CN210221758U - Wide-temperature-range two-dimensional extension rheometer and high-polymer film performance detection device - Google Patents
Wide-temperature-range two-dimensional extension rheometer and high-polymer film performance detection device Download PDFInfo
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- CN210221758U CN210221758U CN201920848196.8U CN201920848196U CN210221758U CN 210221758 U CN210221758 U CN 210221758U CN 201920848196 U CN201920848196 U CN 201920848196U CN 210221758 U CN210221758 U CN 210221758U
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Abstract
The application provides a wide temperature range two dimension extends rheometer, polymer film performance detection device, wide temperature range two dimension extends rheometer carries out the blown film through gas, realizes the two-dimensional even stretching to polymer film, and can control the alternating temperature rate and fall to required low temperature, perhaps rises required high temperature, and polymer film structure evolution under the harsh environment of simulation high and low temperature explores the performance of macromolecular material under wide temperature range. And the light inlet window and the light outlet window are arranged, so that the system can be used together with a synchrotron radiation X-ray scattered ray station, and the in-situ research on the relationship between the structure evolution behavior in the stretching process of the polymer film and the use performance under the harsh conditions of high temperature and low temperature is realized.
Description
Technical Field
The utility model relates to a polymer film processing technology field especially relates to a wide temperature domain two dimension extends rheometer, polymer film performance detection device.
Background
Biaxial stretching is widely used in the field of polymer processing, and a sample subjected to biaxial stretching at a temperature equal to or higher than the glass transition temperature but lower than the equilibrium melting point has molecular chains oriented in both the transverse and longitudinal directions, and is generally considered to be isotropic in the direction parallel to the film plane. Biaxial stretching is not necessary for processing of lithium ion battery separators and optical films for polarizing plates.
However, biaxial stretching is not true two-dimensional isotropy, but molecular chains of a polymer sample are relatively flexible, and relatively uniform orientation distribution can be formed after stretching in the transverse and longitudinal vertical directions, so that ordinary biaxial stretching cannot meet the strict requirement of true isotropy.
Moreover, the glass transition temperature is one of the important parameters of the polymer material, and some typical polymer materials such as rubber tend to have very low glass transition temperature, and theoretically, the glass transition temperature is the lowest critical temperature for the use; on the other hand, due to some harsh using modes of the high polymer material, such as an aerial sounding balloon flying at high altitude, when flying at high altitude over ten thousand meters, the transition of temperature reduction and then temperature rise can be completed by a troposphere and a stratosphere, which is a typical example of application of keeping fixed and uniform deformation at different temperatures. The double-drawn films such as double-drawn polyethylene films, polypropylene films and double-drawn poly-p-phthalic acid plastic films are widely applied in the fields of packaging films, optical compensation films and the like, but the balanced melting points of the materials are higher.
Therefore, it is an urgent problem to provide a two-dimensional extensional rheometer capable of achieving two-dimensional uniform stretching, capable of being used in combination with a synchrotron radiation X-ray scattering station, and having a wide temperature range.
SUMMERY OF THE UTILITY MODEL
In view of this, the utility model provides a wide temperature range two dimension extends rheometer, polymer film performance detection device to solve among the prior art two dimension and extend the problem that the rheometer can't satisfy two-dimentional even stretching, with X ray scattering ally oneself with usefulness, and realize wide temperature range experimental environment simultaneously.
In order to achieve the above object, the utility model provides a following technical scheme:
a wide temperature range two-dimensional extension rheometer is applied to polymer film performance detection, and the two-dimensional extension rheometer comprises:
the gas cavity comprises a gas cavity body, a temperature rise and drop base, a gas pressure gauge, a temperature measuring instrument, a light outlet flange, a gas mass flow controller, an outer cover, a cold source and a heat source;
the opposite two sides of the gas cavity body are respectively provided with a light inlet window and a light outlet window;
the light-emitting flange is fixed on the gas cavity body, covers the light-emitting window and is used for fixing the polymer film on the light-emitting window, and the center of the light-emitting flange is arranged corresponding to the center of the light-emitting window;
the gas cavity body is embedded on the temperature rising and lowering base, and the cold source and the heat source are connected with the temperature rising and lowering base to provide a low-temperature environment and a high-temperature environment for the gas cavity body;
the gas pressure gauge and the temperature measuring instrument are arranged on the gas cavity main body and used for measuring the gas pressure and the gas temperature in the gas cavity main body;
the outer cover is arranged on one side, away from the gas cavity body, of the light outlet flange;
the gas mass flow controller is used to control the flow and velocity of gas entering the gas chamber body.
