CN112485235A - Transmission electron microscope sample rod system with ultrafast time resolution spectral capability and application - Google Patents

Transmission electron microscope sample rod system with ultrafast time resolution spectral capability and application Download PDF

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CN112485235A
CN112485235A CN202011272102.0A CN202011272102A CN112485235A CN 112485235 A CN112485235 A CN 112485235A CN 202011272102 A CN202011272102 A CN 202011272102A CN 112485235 A CN112485235 A CN 112485235A
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sample rod
transmission electron
electron microscope
optical fiber
light
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CN112485235B (en
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马超杰
刘畅
孙华聪
刘开辉
王恩哥
白雪冬
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Institute of Physics of CAS
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64Fluorescence; Phosphorescence
    • G01N21/645Specially adapted constructive features of fluorimeters
    • G01N21/6456Spatial resolved fluorescence measurements; Imaging
    • G01N21/6458Fluorescence microscopy
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B21/00Microscopes
    • G02B21/0004Microscopes specially adapted for specific applications
    • G02B21/002Scanning microscopes
    • G02B21/0024Confocal scanning microscopes (CSOMs) or confocal "macroscopes"; Accessories which are not restricted to use with CSOMs, e.g. sample holders
    • G02B21/0036Scanning details, e.g. scanning stages
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B21/00Microscopes
    • G02B21/0004Microscopes specially adapted for specific applications
    • G02B21/002Scanning microscopes
    • G02B21/0024Confocal scanning microscopes (CSOMs) or confocal "macroscopes"; Accessories which are not restricted to use with CSOMs, e.g. sample holders
    • G02B21/0052Optical details of the image generation
    • G02B21/0076Optical details of the image generation arrangements using fluorescence or luminescence
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64Fluorescence; Phosphorescence
    • G01N2021/6417Spectrofluorimetric devices
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64Fluorescence; Phosphorescence
    • G01N21/645Specially adapted constructive features of fluorimeters
    • G01N2021/6463Optics

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Abstract

The invention discloses a transmission electron microscope sample rod system with ultrafast time resolution spectral capability, which at least comprises an optical system and a mechanical system, wherein the optical system is composed of a sample rod provided with optical fibers, an ultrafast laser, a dispersion compensation element, a spectrometer, a time-dependent single photon counter and the like, and the mechanical system is composed of a piezoelectric ceramic tube, a differential micrometer head, a three-dimensional displacement platform and the like. The optical system and the mechanical system are used for realizing in-situ focusing of pulsed light and three-dimensional scanning of focused light spots in a transmission electron microscope, and finally measuring fluorescence spectrum and fluorescence service life by using the spectrometer and a time-dependent single photon counter through signals such as fluorescence and the like excited and collected by the sample rod provided with the optical fiber. The invention realizes a transmission electron microscope sample rod system with ultrafast time resolution spectral capability, which is used for introducing focused femtosecond pulse light into a transmission electron microscope to perform fluorescence spectrum characterization and fluorescence life measurement, and realizing the ultrafast spectroscopy measurement in the transmission electron microscope.

Description

Transmission electron microscope sample rod system with ultrafast time resolution spectral capability and application
Technical Field
The invention relates to the technical field of accessories of transmission electron microscopes, in particular to a transmission electron microscope sample rod system with ultrafast time resolution spectral capability and application thereof, and more particularly relates to a transmission electron microscope sample rod with ultrafast pulse optical focusing and ultrafast time resolution spectral capability and a corresponding transmission electron microscope system.
Background
Exploring the correspondence between the structural characteristics and physical properties of materials is one of the hot spots in condensed state physical research. In condensed state physical research, when the dimension of a solid approaches to the length of a quantum feature in one or more dimensions, due to the influence of quantum confinement effect and quantum fluctuation effect, electronic structural features which are quite different from those of the bulk material of the solid are shown, most typically, the electronic structure shows discrete energy levels of like atoms or molecules, so that a series of processes such as excitation, relaxation, transportation and the like correspondingly show brand-new features. The measurement and research of the micro mechanism of the excited state and the dynamic process of the nano system are of great significance for developing new research directions and application fields of condensed state physical research.
