In-situ stretching multi-photon laser confocal imager and method for real-time in-situ three-dimensional observation of internal structure of blended polymer

文档序号:405105 发布日期:2021-12-17 浏览:18次 中文

阅读说明:本技术 原位拉伸多光子激光共聚焦成像仪、实时原位三维观测共混聚合物内部结构的方法 (In-situ stretching multi-photon laser confocal imager and method for real-time in-situ three-dimensional observation of internal structure of blended polymer ) 是由 徐斌 武志远 田文晶 于 2021-09-18 设计创作,主要内容包括:本发明涉及原位成像技术领域,尤其涉及一种原位拉伸多光子激光共聚焦成像仪,实时原位三维观测共混聚合物内部结构的方法。本发明提供的原位拉伸多光子激光共聚焦成像仪,包括可调节自动拉伸试验机(1)和成像装置(2);所述成像装置(2)包括依次连接的飞秒激光器(3)、扫描部件(4)、光学显微镜(5)和CCD传感器(6)。所述原位拉伸多光子激光共聚焦成像仪可以实现实时原位三维观测两种以上不同的聚合物的内部结构。(The invention relates to the technical field of in-situ imaging, in particular to an in-situ stretching multi-photon laser confocal imager and a method for real-time in-situ three-dimensional observation of an internal structure of a blending polymer. The invention provides an in-situ stretching multi-photon laser confocal imager, which comprises an adjustable automatic stretching testing machine (1) and an imaging device (2); the imaging device (2) comprises a femtosecond laser (3), a scanning component (4), an optical microscope (5) and a CCD sensor (6) which are connected in sequence. The in-situ stretching multi-photon laser confocal imager can realize real-time in-situ three-dimensional observation of the internal structures of more than two different polymers.)

1. An in-situ stretching multi-photon laser confocal imager is characterized by comprising an adjustable automatic stretching testing machine (1) and an imaging device (2);

the imaging device (2) comprises a femtosecond laser (3), a scanning component (4), an optical microscope (5) and a CCD sensor (6);

the femtosecond laser (3), the scanning component (4), the optical microscope (5) and the CCD sensor (6) are sequentially and optically connected.

2. The in-situ stretching multiphoton laser confocal imager of claim 1, wherein the adjustable automatic tensile tester (1) comprises a motor (7) and a specimen stretcher (8);

the motor (7) is in telecommunication connection with the sample tensioner (8).

3. The in-situ stretching multiphoton laser confocal imager of claim 1, wherein a first dichroic mirror (18) is disposed between the optical microscope (5) and the CCD sensor (6).

4. The in-situ stretching multi-photon laser confocal imager as claimed in any one of claims 1 to 3, wherein the optical microscope (5) comprises an objective lens (9), a second dichroic mirror (10), a long-range filter (11), a first total reflection mirror (12), a second total reflection mirror (13) and an eyepiece (14) which are sequentially arranged from bottom to top.

5. The in-situ stretched multiphoton confocal laser imager of claim 4, wherein the first total reflection mirror (12) is optically connected to the first dichroic mirror (18).

6. The in-situ stretched multiphoton laser confocal imager of claim 5, wherein the imaging device (2) further comprises an imaging display device (15);

the imaging display device (15) is in telecommunication connection with the CCD sensor (6).

7. A method for real-time in-situ three-dimensional observation of the internal structure of a blended polymer, which is carried out by using the in-situ stretching multi-photon laser confocal imager as claimed in any one of claims 1 to 6, and comprises the following steps:

placing a polymer blend sample containing a fluorescent probe on an adjustable automatic tensile testing machine (1), enabling a femtosecond laser (3) to emit laser, enabling the laser emitted by the femtosecond laser (3) to be focused on the surface of the polymer blend sample containing the fluorescent probe sequentially through a scanning component (4) and an optical microscope (5), enabling the obtained optical signal to realize conversion from the optical signal to the electrical signal through a CCD (charge coupled device) sensor (6), realizing fluorescent imaging, and obtaining the internal structures of more than two different polymers.