Preferably, the housing is a transparent housing.
Preferably, the outer cover is further provided with a deformation measurement scale for measuring the deformation amount of the polymer film.
Preferably, the outer cover is an acrylic outer cover.
Preferably, the outer cover is provided with an air inlet for introducing air so as to maintain the temperature of the two sides of the polymer film to be approximately the same.
Preferably, the cold source is a self-pressurization liquid nitrogen tank, and the self-pressurization liquid nitrogen tank is communicated with the cooling medium inlet of the temperature rise and decrease base through a liquid nitrogen electromagnetic valve.
Preferably, the heat source is a heating rod.
Preferably, the heating rod further comprises a thermocouple, wherein the thermocouple is arranged on one side of the heating rod and used for feeding back the temperature of the heating rod.
The utility model also provides a polymer film performance detection device, include:
a wide temperature range two-dimensional extensional rheometer as claimed in any one of the preceding claims;
and the X-ray source is used for emitting X-rays and passes through the light inlet window and the light outlet window on the gas cavity body of the wide-temperature-range two-dimensional extension rheometer.
According to the technical scheme, the utility model provides a wide temperature range two-dimentional extension rheometer carries out the blown film through gas, realizes the two-dimentional even tensile to polymer film, and can control the alternating temperature rate and fall to required low temperature, perhaps rises required high temperature, and polymer film structure evolution under the harsh environment of simulation high and low temperature explores polymer material's performance under wide temperature range. And the light inlet window and the light outlet window are arranged, so that the system can be used together with a synchrotron radiation X-ray scattered ray station, and the in-situ research on the relationship between the structure evolution behavior in the stretching process of the polymer film and the use performance under the harsh conditions of high temperature and low temperature is realized.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required to be used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
Fig. 1 is a schematic structural diagram of a wide temperature range two-dimensional stretching rheometer provided in an embodiment of the present invention;
FIG. 2 is a computer-side output interface of a high-precision gas pressure gauge resistant to high temperature and low temperature;
FIG. 3 is a LabVIEW software control interface for a gas mass flow controller;
FIG. 4 is a schematic diagram of the wide-angle X-ray diffraction pattern of a natural rubber sample at-20 ℃ and a gas flow rate of 50SCCM, wherein the upper left figure is the corresponding gas chamber internal pressure;
FIG. 5 is a one-dimensional integral photograph of the wide angle X-ray diffraction pattern at 25.8kPa of FIG. 4.
Detailed Description
As described in the background section, the two-dimensional stretching in the prior art is biaxial stretching, and two-dimensional isotropy in the true sense cannot be realized, and the performance detection of the polymer film cannot be realized.
If uniform two-dimensional stretching can be realized, the mechanical property of the composite material can be improved to a greater extent, and the composite material has guiding significance to the technical field of polymer processing. And if the two-dimensional extensional rheometer can be used together with X-ray scattering for in-situ structure detection, and can provide high-temperature and low-temperature environments, the application range of the two-dimensional extensional rheometer is wider.
In summary, the wide temperature range two-dimensional extensional rheometer for in-situ structure detection in combination with X-ray scattering needs to have the following features: 1. the stretching mode is two-dimensional uniform stretching, and the central position of the sample is kept unchanged during stretching; 2. the device should be easy to disassemble and assemble for use with synchrotron radiation X-ray scattering stations; 3. different high polymer materials, temperature and deformation quantity, and the temperature and deformation rate of the device are continuously adjustable; 4. the two-dimensional uniform stretching can be performed on the sample in a wide temperature range from low temperature to high temperature.
