In-situ spectroscopy apparatus for composites under load conditions
By designing a sealed sample chamber and anvil structure and a multi-parameter adjustable spectroscopic device, the problem of insufficient multi-parameter control in existing high-temperature and high-pressure spectroscopic characterization equipment has been solved. This enables efficient and accurate composite material research, supports various spectral detection methods, and meets the experimental requirements of composite materials in multi-field coupling environments.
Patent Information
- Application Number
- CN202510462352.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-14
- Publication Date
- 2025-11-18
- Estimated Expiration
- 2045-04-14
AI Technical Summary
Existing high-temperature and high-pressure spectroscopic characterization techniques cannot simultaneously meet the multi-parameter control requirements of high temperature, high pressure, and dynamic force loading, resulting in insufficient experimental stability and accuracy of the equipment in complex environments, making it difficult to meet the multi-dimensional research needs of composite materials.
An in-situ spectroscopic device for composite materials under force loading conditions was designed, including a press assembly and a gas pressurization assembly. A sealed test chamber is formed by the sample chamber and the anvil. Combined with the temperature control component and the gas pressurization assembly, the device can achieve precise adjustment of pressure and temperature and coordinated control of multiple parameters, and supports flexible switching of multiple spectral detection functions.
It achieves sealing and stability under high temperature and high pressure conditions, supports multiple spectral detection, improves experimental efficiency and accuracy, and can comprehensively simulate the multi-field coupling effect of composite materials in actual environment, providing a precise experimental means for the study of failure mechanism of composite materials.
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Figure CN120275158B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of in-situ characterization technology, and more particularly to an in-situ spectroscopic device. Background Technology
[0002] While significant progress has been made in characterizing composite materials under high temperature, high pressure, and dynamic force loading conditions, certain limitations remain. Currently widely used research methods include high-pressure chambers, tensile devices, and equipment combined with spectroscopic analysis techniques, such as high-pressure Raman spectrometers and high-temperature infrared spectrometers. These devices play a crucial role in studying the physicochemical properties of materials, particularly in investigating structural changes, chemical reactions, and mechanical properties under high temperature and high pressure conditions, demonstrating significant technological advantages. However, these devices often have limitations in combining pressure, temperature, and spectroscopic functions, making in-situ characterization of composite materials under complex environments difficult. Specifically, current high-pressure chambers typically utilize diamond anvil cells, applying ultra-high pressure to the sample to achieve high-pressure research. However, traditional diamond anvil cell devices still face challenges in the accuracy and repeatability of pressure control. Furthermore, these devices have limitations in controlling the sample environment (such as temperature and fluid environment) after pressure application, especially under multi-parameter coupling conditions, making it difficult to achieve comprehensive modulation of sample properties. Furthermore, traditional high-pressure chamber devices primarily target solid samples, lacking effective methods for loading and controlling liquid or gaseous samples, and their dynamic control capabilities for the fluid environment are insufficient. For example, in scenarios involving complex chemical reactions, precise injection of liquid reagents and dynamic control of atmospheric conditions are often difficult to achieve, thus limiting the application scenarios of the equipment. In addition, existing technologies also have certain deficiencies in the sealing design of the sample chamber, making fluid leakage or contamination of the sample within the chamber difficult to avoid under high temperature and high pressure environments. These problems, to some extent, limit the practicality and reliability of high-pressure chamber devices.