8. The method according to claim 7, wherein the stretching speed of the blended polymer sample containing the fluorescent probe on the automatic tensile testing machine (1) is 0 to 100 mm/min;

the drawing speed is different from 0.

9. The method of claim 7, wherein the laser has a wavelength of 800 nm.

10. The method of claim 7, wherein the polymer blend in the polymer blend sample containing the fluorescent probe is a blend of polypropylene and polystyrene;

the fluorescent probe in the blended polymer sample containing the fluorescent probe is 2- (4-bromophenyl) -3- (4- (4- (diphenylamino) styryl) phenyl) fumaronitrile.

Technical Field

The invention relates to the technical field of in-situ imaging, in particular to an in-situ stretching multi-photon laser confocal imager and a method for real-time in-situ three-dimensional observation of an internal structure of a blended polymer.

Background

Substances are the basis for the progress and development of human society. The polymer material has rich source, low density, corrosion resistance and low energy consumption, and is widely applied to various fields of national economy, including industry, agriculture, traffic, communication and even daily life, and becomes the fourth major material following wood, steel and cement. In order to meet the needs of new technologies and new applications, researchers need to develop new materials with unique and superior properties as soon as possible. However, the chemical synthesis of new materials has the disadvantages of high cost, long cycle, and the like, and is not beneficial to processing and production. Fortunately, the polymer blending method is convenient, has good linearity and good repeatability, and is an important means for modifying the polymer. For blending, the properties of the material are affected not only by the chemical composition and structure of the various polymers, but also by the microscopic phase separation obtained during the forming process. In two-phase blends, four common morphologies were found: droplets, fibers, layers, and co-continuous microstructures. The phase-separated structure has a great influence on macroscopic properties of the material, such as toughness, transparency, processability, chemical resistance, thermal stability and flowability. Most polymer blends are thermodynamically incompatible, with "islands-in-the-sea" phase morphology. Unfortunately, the "islands-in-the-sea" phase morphology has too many defects. The properties may be improved when the micro-phase structure is transformed from a "sea-island" structure to a co-continuous structure. Therefore, the visualization of the micro-phase separation of the polymer blend has great academic and industrial significance, which is beneficial to understanding the relationship between the morphology and the properties, and finally realizes the control of the properties of more than two different polymers after blending by regulating and controlling the phase separation of the polymer blend.

Currently, many researchers typically study polymer morphology using two-dimensional techniques, such as Transmission Electron Microscopy (TEM) and Scanning Electron Microscopy (SEM). Images obtained by these techniques provide information about two-dimensional mixed morphology, but lack of three-dimensional information is likely to result in misinterpretation of the true morphology by the two-dimensional image information. Therefore, it is important to develop a device and a method for real-time in-situ three-dimensional observation of the internal structure of two or more different polymers.

Disclosure of Invention

The invention aims to provide an in-situ stretching multi-photon laser confocal imager and a method for real-time in-situ three-dimensional observation of the internal structure of a polymer blend.

In order to achieve the above object, the present invention provides the following technical solutions:

the invention provides an in-situ stretching multi-photon laser confocal imager, which comprises an adjustable automatic stretching testing machine 1 and an imaging device 2;

the imaging device 2 comprises a femtosecond laser 3, a scanning component 4, an optical microscope 5 and a CCD sensor 6;

the femtosecond laser 3, the scanning component 4, the optical microscope 5 and the CCD sensor 6 are sequentially and optically connected.

Preferably, the adjustable automatic tensile testing machine 1 comprises a motor 7 and a sample stretcher 8;

the motor 7 is in telecommunication connection with a sample stretcher 8.

Preferably, a first dichroic mirror 18 is disposed between the optical microscope 5 and the CCD sensor 6.

Preferably, the optical microscope 5 includes an objective lens 9, a second dichroic mirror 10, a long-range filter 11, a first total reflection mirror 12, a second total reflection mirror 13, and an eyepiece 14, which are sequentially arranged from bottom to top.

