Stretching rheometer, microstructure detection device and birefringence detection device suitable for polymer sample

Abstract

The invention provides an extensional rheometer suitable for a polymer sample. The extensional rheometer comprises a base; the high-pressure cavity is mounted on the base, and the high-pressure cavity is suitable for providing different pressure environments; the two stretching rollers are arranged in the high-pressure cavity in parallel at intervals, and the two ends of the sample are connected to the two stretching rollers; the driving assembly is suitable for driving the stretching roller to rotate so as to stretch the sample; the two characterization windows are respectively arranged on two opposite side walls of the high-pressure cavity, and the characterization windows are suitable for allowing detection light beams generated by an external detection light source to penetrate through so as to obtain change information of a microstructure of the sample in a stretching process; and the torque sensor is arranged between the stretching roller and the driving assembly and is suitable for acquiring data that the stretching force generated by the sample in the stretching process changes along with different pressure environments.

Description

Technical Field

[0001] At least one embodiment of the present disclosure relates to the technical field of polymer product processing and performance testing and characterization, and more specifically to an extensional rheometer, a microstructure detection device, and a birefringence detection device suitable for polymer samples. Background Art

[0002] Polymer products must be processed before use to further improve their performance. For some products that originally had poor performance, after stretching, the molecular chains in the polymer are oriented along the direction of the force driven by the external force, and the structure and mechanical properties of the polymer will be improved. Many functional films and fibers are obtained by stretching. For example, polylactic acid (PLA) is very brittle before processing and has insufficient mechanical properties. After stretching, it can not only be toughened, but also greatly increase the mechanical properties. The elongation at break and modulus are greatly increased, expanding the scope of use.

[0003] Some polymer films have different structural changes and deformation mechanisms in different temperature and pressure ranges. At the same time, different gas atmospheres, such as water vapor (water vapor can weaken the hydrogen bonding between cellulose molecules), will affect the structural evolution, and then affect the change of crystallinity, and ultimately change the performance of polymer products.

[0004] The related technology is unable to study the data of how the tensile force generated by the polymer sample during the stretching process changes with different pressure environments, and is unable to realize in-situ research on the structural evolution information of the polymer sample. Summary of the invention

[0005] In order to solve at least one of the above-mentioned and other technical problems in the prior art, the present disclosure provides an extensional rheometer suitable for polymer samples, which can obtain data on the variation of the stretching force generated by the polymer samples during the stretching process with different stretching environments, and obtain information on the changes in the microstructure of the polymer samples during the stretching process.

[0006] According to a first aspect of the present disclosure, there is provided an extensional rheometer suitable for polymer samples, comprising:

[0007] Pedestal;

[0008] A high-pressure chamber is installed on the base, and the high-pressure chamber is suitable for providing different pressure environments;

[0009] Two stretching rollers are arranged in parallel and at intervals inside the high-pressure chamber, and both ends of the sample are connected to the two stretching rollers;

[0010] A driving assembly, adapted to drive the stretching roller to rotate so as to stretch the sample;

[0011] two characterization windows, respectively disposed on two opposite side walls of the high-pressure chamber, the characterization windows being adapted to allow a detection light beam generated by an external detection light source to pass through, so as to obtain information on changes in the microstructure of the sample during the stretching process; and

[0012] The torque sensor is installed between the stretching roller and the driving assembly, and is suitable for obtaining data on the variation of the stretching force generated by the sample during the stretching process with different pressure environments.

[0013] According to an embodiment of the present disclosure, a heating assembly is further included, which is adapted to adjust the temperature inside the high pressure chamber so that:

[0014] The torque sensor obtains data on the variation of the tensile force generated by the sample during the stretching process under the preset temperature inside the high pressure chamber, and / or

[0015] The torque sensor obtains data on the variation of the tensile force generated by the sample during the stretching process under the preset pressure inside the high-pressure chamber as a function of different temperature environments.

[0016] According to an embodiment of the present disclosure, it also includes:

[0017] The gas generating assembly is adapted to input the target gas into the interior of the high pressure chamber, and / or adapted to input the fluid medium into the interior of the high pressure chamber,

[0018] In which, the above-mentioned fluid medium forms steam under the action of the above-mentioned heating component to provide the gas atmosphere required for the experiment based on the above-mentioned target gas and steam, so that the above-mentioned torque sensor can obtain data on the change of the stretching force generated by the above-mentioned sample during the stretching process with different gas atmospheres at the preset temperature and / or preset pressure inside the above-mentioned high-pressure chamber.

[0019] According to an embodiment of the present disclosure, it also includes:

[0020] A pressure gauge is disposed above the high-pressure chamber and is suitable for monitoring pressure changes inside the high-pressure chamber.