[0003] In terms of spectroscopic detection, existing high-temperature and high-pressure in-situ spectroscopic analysis equipment mostly adopts a fixed optical path design, supporting only a single type of spectroscopic detection function, such as Raman spectroscopy or infrared spectroscopy. This single spectroscopic function limits the equipment's application capabilities in multiple scenarios and dimensions. The properties of composite materials often involve parameter variations in multiple physical and chemical dimensions, and a single spectroscopic method cannot comprehensively reveal the behavior of materials in complex environments. For example, infrared spectroscopy can characterize the chemical bond vibration characteristics of materials, while Raman spectroscopy is better at revealing crystal structure and molecular symmetry, both of which are indispensable for the comprehensive characterization of materials. However, due to the limitations of existing equipment design, researchers often need to use multiple sets of equipment for separate testing, resulting in low experimental efficiency. At the same time, inconsistencies in the testing environment may introduce experimental errors, further affecting the accuracy of the research. Existing technologies also have technical bottlenecks in the dynamic control of temperature and pressure. The heating and pressure control devices of most devices are independent of each other, resulting in weak multi-parameter coordinated control capabilities. For example, CN202210572912.0 - A diamond anvil press with an in-situ heating device - only discloses the temperature control method. Especially under load conditions, existing equipment struggles to simultaneously regulate pressure, temperature, and mechanical stress, parameters that often have significant coupling relationships in material performance testing. For instance, in the study of failure mechanisms of composite materials, the combined effects of mechanical stress and high-temperature environments significantly influence the microstructure and performance changes of the material; independent control of a single parameter is insufficient to meet the demands of high-precision research. Furthermore, traditional equipment has limited temperature control range and insufficient stability under high-temperature environments, restricting the depth and breadth of research.
[0004] Based on the aforementioned shortcomings, many research teams and companies have begun to attempt to improve existing equipment to better meet the in-situ characterization needs of composite materials under high temperature, high pressure, and force loading conditions. For example, improvements have been made to the design of diamond anvil cells to optimize the sealing and fluid injection capabilities of the chamber; or to introduce adjustable multi-path designs to enable the equipment to adapt to various spectroscopic analysis techniques. However, these improvements still face many technical challenges, such as increased operational difficulty due to increased complexity of the equipment structure, enhanced interference of spectral signals in complex environments, and insufficient stability of multi-parameter control systems. Overall, existing high-temperature and high-pressure spectroscopic characterization techniques still have significant room for improvement in terms of equipment versatility, environmental control flexibility, and experimental efficiency.
[0005] The information disclosed in this background section is intended only to enhance the understanding of the overall background of the invention and should not be construed as an admission or in any way implying that the information constitutes prior art known to those skilled in the art. Summary of the Invention
[0006] The technical problem to be solved by this invention is: how to solve the problem that existing high temperature and high pressure spectral characterization techniques cannot simultaneously meet the multi-parameter control requirements of high temperature, high pressure and dynamic force loading.
[0007] The present invention solves the above-mentioned technical problems through the following technical means:
[0008] An in-situ spectroscopic device for composite materials under load conditions includes a press assembly and a gas pressurization assembly. The press assembly includes a sample chamber, an anvil, a clamping assembly, a temperature control assembly, and a housing assembly. The sample chamber has a through-structure in the middle, and the anvils are clamped on both sides of the through-structure to form a sealed test chamber. The detachable housing assembly is positioned opposite to and clamps the clamping assembly located inside it. The clamping assembly is pressed against the anvil, and the temperature control assembly surrounds the outside of the sample chamber.
[0009] The sample chamber has a first pipe and a second pipe that are connected to the through structure at both ends. The first pipe and the second pipe extend to the outside of the compressor assembly. The gas pressurization assembly is connected to the other end of the first pipe and the second pipe respectively. The gas pressurization assembly injects the sample into the test chamber and applies pressure.
[0010] This invention forms a sealed test chamber through the sample chamber and anvil, under the mechanical force of the shell assembly and clamping assembly, ensuring the accuracy and stability of pressure application within the chamber and exhibiting higher reliability and repeatability under high temperature and high pressure conditions. Simultaneously, the sealed design of the sample chamber effectively avoids fluid leakage and sample contamination under high temperature and high pressure conditions. This technological breakthrough improves the experimental stability of the equipment in complex environments and ensures the accuracy of test data. This invention also enables testing in high-temperature environments through a temperature control assembly and pressurization of the sample through a gas pressurization assembly. It allows for precise adjustment of the pressure and temperature of the sample within the chamber, especially under dynamic force loading conditions, enabling coordinated control of multiple parameters. Compared to the limitations of traditional equipment that cannot simultaneously adjust multiple environmental fields, the technical advantage of this embodiment lies in its ability to comprehensively simulate the multi-field coupling effects of composite materials in actual use environments, providing a more comprehensive and accurate experimental means for the study of composite material failure mechanisms and structural performance analysis. Preferably, the clamping assembly includes a high-pressure pad and an insulating ceramic cylinder. One end of the high-pressure pad on each side abuts against the anvils on both sides, and the other end of the high-pressure pad abuts against the insulating ceramic cylinder. The insulating ceramic cylinder is clamped by the clamping assembly.
