In-situ variable-temperature tensile device and testing method for grazing-incidence X-ray scattering characterization

Abstract

This application relates to the field of thin film testing technology, and discloses an in-situ variable temperature tensile device and a testing method for grazing incidence X-ray scattering characterization. The device includes a power assembly, a base, a slide rail, a support assembly, and a heating assembly. The slide rail is arranged at the upper end of the base; the support assembly includes a first platform support and a second platform support. A first pressing piece is arranged at the upper end of the first platform support, and a second pressing piece and a tensile sensor are arranged at the upper end of the second platform support. Both the first platform support and the second platform support are movably arranged on the slide rail. The first pressing piece cooperates with the second pressing piece to fix the thin film sample. The first platform support and the second platform support are connected to the power assembly; the heating assembly is arranged on the base and is located between the first platform support and the second platform support. This application provides valuable information for the in-situ structural evolution of various functional thin films under tensile conditions, and can also characterize the temperature dependence of the molecular packing structure of functional thin films under uniaxial tension.

Description

Technical Field

[0001] This application relates to the technical field of thin film testing, and particularly relates to an in-situ variable temperature tensile device and a testing method for grazing incidence X-ray scattering characterization. Background Art

[0002] Synchrotron radiation light source is a light source with high energy, high brightness and high stability, providing advanced research means for various experimental technologies. Among them, grazing incidence X-ray scattering (GIXS) testing technology, as a non-destructive and surface-sensitive characterization means, has gradually become a hot topic in the field of materials science. The GIXS testing technology obtains the surface structure and order information of substances by measuring the reflection degree of X-rays on the surface of substances. The application of synchrotron radiation GIXS testing technology in materials science is extensive, and the research on the surface structure and order of thin film materials is a very important part of it. The GIXS testing technology can non-destructively characterize the surface structure, lattice vibration, order, etc. of various thin film materials (such as metal thin films, semiconductor thin films, organic thin films, etc.).

[0003] Taking semiconductor thin films as an example, semiconductor polymers usually exhibit stretchability due to their intrinsic flexibility, and combined with the advantages of solution processability, they are widely used in the fields of flexible electronics, wearable devices, etc. In the national subversive innovation field, flexible electronic technology ranks first. In order to optimize the mechanical and optoelectronic properties of semiconductor polymer thin films, it is crucial to comprehensively understand the structural changes that occur in these thin films under tensile conditions. Tensile or mechanical deformation can significantly affect the molecular packing, chain orientation and crystallinity of semiconductor polymer thin films. These structural changes also affect the charge transport behavior, exciton diffusion and overall device performance in electronic devices. By studying the structural evolution of semiconductor polymer thin films in a stress field, the mechanism of these structural modifications and their effects on electrical properties can be deeply understood. Understanding the relationship between the structural changes caused by tensile stress and the resulting optoelectronic properties can optimize device performance, including charge carrier mobility, charge injection and device stability, and contribute to the construction of high-performance stretchable and flexible electronic devices.

[0004] The Grazing-incidence X-ray scattering (GIXS) characterization method is the most powerful tool for studying the structural changes of semiconductor polymers under tensile conditions. Prior art has studied the in-situ wide-angle and small-angle X-ray scattering of 50-μm-thick poly(3-dodecylthiophene) films during tensile deformation and performed off-situ scattering pole figure analysis on the deformed polymer films. Although this study provided new insights into the deformation mechanism of semiconductor polymers, these films are much thicker than the polymer optoelectronic films used in stretchable electronics, which typically have a thickness of 100 nm or less. With the increasing interest in stretchable organic electronics, there is a growing need to understand the structural characteristics of ultrathin polymer films under tensile conditions. However, due to the complexity of sample preparation and the lack of ready-made free-standing films, off-situ methods are generally used to study the mechanical behavior of these films. Off-situ methods involve separately preparing polymer films and subjecting them to controlled tensile conditions outside the experimental setup. This method can characterize the structural changes in the films after stretching. Although off-situ methods provide valuable insights into the structural changes in the films, they cannot capture the real-time behavior and dynamic processes that occur during stretching.