The recent decades of transmission electron microscopy have advanced the structure characterization capabilities to the atomic scale and can characterize electronic structures at the atomic scale. However, a commercial electron microscope only has structural characterization capability and single function, and cannot be directly related to physical properties of materials. Spectroscopic techniques can be used to study the spectral generation of materials and their interactions with substances, especially with the advent of femtosecond laser technology and the development of ultrafast spectroscopic techniques, the interaction of light with substances can be studied on the femtosecond or even attosecond scale, making it possible to probe ultrafast physical and chemical processes, especially dynamic transient and intermediate processes. Ultrafast processes with different time scales exist in natural science, such as the movement of atomic nuclei, the breakage and the formation of chemical bonds occur in the time range from femtosecond to picosecond, the fluorescence lifetime of a luminescent material is generally in the nanosecond level, the study on the microstructure and the material intrinsic characteristics of a micro substance is a direction which is always regarded in the natural science research, and the important application prospect is also developed.
In-situ electron microscope research is aimed at researching the properties of materials such as force, heat, electricity, light and the like in situ in a transmission electron microscope by introducing signal excitation such as mechanics, thermal, electricity or optics and the like into a transmission electron microscope cavity so as to directly relate the structure and physical properties of the materials. Optical technology is a very important effective means for studying physical properties of materials, for example, spectroscopy technology can study the interaction between light and materials through the spectral response of materials, and the development of ultrafast spectroscopy also improves the time detection resolution of spectroscopy technology to the order of femtoseconds, so that the ultrafast kinetic processes of material electrons or excitons and the like can be further studied. Therefore, it would be of great significance, both in basic scientific research and in applied technology, if an in-situ ultrafast spectral characterization system in a transmission electron mirror could be developed for studying the direct connection between the microstructure and properties of materials.
Disclosure of Invention
Therefore, the present invention is directed to overcoming the drawbacks of the prior art and providing a sample rod system and applications of a transmission electron microscope with ultrafast time-resolved spectroscopy.
To achieve the above object, a first aspect of the present invention provides a tem sample rod system with ultrafast time resolved spectroscopy capability, comprising: the system comprises a femtosecond laser, a beam expanding collimator, a first turning reflector, a dispersion compensation element, a second turning reflector, a first light splitting prism, a microscope objective, a sample rod provided with an optical fiber and a 4f zooming system, a light source, a first lens, a second light splitting prism, a second lens, a third turning reflector, an image acquisition device, an optical filter, a spectrometer, a third lens, a time-dependent single photon counter and an auxiliary optical imaging system;
the 4f zooming system consists of two small-caliber lenses.
The system according to the first aspect of the present invention, wherein the aperture of the small-aperture lens of the 4f zoom system is 2mm to 8mm, preferably 5mm to 6.25 mm.
The system according to the first aspect of the present invention, wherein the laser is a femtosecond laser;
preferably, the laser is selected from a solid femtosecond laser or a fiber femtosecond laser; preferably, the laser is a solid femtosecond laser.
The system according to the first aspect of the present invention, wherein the optical fiber in the sample rod with the optical fiber and 4f zoom system installed is a single mode or few mode optical fiber at the operating wavelength;
preferably, the optical fiber is a fiber bundle consisting of single mode or few mode fibers.
The system according to the first aspect of the present invention, wherein the dispersion compensating element is selected from one or more of: grating pair, prism pair, chirp reflector, programmable phase compensation system and acousto-optic programmable dispersion filter;
preferably a grating pair.
The system according to the first aspect of the present invention, wherein the sample rod with the optical fiber and the 4f zoom system mounted thereon further comprises:
the near end of the optical fiber is fixed on the three-dimensional displacement table;
a front end;
a sample-carrying clamp;
the piezoelectric ceramic tube is used for accurately adjusting the position of a focusing light spot in a plane perpendicular to the light propagation direction;
a centering device; and
and a differential micrometer head.
The system according to the first aspect of the present invention, wherein the sample support fixture is selected from one or more of: a tungsten needle tip, a gold needle tip, and a micro-grid placed obliquely; preferably a tungsten tip.
The system according to the first aspect of the present invention, wherein the sample rod with the optical fiber and the 4f zoom system mounted thereon emits focused pulsed light.
The system according to the first aspect of the present invention, wherein the light source is selected from a white light source or a light emitting diode.
A second aspect of the invention provides a transmission electron microscope comprising a transmission electron microscope sample rod system with ultrafast time-resolved spectroscopic capability as described in the first aspect.
