray emitted by the X-ray emitter (9) in the X-ray imaging assembly is coaxial with the push rod (2) and the movable sample clamp (1); the motor assembly is connected to the guide rail assembly to drive the movable sample clamp (1) to move towards 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, so as to collect and export real-time mechanical data and real-time scattering or diffraction intensity data while puncturing.

2. The synchrotron radiation source-coupled online puncture device according to claim 1, characterized in that, The movable sample holder (1) includes an upper pressure plate (11) and a lower pressure plate (12). The lower pressure plate (12) is detachably connected to the upper pressure plate (11) and both have through holes in their centers. The top rod (2) is any one of a hollow top rod (22), a window top rod (23), or a ball-head top rod (24); the hollow top rod (22) has a circular through hole in the axial direction; the window top rod (23) has a circular through hole in the axial direction and a window is inlaid at the head; the ball-head top 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 at the head.

3. The synchrotron radiation source-coupled 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 clamp (1), the nut seat I (44), and the slider (47) are connected sequentially from top to bottom; the slider (47) is slidably connected to the guide rail (41); the guide rail (41) is parallel to the lead screw (43) and is in the same direction as the puncture; 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); the fixed sensor (3) is connected to the nut seat II (46).

4. The synchrotron radiation source-coupled online puncture device according to claim 3, characterized in that, The motor assembly includes a motor (51), a worm (53) and a worm wheel (55); the motor (51) is fixedly connected to the worm (53); the worm (53) is meshed and driven by the worm wheel (55); the worm wheel (55) is fixedly connected to the end of the lead screw (43) near the fixed sensor (3).

5. The synchrotron radiation source-coupled online puncture device according to claim 4, characterized in that, 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.

6. The synchrotron radiation source-coupled 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 that are connected in communication with the computer.

7. The synchrotron radiation source-coupled 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 acquire the mechanical signals acquired 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) based on the pulse signals and calculates the mechanical data based on the mechanical signals. The mechanical data and displacement data are then transmitted to the computer, and the computer plots 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, 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 the computer by the data transmission module. The computer then draws X-ray scattering or diffraction patterns in real time.

8. A method of using the synchrotron radiation source coupled with an online puncture device as described in claim 7, characterized in that, Includes the following steps: S1: Fix the sample to be tested between the upper pressure plate (11) and the lower pressure plate (12) of the movable sample clamp (1); S2: The X-ray emission module drives the X-ray emitter (9), and the detection module activates the X-ray detector. The X-ray emitted by the X-ray emitter (9) is adjusted 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 sample to be pierced in sequence, and be received by the X-ray detector; if the light spot of the X-ray on the sample is greater than 300×400 μm 2 Proceed to step S3; If the X-ray source spot on the sample is less than 300 × 400 μm 2 Then proceed to step S4; S3: The control module simultaneously starts the fixed sensor (3) and the motor (51), and the nut seat I (44) drives the movable sample clamp (1) to move towards the top rod (2); the computer outputs 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 clamps (1), the control module starts the fixed sensor (3) and motor (51), the nut seat I (44) drives the movable sample clamps (1) to move to the top rod (2) to the first preset position 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 and left and right directions of the sample to be pierced; continue to advance the movable sample clamps (1) to the next position and repeat the scanning process; the computer exports the real-time mechanical curves and real-time X-ray scattering or diffraction patterns of the sample under different deformation states during the piercing process; until the sample is pierced.

9. The method of using the synchrotron radiation source coupled with the online puncture device according to claim 8, characterized in that, The speed at which the driven moving sample holder (1) described in S3 moves is 10~1000 mm / min.

10. An application of an online puncture device coupled with a synchrotron radiation source as described in any one of claims 1-7, characterized in that, It is applied to the study of the correlation mechanism between the microstructure and macroscopic mechanical properties of polymer films, composite materials and other samples under puncture load.

Images