[0005] As the field continues to develop, efforts are being made to overcome the challenges posed by off-situ methods and shift towards in-situ or real-time characterization techniques. These methods aim to provide a more comprehensive understanding of the behavior of ultrathin polymer films under tensile conditions. For example, in prior art, hard and soft X-ray scattering techniques have been used to explore the strain-induced structural changes in semiconductor polymer films, and in-situ transmission X-ray scattering of ternary organic photovoltaic blends has been utilized. In subsequent studies, a series of elastomer-containing ternary blend systems have been thoroughly investigated by transmission X-ray scattering methods. However, this method can only provide structural information in the in-plane direction.

[0006] Advances in GIXS technology at synchrotron radiation facilities play a crucial role in promoting the understanding of semiconductor polymers. In particular, GIXS has been widely used to characterize polymer films in intrinsically stretchable organic photovoltaic cells. However, there is still a lack of real-time detection of the microstructural changes in ultrathin polymer films during stretching, and there is an urgent need to develop new devices and characterization methods for in-situ characterizing the structural evolution of stretched films.

[0007] Application Content

[0008] The purpose of this application is to provide an in-situ variable-temperature tensile device and testing method for grazing-incidence X-ray scattering characterization, which can provide valuable information on the in-situ structural evolution of various functional films under tensile conditions and can also characterize the temperature dependence of the molecular packing structure of functional films under uniaxial stretching.

[0009] To achieve the above objective, the technical solution adopted in this application is as follows:

[0010] In a first aspect of the present application, there is provided an in-situ variable-temperature tensile device for grazing-incidence X-ray scattering characterization, comprising: a power assembly; a base; a slide rail disposed at the upper end of the base; a support assembly including a first platform support, a second platform support, a first pressing piece, a second pressing piece and a tensile sensor, wherein the first pressing piece is disposed at the upper end of the first platform support, the second pressing piece and the tensile sensor are disposed at the upper end of the second platform support, the first platform support and the second platform support are both movably disposed on the slide rail, the first pressing piece cooperates with the second pressing piece to fix a thin film sample, the first platform support and the second platform support are connected to the power assembly, and under the action of the power assembly, the first platform support and the second platform support move towards or away from each other along the slide rail; a heating assembly disposed on the base and located between the first platform support and the second platform support.

[0011] Further, the power assembly includes a motor and a lead screw, an output end of the motor is connected to one end of the lead screw, the other end of the lead screw is rotatably disposed on an end support, the end support is disposed on the base, and the first platform support and the second platform support are connected to the lead screw.

[0012] Further, it further includes a rotating platform, the power assembly is installed on one side of the base, and the base is installed on the upper end of the rotating platform to rotate under the action of the rotating platform.

[0013] Further, the thin film sample includes a substrate and a functional thin film deposited on the substrate, and the substrate is an elastomer thin film.

[0014] Further, the elastomer thin film includes, but is not limited to, one of polysiloxane-based elastomers, thermoplastic polyurethane elastomers, styrene-based thermoplastic elastomers, polyolefin-based thermoplastic elastomers, polyamide-based thermoplastic elastomers.

[0015] Further, the functional thin film includes, but is not limited to, one of conjugated polymer thin films, polyolefin polymer thin films, elastomer thin films, ductile metal thin films.

[0016] In a second aspect of the present application, there is provided an in-situ variable-temperature tensile method for grazing-incidence X-ray scattering characterization, based on the in-situ variable-temperature tensile device for grazing-incidence X-ray scattering characterization provided in the first aspect of the present application. The detection method includes: using an elastomer thin film as a substrate, depositing a functional thin film on the substrate to obtain a thin film sample; fixing the thin film sample on the upper end of the support assembly; irradiating the thin film sample with X-rays, setting the tensile strain and temperature, and obtaining in-situ information on the structural evolution of the thin film under different stress fields and / or different temperature fields.