Preferably, the first total reflecting mirror 12 is optically connected to the first dichroic mirror 18.

Preferably, the imaging device 2 further includes an imaging display device 15;

the imaging display device 15 is in telecommunication connection with the CCD sensor 6.

The invention also provides a method for real-time in-situ three-dimensional observation of the internal structure of the polymer blend, which is carried out by adopting the in-situ stretching multi-photon laser confocal imager in the technical scheme and comprises the following steps:

placing a polymer blend sample containing a fluorescent probe on an adjustable automatic tensile testing machine 1, enabling a femtosecond laser 3 to emit laser, enabling the laser emitted by the femtosecond laser 3 to be focused on the surface of the polymer blend sample containing the fluorescent probe sequentially through a scanning component 4 and an optical microscope 5, realizing fluorescence imaging inside the structure of the polymer blend sample containing the fluorescent probe, enabling the obtained optical signal to realize conversion from an optical signal to an electrical signal through a CCD (charge coupled device) sensor 6, realizing fluorescence imaging, and obtaining the internal structures of more than two different polymers.

Preferably, the stretching speed of the blended polymer sample containing the fluorescent probe on the automatic tensile testing machine 1 is 0-100 mm/min;

the drawing speed is different from 0.

Preferably, the laser has a wavelength of 800 nm.

Preferably, the polymer blend in the polymer blend sample containing the fluorescent probe is a blend of polypropylene (PP) and Polystyrene (PS);

the fluorescent probe in the blended polymer sample containing the fluorescent probe is 2- (4-bromophenyl) -3- (4- (4- (diphenylamino) styryl) phenyl) fumaronitrile.

The invention provides an in-situ stretching multi-photon laser confocal imager, which comprises an adjustable automatic stretching testing machine 1 and an imaging device 2; the imaging device 2 comprises a femtosecond laser 3, a scanning component 4, an optical microscope 5 and a CCD sensor 6; the femtosecond laser 3, the scanning component 4, the optical microscope 5 and the CCD sensor 6 are sequentially and optically connected. The in-situ stretching multi-photon laser confocal imager is provided with the femtosecond laser, the effective penetration depth of an excitation light source emitted by the femtosecond laser is deeper, so that a sample to be detected can be subjected to three-dimensional imaging without being limited to a transparent sample or a slice, and the application range is wide; the adjustable automatic tensile testing machine can realize dynamic stretching of a sample in the detection process and realize the purpose of real-time imaging; the in-situ stretching multi-photon laser confocal imager does not need special requirements of high vacuum, heavy metal dyeing, slicing and the like when in use, is simple and rapid to operate, and cannot cause irreparable damage to a sample.

The invention also provides a method for real-time in-situ three-dimensional observation of the internal structure of the polymer blend, which is carried out by adopting the in-situ stretching multi-photon laser confocal imager in the technical scheme and comprises the following steps: placing a polymer blend sample containing a fluorescent probe on an adjustable automatic tensile testing machine 1, enabling a femtosecond laser 3 to emit laser, enabling the laser emitted by the femtosecond laser 3 to be focused on the surface of the polymer blend sample containing the fluorescent probe sequentially through a scanning component 4 and an optical microscope 5, realizing fluorescence imaging inside the structure of the polymer blend sample containing the fluorescent probe, enabling the obtained optical signal to realize conversion from an optical signal to an electrical signal through a CCD (charge coupled device) sensor 6, realizing fluorescence imaging, and obtaining the internal structures of more than two different polymers. The invention utilizes the different dispersivity of the fluorescent probe in different polymer phases to lead the different aggregation structures of the fluorescent probe in different polymers to lead the fluorescent probe to have different fluorescence intensity in different polymers, realizes the specific identification under a multi-photon laser confocal microscope, can clearly observe the micro-morphology and the distribution condition of one polymer in more than two different polymers at the same time, and further observes the micro-phase separation condition of more than two incompatible different polymers.