[0021] According to an embodiment of the present disclosure, a single film coupling is further included, which is arranged between the above-mentioned torque sensor and the above-mentioned stretching roller, and the above-mentioned single film coupling is suitable for transmitting the stretching force exerted on the above-mentioned sample to the above-mentioned torque sensor.

[0022] According to an embodiment of the present disclosure, the above-mentioned driving assembly includes:

[0023] A servo motor, suitable for providing a driving force; and

[0024] The double film coupling is connected with the torque sensor and the servo motor, and is suitable for transmitting the driving force to the stretching roller to drive the stretching roller to rotate.

[0025] According to an embodiment of the present disclosure, a pressure relief valve is further included, which is suitable for outputting the above-mentioned target gas and / or the above-mentioned steam to adjust the pressure inside the above-mentioned high-pressure chamber.

[0026] According to an embodiment of the present disclosure, the heating assembly comprises:

[0027] A heating chamber body is arranged inside the high pressure chamber;

[0028] A heating plate is arranged on the inner wall of the heating chamber, and the heating plate is suitable for generating heat to adjust the ambient temperature of the sample;

[0029] A temperature sensor, adapted to monitor the temperature inside the heating chamber; and

[0030] The controller is adapted to adjust the temperature inside the heating chamber by controlling the voltage applied to the heating plate.

[0031] According to a second aspect of the present disclosure, there is provided a microstructure detection device suitable for polymer samples, comprising:

[0032] The above extensional rheometer;

[0033] An X-ray light source, adapted to provide initial X-rays, the initial X-rays being incident vertically from the characterization window onto the sample surface;

[0034] A detection assembly, adapted to obtain a microstructure image of the sample by detecting an X-ray beam emitted from a surface of the sample; and

[0035] The three-axis translation stage is configured to movably support the extensional rheometer to adjust the position where the initial X-ray is incident on the sample surface.

[0036] According to a third aspect of the present disclosure, there is provided a birefringence detection device suitable for polymer samples, comprising:

[0037] The above extensional rheometer;

[0038] A laser, adapted to provide an initial laser beam, wherein the initial laser beam is incident vertically from the characterization window to the sample surface;

[0039] An optical path component, adapted to cause the first laser beam after the initial laser beam passes through the sample to undergo birefringence;

[0040] A detector, adapted to obtain the birefringence index of the sample by detecting the first laser beam that undergoes birefringence; and

[0041] The three-axis translation stage is configured to movably support the extensional rheometer to adjust the position where the initial laser beam is incident on the sample surface.

[0042] According to an embodiment of the present disclosure, a base and a high-pressure chamber are provided, and the high-pressure chamber is installed on the base to provide different pressure environments by using the high-pressure chamber; two stretching rollers are provided in parallel and spaced apart inside the high-pressure chamber, and both ends of the polymer sample are connected to the two stretching rollers; a driving assembly is provided to drive the stretching rollers to rotate so as to stretch the sample; two characterization windows are provided on two opposite side walls of the high-pressure chamber, and the characterization windows allow a detection light beam generated by an external detection light source to pass through, so as to obtain information on changes in the microstructure of the sample during the stretching process; a torque sensor is provided between the stretching roller and the driving assembly, so as to obtain data on changes in the stretching force generated by the polymer sample during the stretching process with different stretching environments, and obtain information on changes in the microstructure of the polymer sample during the stretching process. BRIEF DESCRIPTION OF THE DRAWINGS

[0043] The above contents and other objects, features and advantages of the present disclosure will become more apparent through the following description of the embodiments of the present disclosure with reference to the accompanying drawings, in which:

[0044] Figure 1 The working principle diagram of the extensional rheometer applicable to polymer samples according to an embodiment of the present disclosure is schematically shown;

[0045] Figure 2 The working principle diagram of the extensional rheometer with a three-axis translation stage suitable for polymer samples according to an embodiment of the present disclosure is schematically shown;

[0046] Figure 3 A schematic diagram showing the working principle of a microstructure detection device for polymer samples according to an embodiment of the present disclosure; and

[0047] Figure 4 The working principle diagram of the birefringence detection device suitable for polymer samples according to an embodiment of the present disclosure is schematically shown.