[0011] Preferably, the temperature control component includes a heating element, a heat insulation sleeve, and a water cooling sleeve. The heating element has a ring structure and is located outside the sample cavity. The heating element is connected to the heat insulation sleeve, which is connected to the housing assembly. The water cooling sleeve has a ring-shaped cavity structure, which surrounds the outside of the heat insulation sleeve and is connected to the housing assembly.
[0012] The heating element has a built-in resistance wire, which is electrically connected to the controller in the temperature control box. The current of the resistance wire can be adjusted by the controller. The heat insulation sleeve is responsible for effectively wrapping the heat inside the sample cavity 31 and preventing it from easily flowing out. Its material includes, but is not limited to, various porous materials.
[0013] The heating element is used in conjunction with a water-cooled jacket to precisely control the test temperature.
[0014] Preferably, the housing assembly includes a first housing and a second housing, wherein the first housing and the second housing are located on opposite sides of the clamping assembly, and the first housing and the second housing are connected by a plurality of studs.
[0015] Preferably, the press assembly also includes a temperature sensing element that passes through the pressing assembly, the temperature control assembly, and the housing assembly from the side, with the temperature sensing head of the temperature sensing element embedded in the sample cavity.
[0016] Preferably, the sample cavity, the clamping assembly, and the housing assembly are all provided with conical holes in the middle, and the center lines of each conical hole coincide to form a through optical path.
[0017] The large-open-angle optical path design enables flexible switching between multiple spectral functions. This design breaks through the limitations of traditional single-spectral detection functions, allowing the device to support various spectral detection techniques, including Raman, infrared, and XRD, thereby significantly improving experimental efficiency and the comprehensiveness of material characterization. Users can select different spectral techniques according to experimental needs to achieve multi-dimensional characterization from the chemical composition to the crystal structure of materials, without the need to switch between multiple sets of equipment in different experimental environments. This not only significantly improves experimental efficiency but also effectively avoids data errors that may be introduced due to differences in experimental conditions.
[0018] Preferably, the gas pressurization assembly includes a piston assembly, a pressure transmitter, a high-pressure ball valve, and a connector; the piston assembly is connected to a first pipe at the top of the sample chamber, the pressure transmitter is connected to the high-pressure ball valve and the connector in sequence, and the connector is connected to a second pipe at the bottom of the sample chamber; the high-pressure gas injection piston assembly injects the sample into the sample chamber and applies pressure.
[0019] Preferably, the piston assembly includes a piston chamber, a piston body, a high-pressure plug, and a sample delivery tube; the piston chamber is filled with a liquid sample, one end of the piston chamber is connected to the sample delivery tube, the sample delivery tube is connected to a first pipe at the top of the sample chamber, the piston body is connected inside the piston chamber, one end of the piston chamber is also connected to the high-pressure plug, the high-pressure plug is threaded to the piston chamber, the high-pressure plug is penetrating through the middle, and high-pressure gas is injected into the piston chamber along the high-pressure plug to apply pressure.
[0020] Preferably, it also includes an adapter plate, on which the compressor assembly and the gas booster assembly are connected.
[0021] Preferably, it also includes a displacement table, the press assembly is connected to the displacement table, and the displacement table is connected to the adapter plate.
[0022] The displacement stage is an XYZ displacement device that can achieve multi-directional and multi-angle adjustment. The bottom of the displacement stage is connected to the adapter plate, which can be connected and fixed with various spectrometers. The adapter plate is connected to the press assembly. By adjusting the displacement stage with the knob, the relative position of the light source of the spectrometer and the center of the window of the press assembly is changed to obtain better acquisition effect.