The technology aims to solve the technical problems that the existing transmission electron microscope technology does not have time resolution capability and cannot measure the ultrafast dynamic process, so that the transmission electron microscope technology with ultrafast time resolution spectral capability is realized.
The idea of the invention is that: the 4f system that the optic fibre bundle that utilizes single mode or few mode optic fibre or constitute by a large amount of single mode or few mode optic fibre and two small-bore lenses is constituteed is installed in the sample holder, through the sample holder introduces transmission electron microscope with the ultrafast pulsed light of focus, realizes possessing ultrafast time resolution spectral power transmission electron microscope sample holder system. Firstly, a dispersion compensation element is used for compensating pulse broadening (second-order dispersion) caused by an optical fiber, then pulse light after being broadened in a reverse direction is coupled into a single fiber core at the near end of an optical fiber bundle by means of a reflection imaging system, and the pulse light emitted from the far end of the optical fiber bundle passes through a fiber core 2: the 4f zooming system of the 1 enables femtosecond laser to be focused on a sample chamber, and an excited spectrum signal is collected through the optical fiber bundle and finally enters a spectrometer and a time-dependent single photon counter, so that the transmission electron microscope sample rod system with ultra-fast time resolution spectrum capability is realized.
The transmission electron microscope sample rod system with the ultrafast time resolution spectrum capability of the invention has the following operation steps:
step 1: laser emitted by the femtosecond laser is firstly widened through a dispersion compensation element, then, by means of a white light reflection imaging system, pulse light with the reversed direction widened is coupled into a single fiber core at the near end of an optical fiber bundle, and the pulse light emitted by the far end of the optical fiber bundle is 2: the 4f zooming system of the optical fiber bundle 1 generates femtosecond pulse focusing light spots, the coupling position of the pulse light is changed by adjusting the near end of the optical fiber bundle, and the femtosecond pulse focusing light spots can be scanned in a two-dimensional plane;
step 2: the piezoelectric ceramic tube is used for electrically adjusting the far end of the optical fiber bundle, the focusing light spot generated in the step (1) can be accurately adjusted in a two-dimensional plane, and the differential micrometer head is used for manually adjusting the far end of the optical fiber bundle out of the plane, so that the focusing plane of the focusing light spot is adjusted;
and step 3: and (3) using quantum dots dripped on a tungsten needle point as a measuring object, repeating the steps (1) and (2), changing the position of a focusing light spot, enabling pulsed light to be just focused on the surface of a sample according to the fluorescence spectrum signal intensity detected by a spectrometer, and introducing a fluorescence spectrum into a time-dependent single photon counter to realize ultrafast spectral characterization in a transmission electron microscope.
The transmission electron microscope sample rod system of the present invention may have the following beneficial effects, but is not limited to:
the invention provides a transmission electron microscope sample rod system with ultrafast time resolution spectral capability, which can introduce focused ultrafast pulse light into a transmission electron microscope and realize the detection of ultrafast time spectrum, thereby realizing the transmission electron microscope system for synchronously researching the microstructure of a substance and ultrafast spectroscopy in situ.
Drawings
Embodiments of the invention are described in detail below with reference to the attached drawing figures, wherein:
FIG. 1 shows the structure of a TEM sample rod system with ultrafast time-resolved spectroscopic capability according to the present invention.
FIG. 2 shows a detailed view of the sample rod portion with the fiber optic bundle installed.
FIG. 3 shows a graph of the intensity of the reflection at the proximal end face of the fiber bundle recorded by the image capture device; in which fig. 3(a) shows a reflection intensity map when only white light is irradiated on an end face, fig. 3(b) shows a reflection intensity map when a white light source and femtosecond pulse light are simultaneously irradiated on an end face, and an inset of fig. 3(b) shows a partially enlarged view of an area near a focused end face of the femtosecond pulse light, indicating that the pulse light is focused on a single core.
FIG. 4 shows the result of optical focusing via a sample rod when femtosecond pulsed light is coupled into a single core; wherein, fig. 4(a) shows an intensity map of a focused spot recorded by the auxiliary optical imaging system, and fig. 4(b) shows an intensity distribution of the focused spot in a horizontal direction.
Fig. 5 shows the intensity distribution of the focused spots generated by coupling femtosecond pulsed light into the fiber bundle from different cores after superposition.
