CN107063889B - Creep stretching device combined with X-ray scattering and experimental method thereof - Google Patents
Creep stretching device combined with X-ray scattering and experimental method thereof Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/22—Investigating strength properties of solid materials by application of mechanical stress by applying steady torsional forces
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/026—Specifications of the specimen
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
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- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/06—Indicating or recording means; Sensing means
- G01N2203/0641—Indicating or recording means; Sensing means using optical, X-ray, ultraviolet, infrared or similar detectors
Abstract
The invention provides a creep stretching device combined with X-ray scattering and an experimental method thereof. The device adopts an Anchuan servo motor synchronous drive as a power source, and simultaneously utilizes a torque limiter to keep constant output torque so as to realize creep stretching. The device is provided with a torque sensor and an angle sensor, synchronously measures rheological information in the creep process, and monitors the running state stability of the device. The stretching mechanism adopts a hollow detachable separating roller, reduces the rotational inertia of the mechanism, improves the linear speed at the same rotating speed, can provide various mounting modes, and meets the testing requirements of different sample strengths and categories. The forced nitrogen flow is adopted to ensure the temperature uniformity of the sample cavity and prevent the thermal degradation of the sample at high temperature. The invention has the advantages of easy disassembly and installation, is very suitable for being used together with a synchrotron radiation experiment line station, and provides more favorable conditions for representing rheological and phase change behaviors in the flow field induced crystallization process.
Description
Technical Field
The invention relates to the technical field of research on the coupling relation between polymer structure evolution and different external field parameters by using synchrotron radiation X-ray scattering, in particular to a creep stretching device combined with X-ray scattering and an experimental method thereof.
Background
The research of the crystallization of the polymer material induced by the flow field has important guiding significance for the processing of the polymer material. Under industrial production and material service conditions, different external field parameters, including strain, strain rate, stress, etc., can affect the final structure and performance of the finished product. Based on these factors, it is important to study the mechanism of action of different external field parameters on the structural evolution of flow field induced crystallization. The basic idea of the research is to apply a flow field to a material under the set conditions of temperature, pressure and the like, and analyze the structure and performance characteristics of different dimensions by using different optical characterization means. In the stretching process, the strain rate is controlled to be unchanged under the general condition, the stretching with different strains is carried out, and due to the unique long-chain structure of the high polymer material, the relaxation mechanical behavior and the structural evolution of different microscale structures are more focused in many times. However, in many studies, especially those involving phase transitions under unbalanced conditions, stresses actually play a greater role. Therefore, creep stretching, which keeps the tensile stress constant, is of great importance in this study.
Meanwhile, for the research of structural transformation during stretching, various in-situ optical detection means are the most suitable methods. Particularly, ultra-fast X-ray scattering is sensitive to various stable and metastable ordered structures in a high molecular crystalline material, and can be used for researching the structure type, content, morphology, structure transformation rate and dynamics of ultra-fast structure transformation. The common X-ray scattering means mainly comprise small-angle and wide-angle X-ray scattering, and structures of different spatial dimensions of materials can be tracked respectively by adjusting the detection distance from a sample to the sample and combining the structure information dimensions of the materials.
In order to perform in-situ research on the relationship between different external field parameters and structural transformation in the stretching process of the high polymer material, the experimental device must meet the following conditions: 1. the stress, the strain rate and the strain can be controlled respectively and the different control modes can be switched. 2. And aiming at the characteristics of different detection materials, the coupling of the linear speed and the stress is regulated and controlled under the condition of constant power of the power source. 3. Portable, small in installation size, and convenient to be combined with a synchrotron radiation light source. 4. A light-passing hole for passing scattered light is arranged, and the temperature of the sample must be controlled.