[0048] In the above drawings, the meanings of the reference numerals are as follows:

[0049] 1- Subject;

[0050] 2-heating chamber body;

[0051] 3- High pressure chamber;

[0052] 4-heating plate;

[0053] 5- stretching roller;

[0054] 6- Characterization window;

[0055] 7- Pressure gauge;

[0056] 8-intake valve;

[0057] 9-heating chamber sealing plate;

[0058] 10- high pressure chamber sealing plate;

[0059] 11-Single film coupling;

[0060] 12- torque sensor;

[0061] 13- driving assembly;

[0062] 131-Servo motor;

[0063] 132-Double film coupling;

[0064] 14- Gas source;

[0065] 15-pressure relief valve;

[0066] 16-Three-axis translation stage;

[0067] 17-Laser;

[0068] 18-X-ray light source;

[0069] 19-conical vacuum tube;

[0070] 20- a first diffraction detector;

[0071] 21- second diffraction detector;

[0072] 22- optical path component;

[0073] 23- Extensional rheometer. DETAILED DESCRIPTION

[0074] Hereinafter, embodiments of the present disclosure will be described with reference to the accompanying drawings. However, it should be understood that these descriptions are exemplary only and are not intended to limit the scope of the present disclosure. In the following detailed description, for ease of explanation, many specific details are set forth to provide a comprehensive understanding of the embodiments of the present disclosure. However, it is apparent that one or more embodiments may also be implemented without these specific details. In addition, in the following description, descriptions of known structures and technologies are omitted to avoid unnecessary confusion of the concepts of the present disclosure.

[0075] The terms used herein are only for describing specific embodiments and are not intended to limit the present disclosure. The terms "comprise", "include", etc. used herein indicate the existence of the features, steps, operations and / or components, but do not exclude the existence or addition of one or more other features, steps, operations or components.

[0076] All terms (including technical and scientific terms) used herein have the meanings commonly understood by those skilled in the art unless otherwise defined. It should be noted that the terms used herein should be interpreted as having a meaning consistent with the context of this specification and should not be interpreted in an idealized or overly rigid manner.

[0077] When using expressions such as "at least one of A, B, and C, etc.", they should generally be interpreted according to the meaning of the expression commonly understood by those skilled in the art (for example, "a system having at least one of A, B, and C" should include but is not limited to a system having A alone, B alone, C alone, A and B, A and C, B and C, and / or A, B, C, etc.).

[0078] The related technology is unable to study the data of how the tensile force generated by the polymer sample during the stretching process changes with different pressure environments, and is unable to realize in-situ research on the structural evolution information of the polymer sample.

[0079] In view of this, the present disclosure provides an extensional rheometer suitable for polymer samples, which is provided with a base and a high-pressure chamber. The high-pressure chamber is installed on the base to provide different pressure environments; two stretching rollers are arranged in parallel and spaced apart inside the high-pressure chamber, and both ends of the polymer sample are connected to the two stretching rollers; a driving assembly is arranged to drive the stretching rollers to rotate so as to stretch the sample; two characterization windows are arranged on two opposite side walls of the high-pressure chamber, and the characterization windows allow a detection light beam generated by an external detection light source to pass through, so as to obtain information on changes in the microstructure of the sample during the stretching process; a torque sensor is arranged between the stretching roller and the driving assembly, so as to obtain data on changes in the stretching force generated by the polymer sample during the stretching process with different stretching environments, and obtain information on changes in the microstructure of the polymer sample during the stretching process.

[0080] Figure 1 The working principle diagram of the extensional rheometer suitable for polymer samples according to an embodiment of the present disclosure is schematically shown.

[0081] According to the first aspect of the present disclosure, Figure 1As shown, an extensional rheometer suitable for polymer samples is provided, including a base 1, a high-pressure chamber 3, two stretching rollers 5, a driving assembly 13, two characterization windows 6, and a torque sensor 12. The high-pressure chamber 3 is installed on the base 1, and the high-pressure chamber 3 is suitable for providing different pressure environments; the two stretching rollers 5 are arranged in parallel and spaced inside the high-pressure chamber 3, and the two ends of the sample are connected to the two stretching rollers 5; the driving assembly 13 is suitable for driving the stretching rollers 5 to rotate to stretch the sample; the two characterization windows 6 are respectively arranged on the two opposite side walls of the high-pressure chamber 3, and the characterization windows 6 are suitable for allowing the detection light beams generated by the external detection light source to pass through, so as to obtain the change information of the microstructure of the sample during the stretching process; the torque sensor 12 is installed between the stretching roller 5 and the driving assembly 13, and the torque sensor 12 is suitable for obtaining the data of the tensile force generated by the sample during the stretching process changing with different pressure environments.

[0082] According to some embodiments of the present disclosure, a high-pressure chamber 3 is installed on a base 1, and different pressure environments are provided by utilizing the high-pressure chamber 3; two stretching rollers 5 are arranged in parallel and spaced apart inside the high-pressure chamber 3, and both ends of the polymer sample are connected to the two stretching rollers 5; a driving assembly 13 is arranged to drive the stretching rollers 5 to rotate so as to stretch the sample; two characterization windows 6 are arranged on two opposite side walls of the high-pressure chamber 3, and the characterization windows 6 allow a detection light beam generated by an external detection light source to pass through so as to obtain information on changes in the microstructure of the sample during the stretching process; a torque sensor 12 is arranged between the stretching roller 5 and the driving assembly 13, and data on changes in the stretching force generated by the polymer sample during the stretching process with different pressure environments are obtained, and information on changes in the microstructure of the polymer sample during the stretching process is obtained.