[0023] The advantages of this invention are:
[0024] The in-situ spectroscopic apparatus for composite materials under force loading proposed in this invention represents a significant improvement over existing technologies in terms of functionality, accuracy, applicability, and efficiency. Its multi-parameter synergistic control capability, dynamic liquid sample loading function, and flexible multispectral switching design provide a novel technical approach for in-depth research on composite materials under complex environments, possessing significant scientific value and broad application prospects. This apparatus demonstrates great potential in multiple fields, including composite material failure mechanism research, chemical reaction characterization under high temperature and pressure, and multi-field coupling effect analysis, providing more efficient, comprehensive, and reliable solutions for related research. Attached Figure Description
[0025] Figure 1 This is a schematic diagram of the in-situ spectroscopic device for composite materials under force loading conditions according to an embodiment of the present invention;
[0026] Figure 2 This is a top view of the in-situ spectroscopic device for composite materials under force loading conditions according to an embodiment of the present invention;
[0027] Figure 3 yes Figure 2 Sectional view at point BB;
[0028] Figure 4 yes Figure 2 Sectional view at point AA;
[0029] Figure 5 This is a schematic diagram of the sample cavity structure according to an embodiment of the present invention;
[0030] Figure 6 This is an exploded view of the in-situ spectroscopic apparatus of the composite material under force loading conditions according to an embodiment of the present invention;
[0031] Figure 7 This is a schematic diagram of the operation of the gas booster assembly according to an embodiment of the present invention;
[0032] Numbering on the map:
[0033] 1. Adapter board;
[0034] 2. Displacement stage;
[0035] 3. Press assembly; 31. Sample chamber; 311. First pipe; 312. Second pipe; 32. Anvil; 33. High-pressure pad; 34. Insulating ceramic cylinder; 35. Heating element; 36. Insulation jacket; 37. Water cooling jacket; 371. Liquid inlet; 372. Liquid outlet; 38. First housing; 39. Second housing;
[0036] 4. Gas booster assembly; 41. Piston assembly; 411. Piston chamber; 412. Piston body; 413. High-pressure plug; 414. Sample delivery tube; 42. Pressure transmitter; 43. High-pressure ball valve; 44. T-connector;
[0037] 5. Temperature sensing element. Detailed Implementation
[0038] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0039] Example 1:
[0040] like Figure 1 , Figure 2 As shown, the in-situ spectroscopic device for composite materials under force loading includes a transfer plate 1, a displacement stage 2, a press assembly 3, and a gas pressurization assembly 4.
[0041] The displacement stage 2 is an XYZ displacement device that can achieve multi-directional and multi-angle adjustment. The bottom of the displacement stage 2 is connected to the adapter plate 1, which can be connected and fixed with various spectrometers. The adapter plate 1 is connected to the press assembly 3. By adjusting the displacement stage 2 with the knob, the relative position of the light source of the spectrometer and the center of the window of the press assembly 3 is changed, so as to obtain better acquisition effect.
[0042] like Figure 3 , Figure 4 As shown, the press assembly 3 includes a sample chamber 31, an anvil 32, a clamping assembly, a temperature control assembly, and a housing assembly. The sample chamber 31 has a through-structure in the middle, and the anvils 32 are clamped on both sides of the through-structure to form a sealed test chamber. The detachable housing assembly is positioned opposite to and clamps the clamping assembly located inside it. The clamping assembly abuts against the anvil, and the temperature control assembly surrounds the outside of the sample chamber. The clamping assembly includes a high-pressure pad 33 and an insulating ceramic cylinder 34. The ambient temperature assembly includes a heating element 35 and a heat insulation sleeve 36. The housing assembly includes a first housing 38 and a second housing 39.