Disclosure of Invention
The invention aims to provide a creep stretching device used together with X-ray scattering and an experimental method thereof. The stretching device has the characteristics of easy disassembly and installation and convenient combination with synchrotron radiation X-ray in-situ experiment technology; the strain, the strain rate and the stress can be respectively controlled; the stretching mode is uniaxial roller stretching, so that constant stretching speed and strain rate can be ensured under the same stretching mode; the temperature of the sample is accurately controlled; the controllable range of stress and strain rate is wide, and the device can be conveniently adjusted and replaced without disassembling the device; the method has the characteristics of multichannel real-time data acquisition and the like. The morphological structure information such as crystallinity, orientation degree and rheological information (stress and strain change) of the high polymer material can be obtained, and the relation between the external field parameter and the structural evolution is obtained.
The invention adopts the technical scheme that: the utility model provides a creep stretching device with X ray scattering allies oneself with, includes high accuracy servo motor, motion controller, constant force output control, torque sensor, angle sensor and hollow disconnect-type roller anchor clamps, and the sample is the polymer film sample, wherein:
the high-precision servo motor is controlled by the motion controller to stretch, the high-precision servo motor and the constant force output control are used for controlling and switching the operation mode, meanwhile, the hollow split roller clamp is used for improving the stretching speed at the same motor rotating speed so as to improve the strain rate, in the stretching process, the torque sensor and the angle sensor track the change of stress and strain, the rheological behavior is represented, the stretching temperature is accurately controlled by the double-channel temperature controller, the sample heating cavity is provided with two thermal resistors, the detected temperature information is fed back to the temperature controller, and the temperature controller automatically adjusts the working state so as to achieve the aim of accurately controlling the temperature; the nitrogen is introduced to ensure the uniformity of the film temperature.
The device can realize three different operation modes, namely:
(1) the high-precision servo motor continuously runs, and torque control is performed by using a constant force output control, so that creep stretching is realized;
(2) the constant force output control is locked, and the strain and strain rate controllable stretching is performed by utilizing the high-precision servo motor;
(3) firstly, performing creep stretching, then positioning at specific strain by a high-precision servo motor, reversely locking a constant force output control, and observing the evolution process of a creep-induced generated microstructure in a relaxation stage.
The coupling control of the constant force output control and the high-precision servo motor can respectively control the stress and the strain in the stretching process; meanwhile, the structural information in the flow field of the stretching/creeping process is tracked by utilizing an X-ray ultra-high time resolution in-situ characterization technology, and the phase change theory and the scientific problems related to actual production and processing are researched.
The invention further provides a creep stretching experimental method combined with X-ray scattering, and by utilizing the creep stretching device, the phase change characteristics of flow field induced polymer crystallization and the action mechanisms of different external field parameters are studied in situ by combining with synchronous radiation wide-angle X-ray scattering and small-angle X-ray scattering experimental technologies.
The device and the X ray experimental technique are combined, and the main experimental steps are as follows:
step (1), a motor driver is respectively connected with a high-precision servo motor and a motion controller, a sensor is connected with an acquisition system, a temperature controller is used for controlling the temperature of a heating rod, and then a power supply is started;
step (2), setting the parameters of the constant force output control,
step (3), clamping a high polymer film sample;
setting the stretching temperature of the polymer film sample, and starting an X-ray light source when the polymer film sample reaches the set temperature;
step (5), controlling the high-precision servo motor to start to rotate continuously, and stretching in a set stretching mode;
and (6) simultaneously recording tension and strain changes and structural evolution of the stretched polymer film sample in the stretching process. By implementing different stretching rates, stretching ratios or stretching stresses on different polymer samples, the system researches the influence of molecular parameters and external field parameters on the crystal structure and dynamics, and couples the data to obtain the relationship between the phase change behavior and the rheological behavior of the polymer melt under the flow field.
The device can realize accurate temperature control of the film sample, and can realize the uniformity of the surface temperature of the polymer sample through nitrogen flow.