Based on this, the embodiment of the utility model provides a wide temperature domain two dimension extends rheometer is applied to the polymer film performance and detects, include:
the gas cavity comprises a gas cavity body, a temperature rise and drop base, a gas pressure gauge, a temperature measuring instrument, a light outlet flange, a gas mass flow controller, an outer cover, a cold source and a heat source;
the opposite two sides of the gas cavity body are respectively provided with a light inlet window and a light outlet window;
the light-emitting flange is fixed on the gas cavity body, covers the light-emitting window and is used for fixing the polymer film on the light-emitting window, and the center of the light-emitting flange is arranged corresponding to the center of the light-emitting window;
the gas cavity body is embedded on the temperature rising and lowering base, and the cold source and the heat source are connected with the temperature rising and lowering base to provide a low-temperature environment and a high-temperature environment for the gas cavity body;
the gas pressure gauge and the temperature measuring instrument are arranged on the gas cavity main body and used for measuring the gas pressure and the gas temperature in the gas cavity main body;
the outer cover is arranged on one side, away from the gas cavity body, of the light outlet flange;
the gas mass flow controller is used to control the flow and velocity of gas entering the gas chamber body.
The utility model provides a wide temperature range two dimension extends rheometer carries out the blown film through gas, realizes the two-dimensional even stretching to polymer film, and can control alternating temperature speed and fall to required low temperature, perhaps rises required high temperature, and polymer film structure evolution under the harsh environment of simulation high and low temperature explores the performance of macromolecular material under wide temperature range. And the light inlet window and the light outlet window are arranged, so that the system can be used together with a synchrotron radiation X-ray scattered ray station, and the in-situ research on the relationship between the structure evolution behavior in the stretching process of the polymer film and the use performance under the harsh conditions of high temperature and low temperature is realized.
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
Please refer to fig. 1, fig. 1 is a wide temperature range two-dimensional extension rheometer provided by an embodiment of the present invention, which is applied to polymer film performance detection, and the two-dimensional extension rheometer includes: the gas cavity comprises a gas cavity body 1, a temperature rise and drop base 2, a gas pressure gauge 3, a temperature measuring instrument 4, a light emitting flange 6, a gas mass flow controller 5, an outer cover 10, a cold source (not shown in the figure) and a heat source 8.
Wherein, the two opposite sides of the gas cavity body 1 are respectively provided with a light inlet window and a light outlet window; the light-emitting flange 6 is fixed on the gas cavity body 1, covers the light-emitting window and is used for fixing the polymer film on the light-emitting window, and the center of the light-emitting flange 6 corresponds to the center of the light-emitting window; the gas cavity body 1 is embedded on the temperature rising and lowering base 2, and the cold source and the heat source 8 are connected with the temperature rising and lowering base to provide a low-temperature environment and a high-temperature environment for the gas cavity body 1; the gas pressure gauge 3 and the temperature measuring instrument 4 are arranged on the gas cavity main body 1 and used for measuring the gas pressure and the gas temperature in the gas cavity main body 1; the outer cover 10 is arranged on one side of the light-emitting flange 6, which is far away from the gas cavity body 1; the gas mass flow controller 5 is used to control the flow and velocity of gas into the gas chamber body 1.
It should be noted that, in this embodiment, the specific material of the outer cover is not limited, and optionally, the outer cover may be an acrylic outer cover and made of a transparent material, so that a deformation measurement scale may be further disposed on the outer cover for measuring the deformation amount of the polymer film.
The embodiment of the utility model provides an dustcoat has two effects: firstly, a low-temperature environment can be provided for the outside of the polymer film through the gas inlet 11 (corresponding to the low-temperature nitrogen gas inlet at this time) in a low-temperature experiment, and the outside of the polymer film through the gas inlet 11 (corresponding to the high-temperature gas inlet at this time) in a high-temperature experiment, that is, the temperatures at the two sides of the polymer film are kept to be the same; and secondly, the damage to the external detector when the polymer film is broken can be avoided, and the external detector is protected.
The concrete structure of cold source and heat source is not limited in this embodiment, and optionally, the cold source is a self-pressurization liquid nitrogen container, and the self-pressurization liquid nitrogen container is communicated with a cooling medium inlet 7 (corresponding to a liquid nitrogen inlet here) of the temperature raising and lowering base 2 through a liquid nitrogen electromagnetic valve. The heat source is a heating rod 8 and is used for heating the temperature raising and lowering base 2; in addition, in order to accurately control the heating temperature in the temperature raising and lowering base 2, a thermocouple 9 may be further included in the present embodiment, and the thermocouple 9 is disposed on one side of the heating rod 8 and used for feeding back the temperature of the heating rod 8. During high temperature experiment, the temperature controller is adopted to control the working state of the heating rod to realize the temperature control of the polymer film, the thermocouple has a feedback effect, and the temperature in the heating and cooling base 2 is accurately controlled by adjusting PID parameters.