[0043] The sample chamber 31 is located at the center of the press assembly 3. The sample chamber 31 extends to the outside of the press assembly 3 through a first pipe 311 and a second pipe 312 at both ends. Figure 5 As shown, the sample cavity 31 has a disc-shaped structure in the middle with a horizontal through-hole. There are platforms on both sides of the through-hole, with conical holes on the outer sides of the platforms. Anvils 32 are respectively placed on the platforms on both sides, thus forming a sealed test chamber with the sample cavity 31. The test chamber is filled with a liquid sample via the first conduit 311, and then the test can be performed. The material of the sample cavity 31 needs to withstand high pressure and high temperature and be resistant to deformation; therefore, the material selection includes, but is not limited to, various high-pressure alloys. Its geometry features a conical hole in the middle to ensure a thin liquid layer for observation, thereby maximizing the spectral analysis of the sample relative to the incident light source. A groove on one side of the middle of the sample cavity 31 is used to place the test head of the temperature sensing element 5.
[0044] Combination Figure 3 , Figure 4 , Figure 6 As shown, the outer sides of the pressure anvils 32 on both sides are abutted by high-pressure pads 33, which in turn are abutted by insulating ceramic cylinders 34. The insulating ceramic cylinders 34 on both sides are respectively bolted to the first housing 38 and the second housing 39 for compression. If the compression assembly, temperature control assembly, and housing assembly may interfere with the first pipe 311 and the second pipe 312, clearance holes or grooves can be provided.
[0045] The high-pressure pad 33, the heat-insulating ceramic cylinder 34, the first shell 38, and the second shell 39 are all provided with conical holes in the middle, and the center lines of each conical hole roughly coincide to form an optical path.
[0046] The heating element 35 is a ring-shaped structure, fitted onto the outside of the high-pressure pad 33 and / or the insulating ceramic cylinder 34. The heating element 35 can be made of heating resistance wire or similar materials, enabling the heating function of the sample cavity 31 and altering its internal pressure environment through heating. Specifically, the heating element 35 contains various types of resistance wires as heating elements, including but not limited to conventional resistance wires, Pt wires, and W wires. The furnace body is ring-shaped, enclosing the sample cavity 31 for heating. The resistance wires are electrically connected to a controller in the temperature control box, allowing adjustment of the current in the resistance wires via the controller.
[0047] The heating element 35 is fixed to the heat insulation sleeve 36. Specifically, the heat insulation sleeve 36 is also annular and is fitted over the heating element 35. In this embodiment, the heat insulation sleeve 36 includes a concave cavity and a connecting plate. The concave cavity and the connecting plate are connected together to form a horizontally penetrating cavity structure. The heating element 35 can be fixed to the concave cavity or the connecting plate by bolts or other means.
[0048] The heat insulation sleeve 36 is connected to the inner side of the second housing 39. After the first housing 38 and the second housing 39 are connected together, on the one hand, it can press the high-pressure pad 33 and the anvil 32 in sequence by abutting against the heat-insulating ceramic cylinder 34, so that the anvil 32 and the sample cavity 31 form a sealed cavity. On the other hand, it seals the heating element 35 and the heat insulation sleeve 36 between the first housing 38 and the second housing 39. The heat insulation sleeve 36 is responsible for effectively wrapping the heat inside the sample cavity 31 and preventing it from easily flowing out. Its material includes, but is not limited to, various porous materials.
[0049] The first housing 38 and the second housing 39 are connected by multiple studs. By turning the studs, the distance between the first housing 38 and the second housing 39 can be changed, thereby achieving the clamping of the anvil 32. Multiple guide posts can also be connected between the first housing 38 and the second housing 39 for guidance.
[0050] Temperature sensing elements 5 are inserted into the side of the press assembly 3. Different types of temperature sensing elements 5 can be placed there. The high-pressure pad 33, the insulating ceramic cylinder 34, and the heating element 35 are provided with clearance holes for the insertion of temperature sensing elements 5. The temperature sensing elements 5 include, but are not limited to, various thermocouples or Pt100 temperature sensing elements, which are used to monitor the temperature changes inside the device in real time. The temperature sensing elements 5 are also responsible for transmitting the real-time temperature data to the controller in the temperature control box. The current is adjusted by the temperature control parameters so that the measured temperature fluctuates slightly at the target temperature.