The method comprises the steps of controlling the rotation of a motor, collecting the changes of internal stress and strain of a sample, and obtaining different samples, wherein different external parameters influence the structure transformation process in the crystallization process induced by a flow field.
The device can be used together with synchrotron radiation X-ray experimental technology to track the structure evolution of the film in situ.
Compared with a common stretching device, the invention has the main innovation points that:
1. the device of the invention is easy to disassemble and assemble, and is convenient to be used together with synchrotron radiation X-ray experimental technology.
2. The invention has continuously adjustable stretching rate, stretching ratio and tension, and accurate control;
3. according to the invention, through the coupling control of the high-precision servo motor and the constant force output control, different stretching modes are switched, and the action mechanisms of different types of external field parameters are researched.
4. The stretching mode of the invention is uniaxial hollow roller stretching, the linear speed is improved under the same motor rotation speed, and the moment of inertia is reduced; the split type clamp is convenient to replace, and can be debugged according to different samples;
5. the invention has the characteristics of large controllable tension and stretching speed range, multichannel real-time data acquisition and the like.
6. The invention can obtain morphological structure information such as crystallinity, orientation degree and rheological information (strain and stress change) of the high polymer material, and obtain the relation between different external field parameters and microstructure evolution.
7. The application prospect of the invention: 1) The method is combined with a synchrotron radiation X-ray scattering experimental technology, and the action mechanism of regulating and controlling the product performance by different processing parameters in the processing process of the polymer material is systematically researched; 2) And researching the corresponding relation between the microstructure transformation process in the flow field induced crystallization and external action parameters, and explaining the phase change theory in the unbalanced substance.
In summary, the invention can study the structure evolution behavior of different polymer materials under different stretching temperatures and different types of stretching modes, and study the action mechanism of the structure evolution of different types of external field parameters in the induced crystallization process of the flow field. And coupling the crystallinity, the crystal form, the orientation degree and the tensile mechanical data of the film sample obtained by X-ray scattering, so that the relationship between the external field parameter and the phase change structure and performance can be obtained. The method is used for simulating actual film stretching processing conditions in a laboratory and disclosing scientific problems of film industrial processing.
Drawings
FIG. 1 is a schematic view of a creep stretching apparatus for use with X-ray scattering according to the present invention, wherein: 1 is a high-precision servo motor, 2 is a motion controller, 3 is a constant force output control, 4 is a torque sensor, 5 is an angle sensor, 6 is a hollow separation type roller clamp, and 7 is a high polymer film sample;
FIG. 2 is a schematic view of a hollow split roller clamp according to the present invention;
FIG. 3 is rheological data obtained in the present invention, including strain and stress information;
FIG. 4 is a strain and stress curve in a mode 3 experiment;
FIG. 5 is a wide angle X-ray scattering plot of stretch induced natural rubber crystallization at different strain rates;
FIG. 6 is quantitative data of structural evolution during creep-relaxation.
Detailed Description
The invention is further described below with reference to the drawings and examples.
Referring to fig. 1, a creep stretching device used in combination with X-ray scattering comprises a high-precision servo motor 1, a motion controller 2, a constant force output control 3, a torque sensor 4, an angle sensor 5 and a hollow separation type roller clamp 6, wherein a sample is a high-molecular film sample 7, and the high-precision servo motor 1 is controlled by the motion controller 2 to stretch. The operation mode is controlled and switched by using the high-precision servo motor 1 and the constant force output control 3. Simultaneously, the stretching speed is increased by using the hollow split roller clamp 6 at the same motor rotation speed, so that the strain rate is increased. During stretching, the torque sensor 4 and the angle sensor 5 track changes in stress and strain, characterizing rheological behavior. The stretching temperature is accurately controlled by a double-channel temperature controller, two thermal resistors are arranged in a sample heating cavity, detected temperature information is fed back to the temperature controller, and the temperature controller automatically adjusts the working state so as to achieve the aim of accurately controlling the temperature; the nitrogen is introduced to ensure the uniformity of the film temperature.