[0017] Further, a thin film sample is prepared by the following method: the silicon wafer is ultrasonically cleaned and soaked in isopropyl alcohol, distilled water, acetone, and isopropyl alcohol in sequence; the soaked silicon wafer is subjected to ultraviolet ozone modification; octadecyltrichlorosilane (OTS) and toluene are mixed to form an OTS-toluene solution, and the modified silicon wafer is covered with the OTS-toluene solution, followed by cleaning and annealing to obtain an OTS-modified silicon substrate; the elastomer particles are dissolved in toluene to form an elastomer solution; the elastomer solution is poured onto the OTS-modified silicon substrate to form a film, and dried to obtain an elastomer substrate; a functional film is deposited on the elastomer substrate to obtain a thin film sample. Further, the thin film sample is irradiated with X-rays, and the tensile strain and temperature are set to obtain in-situ information on the structural evolution of the thin film under different stress fields and / or different temperature fields, including: setting the tensile strain at 0%, 5%, 10%, 20%, 30%, 40%, 50%, 80%, and 100%, and rotating the base 90° each time the tensile strain is adjusted. At each tensile strain, the X-ray is controlled to irradiate the thin film sample with set parameters to obtain in-situ information on the structural evolution of the thin film under different stress fields; under the condition of a fixed tensile strain, the temperature is varied between 40°C, 50°C, 60°C, 70°C, 80°C, and 90°C, and the base is rotated 90° each time the temperature is adjusted. At each temperature, the X-ray is controlled to irradiate the thin film sample with set parameters to obtain in-situ information on the structural evolution of the thin film under different temperature fields at the set stress field.

[0018] Further, the set parameters are: an exposure time of 1 to 600 seconds.

[0019] The beneficial effects of this application are:

[0020] Using an elastomer thin film as the substrate, depositing a functional film on the substrate, fixing it on the fixture of a uniaxial tensile device, and setting a certain tensile rate / strain and temperature, in-situ information on the structural evolution of the thin film under stress and temperature fields can be obtained, thereby providing valuable information for the in-situ structural evolution of various functional films under tensile conditions, and the temperature dependence of the molecular packing structure of the functional film under uniaxial tension can be characterized. Description of the Drawings

[0021] Figure 1 Shows a structural diagram of an in-situ variable temperature tensile device for grazing incidence X-ray scattering characterization according to an embodiment of the present application.

[0022] Figure 2 Shows a perspective view of the base in an in-situ variable temperature tensile device for grazing incidence X-ray scattering characterization according to an embodiment of the present application.

[0023] Figure 3 Shows schematic diagrams of the displacement-time graph, stress-time graph, and stress-displacement graph during the detection process according to an embodiment of the present application.

[0024] Figure 4 Shows a flowchart of an in-situ variable-temperature tensile method for grazing-incidence X-ray scattering characterization according to an embodiment of the present application.

[0025] Figure 5 Shows a flowchart of the preparation of an elastic substrate according to an embodiment of the present application.

[0026] Figure 6 Shows one-dimensional curves and two-dimensional images of in-plane / out-of-plane information of the N2200 sample varying with tensile strain in two incident directions according to an embodiment of the present application.

[0027] Figure 7 Shows one-dimensional curves and two-dimensional images of in-plane / out-of-plane information of (010)-oriented N2200 varying with temperature when the incident light is parallel to the tensile direction at different temperatures according to an embodiment of the present application.

[0028] Figure 8 Shows two-dimensional GIWAXS images and one-dimensional curves of an elastic substrate according to an embodiment of the present application.

[0029] In the figure, 1 is a power assembly, 11 is a motor, 12 is a lead screw, 2 is a base, 3 is a slide rail, 4 is a support assembly, 41 is a first platform support, 42 is a second platform support, 43 is a first pressing piece, 44 is a second pressing piece, 45 is a second pressing piece, 5 is a heating assembly, 6 is an end support, 7 is a transmission box body, 71 is an input port, and 72 is an output port. Specific Embodiments

[0030] The following uses specific specific examples to illustrate the embodiments of the present application. Those skilled in the art can easily understand other advantages and effects of the present application from the content disclosed in this specification. The present application can also be implemented or applied through other different specific embodiments, and various details in this specification can also be modified or changed based on different viewpoints and applications without departing from the spirit of the present application. It should be noted that, without conflict, the following embodiments and the features in the embodiments can be combined with each other.

[0031] The following further describes in detail the specific embodiments of the present application in conjunction with the drawings and embodiments.