[0051] The first housing 38 and the second housing 39 of the press assembly 3 serve as the support source for the mechanical loading pressure. The mechanical force is directly transferred to the sample in the sample chamber 31 through the high-pressure pad 33 and the anvil 32. The material of the press assembly 3 in this embodiment can be consistent with that of existing DAC presses. The high-pressure pad 33 can be made of a hard material capable of withstanding high pressure, such as tungsten carbide (WC), and the material of the anvil 32 can include, but is not limited to, various hard materials, such as diamond and single-crystal alumina.
[0052] In this embodiment, the sealed space of the test chamber is composed of an anvil 32 and a sample chamber 31. A platform is made inside the conical hole of the sample chamber 31. By tightening the pressure bolt on the press assembly 3, the anvil 32 is pressed against the platform, thereby forming a sealed space in the center of the sample chamber 31, which can withstand a pressure of 30 MPa.
[0053] The gas pressurization assembly 4 is the main component for pressurizing and controlling the pressure of the sample. The gas pressurization assembly 4 includes a piston assembly 41, a pressure transmitter 42, a high-pressure ball valve 43, and a three-way connector 44. The gas pressurization assembly 4 is connected to an external high-pressure gas source and is used to push the sample into the sample chamber 31 and to pressurize it. The piston assembly 41 is connected to the first pipe 311 at the top of the sample chamber 31. The pressure transmitter 42 is sequentially connected to the high-pressure ball valve 43 and the three-way connector 44. In this embodiment, two high-pressure ball valves 43 are included, and the three-way connector 44 is connected to both high-pressure ball valves 43 and the second pipe 312 at the bottom of the sample chamber 31. High-pressure gas is introduced into the piston assembly 41 and simultaneously pressurizes the liquid sample in the sample chamber 31 from the input pressure transmitter 42, high-pressure ball valve 43, and three-way connector 44 through the second pipe 312.
[0054] Specifically, such as Figure 7 As shown, the piston assembly 41 includes a piston chamber 411, a piston body 412, a high-pressure plug 413, and a sample delivery tube 414. The piston chamber 411 is filled with a liquid sample. The right end of the piston chamber 411 is connected to the sample delivery tube 414, which is connected to the first pipe 311 at the top of the sample chamber 31. The left end of the piston chamber 411 is connected to the piston body 412. When the piston body 412 moves to the right, the liquid sample can be injected into the sealed test chamber along the sample delivery tube 414 and the first pipe 311. The left end of the piston chamber 411 is also connected to the high-pressure plug 413, which is threaded to the inner surface of the piston chamber 411. The high-pressure plug 413 has a through-hole in the middle, allowing high-pressure gas to be injected into the piston chamber 411 along the high-pressure plug 413 to apply pressure. At the same time, high-pressure gas also enters the bottom of the sample chamber 31 from the pressure transmitter 42, the high-pressure ball valve 43, and the three-way connector 44, thereby applying pressure to the liquid in the test chamber. This increases the internal pressure of the device to the target pressure value, thus completing the pressurization.
[0055] In this embodiment, the liquid sample is injected into the entire device pipeline through the piston chamber 411 and the internal piston body 412 in the piston assembly 41. Then, high-pressure gas is injected into the piston chamber 411 through the high-pressure plug 413, which reduces the volume of the liquid sample in the device pipeline and increases the internal pressure. Secondly, since the sample is a solution, it will generate saturated vapor pressure after heating. The presence of the piston assembly 41 can play a pressure buffering role, ensuring that the internal pressure of the device remains unchanged after heating.
[0056] The pressure transmitter 42 can monitor pressure changes inside the device in real time and feed the data back to the system controller. A pressure testing element can also be built into the sample chamber 31 to obtain the test pressure.
[0057] The high-pressure ball valve 43 can adjust the valve opening.