The creep stretching device can realize three different operation modes, namely:
1. the high-precision servo motor 1 runs continuously, and torque control is performed by using the constant force output control 3, so that creep stretching is realized;
2. the constant force output control 3 is locked, and the high-precision servo motor 1 is utilized to stretch the constant strain rate with controllable strain and strain rate;
3. firstly, creep stretching is carried out, then the high-precision servo motor 1 is positioned at specific strain, the constant force output control 3 is reversely locked, and the evolution process of a microstructure generated by creep induction in a relaxation stage is observed.
Under the high-speed stretching condition, the device can carry out coupling control on the highest rotating speed and the highest stress of the system by assembling hollow rollers and clamps with different types as shown in fig. 2, so that the testing requirements on samples with different performances are met, and the power of a motor is fully utilized. Meanwhile, the change of stress and strain in the stretching process can be collected, and the phase change characteristics of flow field induced crystallization and the physical mechanism of external field parameter action are researched. The roller is designed to be separable, and the two parts are respectively connected with the transmission shaft, so that the roller can be replaced according to different experimental requirements without a dismounting device in the experimental process. According to the space design of the device, the distance between the rollers needs 9 mm to ensure the X-ray to pass, so that the controllable range of the diameter of the rollers is 8-26 mm, the highest rotating speed of the motor is 3000 rpm, the maximum torque value of the constant force output control is 0.5 nm, the thickness of the sample is 0.5 mm, and the width of the sample is 5 mm. According to the above parameters, the formula is as follows:
linear speed = rotational speed x drum circumference x 2
The maximum achievable speed of the device can be calculated to be 8.16 m/s with a maximum stress of 25 mpa.
The device adopts the binary channels temperature controller to control the operating condition of heating rod and realizes controlling the temperature to the sample, and temperature probe has feedback effect. And the temperature of the cavity and the temperature rising and falling rate are precisely controlled by adjusting PID parameters.
Experimental example:
the effect of ultra-fast stretching rate on stretch-induced natural rubber crystallization was studied in situ by wide angle X-ray scattering.
The purpose of the experiment is as follows:
natural rubber can crystallize under stretching conditions. It is generally recognized that in the crystallization of stretch-induced natural rubber, there is a clear correspondence between the crystallization behavior and strain of the rubber, without taking into account the effects of relaxation and crystallization kinetics of the rubber. Moreover, the conventional stretching device can only control constant strain rate stretching and has limited stretching speed, so that the relationship between the crystallization dynamics of the natural rubber and different flow field parameters cannot be well reflected. In the experiment, by utilizing a creep stretching device and combining an ultra-fast X-ray wide angle and small angle detection experiment technology, we can observe the multiscale influence of different external field parameters on the crystallization and crystallization kinetics of the natural rubber.
The experimental process comprises the following steps:
the natural rubber raw material is Indonesia No. 1 tobacco flake rubber, the natural rubber raw material is pressed into tablets by a flat vulcanizing machine after being mixed with sulfur, and the sample size is 0.4-5-45 mm. The X-ray line width angle scattering tracks the evolution of the sample morphology before and after stretching, and the torque and angle sensors record the changes of stress and strain in the stretching process respectively. By combining the tensile force and the sample morphology, the phase change and rheological information of the natural rubber crystallization induced by different stretching conditions can be obtained. The present example uses modes 2 and 3 of operation described previously to study stress induced crystallization and the evolution of structural relaxation under creep conditions.
Experimental results:
FIG. 3 is a graph of rheological data obtained in the present invention for different creep stresses, i.e., the change in creep process strain over time; under high stress creep, the strain of the sample is observed to be gradually increased, and obvious creep phenomenon is shown; as can be seen from the enlarged view of fig. b, the sample requires a certain settling time to start the creep process, and at the lowest experimental value of 3.8 mpa, the longest settling time can be found to be about 0.2 seconds. The effect of creep stabilization time can be ignored during data analysis compared to experimental times of tens of seconds.