Drawings

FIG. 1 is a schematic structural diagram of an in-situ stretching multi-photon laser confocal imager, wherein 1-an adjustable automatic stretching tester, 2-an imaging device, 3-a femtosecond laser, 4-a scanning component, 5-an optical microscope, 6-a CCD sensor, 7-a motor, 8-a sample stretcher, 9-an objective lens, 10-a second dichroic mirror, 11-a long-range filter, 12-a first total reflector, 13-a second total reflector, 14-an eyepiece, 15-an imaging display device, 16-a mechanical moving platform, 17-an expansion platform and 18-a first dichroic mirror;

FIG. 2 is a fluorescence image of the polymer blend sample of example 1 in the in situ stretched multiphoton confocal laser imager of the present invention;

FIG. 3 is a life and fluorescence image of a sample of the polymer blend of comparative example 1 under a conventional fluorescence microscope;

FIG. 4 is an SEM image of a polymer blend sample of example 2;

FIG. 5 is a fluorescence image of the polymer blend sample of example 2 in the in situ stretched multiphoton confocal laser imager of the present invention.

Detailed Description

As shown in fig. 1, the present invention provides an in-situ stretching multi-photon laser confocal imager, which comprises an adjustable automatic stretching testing machine 1 and an imaging device 2;

the imaging device 2 comprises a femtosecond laser 3, a scanning component 4, an optical microscope 5 and a CCD sensor 6;

the femtosecond laser 3, the scanning component 4, the optical microscope 5 and the CCD sensor 6 are sequentially and optically connected.

As a specific embodiment of the present invention, the optical microscope 5 includes an objective lens 9, a second dichroic mirror 10, a long-range filter 11, a first total reflection mirror 12, a second total reflection mirror 13, and an eyepiece 14, which are sequentially arranged from bottom to top.

As a specific embodiment of the present invention, the optical microscope 5 further includes a stage, a 5-aperture objective lens converter, and a focusing mechanism.

In the present invention, the parameters of the optical microscope 5 are preferably: magnification of objective lens 9: 4-40X. Objective lens 9: an inner positioning 5-hole objective converter; the overlength working distance infinite flat field achromatic phase contrast objective lens is 4X/N.A. more than or equal to 0.13/W.D. more than or equal to 10.43mm, and the diameter of a clear imaging circle (based on data in a detection report) is more than or equal to 16.8 mm; the diameter of a clear imaging circle (based on data in a detection report) is more than or equal to 16.5 mm; the diameter of a clear imaging circle (based on data in a detection report) is not less than 15.9 mm; the diameter of a clear imaging circle (based on data in a detection report) is more than or equal to 16 mm; the ocular lens 14 is fixed by adopting an observation tube, the observation tube is hinged three-eye, is inclined at 45 degrees, and has a pupil distance adjusting range of 50-75 mm; the eyepiece 14: a high-eyepoint large-visual field flat eyepiece PL10X/22mm with self-visibility adjustment; a focusing mechanism: coarse and fine coaxial focusing; the coarse adjustment stroke is more than or equal to 9mm, and the fine adjustment precision is 0.002 mm; the torque of the rough adjusting hand wheel can be adjusted by the rough adjusting tightness adjusting device.

As a specific embodiment of the present invention, the adjustable automatic tensile testing machine 1 includes a motor 7 and a specimen tensile tester 8; the motor 7 is in telecommunication connection with a sample stretcher 8. The sample stretcher 8 is arranged on a fixed carrying platform of the optical microscope 5, and the sample stretcher 8 comprises a mechanical moving platform 16 and an expansion platform 17; the area of the fixed loading platform is more than or equal to 250X215 mm; the moving range of the mechanical moving platform 16 is more than or equal to 120mmX80 mm. In the present invention, the fixed stage, the mechanically moving stage 16 and the expansion stage 17 are preferably metal stages.

In the present invention, the adjustable automatic tensile testing machine 1 is preferably fully automatically controlled, i.e. automatically returns to the original point, and the machine stroke of the adjustable automatic tensile testing machine 1 is as follows: 650mm (without clamp); standard travel: 1000mm (with clamp); load capacity: 5 to 100N.