The utility model provides a wide temperature range two dimension extends rheometer carries out the blown film through gas, realizes the two-dimensional even stretching to polymer film, and can control alternating temperature speed and fall to required low temperature, perhaps rises required high temperature, and polymer film structure evolution under simulation high temperature, the harsh environment of low temperature explores the performance of macromolecular material under wide temperature range. And the light inlet window and the light outlet window are arranged, so that the system can be used together with a synchrotron radiation X-ray scattered ray station, and the in-situ research on the relationship between the structure evolution behavior in the stretching process of the polymer film and the use performance under the harsh conditions of high temperature and low temperature is realized.
Based on the same utility model discloses think, the utility model discloses still provide a polymer film performance detection device, include: the wide temperature range two-dimensional extensional rheometer described in the above example; and the X-ray source is used for emitting X-rays and passing through the light inlet window and the light outlet window on the gas cavity body of the wide-temperature-range two-dimensional extension rheometer.
Similarly, the embodiment of the utility model provides a still provide a polymer film performance detection method, include:
fixing a polymer film to be detected at a light outlet window of the wide-temperature-range two-dimensional stretching rheometer in the embodiment;
introducing gas into a gas cavity main body of the wide-temperature-range two-dimensional stretching rheometer to enable the high polymer film to be stretched in two dimensions;
opening a cold source, closing a heat source, and detecting the low-temperature performance of the polymer film;
and opening a heat source, closing a cold source, and detecting the high-temperature performance of the polymer film.
In order to more clearly illustrate the structure and the working principle of the wide temperature range two-dimensional extension rheometer provided by the present invention, the present invention is described in detail in the following embodiments.
The embodiment of the utility model provides a wide temperature range two dimension that carries out normal position structure detection with X ray scattering allies oneself with uses extends rheometer, including gas chamber main part, low temperature rise and fall warm base, high accuracy gas pressure table, high accuracy thermoscope, gaseous mass flow controller, light-emitting flange, liquid nitrogen import, heating rod, thermocouple, ya keli dustcoat, low temperature nitrogen gas import and deformation measurement scale.
Dry nitrogen is introduced into the gas cavity body 1, the flow speed and the flow of the nitrogen entering the gas cavity body are regulated and controlled by the gas mass flow controller and the data conversion module, so that the pressure difference between two sides of a polymer film is generated, uniform two-dimensional stretching is realized, digital control is realized by the data conversion module, the deformation rate of a polymer film sample is accurately controlled and adjusted, and the response of different materials to the deformation rate can be well matched.
The high-precision (precision is-199.9 ℃ to +199.9 ℃) thermometer 4 displays the temperature in real time, the internal pressure is displayed in real time through the high-precision (precision is 0-5.0000 MPa) gas pressure gauge 3, and remote computer display is realized through the RS485 conversion module (as shown in figure 2, the board card temperature is the display temperature of the thermometer).
The polymer film clamping mode is the sealed double-layered appearance of light-emitting flange 6, outside assembly ya keli dustcoat 10, the ya keli dustcoat can provide low temperature environment (for letting in high temperature nitrogen gas in air inlet 11 in the high temperature experiment) for the sample outside in the low temperature experiment through low temperature nitrogen gas import 11, can avoid the sample to break the destruction of external detector when breaking again, for demarcating sample deformation size, the laminating of deformation measurement scale 12 is outside and with CCD camera real-time recording deformation volume at ya keli dustcoat 10. During the experiment, a sample is clamped firstly, the high and low temperature is regulated after the sample is sealed, when the temperature reaches the required temperature, an X-ray light source is started, and meanwhile, a LabVIEW software control system is started to set the gas flow velocity and flow rate, so that the sample is stretched in two dimensions. LabVIEW software control system carries out accurate regulation and control, data conversion module to gas flow velocity and flow the embodiment of the utility model provides an in not inject, the output signal mode is RS 232.
In the low temperature experiment, through letting in the low temperature environment for the base of cooling and heating, the liquid nitrogen is as low temperature heat transfer medium, can fall very low temperature rapidly, and the liquid nitrogen is also very long in the normal atmospheric temperature container save time, satisfies whole low temperature stretching process constancy of temperature.