[0083] According to some embodiments of the present disclosure, two handles are provided on the top of the base 1, and the handles are suitable for providing convenience for moving the extensional rheometer.

[0084] According to some embodiments of the present disclosure, the stretching rate and the stretching length of the two stretching rollers 5 are constant. The stretching roller 5 is provided with a frosted layer and a screw to ensure that the sample does not fall off. The two stretching rollers rotate in opposite directions.

[0085] According to some optional embodiments of the present disclosure, the stretching roller 5 is capable of stretching the sample within a stretching rate range of 0-150 mm / s.

[0086] According to some optional embodiments of the present disclosure, the polymer sample is a polymer film, such as a polyethylene (PE) film, a polypropylene (PP) film, a polyvinyl alcohol (PVA) film, and the like.

[0087] According to some embodiments of the present disclosure, the above-mentioned extensional rheometer suitable for polymer samples also includes a heating component, which is suitable for adjusting the temperature inside the high-pressure chamber 3, so that the torque sensor 12 obtains data on the variation of the tensile force generated by the sample during the stretching process with different pressure environments at a preset temperature inside the high-pressure chamber 3, and / or the torque sensor 12 obtains data on the variation of the tensile force generated by the sample during the stretching process with different temperature environments under a preset pressure inside the high-pressure chamber 3.

[0088] According to some embodiments of the present disclosure, by utilizing a heating assembly to adjust the temperature inside the high-pressure chamber 3, the torque sensor 12 can obtain data on how the tensile force generated by the sample during the stretching process varies with different pressure environments at a preset temperature inside the high-pressure chamber 3; the torque sensor 12 can also obtain data on how the tensile force generated by the sample during the stretching process varies with different temperature environments at a preset pressure inside the high-pressure chamber 3.

[0089] According to some embodiments of the present disclosure, the preset temperature is a target temperature required for the experiment, and the preset pressure is a target pressure required for the experiment.

[0090] According to some optional embodiments of the present disclosure, the temperature range of the internal environment of the high-pressure chamber 3 is 0℃-180℃, for example, the temperature of the internal environment of the high-pressure chamber 3 includes 0℃, 10℃, 20℃, 30℃, 40℃, 50℃, 60℃, 70℃, 80℃, 90℃, 100℃, 110℃, 120℃, 130℃, 140℃, 150℃, 160℃, 170℃, and 180℃; the pressure range that the high-pressure chamber 3 can withstand is 0Mpa-0.6Mpa, for example, the pressure that the high-pressure chamber 3 can withstand includes 0Mpa, 0.1Mpa, 0.2Mpa, 0.3Mpa, 0.4Mpa, 0.5Mpa, and 0.6Mpa.

[0091] According to some embodiments of the present disclosure, the above-mentioned extensional rheometer suitable for polymer samples also includes a gas generating component, which is suitable for inputting a target gas into the high-pressure chamber 3, and / or suitable for inputting a fluid medium into the high-pressure chamber 3, wherein the fluid medium forms steam under the action of the heating component to provide a gas atmosphere required for the experiment based on the target gas and the steam, so that the torque sensor 12 obtains data on the variation of the tensile force generated by the sample during the stretching process with different gas atmospheres at a preset temperature and / or preset pressure inside the high-pressure chamber 3.

[0092] According to some embodiments of the present disclosure, by using a gas generating assembly to input a target gas into the high pressure chamber 3, or by using a gas generating assembly to input a fluid medium into the high pressure chamber 3, the fluid medium forms steam under the action of a heating assembly, so that the gas atmosphere required for the experiment is provided based on the target gas and the steam. Therefore, the gas atmosphere required for the experiment in the high pressure chamber 3 can be achieved by inputting the target gas, or by inputting the fluid medium into the high pressure chamber 3 and then evaporating it into a steam atmosphere through heating.

[0093] According to some embodiments of the present disclosure, under the condition of constant temperature, that is, when the temperature is a preset temperature, the torque sensor 12 can obtain data on how the stretching force generated by the sample during the stretching process varies with different gas atmospheres; under the condition of constant pressure, that is, when the pressure is a preset pressure, the torque sensor 12 can obtain data on how the stretching force generated by the sample during the stretching process varies with different gas atmospheres.