As a specific embodiment of the present invention, a first dichroic mirror 18 is disposed between the optical microscope 5 and the CCD sensor 6.

As a specific embodiment of the present invention, the first total reflection mirror 12 is optically connected to the first dichroic mirror 18.

As a specific embodiment of the present invention, the imaging device 2 further includes an imaging display device 15; the imaging display device 15 is in telecommunication connection with the CCD sensor 6.

In the present invention, the CCD sensor 6 is preferably a Sony ICX205140 ten thousand pixel color CCD sensor.

In the invention, the adjustable range of the wavelength of the femtosecond laser 3 is preferably 300-1500 nm.

The invention also provides a method for real-time in-situ three-dimensional observation of the internal structure of the polymer blend, which is carried out by adopting the in-situ stretching multi-photon laser confocal imager in the technical scheme and comprises the following steps:

placing a polymer blend sample containing a fluorescent probe on an adjustable automatic tensile testing machine 1, enabling a femtosecond laser 3 to emit laser, enabling the laser emitted by the femtosecond laser 3 to be focused on the surface of the polymer blend sample containing the fluorescent probe sequentially through a scanning component 4 and an optical microscope 5, enabling the obtained optical signal to realize conversion from an optical signal to an electrical signal through a CCD (charge coupled device) sensor 6, realizing fluorescent imaging, and obtaining the internal structures of more than two different polymers.

In the present invention, unless otherwise specified, the raw materials used in the preparation of the polymer blend sample containing the fluorescent probe are all commercially available products well known to those skilled in the art.

The invention mixes more than two different polymers and the fluorescent probe, and carries out granulation or melt tabletting to obtain the blended polymer sample containing the fluorescent probe.

The preparation process of the blended polymer sample containing the fluorescent probe is not limited in any way, and can be carried out by adopting a process well known to those skilled in the art.

The shape and thickness of the polymer blend sample containing the fluorescent probe are not limited in any way, and those familiar to those skilled in the art can be used.

In the present invention, the types of the polymers in the polymer blend containing the fluorescent probe are preferably two. The polymer of the present invention is not particularly limited in kind, and those known to those skilled in the art can be used. In a specific embodiment of the present invention, the polymer blend in the polymer blend sample containing the fluorescent probe is a blend of polypropylene and polystyrene; the invention has no special limit on the proportion of each polymer in the polymer blend, and the polymer blend can be mixed according to any proportion.

The invention does not have any special limitation on the types of the fluorescent probes in the blended polymer sample containing the fluorescent probes, and the types well known to those skilled in the art can be adopted to meet the requirement that the fluorescent probes have different dispersities in the phases of different polymer types. In a specific embodiment of the invention, the fluorescent probe is specifically 2- (4-bromophenyl) -3- (4- (4- (diphenylamino) styryl) phenyl) fumaronitrile (TB).

In the present invention, the mass percentage of the fluorescent probe to the total mass of the two or more different polymers is preferably 0.1 to 1%, more preferably 0.5 to 1%, and most preferably 1%.

In the invention, the stretching speed of the blended polymer sample containing the fluorescent probe on the automatic tensile testing machine 1 is preferably 0-100 mm/min, and the stretching speed is not 0; more preferably 10 to 20mm/min, most preferably 15 mm/min.

In the present invention, the wavelength of the laser light is preferably 800 nm.

In the present invention, the focusing is preferably performed by focusing the laser at a position 50 μm or less from the surface of the polymer blend specimen containing the fluorescent probe.

In the present invention, after the focusing is completed, the fluorescence imaging is preferably realized in a Z-axis scanning manner. The Z-axis scanning is a process that the objective lens 9 continuously moves downwards in a direction vertical to the direction of the blended polymer sample containing the fluorescent probe under the control of software; the pattern of the Z-axis scan is preferably one coal three second scan.