[0058] High-pressure gas can be generated by gas boosting devices in the prior art, and this embodiment does not impose specific limitations.
[0059] The working process of this embodiment:
[0060] First, connect the adapter plate 1 of the in-situ spectroscopic equipment for composite materials under full force loading to the spectrometer, and then adjust the optical path using the XYZ displacement stage. After aligning the sample chamber 31 of the device with the optical path of the spectrometer, unscrew the high-pressure plug 413, and use the piston to fill the first pipe 311 and the test chamber with the liquid sample. Then tighten the high-pressure plug 413 to complete the sample loading. Next, use the high-pressure gas generated by the gas pressurization device to compress the volume of the liquid sample, thereby increasing the internal pressure of the device to the target pressure value, completing the pressurization. Heat the sample chamber 31 using the heating element 35. When the temperature reaches the target temperature, the spectrometer can begin collecting the corresponding experimental data.
[0061] The in-situ spectroscopic device for composite materials under force loading proposed in this embodiment has significant advantages over existing technologies.
[0062] First, this embodiment ensures the accuracy and stability of pressure application within the chamber through the sealed design of the anvil 32 and the sample chamber 31, resulting in higher reliability and repeatability under high temperature and high pressure conditions. Simultaneously, the sealed design of the sample chamber effectively avoids fluid leakage and sample contamination under high temperature and high pressure conditions. This technological breakthrough improves the experimental stability of the equipment in complex environments and ensures the accuracy of test data.
[0063] Furthermore, the device in this embodiment achieves dynamic loading capability for liquid samples through an external liquid delivery pipeline. This design overcomes the shortcomings of existing technologies in fluid environment control and can meet the needs of composite material research in multiple fields such as chemical reactions, phase transitions, and mechanical properties. Combined with a gas pressurization device and a heating element 35, this device can achieve precise adjustment of the pressure and temperature of the sample within the chamber, especially under dynamic force loading conditions, enabling coordinated control of multiple parameters. Compared to the limitations of traditional devices that cannot simultaneously adjust multiple environmental fields, the technical advantage of this embodiment lies in its ability to comprehensively simulate the multi-field coupling effects of composite materials in actual use environments, providing a more comprehensive and accurate experimental means for the study of composite material failure mechanisms and structural performance analysis.
[0064] This embodiment also achieves flexible switching between multiple spectral functions through a large-open-angle optical path design. This design breaks the limitation of traditional equipment's single spectral detection function, enabling the device to support multiple spectral detection technologies, including Raman, infrared, and XRD, thereby significantly improving experimental efficiency and the comprehensiveness of material characterization. Users can select different spectral technologies according to experimental needs to achieve multi-dimensional characterization from the chemical composition to the crystal structure of materials, without the need to switch between multiple sets of equipment in different experimental environments. This not only significantly improves experimental efficiency but also effectively avoids data errors that may be introduced due to differences in experimental conditions.
[0065] In summary, the in-situ spectroscopic apparatus for composite materials under force loading conditions proposed in this embodiment represents a significant improvement over existing technologies in terms of functionality, accuracy, applicability, and efficiency. Its multi-parameter synergistic control capability, dynamic liquid sample loading function, and flexible multispectral switching design provide a novel technical approach for in-depth research on composite materials under complex environments, possessing significant scientific value and broad application prospects. This apparatus demonstrates great potential in multiple fields, including composite material failure mechanism research, chemical reaction characterization under high temperature and pressure, and multi-field coupling effect analysis, providing a more efficient, comprehensive, and reliable solution for related research.
[0066] Example 2:
[0067] like Figure 3 As shown, in this embodiment, based on Embodiment 1, the press assembly 3 further includes a water-cooling jacket 37. The water-cooling jacket 37 has an annular cavity structure, with an inlet 371 and an outlet 372 connected to it. The water-cooling jacket 37 is used to control the external surface temperature of the entire device. Its interior is hollow for the circulation of the water cooling system, while the external annular structure can be directly connected to the second housing 39 via bolts or other means, cooling the entire device through direct heat conduction.