[0094] It can be understood that the experimental environment in the high-pressure chamber 3 can be characterized by the pressure, temperature and gas atmosphere in the high-pressure chamber. According to actual needs, one or two of the pressure, temperature and gas atmosphere can be set as predetermined constant conditions, and the other two or one of the pressure, temperature and gas atmosphere can be set as variable conditions. Under the constant conditions, data on the change of the tensile force generated by the sample during the stretching process with the changing conditions can be obtained, thereby measuring the tensile properties of the sample from multiple dimensions.

[0095] According to some optional embodiments of the present disclosure, the gas atmosphere includes any one of air, nitrogen, and water vapor.

[0096] According to some optional embodiments of the present disclosure, when the preset temperature is 70°C and the preset pressure is 0.3Mpa, the torque sensor 12 can obtain data on how the stretching force generated by the sample during the stretching process varies with different gas atmospheres; when the preset pressure is 0.3Mpa and the gas atmosphere is air, the torque sensor 12 can obtain data on how the stretching force generated by the sample during the stretching process varies with different temperatures; when the gas atmosphere is air and the preset temperature is 70°C, the torque sensor 12 can obtain data on how the stretching force generated by the sample during the stretching process varies with different pressures.

[0097] According to some embodiments of the present disclosure, the extensional rheometer suitable for polymer samples further includes a pressure gauge 7 disposed above the high-pressure chamber 3 , and the pressure gauge 7 is suitable for monitoring the pressure change inside the high-pressure chamber 3 .

[0098] According to some embodiments of the present disclosure, by utilizing a pressure gauge 7 disposed above the high-pressure chamber 3 to monitor the pressure changes inside the high-pressure chamber 3, and by observing the pressure changes inside the high-pressure chamber 3 in real time, the flow rate of the target gas and the fluid medium input into the high-pressure chamber 3 can be adjusted in real time, thereby further adjusting the pressure inside the high-pressure chamber 3.

[0099] According to some embodiments of the present disclosure, a high-pressure chamber sealing plate 10 is provided on one side of the high-pressure chamber 3 and is sealed with a polyimide (PI) film, thereby enhancing the sealing of the interior of the high-pressure chamber 3 and allowing different types of detection beams such as X-rays or laser beams to pass through without interfering with the scattering signal, reflection signal or transmission signal generated by the polymer sample on the detection beam.

[0100] According to some optional embodiments of the present disclosure, the high-pressure chamber 3 is tightly connected to the high-pressure chamber sealing plate 10 by screws.

[0101] According to some embodiments of the present disclosure, the above-mentioned extensional rheometer suitable for polymer samples also includes a single film coupling 11, which is arranged between the torque sensor 12 and the stretching roller 5. The single film coupling 11 is suitable for transmitting the stretching force exerted on the sample to the torque sensor 12.

[0102] According to some embodiments of the present disclosure, a single film coupling 11 is disposed between the torque sensor 12 and the stretching roller 5 , and the stretching force applied to the sample is transmitted to the torque sensor 12 by the single film coupling 11 , so that the required mechanical experimental data can be obtained through the torque sensor 12 .

[0103] According to some embodiments of the present disclosure, the driving assembly 13 includes a servo motor 131 and a double film coupling 132. The servo motor 131 is suitable for providing driving force; the double film coupling 132 is connected to the torque sensor 12 and the servo motor 131, and the double film coupling 132 is suitable for transmitting the driving force to the stretching roller 5 to drive the stretching roller 5 to rotate.

[0104] According to some embodiments of the present disclosure, the extensional rheometer suitable for polymer samples further includes a pressure relief valve 15 , which is suitable for outputting target gas and / or steam to adjust the pressure inside the high-pressure chamber 3 .

[0105] According to some embodiments of the present disclosure, the pressure inside the high-pressure chamber 3 is adjusted by providing a pressure relief valve 15 to output the target gas and / or steam.

[0106] According to some embodiments of the present disclosure, the double film coupling 132 and the single film coupling 11 are capable of transmitting motion and torque, and compensating for the offset between the torque sensor 12 and the stretching roller 5 and between the torque sensor 12 and the servo motor 131 caused by misalignment during installation or other reasons, such as thermal expansion and contraction.

[0107] According to some embodiments of the present disclosure, the heating assembly includes a heating chamber body 2, a heating plate 4, a temperature sensor, and a controller. The heating chamber body 2 is disposed inside the high-pressure chamber 3; the heating plate 4 is disposed on the inner wall of the heating chamber body 2, and the heating plate 4 is adapted to generate heat to adjust the ambient temperature of the sample; the temperature sensor is adapted to monitor the temperature inside the heating chamber body 2; and the controller is adapted to adjust the temperature inside the heating chamber body 2 by controlling the voltage applied to the heating plate 4.