In a high-temperature experiment, the working state of the heating rod is controlled by the temperature controller to realize the temperature control of the sample, the thermocouple has a feedback effect, and the temperature in the sample heating cavity is accurately controlled by adjusting PID parameters.
The embodiment of the utility model provides a wide temperature range two dimension extends rheometer has following characteristics:
1. easy to be disassembled and assembled, and convenient to be used together with a synchrotron radiation X-ray scattering experiment station.
2. The stretching temperature can be reduced to-60 ℃ at the lowest, can be increased to +180 ℃ at the highest, and the temperature rising and reducing rates are adjustable, and the temperature is uniform and constant.
3. The deformation rate is continuously adjustable and the control is accurate.
4. The pressure and deformation quantity of the inner side of the sample can be accurately collected in real time.
5. The method is suitable for parameter setting aiming at different polymer film materials, and has universality for disclosing the scientific problem of two-dimensional stretching of the polymer film.
6. The application prospect is as follows: 1) the system is used together with a synchrotron radiation X-ray scattering experiment station to systematically research the basic scientific problem in the two-dimensional stretching process of the high molecular film; 2) simulating a harsh environment with high temperature and low temperature, and revealing the relationship between the film structure evolution behavior and the use performance under the condition of low temperature and wide temperature range.
The main experimental steps of the device when used with a synchrotron radiation X-ray scattering station comprise:
the method comprises the following steps: a gas pressure gauge, a temperature measuring instrument and a gas mass flow controller are connected to a gas cavity main body, and a liquid nitrogen tank and a liquid nitrogen electromagnetic valve are connected to a liquid nitrogen inlet of a temperature rise and drop base after being connected in a low-temperature experiment;
in the high-temperature experiment, the heating rod and the thermocouple are directly opened, and the gas cavity body is clamped in the temperature rise and fall base.
Step two: clamping polymer film sample, covering the light-emitting flange, chucking the ya keli dustcoat, low temperature experiment need with low temperature nitrogen gas pipe insert in the low temperature nitrogen gas import.
Step three: opening a software control system interface (shown in figure 3) of the gas mass flow controller, setting the gas flow rate, simultaneously opening an RS485 output interface and a CCD of a gas pressure gauge, and waiting for acquiring gas pressure and real-time deformation of a sample;
step four: in the low-temperature experiment, valves of a self-pressurization liquid nitrogen tank and a liquid nitrogen electromagnetic valve need to be opened, when the high molecular film sample reaches a preset temperature, the liquid nitrogen electromagnetic valve is closed, a nitrogen tube is immersed in a Dewar flask filled with liquid nitrogen, the nitrogen valve is opened, an X-ray light source is started, the high molecular film sample is uniformly stretched in two dimensions, the gas pressure and deformation in the stretching process and the structural evolution of the high molecular film sample in the stretching process are recorded, and once the temperature rises, the liquid nitrogen electromagnetic valve is immediately opened to introduce liquid nitrogen for cooling;
in the high-temperature experiment, a heating rod and a thermocouple need to be opened, and the temperature in the sample heating cavity is accurately controlled by adjusting PID parameters.
Step five: by implementing different temperatures and deformation quantities on different polymer film samples, the influence of polymer parameters and external field parameters on film structure evolution is systematically researched, and the data are coupled to finally obtain the service performance of the polymer at different temperatures.
The polymer sample is uniformly stretched in two dimensions, the central position, namely the position through which the X-ray passes, can be guaranteed to be always in a stretching state, can not be limited by the strain magnitude, is stretched to a specified deformation amount or even is broken, and the polymer film stretching device is used for simulating the real use environment of polymer film two-dimensional stretching at high and low temperatures in a laboratory. The wide-temperature-range two-dimensional stretching rheometer can realize accurate temperature control of a film sample and can realize uniformity of surface temperature of the film sample. The deformation of a polymer film sample is recorded in real time by using a CCD (charge coupled device), the areas of the samples at different moments are calculated by using high-throughput image processing software, the deformation quantity of the samples is obtained, different samples are obtained, and the influence of different external field parameters on the tensile rheological property of the film.
The embodiment of the utility model provides an extend rheometer can be applied to synchrotron radiation X ray scattering research for the technique of research polymer film structure evolution and outfield parameter relation can be researched different film samples under different tensile temperatures, the structure evolution action under the different deformation volume. The crystallinity and orientation of the film sample obtained by X-ray scattering are coupled with the two-position stretching data, so that the relationship between the external field parameters and the film structure performance can be obtained. The method is used for simulating the mechanical properties of materials, especially high polymer materials, in high-temperature and low-temperature harsh environments in a laboratory and researching the use conditions of the high polymer materials under the harsh conditions.