Fig. 4 is a rheological profile for operation in mode 3. At a stress of 9.6 mpa, creep was first carried out for 20 seconds, followed by a relaxation process. Typical creep and relaxation curves can be observed in the graph, namely: stress is unchanged and strain is increased in the creep process; the strain is unchanged and the stress is reduced during relaxation.
FIG. 5 is a two-dimensional plot of WAXS and SAXS at the beginning of the creep process. It can be seen from the figure that a weak orientation signal starts to appear at 0.06 seconds SAXS, whereas a crystal signal can only be seen in WAXS at 0.18 seconds. The crystal signal is highly oriented, indicating that there is an amorphous pre-ordered structure between 0.06 seconds and 0.18 seconds. After 6 seconds the morphology of the signal no longer changes significantly, only the intensity.
FIG. 6 is a graph of the crystal plane peak intensity and crystallinity of the creep-relaxation process. From 20 seconds, the relaxation process, both the crystal plane strength and the crystallinity start to decrease. This means that the decrease in stress leads to a decrease in crystallinity with unchanged strain.
Conclusion of experiment:
the structure information and crystallization kinetics of the natural rubber under different conditions are successfully observed by utilizing a creep stretching device combined with X-ray scattering. From the rheological data and the X-ray structure evolution, the following two conclusions can be drawn:
1) During crystallization of natural rubber, an amorphous pre-ordered structure exists.
2) The stress itself affects the crystallization behavior. The decrease in stress during relaxation results in a decrease in crystallinity.
Parts of the invention not described in detail are well known in the art.
While the foregoing describes illustrative embodiments of the present invention to facilitate an understanding of the present invention by those skilled in the art, it should be understood that the present invention is not limited to the scope of the embodiments, but is to be construed as protected by the accompanying claims insofar as various changes are within the spirit and scope of the present invention as defined and defined by the appended claims.
Claims (9)
1. A creep stretching device for use with X-ray scattering, characterized by: including high accuracy servo motor (1), motion controller (2), constant force output control (3), torque sensor (4), angle sensor (5) and hollow disconnect-type roller anchor clamps (6), the sample is polymer film sample (7), wherein:
the high-precision servo motor (1) is controlled to stretch through the motion controller (2), the high-precision servo motor (1) and the constant force output control (3) are used for controlling and switching the operation mode, meanwhile, the hollow separation type roller clamp (6) is used for improving the stretching speed at the same motor rotating speed so as to improve the strain rate, in the stretching process, the torque sensor (4) and the angle sensor (5) track the change of stress and strain, the rheological behavior is represented, the stretching temperature is accurately controlled by the double-channel temperature controller, the sample heating cavity is provided with two thermal resistors, the detected temperature information is fed back to the temperature controller, and the temperature controller automatically adjusts the working state so as to achieve the aim of accurately controlling the temperature; the nitrogen is introduced to ensure the uniformity of the film temperature.
2. A creep stretching apparatus for use in combination with X-ray scattering as claimed in claim 1, wherein: the device can realize three different operation modes, respectively:
(1) the high-precision servo motor (1) runs continuously, and torque control is carried out by using the constant force output control (3) so as to realize creep stretching;
(2) the constant force output control (3) is locked, and the strain and strain rate controllable stretching is carried out by utilizing the high-precision servo motor (1);
(3) firstly, performing creep stretching, then positioning by a high-precision servo motor (1) at a specific strain, reversely locking a constant force output control (3), and observing the evolution process of a creep-induced generated microstructure in a relaxation stage.
3. A creep stretching apparatus for use in combination with X-ray scattering as claimed in claim 1, wherein: the constant force output control (3) and the high-precision servo motor (1) are coupled and controlled, so that the stress and the strain in the stretching process can be controlled respectively; meanwhile, the structural information in the flow field of the stretching/creeping process is tracked by utilizing an X-ray ultra-high time resolution in-situ characterization technology, and the phase change theory and the scientific problems related to actual production and processing are researched.