[0108] According to some embodiments of the present disclosure, two opposite side walls of the heating chamber body 2 are also provided with characterization windows 6, and the central axes of the multiple characterization windows 6 coincide. A heating chamber sealing plate 9 is installed on one side of the heating chamber body 2, and is sealed with a polyimide (PI) film, which enhances the sealing of the interior of the heating chamber, allows different types of detection beams such as X-rays or laser beams to pass through, and does not interfere with the scattering signal, reflection signal or transmission signal generated by the polymer sample on the detection beam.

[0109] According to some optional embodiments of the present disclosure, the heating chamber body 2 and the heating chamber sealing plate 9 are tightly connected by screws; other joints such as the rotating shaft are sealed by flanges or sealing rings.

[0110] Figure 2 The working principle diagram of an extensional rheometer suitable for polymer samples with a three-axis translation stage according to an embodiment of the present disclosure is schematically shown.

[0111] According to some embodiments of the present disclosure, Figure 2 As shown, the gas generating assembly includes a gas source 14 and an inlet valve 8, and the target gas is input into the high pressure chamber 3 through the gas source 14. The fluid medium is directly input into the heating chamber body 2 from the outside, and the controller is used to control the voltage applied to the heating plate 4 to adjust the temperature inside the heating chamber 2, further changing the fluid medium from liquid to gas to form steam, so as to provide the gas atmosphere required for the experiment.

[0112] According to some embodiments of the present disclosure, a three-axis translation stage 16 is used to movably support the extensional rheometer in three directions: X-axis, Y-axis and Z-axis.

[0113] According to some embodiments of the present disclosure, the three-axis translation stage 16 can provide a travel range of 100 mm in both the X-axis and the Y-axis, and a travel range of 25 mm in the Z-axis.

[0114] Figure 3 The working principle diagram of the microstructure detection device suitable for polymer samples according to an embodiment of the present disclosure is schematically shown.

[0115] According to the second aspect of the present disclosure, Figure 3 As shown, a microstructure detection device suitable for polymer samples is provided, comprising the above-mentioned extensional rheometer 23, an X-ray light source 18, a detection assembly and a three-axis translation stage 16. The X-ray light source 18 is suitable for providing initial X-rays, which are vertically incident on the sample surface from the characterization window 6; the detection assembly is suitable for obtaining a microstructure image of the sample by detecting the X-ray beam emitted from the sample surface; the three-axis translation stage 16 is configured to movably support the extensional rheometer 23 to adjust the position where the initial X-rays are incident on the sample surface.

[0116] According to some embodiments of the present disclosure, an extensional rheometer 23 is provided, and an X-ray light source 18 is used to provide initial X-rays, which are vertically incident on the sample surface from the characterization window 6; a detection component is used to detect the X-ray beam emitted from the sample surface to obtain a microstructure image of the sample; a three-axis translation stage 16 is used to movably support the extensional rheometer 23 to adjust the position where the initial X-rays are incident on the sample surface, and the above-mentioned microstructure detection device can detect the microstructure of the sample in situ using X-rays under different temperature, pressure and gas atmosphere conditions, and record mechanical data using the torque sensor 12. The mechanical data includes data on the variation of the tensile force generated by the sample during the stretching process with different pressure environments, data on the variation of the tensile force generated by the sample during the stretching process with different temperatures, and data on the variation of the tensile force generated by the sample during the stretching process with different atmospheric conditions.

[0117] According to some embodiments of the present disclosure, the detection assembly includes a conical vacuum tube 19, a first diffraction detector 20, and a second diffraction detector 21. The conical vacuum tube 19 is arranged to receive the first X-ray after the initial X-ray passes through the sample to obtain the second X-ray; the first diffraction detector 20 is arranged near one end of the cone of the conical vacuum tube 19, and the first diffraction detector 20 is suitable for imaging the first X-ray to obtain a microscopic structure image of the sample in a larger angle range; the second diffraction detector 21 is arranged near one end of the cylinder of the conical vacuum tube 19, and the second diffraction detector 21 is suitable for imaging the second X-ray to obtain a microscopic structure image of the sample in a smaller angle range.

[0118] According to some embodiments of the present disclosure, the signal received by the detection component is a scattered signal, a reflected signal or a transmitted signal generated by the sample to the initial X-ray.

[0119] According to some embodiments of the present disclosure, the above-mentioned microstructure detection device suitable for polymer samples also includes a computer, which is suitable for analyzing the microstructure images of multiple samples obtained by the detection component and multiple sets of mechanical data on the changes in the tensile force generated by the samples during the stretching process under different temperature, pressure and gas atmosphere conditions.