[0068] In this embodiment, both the heating element 35 and the water-cooling jacket 37 can be turned on during operation. By using the heating element 35 and the water-cooling jacket 37 in combination, precise temperature regulation can be achieved.
[0069] The above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit it. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims
1. An in-situ spectroscopy apparatus for composites under force loading conditions, characterized by, The press assembly comprises a sample cavity, an anvil, a compression assembly, a temperature control assembly, and a shell assembly; the sample cavity has a through structure in the middle, the anvil is tightly pressed on both sides of the through structure to form a sealed test cavity, the detachable shell assembly is oppositely arranged and tightly presses the compression assembly inside, the compression assembly is tightly pressed on the anvil, and the temperature control assembly is arranged outside the sample cavity; The sample cavity has a first pipeline and a second pipeline at both ends, which are in communication with the through structure, and the first pipeline and the second pipeline extend to the outside of the press assembly; the gas pressurization assembly is connected with the other ends of the first pipeline and the second pipeline respectively; the gas pressurization assembly injects the sample into the test cavity and applies pressure. The compression assembly comprises high-pressure pads and an adiabatic ceramic cylinder, one end of the high-pressure pads on both sides is tightly pressed on the anvil on both sides, the other end of the high-pressure pads is tightly pressed on the adiabatic ceramic cylinder, and the adiabatic ceramic cylinder is tightly pressed by the compression assembly. The sample cavity, the compression assembly, and the shell assembly all have a tapered hole in the middle, and the center lines of the tapered holes coincide to form a through optical path. The gas pressurization assembly comprises a piston assembly, a pressure transmitter, a high-pressure ball valve, and a joint; the piston assembly is in communication with the first pipeline at the top end of the sample cavity, the pressure transmitter is sequentially connected with the high-pressure ball valve and the joint, and the joint is connected with the second pipeline at the bottom of the sample cavity; high-pressure gas is injected into the piston assembly to inject the sample into the sample cavity and apply pressure.
2. The in-situ spectroscopy apparatus for composites under force loading conditions of claim 1, wherein, The temperature control assembly comprises a heating body, a heat insulation sleeve, and a water cooling sleeve; the heating body is in an annular structure and is arranged outside the sample cavity; the heating body is connected with the heat insulation sleeve, the heat insulation sleeve is connected with the shell assembly, and the water cooling sleeve is in an annular cavity structure and is arranged outside the heat insulation sleeve and connected with the shell assembly.
3. The in-situ spectroscopy apparatus for composites under applied force of claim 1, wherein, The shell assembly comprises a first shell and a second shell; the first shell is arranged on one side of the compression assembly, and the second shell is arranged on the other side of the compression assembly; the first shell and the second shell are connected by a plurality of studs.
4. The in-situ spectroscopy apparatus for composites under applied force of claim 1, wherein, The press assembly further comprises a temperature measuring element, which passes through the compression assembly, the temperature control assembly, and the shell assembly from the side, and the temperature measuring head of the temperature measuring element is embedded in the sample cavity.
5. The in-situ spectroscopy apparatus for composites under applied force of claim 1, wherein, The piston assembly comprises a piston cavity, a piston body, a high-pressure plug, and a sample feeding tube; the piston cavity is filled with a liquid sample, one end of the piston cavity is connected with the sample feeding tube, the sample feeding tube is in communication with the first pipeline at the top end of the sample cavity, the piston cavity is connected with the piston body, and the high-pressure plug is further connected with one end of the piston cavity; the high-pressure plug is threadedly connected with the piston cavity, the high-pressure plug is penetrated in the middle, high-pressure gas is injected into the piston cavity along the high-pressure plug to apply pressure.
6. The in-situ spectroscopy apparatus for composites under applied force of claim 1, wherein, The press assembly and the gas pressurization assembly are connected on the adapter plate.
7. The in-situ spectroscopy apparatus for composites under applied force of claim 1, wherein, The press assembly is connected on the displacement table, and the displacement table is connected on the adapter plate.
Citation Information
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