4. A creep stretching experiment method combined with X-ray scattering, which utilizes the creep stretching device of claim 1 to be combined with synchronous radiation wide-angle X-ray scattering and small-angle X-ray scattering experiment technology to study the relation between the structure evolution behavior and the processing performance in the process of inducing crystallization of different types of flow fields in situ; the method is characterized in that: the device and the X ray experimental technique are combined, and the main experimental steps are as follows:
step (1), a motor driver is respectively connected with a high-precision servo motor (1) and a motion controller (2), a sensor is connected with an acquisition system, a temperature controller is used for controlling the temperature of a heating rod, and then a power supply is started;
setting parameters of a constant force output control (3),
step (3), clamping a polymer film sample (7);
setting the stretching temperature of the polymer film sample (7), and starting an X-ray light source when the polymer film sample (7) reaches the set temperature;
step (5), controlling the high-precision servo motor (1) to start to rotate continuously, and stretching in a set stretching mode;
and (6) simultaneously recording stress and strain changes and structural evolution of a stretched polymer film sample (7) in the stretching process, systematically researching the influence of molecular parameters and external field parameters on the crystalline structure and dynamics by implementing different stretching rates, stretching ratios or stretching stresses on different polymer samples, and coupling the data to obtain the relationship between the phase change behavior and rheological behavior of the polymer melt under a flow field.
5. A creep-stretching test method for use in combination with X-ray scattering as claimed in claim 4, wherein: the experimental forms of three different stretching modes are realized by utilizing the coupling installation and control of the high-precision servo motor and the constant force output control, and different rheological parameters and structural parameters in the research of the induced crystallization of the flow field are tracked.
6. A creep-stretching test method for use in combination with X-ray scattering as claimed in claim 4, wherein: by adopting a detachable split type hollow roller clamp, the rotational inertia is reduced, and the stretching speed is improved; the device is convenient to detach, can be installed and replaced in the sample cavity, can realize different testing stress and strain rate ranges, meets testing requirements of different materials, and can be coupled with material strength and phase change conditions.
7. A creep-stretching test method for use in combination with X-ray scattering as claimed in claim 4, wherein: the accurate temperature control of the film sample can be realized, and the uniformity of the surface temperature of the film sample can be realized.
8. A creep-stretching test method for use in combination with X-ray scattering as claimed in claim 4, wherein: the method can record the internal strain and stress information of the material in the high-speed stretching process, and simultaneously, the internal structural change of the structural material is characterized by utilizing x-rays to obtain multi-scale data of material phase change.
9. A creep-stretching test method for use in combination with X-ray scattering as claimed in claim 4, wherein: the device can be used together with synchrotron radiation X-ray experimental technology to track the structural evolution of materials in situ.
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| CN201710191037.0A CN107063889B (en) | 2017-03-27 | 2017-03-27 | Creep stretching device combined with X-ray scattering and experimental method thereof |
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| CN107063889B true CN107063889B (en) | 2023-04-28 |
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| CN111665273B (en) * | 2020-06-17 | 2022-05-17 | 中国科学院长春应用化学研究所 | High-low temperature environment box for combined use of testing machine and X-ray light source characterization |
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| JP2003202279A (en) * | 2001-10-25 | 2003-07-18 | Keigo Kamabayashi | Creep testing machine |
| CN103063689A (en) * | 2012-12-27 | 2013-04-24 | 中国科学技术大学 | Constant width film stretching device combined with X-ray scattering, and experimental method thereof |
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| CN203241364U (en) * | 2013-04-08 | 2013-10-16 | 中国科学技术大学 | Double-shaft unidirectional stretching device for in-situ structure detection by being combined with X-ray scattering |
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