[0120] According to some optional embodiments of the present disclosure, the first diffraction detector 20 is a wide-angle diffraction detector capable of detecting a larger angle range, the larger angle range is 5°~80°, for example 5°, 10°, 15°, 20°, 25°, 35°, 55°, 65°, 75°, 80°; the second diffraction detector 21 is a small-angle diffraction detector capable of detecting a smaller angle range, the smaller angle range is 0°~5°, for example 0°, 1°, 2°, 3°, 4°, 5°.

[0121] According to some embodiments of the present disclosure, the three-axis translation stage 16 can conveniently and accurately adjust the position of the sample in the entire optical path, that is, the position where the initial X-ray is incident on the sample surface.

[0122] According to some embodiments of the present disclosure, before the experimental test, the three-axis translation stage 16 is used to adjust the X-ray optical path and the position of the extensional rheometer in the optical path to ensure that the detection component can receive clear imaging. After the above preparations are completed, the film sample is clamped at the stretching roller 5, and the heating chamber sealing plate 9 and the high-pressure chamber sealing plate 10 are fixed and tightened with screws to ensure the sealing of the high-pressure chamber 3 and the heating chamber body 2. Subsequently, according to the needs of the experiment, the corresponding gas atmosphere, preset temperature, preset pressure and heating time are set. The servo motor 131 can simultaneously drive the stretching roller 3 polymer sample in reverse to stretch. Before stretching, the X-ray light source 18 is started. When the stretching starts, the torque sensor 12 will also synchronously record the mechanical changes of the sample during the stretching process. During the stretching process of the polymer sample, the first diffraction detector 20 and the second diffraction detector 21 are synchronously used to perform wide-angle and small-angle diffraction detection respectively to obtain the microscopic structural evolution of the polymer sample.

[0123] Figure 4 The working principle diagram of the birefringence detection device suitable for polymer samples according to an embodiment of the present disclosure is schematically shown.

[0124] According to the third aspect of the present disclosure, Figure 4 As shown, a birefringence detection device suitable for polymer samples is provided, comprising the above-mentioned extensional rheometer 23, laser 17, optical path component 22, detector and three-axis translation stage 16. The laser 17 is suitable for providing an initial laser beam, which is vertically incident on the sample surface from the characterization window 6; the optical path component 22 is suitable for causing the first laser beam after the initial laser beam passes through the sample to undergo birefringence; the detector is suitable for obtaining the birefringence of the sample by detecting the first laser beam undergoing birefringence; the three-axis translation stage 16 is configured to movably support the extensional rheometer 23 to adjust the position where the initial laser beam is incident on the sample surface.

[0125] According to some embodiments of the present disclosure, an extensional rheometer 23 is provided, and an initial laser beam is provided by a laser 17, and the initial laser beam is vertically incident on the sample surface through a characterization window 6; an optical path component 22 is used to cause the first laser beam after the initial laser beam passes through the sample to undergo birefringence; a detector is used to obtain the birefringence of the sample by detecting the first laser beam that undergoes birefringence; and a three-axis translation stage 16 is used to movably support the extensional rheometer 23 to adjust the position at which the initial laser beam is incident on the sample surface. The initial laser beam can be used in situ to detect the birefringence of the sample under different temperature, pressure and gas atmosphere conditions, and a torque sensor 12 is used to record mechanical data, thereby obtaining data on the size and direction of the delay caused by stress when the polymer sample is stretched.

[0126] According to some embodiments of the present disclosure, by comparing the changes in the birefringence of the sample before and after stretching, the stress state of the sample and the magnitude and direction of the retardation caused thereby can be inferred.

[0127] According to some embodiments of the present disclosure, the signal received by the detector is a scattering signal, a reflection signal or a transmission signal generated by the sample to the initial laser beam.

[0128] According to some embodiments of the present disclosure, the three-axis translation stage 16 can conveniently and accurately adjust the position of the sample in the entire optical path, that is, the position where the initial laser beam is incident on the sample surface.

[0129] According to some embodiments of the present disclosure, the above-mentioned birefringence detection device for polymer samples also includes a computer, which is suitable for analyzing the birefringence of the sample obtained by the detector and the data on the size and direction of the delay caused by stress when the sample is stretched.

[0130] It will be appreciated by those skilled in the art that the features described in the various embodiments and / or claims of the present disclosure may be combined and / or combined in a variety of ways, even if such combinations and / or combinations are not explicitly described in the present disclosure. In particular, the features described in the various embodiments and / or claims of the present disclosure may be combined and / or combined in a variety of ways without departing from the spirit and teachings of the present disclosure. All of these combinations and / or combinations fall within the scope of the present disclosure.