In the invention, the above process is specifically: the fluorescent probe of the polymer blend sample containing the fluorescent probe emits fluorescence after being stimulated by laser emitted by a femtosecond laser 3, the fluorescence sequentially passes through an objective lens 9, a second dichroic mirror 10, a long-range filter 11, a first total reflecting mirror 12, a first dichroic mirror 18 and a CCD sensor 6, and is subjected to photoelectric conversion through the CCD sensor 6 and transmitted to an imaging display device 15 to realize fluorescence imaging; meanwhile, the fluorescence passes through the first total reflecting mirror 12 and then passes through the second total reflecting mirror 13, and then is observed through an eyepiece connected with the second total reflecting mirror 13.

The following examples are provided to describe the method for real-time in-situ three-dimensional observation of the internal structure of the polymer blend by the in-situ stretching multi-photon laser confocal imager provided by the present invention, but they should not be construed as limiting the scope of the present invention.

Example 1

Mixing 0.8g of polypropylene, 0.2g of polystyrene and 100mL of toluene solvent, adding 0.01g of TB under the stirring condition, dripping the obtained mixed solution on a polarizer, heating at the temperature of 180 ℃ for 10min to remove the toluene solvent, and cooling to room temperature at the cooling rates of 1 ℃/min, 10 ℃/min and 50 ℃/min respectively to prepare a blended polymer sample containing the fluorescent probe;

placing the blended polymer sample on an adjustable automatic tensile testing machine 1 without stretching, enabling a femtosecond laser 3 to emit laser with the wavelength of 800nm, enabling an objective lens of an optical microscope 5 to move downwards along the direction vertical to the blended polymer sequentially through a scanning component 4 under the control of software, enabling the laser emitted by the femtosecond laser 3 to be focused below 50 micrometers from the surface of the blended polymer sample containing the fluorescent probe, scanning in a Z-axis scanning mode (enabling an objective lens 9 to continuously move downwards in the direction vertical to a sample under the control of the software), scanning downwards every 5 micrometers, enabling the obtained optical signal (610-710 nm) to realize the conversion from the optical signal to the electric signal through a CCD (charge coupled device) sensor 6, realizing fluorescent imaging, and obtaining the internal structures of more than two different polymers;

fluorescence imaging (scale bar is 40 μm) of the blended polymer sample containing the fluorescent probe in the in-situ stretching multi-photon laser confocal imager is shown in fig. 2, wherein a is a top view of in-situ three-dimensional imaging, b is a side view of in-situ three-dimensional imaging, the three-dimensional imaging is formed by overlapping fluorescence imaging acquired by tomography, c is a phase separation micro-topography 20 micrometers below the surface of the blended polymer sample, d is a phase separation micro-topography 40 micrometers below the surface of the blended polymer sample, and e is a phase separation micro-topography 60 micrometers below the blended polymer sample; as can be seen from FIG. 2, the detection method of the present invention can overcome the defects that two-dimensional imaging cannot reveal a real phase separation morphology, and the diameter of the exposed PS microsphere cannot represent the real size of the PS microsphere, and can provide richer and real morphology information from a three-dimensional perspective.

Comparative example 1

Mixing 0.8g of polypropylene, 0.2g of polystyrene and 100mL of toluene solvent, adding 0.01g of TB under the stirring condition, dripping the obtained mixed solution on a polarizer, heating at the temperature of 180 ℃ for 10min to remove the toluene solvent, and cooling to room temperature at the cooling rates of 1 ℃/min, 10 ℃/min and 50 ℃/min respectively to prepare a blended polymer sample;

carrying out fluorescence imaging on the blended polymer sample under a common fluorescence microscope;