[0032] Figure 1 Shows a structural diagram of an in-situ variable-temperature tensile device for grazing-incidence X-ray scattering characterization according to an embodiment of the present application. An embodiment of the present application provides an in-situ variable-temperature tensile device for grazing-incidence X-ray scattering characterization, as Figure 1As shown in the figure, the device includes: a power component 1, a base 2, a slide rail 3, a support component 4, and a heating component 5. The slide rail 3 is arranged at the upper end of the base; the support component 4 includes a first platform support 41, a second platform support 42, a first pressing piece 43, a second pressing piece 44, and a tensile force sensor 45. The first pressing piece 43 is arranged at the upper end of the first platform support 41, and the second pressing piece 43 and the tensile force sensor 44 are arranged at the upper end of the second platform support 42. Both the first platform support 41 and the second platform support 42 are movably arranged on the slide rail 3. The first pressing piece 43 and the second pressing piece 44 cooperate to fix the thin film sample. The first platform support 41 and the second platform support 42 are connected to the power component 1. Under the action of the power component 1, the first platform support 41 and the second platform support 42 move towards or away from each other along the slide rail 3; the heating component 5 is arranged on the base 2 and is located between the first platform support 41 and the second platform support 42.

[0033] In this embodiment, the first pressing piece 43 and the second pressing piece 44 form a fixture for fixing the thin film sample. After the thin film sample is fixed, it is irradiated with X-rays. By controlling the power component 1, the stretching state of the thin film sample can be adjusted. The tensile force sensor 45 can detect the tensile stress of the thin film sample, and then determine its tensile strain, so that the thin film sample can be controlled in the set tensile strain state. Through the detector, the scattering data of the thin film sample can be obtained, and then the in-situ information of the thin film structure evolution under different stress fields can be obtained. The heating component 5 is used to control the temperature environment of the thin film sample. Under the set stress field, by changing the temperature environment of the thin film sample through the heating component 5, irradiating the thin film sample with X-rays, and based on the scattering data of the thin film sample collected by the detector, the in-situ information of the thin film structure evolution under different temperature fields can be obtained. Among them, the heating component 5 can include an electric heating element and a temperature controller. Since the temperature field of the thin film sample is higher than the normal room temperature environment, only heating is required. The electric heating element is used for heating, and a temperature probe is configured in the temperature controller. The current temperature value is collected by the temperature probe. If the current temperature value reaches the set temperature value, the temperature controller controls the electric heating element to stop heating. In this way, the temperature can be controlled within the set temperature range through the heating component 5.

[0034] In some embodiments, as Figure 1 shown, the power component 1 includes a motor 11 and a lead screw 12. The output end of the motor 11 is connected to one end of the lead screw 12. The other end of the lead screw 12 is rotatably arranged on an end support 6. The end support 6 is arranged on the base 2. The first platform support 41 and the second platform support 42 are connected to the lead screw 12.

[0035] In this embodiment, the motor 11 operates and rotates to cause the lead screw 12 to rotate, thereby causing the first platform support 41 and the second platform support 42 connected to the lead screw 12 to move towards or away from each other. By controlling the operating parameters of the motor 11, such as speed, torque, etc., the rate at which the first platform support 41 and the second platform support 42 move towards or away from each other can be controlled, thereby achieving control of the stretching rate of the thin film sample. Among them, two lead screws 12 can be provided to ensure the stability of driving.

[0036] Exemplarily, as Figure 2 shown, a transmission box body 7 is provided on one side of the base 2. The motor 11 is installed on the outside of the transmission box body 7. The motor 11 is also connected to a reducer. The reducer is arranged in the transmission box body 7. The transmission box body 7 has an input port 71 and two output ports 72. The input port 71 is used for connecting the output shaft of the motor 11 to the reducer. The two output ports 72 are matched with a reducer with double output shafts, so that the double output shafts of the reducer are respectively connected to a lead screw 12.

[0037] In some embodiments, the device further includes a rotating platform. The power assembly 1 is installed on one side of the base 2, and the base 2 is installed on the upper end of the rotating platform to rotate under the action of the rotating platform.

[0038] The function of the rotating platform is to control the rotation of the base 2. For example, the rotating platform can be a rotating motor installed on a bottom platform. The output end of the rotating motor is connected to the base 2. Under the drive of the rotating motor, the base 2 rotates, thereby adjusting the angle of the thin film sample fixed on the base 2 by the fixture, so that under X-ray irradiation, measurements can be respectively carried out perpendicular and parallel to the stretching direction.