[0131] The embodiments of the present disclosure are described above. However, these embodiments are only for illustrative purposes and are not intended to limit the scope of the present disclosure. Although the embodiments are described above separately, this does not mean that the measures in the various embodiments cannot be used in combination to advantage. The scope of the present disclosure is defined by the attached claims and their equivalents. Without departing from the scope of the present disclosure, those skilled in the art may make a variety of substitutions and modifications, which should all fall within the scope of the present disclosure.

Claims

1. An extensional rheometer suitable for polymer samples, comprising: Pedestal; A high pressure chamber is installed on the base, and the high pressure chamber is suitable for providing different pressure environments; Two stretching rollers are arranged in parallel and at intervals inside the high-pressure chamber, and two ends of the sample are connected to the two stretching rollers; A driving assembly, adapted to drive the stretching roller to rotate so as to stretch the sample; Two characterization windows are respectively arranged on two opposite side walls of the high-pressure chamber, and the characterization windows are adapted to allow a detection light beam generated by an external detection light source to pass through so as to obtain information on changes in the microstructure of the sample during the stretching process; as well as The torque sensor is installed between the stretching roller and the driving assembly, and is suitable for obtaining data on the variation of the stretching force generated by the sample during the stretching process with different pressure environments.

2. The extensional rheometer for polymer samples according to claim 1, further comprising a heating assembly adapted to adjust the temperature inside the high pressure chamber so that: The torque sensor obtains data on the variation of the tensile force generated by the sample during the stretching process under a preset temperature inside the high-pressure chamber with different pressure environments, and / or The torque sensor obtains data on the variation of the tensile force generated by the sample during the stretching process under a preset pressure inside the high-pressure chamber with different temperature environments.

3. The extensional rheometer suitable for polymer samples according to claim 2, further comprising: A gas generating assembly is adapted to input a target gas into the interior of the high pressure chamber, and / or adapted to input a fluid medium into the interior of the high pressure chamber, In which, the fluid medium forms steam under the action of the heating component to provide the gas atmosphere required for the experiment based on the target gas and the steam, so that the torque sensor can obtain data on the variation of the stretching force generated by the sample during the stretching process with different gas atmospheres at a preset temperature and / or preset pressure inside the high-pressure chamber.

4. The extensional rheometer suitable for polymer samples according to claim 3, further comprising: A pressure gauge is disposed above the high-pressure chamber, and the pressure gauge is suitable for monitoring pressure changes inside the high-pressure chamber.

5. The extensional rheometer suitable for polymer samples according to claim 1 further includes a single film coupling, which is arranged between the torque sensor and the stretching roller, and the single film coupling is suitable for transmitting the stretching force applied to the sample to the torque sensor.

6. The extensional rheometer suitable for polymer samples according to claim 1, wherein: The drive assembly comprises: A servo motor, suitable for providing a driving force; and A double film coupling is connected to the torque sensor and the servo motor, and is suitable for transmitting the driving force to the stretching roller to drive the stretching roller to rotate.

7. The extensional rheometer suitable for polymer samples according to claim 3 further comprises a pressure relief valve suitable for outputting the target gas and / or the steam to adjust the pressure inside the high-pressure chamber.

8. The extensional rheometer suitable for polymer samples according to claim 2, wherein: The heating assembly comprises: A heating chamber body is arranged inside the high-pressure chamber; A heating plate is arranged on the inner wall of the heating chamber, and the heating plate is suitable for generating heat to adjust the ambient temperature of the sample; A temperature sensor, adapted to monitor the temperature inside the heating chamber; and The controller is adapted to adjust the temperature inside the heating chamber by controlling the voltage applied to the heating plate.

9. A microstructure detection device suitable for polymer samples, comprising: The extensional rheometer as claimed in claims 1 to 8; An X-ray light source, adapted to provide initial X-rays, wherein the initial X-rays are incident vertically from the characterization window to the sample surface; A detection assembly, adapted to obtain a microstructure image of the sample by detecting an X-ray beam emitted from a surface of the sample; as well as The three-axis translation stage is configured to movably support the extensional rheometer so as to adjust the position where the initial X-ray is incident on the sample surface.

10. A birefringence detection device suitable for polymer samples, comprising: The extensional rheometer as claimed in claims 1 to 8; A laser, adapted to provide an initial laser beam, wherein the initial laser beam is incident vertically from the characterization window to the sample surface; An optical path component, adapted to cause the first laser beam after the initial laser beam passes through the sample to undergo birefringence; A detector, adapted to obtain the birefringence index of the sample by detecting the first laser beam that undergoes birefringence; as well as The three-axis translation stage is configured to movably support the extensional rheometer so as to adjust the position where the initial laser beam is incident on the sample surface.

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