Experimental examples:
synchronous radiation X-ray in-situ research is carried out on the natural rubber which is uniformly stretched in two dimensions at ultralow temperature.
Purpose of the experiment:
natural rubber is one of the most widely used rubber elastomers, the glass transition temperature of common varieties is often about-68 ℃, although coin-induced crystallization can occur in the natural rubber at low temperature, thermodynamic studies prove that isotropic unstretched samples can only undergo temperature-induced crystallization after being treated at low temperature for about 20 hours, and biaxial stretching at normal temperature can not generate any crystal; the X-ray is one of the important means of crystallography research, is an indispensable characterization method in the field of polymer material research, and along with the discovery and application of the synchrotron radiation X-ray, the detection time resolution is shortened to the millisecond order from the last dozens of hours; whether the two-dimensional stretching can induce the crystallization at low temperature or not has guiding significance on the low-temperature use performance.
The experimental process comprises the following steps:
fixing the cut natural rubber sample on a gas cavity main body through a light-emitting flange screw, opening a self-pressurizing liquid nitrogen tank and a liquid nitrogen electromagnetic valve after sealing, setting the temperature to-20 ℃, and opening a nitrogen cylinder but closing a gas mass flow controller; and (3) starting a CCD camera to record the deformation amount of the sample, starting an X-ray light source, and simultaneously starting a LabVIEW software control system to set the gas flow velocity and flow rate, so as to perform two-dimensional stretching on the sample.
The experimental results are as follows:
FIG. 4 is a wide angle X-ray diffraction pattern of a natural rubber sample at-20 ℃ and an internal pressure of 25.8kPa, the upper left figure is the pressure inside the corresponding gas chamber, it can be seen from the left figure that the initial sample has only one ring, which is a typical rubber amorphous ring, and after uniform two-dimensional stretching, the wide angle X-ray diffraction pattern of the right figure sample shows three new diffraction rings, which is the appearance of a crystal signal, which is different from diffraction spots generated by highly oriented uniaxial stretching induced crystallization, but is an isotropic crystal signal.
In fig. 5, curve a is a result of one-dimensional integration of a wide-angle X-ray diffraction pattern at an internal pressure of 25.8kPa, curve B is a result of machine recognition of a one-dimensional integration curve by a computer, and is fitted to a crystal peak (200) of curve a, a crystal peak (201) of curve B, a crystal peak (120) of curve d, an auxiliary agent peak of curve c, and an amorphous form of curve e, and appearance of a crystal peak indicates occurrence of crystallization by assigning peaks to the obtained one-dimensional integration result curve. It is clear from the figure that new diffraction peaks appear at positions around 11.4 °, 14.2 ° and 17.2 °, and the crystal signals are determined to belong to the (200), (201) and (120) crystal planes of natural rubber by reference to relevant literature. Shows that crystals are generated in the natural rubber after two-dimensional uniform stretching at low temperature.
And (4) experimental conclusion:
the method utilizes a small-sized experimental wide-temperature-range two-dimensional stretching rheometer and combines a synchrotron radiation online X-ray technology to conveniently obtain the structural evolution information of the crystallinity, the orientation degree, the crystallization dynamics and the like of the high polymer material, particularly the elastomer material, at low temperature. The results of the experiments with synchrotron radiation X-rays are combined to conclude that the natural rubber sample is subjected to an online wide-angle X-ray diffraction (WAXD) two-dimensional uniform stretching experiment at the temperature of-20 ℃, compared with the normal-temperature biaxial stretching which only has the high orientation of an amorphous dispersion ring, the uniform two-dimensional stretching result at the low temperature shows that three crystal diffraction rings can appear under large strain, and the natural rubber crystal is formed through crystal structure analysis. The research realizes the online WAXD two-dimensional stretching experiment of the natural rubber at ultralow temperature for the first time, obtains isotropic crystal signals and provides theoretical guidance for processing and low-temperature service performance of the natural rubber.