[0039] In some embodiments, the thin film sample includes a substrate and a functional thin film deposited on the substrate, and the substrate is an elastomeric film. The deposition methods of the functional thin film include, but are not limited to, spin coating, drop coating, blade coating, and vacuum evaporation.

[0040] In some embodiments, the thickness of the substrate is 1 μm to 5 mm, and the thickness of the functional thin film is 10 nm to 10 μm.

[0041] In some embodiments, the elastomeric film includes one of polysiloxane-based elastomers, thermoplastic polyurethane elastomers, styrene-based thermoplastic elastomers, polyolefin-based thermoplastic elastomers, and polyamide-based thermoplastic elastomers.

[0042] In some embodiments, the functional thin film includes one of conjugated polymer thin films, polyolefin polymer thin films, elastomeric thin films, and ductile metal thin films.

[0043] Exemplarily, the conjugated polymer materials used in the conjugated polymer film include, but are not limited to, any one or a blend solution of multiple ones among PDPPTPT, PTQ1, PTB7, PDPP3T, PM6, PM7, PTB7-Th, PTVT-T, PBDB-T, PFBCPZ, TIPS-TPD, PDTP-DPP, PBDTTPD-HT, asy-ranPBTBDT, PBnDT-FTAZ, J71, PTzBi-Si, D18, D18-CI, PDPPSDTPS, PDPP5T, CC1C10-PPV, PCDTBT, PBQx-TC1, PCPDTBT, Si-PCPDTBT, PBT(TH), PBD(EDOT), PBD(TH), PDCBT, PDTPBT, P4T2F-HD, PDCBT-CI, PTQ10, P3HT, PD2FCT-29DPP, P4T2F-HD, PffBT4T-2OD, PNDI-5DD, PNDI-POD, N22O0, IDTBT, PTQ-10, SEBS, PDMS, PS. The molecular structural formula is as follows:

[0044]

[0045]

[0046] The device provided in this embodiment can collect the microscopic structural changes that occur in the functional film under tensile conditions. Through the power assembly 1, the polymer film can be accurately uniaxially stretched, with a strain range from 0% to 1000% and a strain rate range from 0.01 mm / min to 1000 mm / min. To ensure controllable tensile conditions, a load cell and a strain gauge sensor can also be integrated into the device to collect the weight and strain data of the film sample. These sensors help to accurately measure and control the applied strain during the experiment. A heating assembly 5 is installed on the base 2, which can heat the film sample to 300 °C. Importantly, through the rotating platform under the base 2, it can be well interfaced with the beamline 1W1A of BSRF and the beamline 02U2 of SSRF. The stretching device can be rotated to measure the structural differences in two directions parallel and perpendicular to the stretching direction.

[0047] When conducting a tensile test using this device, based on the set sensors and the control of the power assembly 1, some important information can be recorded, such as Figure 3 As shown, the displacement-time graph, stress-time graph, and stress-displacement graph can be recorded during the measurement.

[0048] Therefore, through the device provided in this embodiment, valuable insights into the microstructural changes occurring within the semiconductor polymer thin film under various stretching conditions can be obtained, while the temperature dependence of the molecular packing structure of many functional thin films under uniaxial stretching can be characterized.

[0049] Based on the in-situ variable-temperature stretching device for grazing-incidence X-ray scattering characterization provided in the above embodiments, an embodiment of the present application provides an in-situ variable-temperature stretching method for grazing-incidence X-ray scattering characterization. As Figure 4 shown, this method includes the following steps:

[0050] S1. Using an elastomer thin film as a substrate, deposit a functional thin film on the substrate to obtain a thin film sample.

[0051] In a specific embodiment, the preparation process of the thin film sample is as Figure 5 shown. Before the stretching experiment, prepare the thin film sample on the stretchable substrate according to the following steps:

[0052] First, ultrasonically clean a silicon wafer with dimensions of 10 cm × 10 cm, and continuously soak it in different solvents. As Figure 3 shown, the silicon wafer is successively soaked in isopropyl alcohol, distilled water, acetone, and isopropyl alcohol for 15 minutes. After the cleaning process is completed, the silicon wafer is subjected to ultraviolet ozone modification for 15 minutes. Mix 10 μL of octadecyltrichlorosilane (OTS) with 5 mL of toluene to form a homogeneous mixture. Then pour the OTS-toluene solution into a petri dish and cover the silicon wafer. After the treatment, rinse the silicon wafer with toluene to remove the excess OTS-toluene solution. To stabilize and promote the proper adhesion of the OTS layer, the silicon wafer is annealed on a hot plate at 120 °C for 60 minutes. At the same time, dissolve SEBS particles in toluene to form a homogeneous solution with a concentration of 100 mg / mL. Pour the SEBS solution onto the OTS-modified silicon substrate to form a film, and dry it at room temperature to obtain a SEBS substrate. First, fix the SEBS substrate with a thickness of 0.2 - 0.5 mm on the stretching device, and irradiate the surface of the substrate with X-rays to obtain the diffraction information of the elastomer substrate, as Figure 8 shown.

[0053] Subsequently, cut the SEBS substrate into sample strips with dimensions of 1 cm × 5 cm and paste them onto the glass. Finally, deposit the functional thin film on the SEBS substrate.

[0054] S2. Fix the thin film sample at the upper end of the support assembly.

[0055] S3. Irradiate the thin film sample with X-rays, set the tensile strain and temperature, and obtain the in-situ information on the structural evolution of the thin film under different stress fields and / or different temperature fields.

[0056] The X-ray scattering experiment was mainly carried out on the 1W1A beamline of BSRF. In the tensile experiment, a customized sample stage was used to fix the sample. An X-ray beam with a specific wavelength penetrated the sample, and a 1MEIGER2 X detector was used to collect scattering data simultaneously. The sample-to-detector distance (SDD) was set to a specific value (86.6 mm), and LaB6 was used for SDD calibration. By collecting the scattered X-ray information with a two-dimensional detector, a detailed scattering pattern could be obtained. The height of the central heating copper block was adjusted to be slightly higher than the fixture. The speed was set to 10 mm / min. The distance and height between the sample stage and the detector were adjusted to appropriate values to ensure optimal measurement and data collection.

[0057] The tensile strains of the specimens were 0%, 5%, 10%, 20%, 30%, 40%, 50%, 80%, and 100% respectively. At each strain, the incident angle was 0.2°, and the exposure time was 5 s. Each time the strain was adjusted, the device turntable rotated 90°, and measurements were taken perpendicular and parallel to the tensile direction respectively. For temperature-related measurements, the tensile strain was fixed at 40%. The hot stage temperature varied between 40 °C, 50 °C, 60 °C, 70 °C, 80 °C, and 90 °C. The incident angle was maintained at 0.2°, and the exposure time was 5 s. Each time the temperature was measured, the workbench rotated 90°. Following these steps, in-situ GIXS measurements were carried out using a new tensile device and software to obtain the structural changes of polymer films at different strain levels and temperatures.

[0058] Based on the method steps described above, the following embodiments of this application will further demonstrate the feasibility and progressiveness of this application in combination with specific experiments.

[0059] Example 1:

[0060] The prepared SEBS flexible substrate with a thickness of about 0.2 mm was cut into a size of 1 cm × 5 cm and pasted on a glass substrate of the corresponding size. The scattering information is as Figure 8 shown; a certain mass of N2200 was weighed and added to chloroform to prepare chloroform solutions with concentrations of 15 mg / mL respectively. The solutions were placed on a hot stage at 40 °C and stirred overnight to dissolve into a homogeneous solution. The dissolved N2200 solution was spin-coated on the surface. After film formation, it was annealed on a hot stage at 100 °C for 10 min; the sample was clamped on the fixture, the tensile speed was set to 10 mm / min, and the tensile strains were set to 0%, 5%, 10%, 20%, 30%, 40%, 50%, 80%, and 100% respectively. At each strain, the incident angle was 0.2°, and the exposure time was 5 s. Each time the strain was adjusted, the device turntable rotated 90°, and measurements were taken perpendicular and parallel to the tensile direction respectively. Figure 6 The one-dimensional curves and two-dimensional images of the in-plane and out-of-plane information of the N2200 sample as a function of tensile strain in two incident directions.