the lifetime and fluorescence imaging of the polymer blend sample under a common fluorescence microscope are shown in FIG. 3, wherein a is a bright field photograph of the polymer blend sample under a fluorescence microscope when the rate of 1 ℃/min is reduced to room temperature, b is a bright field photograph of the polymer blend sample under a fluorescence microscope when the rate of 10 ℃/min is reduced to room temperature, c is a bright field photograph of the polymer blend sample under a fluorescence microscope when the rate of 50 ℃/min is reduced to room temperature, d is a fluorescence photograph of the polymer blend sample under a fluorescence microscope when the rate of 1 ℃/min is reduced to room temperature, e is a fluorescence photograph of the polymer blend sample under a fluorescence microscope when the rate of 10 ℃/min is reduced to room temperature, and f is a fluorescence photograph of the polymer blend sample under a fluorescence microscope when the rate of 50 ℃/min is reduced to room temperature, as can be seen from FIG. 3, only polystyrene fluoresces under the action of the fluorescent probe TB, and it can be seen that different annealing rates can significantly affect the phase separation morphology of the polymer blend, when the rate of 1 ℃/min is reduced to room temperature, the PS phase is distributed in the PP in a sea-island structure, and when the rate of 50 ℃/min is reduced to room temperature, the PS phase and the PP are penetrated to form a bicontinuous phase. However, the two-dimensional image cannot obtain the internal structure of the polymer, which is not beneficial to further research on the influence of external processing conditions on the phase separation morphology of the polymer.

Example 2

Uniformly mixing 0.8g of polypropylene, 0.2g of polystyrene and 0.01g of TB, and then sequentially carrying out blending (the blending temperature is 180 ℃, the time is 10min), granulation and injection (the temperature is 180 ℃), so as to prepare a dumbbell-shaped blended polymer sample containing the fluorescent probe, wherein the sample is 6cm in length, 1cm in width and 0.5cm in thickness;

placing the blended polymer sample containing the fluorescent probe on an adjustable automatic tensile testing machine 1, setting the tensile speed of the adjustable automatic tensile testing machine to be 15mm/min, enabling a femtosecond laser 3 to emit laser with the wavelength of 800nm to sequentially pass through a scanning component 4 and enable an objective lens of an optical microscope 5 to move downwards along the direction vertical to the blended polymer under the control of software, enabling the laser emitted by the femtosecond laser 3 to be focused below 50 micrometers away from the surface of the blended polymer sample containing the fluorescent probe, scanning in a Z-axis scanning mode (an eyepiece 14 continuously moves downwards in the direction vertical to the sample under the control of the software), scanning once every 3 seconds, enabling the obtained optical signal (610-710 nm) to realize the conversion from the optical signal to the electric signal through a CCD sensor 6, realizing fluorescence imaging, and obtaining the internal structures of more than two different polymers, completing in-situ real-time observation of the internal structure of the tensile sample;

and (3) putting the blended polymer sample containing the fluorescent probe into liquid nitrogen for brittle fracture, and performing SEM test, wherein the test result is shown in figure 4, a is an electron micrograph of the brittle fracture cross section of the blended polymer sample containing the fluorescent probe, and b is an electron micrograph of the brittle fracture cross section of the blended polymer sample containing the fluorescent probe after the PS is etched away by using a good solvent (toluene). As can be seen from fig. 4, the SEM image can only provide surface topography information, and the internal structure of the polymer blend cannot be observed;

FIG. 5 is a fluorescence image of the polymer blend sample containing the fluorescent probe in the in-situ stretching multi-photon laser confocal imager, wherein a is a two-photon in-situ three-dimensional image of a stretched region and an unstretched region of the polymer blend sample containing the fluorescent probe after stretching, b is a change of a PS phase at 50 microns inside the stretched region of the polymer blend sample containing the fluorescent probe along with the stretching morphology and distribution of the stretching instrument, and c is a deformation amount of the PS and PP phase regions in the stretching process of the polymer blend sample containing the fluorescent probe; as can be seen from FIG. 5, the technique can be used for real-time imaging monitoring of the distribution change of the PS microphase in the stretching process, which cannot be realized by the traditional electron microscope method. Meanwhile, it is known that although the rigidity of PP is increased after doping PS, the toughness is reduced, and it is known from c in fig. 5 that the toughness is reduced because PS is hardly deformed during stretching, which results in that the force is not effectively conducted in the PS phase region, resulting in reduced toughness. Therefore, the set of device can provide beneficial help for researchers to research the relation between the microstructure and the performance of the polymer.

The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

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