The embodiment of the utility model provides a wide temperature range two dimension extends rheometer can jointly use with synchrotron radiation X ray scattered ray station, carries out normal position structure detection, adopts gas mass flow controller, cooperation data conversion module, realizes the digital control to gas flow; gas with certain flow velocity and flow enters the gas cavity, and the pressure difference of two sides of the polymer film sample is utilized to realize uniform stretching of the polymer film sample; meanwhile, a high-precision gas pressure gauge and a high-precision temperature measuring instrument connected to the outside of the gas cavity record the pressure and the temperature inside the gas cavity in real time; during low-temperature two-dimensional stretching, the gas cavity is arranged on a temperature-reducing base, the temperature-reducing medium is liquid nitrogen, the liquid nitrogen inlet and outlet and the flow rate are controlled through a liquid nitrogen flow valve, and the temperature is further controlled to be as low as-60 ℃; when stretching at high temperature, the temperature is accurately controlled by a double-channel temperature controller, and the maximum temperature can reach +180 ℃.
Simultaneously the embodiment of the utility model provides a still provide polymer film performance detection method and detection device for wide temperature range two dimension extends rheometer and synchrotron radiation X ray scattered ray station antithetical couplet and uses, realizes polymer film's normal position structure and detects. The utility model discloses can with the accurate cooling/intensification of polymer film sample to required temperature and realize even two-dimentional drawing, the device main part is small, can portably carry, is a very good set of device of structural evolution under the different temperatures of normal position research material especially macromolecular material.
It should be noted that, in the present specification, the embodiments are all described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments may be referred to each other.
It is further noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that an article or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such article or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in an article or device that comprises the element.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. A wide temperature range two-dimensional extension rheometer is characterized in that, being applied to polymer film performance detection, the two-dimensional extension rheometer comprises:
the gas cavity comprises a gas cavity body, a temperature rise and drop base, a gas pressure gauge, a temperature measuring instrument, a light outlet flange, a gas mass flow controller, an outer cover, a cold source and a heat source;
the opposite two sides of the gas cavity body are respectively provided with a light inlet window and a light outlet window;
the light-emitting flange is fixed on the gas cavity body, covers the light-emitting window and is used for fixing the polymer film on the light-emitting window, and the center of the light-emitting flange is arranged corresponding to the center of the light-emitting window;
the gas cavity body is embedded on the temperature rising and lowering base, and the cold source and the heat source are connected with the temperature rising and lowering base to provide a low-temperature environment and a high-temperature environment for the gas cavity body;
the gas pressure gauge and the temperature measuring instrument are arranged on the gas cavity main body and used for measuring the gas pressure and the gas temperature in the gas cavity main body;
the outer cover is arranged on one side, away from the gas cavity body, of the light outlet flange;
the gas mass flow controller is used to control the flow and velocity of gas entering the gas chamber body.
2. The wide temperature range two-dimensional extensional rheometer of claim 1 wherein the housing is a transparent housing.
3. The wide temperature range two-dimensional extensional rheometer of claim 2, wherein the housing is further provided with a strain gauge for measuring the amount of strain of the polymeric film.
4. A wide temperature range two-dimensional extensional rheometer according to any one of claims 1 to 3 wherein the housing is an acrylic housing.
5. The wide temperature range two-dimensional extensional rheometer of claim 1 wherein the housing is provided with an inlet for admitting gas to maintain the temperature on both sides of the polymer film to be about the same.
6. The wide temperature range two-dimensional stretching rheometer of claim 1, wherein the cold source is a self-pressurizing liquid nitrogen tank, and the self-pressurizing liquid nitrogen tank is communicated with the cooling medium inlet of the temperature raising and lowering base through a liquid nitrogen solenoid valve.
7. The wide temperature range two-dimensional extensional rheometer of claim 1 wherein the heat source is a heating rod.
8. The wide temperature range two-dimensional extensional rheometer of claim 7, further comprising a thermocouple disposed on one side of the heating rod for feeding back the temperature of the heating rod.
9. A polymer film performance detection device is characterized by comprising:
a wide temperature range two-dimensional extensional rheometer according to any one of claims 1 to 8;
and the X-ray source is used for emitting X-rays and passes through the light inlet window and the light outlet window on the gas cavity body of the wide-temperature-range two-dimensional extension rheometer.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201920848196.8U CN210221758U (en) | 2019-06-05 | 2019-06-05 | Wide-temperature-range two-dimensional extension rheometer and high-polymer film performance detection device |
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