[0061] Example 2:

[0062] The prepared SEPS flexible substrate with a thickness of about 0.2 mm was cut into a size of 1 cm × 5 cm and pasted on a glass substrate of corresponding size; a certain mass of N2200 was weighed and added to chloroform to prepare chloroform solutions with concentrations of 15 mg / mL respectively, and they were placed on a hot stage at 40 °C and stirred overnight to dissolve into a homogeneous solution. The dissolved N2200 solution was spin-coated on the surface, and after film formation, it was annealed on a hot stage at 100 °C for 10 min; the sample was clamped on a fixture, the tensile strain was set to 40%, and the hot stage temperatures were set to 40 °C, 50 °C, 60 °C, 70 °C, 80 °C, and 90 °C respectively. At each temperature, the incident angle was 0.2°, and the exposure time was 5 s. Figure 7 They are the one-dimensional curves and two-dimensional images of the in-plane and out-of-plane information of the N2200 sample varying with the tensile strain when the incident light is parallel to the tensile direction; the coherence length, the variation trend of the g parameter, the pole figure of the (010) diffraction peak, and the variation trend of rDoC of N2200 in the (010) direction.

[0063] Example 3:

[0064] The prepared SEPS flexible substrate with a thickness of about 0.2 mm was cut into a size of 1 cm × 5 cm and clamped on a fixture. The tensile speed was set to 10 mm / min, and the tensile strains were set to 0%, 5%, 10%, 20%, 30%, 40%, 50%, 80%, and 100% respectively. At each strain, the incident angle was 0.2°, and the exposure time was 5 s. Each time the strain was adjusted, the turntable of the device rotated 90°, and measurements were carried out perpendicular and parallel to the tensile direction respectively.

[0065] Example 4:

[0066] The prepared SEBS flexible substrate with a thickness of about 0.2 mm was cut into a size of 1 cm × 5 cm and clamped on a fixture. The tensile strain was set to 40%, and the hot stage temperatures were set to 40 °C, 50 °C, 60 °C, 70 °C, 80 °C, and 90 °C respectively. At each temperature, the incident angle was 0.2°, and the exposure time was 5 s.

[0067] Example 5:

[0068] The prepared SEBS flexible substrate with a thickness of about 0.2 mm was cut into a size of 1 cm × 5 cm and pasted on a glass substrate of corresponding size. The scattering information is as Figure 8As shown; Weigh a certain mass of P3HT, add chloroform, and prepare chloroform solutions with concentrations of 15 mg / mL respectively. Place them on a hot plate at 40 °C and stir overnight to dissolve into a homogeneous solution. Spin-coat the dissolved P3HT solution on the surface, and after film formation, place it on a hot plate at 100 °C for annealing for 10 min; Clamp the sample on the fixture, set the stretching speed to 10 mm / min, and set the stretching strains to 0%, 5%, 10%, 20%, 30%, 40%, 50%, 80%, and 100% respectively. At each strain, the incident angle is 0.2°, and the exposure time is 5 seconds. Each time the strain is adjusted, the turntable of the device rotates 90°, and measurements are taken perpendicular and parallel to the stretching direction respectively.

[0069] Example 6:

[0070] Cut the prepared SEPS flexible substrate with a thickness of about 0.2 mm into a size of 1 cm × 5 cm, and paste it on a glass substrate of the corresponding size; Weigh a certain mass of P3HT, add chloroform, and prepare chloroform solutions with concentrations of 15 mg / mL respectively. Place them on a hot plate at 40 °C and stir overnight to dissolve into a homogeneous solution. Spin-coat the dissolved P3HT solution on the surface, and after film formation, place it on a hot plate at 100 °C for annealing for 10 min; Clamp the sample on the fixture, set the stretching strain to 40%, and set the hot plate temperatures to 40 °C, 50 °C, 60 °C, 70 °C, 80 °C, and 90 °C respectively. At each temperature, the incident angle is 0.2°, and the exposure time is 5 seconds.

[0071] The above embodiments are only used to illustrate the present application, rather than limiting the present application. Those of ordinary skill in the relevant technical field can also make various changes and modifications without departing from the spirit and scope of the present application. Therefore, all equivalent technical solutions also belong to the scope of the present application. The patent protection scope of the present application shall be defined by the claims.

Claims

1. An in-situ variable-temperature tensile method for grazing-incidence X-ray scattering characterization, characterized in that An in-situ variable-temperature tensile device for grazing-incidence X-ray scattering characterization, comprising: A power component; A base; A slide rail, which is arranged at the upper end of the base; A support component, including a first platform support, a second platform support, a first pressing piece, a second pressing piece and a tensile sensor. The first pressing piece is arranged at the upper end of the first platform support, the second pressing piece and the tensile sensor are arranged at the upper end of the second platform support. Both the first platform support and the second platform support are movably arranged on the slide rail. The first pressing piece cooperates with the second pressing piece to fix the thin film sample. The first platform support and the second platform support are connected to the power component. Under the action of the power component, the first platform support and the second platform support move towards or away from each other along the slide rail; the thin film sample includes a substrate and a functional thin film deposited on the substrate, and the substrate is an elastomeric thin film; A heating component, which is arranged on the base and located between the first platform support and the second platform support; The method includes: Using an elastomeric thin film as a substrate, depositing a functional thin film on the substrate to obtain a thin film sample; Fixing the thin film sample at the upper end of the support component; Irradiating the thin film sample with X-rays, setting the tensile strain and temperature, to obtain in-situ information on the structural evolution of the thin film under different stress fields and / or different temperature fields; Irradiating the thin film sample with X-rays, setting the tensile strain and temperature, to obtain in-situ information on the structural evolution of the thin film under different stress fields and / or different temperature fields, including: Making the tensile strain be 0%, 5%, 10%, 20%, 30%, 40%, 50%, 80% and 100% respectively. Each time the tensile strain is adjusted, the base rotates 90°, to obtain the stacking structure difference in two X-ray incident directions perpendicular and parallel to the tensile direction; at each tensile strain, controlling the X-ray to irradiate the thin film sample with set parameters, to obtain in-situ information on the structural evolution of the thin film under different stress fields; Under the condition of a fixed tensile strain, making the temperature vary between 40°C, 50°C, 60°C, 70°C, 80°C and 90°C. Each time the temperature is adjusted, the base rotates 90°. At each temperature, controlling the X-ray to irradiate the thin film sample with set parameters, to obtain in-situ information on the structural evolution of the thin film under different temperature fields in a set stress field; The thin film sample is prepared by the following method: Performing ultrasonic cleaning on a silicon wafer, and soaking the silicon wafer in isopropyl alcohol, distilled water, acetone and isopropyl alcohol in sequence; Performing ultraviolet ozone modification on the soaked silicon wafer; Mixing octadecyltrichlorosilane OTS with toluene to form an OTS-toluene solution, covering the modified silicon wafer with the OTS-toluene solution, cleaning and annealing to obtain an OTS-modified silicon substrate; Dissolving elastomeric particles in toluene to form an elastomeric solution; Pouring the elastomeric solution onto the OTS-modified silicon substrate to form a film, and drying to obtain an elastomeric substrate; Depositing a functional thin film on the elastomeric substrate to obtain a thin film sample.

2. The in-situ temperature-variable tensile method for grazing-incidence X-ray scattering characterization according to claim 1, wherein The power assembly includes a motor and a lead screw. The output end of the motor is connected to one end of the lead screw, and the other end of the lead screw is rotatably arranged on an end support. The end support is arranged on the base, and the first platform support and the second platform support are connected to the lead screw.

3. The in-situ variable-temperature tensile method for grazing-incidence X-ray scattering characterization according to claim 1, wherein, It further includes a rotating platform. The power assembly is installed on one side of the base, and the base is installed on the upper end of the rotating platform to rotate under the action of the rotating platform.

4. The in-situ temperature-variable tensile method for grazing-incidence X-ray scattering characterization according to claim 1, wherein The elastomeric film includes, but is not limited to, one of polysiloxane elastomers, thermoplastic polyurethane elastomers, styrenic thermoplastic elastomers, polyolefin thermoplastic elastomers, and polyamide thermoplastic elastomers.

5. The in-situ variable-temperature tensile method for grazing-incidence X-ray scattering characterization according to claim 1, wherein The functional film includes, but is not limited to, one of conjugated polymer films, polyolefin polymer films, elastomeric films, and ductile metal films.

6. The in-situ variable-temperature tensile method for grazing-incidence X-ray scattering characterization according to claim 1, wherein The set parameters are: exposure time of 1 to 600 seconds.

Images