FIG. 6 shows the pulse width measurement of the pulse emitted from the sample rod with the fiber bundle installed when the femtosecond pulse light is coupled into the single fiber core; fig. 6(a) shows the pulse width of the outgoing pulsed light when the grating pair is not compensated, and fig. 6(b) shows the pulse width of the outgoing pulsed light when the grating pair is compensated.
FIG. 7 shows ultrafast spectral characterization results of a sample rod with a fiber bundle mounted thereon for quantum dots drop-coated on a tungsten tip; in this case, fig. 7(a) shows a two-photon fluorescence spectrum of the quantum dot, and fig. 7(b) shows a fluorescence lifetime of the quantum dot measured by the time-dependent single-photon counter.
Description of reference numerals:
1. a femtosecond laser; 2. a beam expanding collimator; 3. a first flip mirror; 4. a dispersion compensating element; 5. a second flipping mirror; 6. a mirror; 7. a first beam splitting prism; 8. a microscope objective; 9. a sample rod mounted with an optical fiber bundle; 10. a white light source; 11. a first lens; 12. a second beam splitting prism; 13. a second lens; 14. a third flipping mirror; 15. an image acquisition device; 16. an optical filter; 17. a spectrometer; 18. a third lens; 19. a time-dependent single photon counter; 20. an auxiliary optical imaging system; 21. a front end; 22. a sample-carrying clamp; 23. a first small-caliber lens; 24. a second small-caliber lens; 25. a fiber optic bundle mounted to the sample rod; 26. a piezoelectric ceramic tube; 27. a centering device; 28. and a differential micrometer head.
Detailed Description
The invention is further illustrated by the following specific examples, which, however, are to be construed as merely illustrative, and not limitative of the remainder of the disclosure in any way whatsoever.
This section generally describes the materials used in the testing of the present invention, as well as the testing methods. Although many materials and methods of operation are known in the art for the purpose of carrying out the invention, the invention is nevertheless described herein in as detail as possible. It will be apparent to those skilled in the art that the materials and methods of operation used in the present invention are well within the skill of the art, provided that they are not specifically illustrated.
Example 1
This example illustrates the structure of a transmission electron microscope sample rod system according to the present invention.
The invention relates to a transmission electron microscope sample rod system with ultra-fast time resolution spectral capability, as shown in figure 1, comprising: the device comprises a femtosecond laser 1, a beam expanding collimator 2, a first turnover reflector 3, a dispersion compensation element 4, a second turnover reflector 5, a reflector 6, a first light splitting prism 7, a microscope objective 8, a sample rod 9 provided with an optical fiber beam, a white light source 10, a first lens 11, a second light splitting prism 12, a second lens 13, a third turnover reflector 14, an image acquisition device 15, an optical filter 16, a spectrometer 17, a third lens 18, a time-dependent single photon counter 19 and an auxiliary optical imaging system 20; the detailed information of the sample rod portion with the fiber bundle mounted thereon is shown in fig. 2 and includes a front end head 21, a sample carrying clamp 22, a first small-caliber lens 23, a second small-caliber lens 24, a fiber bundle 25 mounted on the sample rod, a piezoelectric ceramic tube 26, a centering device 27, and a differential micrometer head 28.
As shown in FIG. 1, the femtosecond pulse light emitted from a femtosecond laser 1 (wavelength 800nm) is first converted into quasi-parallel light by a beam expanding collimator 2, then reflected by a first turning mirror 3 and irradiated to a dispersion compensation element 4 (including a parallel-arranged grating pair and a mirror) to widen the pulse, the pulse light which is reversely widened is firstly reflected by a second turning mirror 5, the propagation direction of the optical fiber is the same as that before reflection of the first turnover mirror 3, and then the optical fiber is reflected by the first reflection mirror 6 and the first beam splitter prism 7, focused on the near end of the optical fiber bundle 25 arranged on the sample rod through the microscope objective 8, wherein the near end of the optical fiber bundle is fixed on a three-dimensional displacement table, the pulse light is firstly collected through a microscope objective 8 after being reflected by the end face, then, after being reflected by the first beam splitter prism 7 and the second beam splitter prism 12, the reflected light finally reaches the target surface of the collecting device 15 through the second lens 1; in the white light imaging system, white light emitted by a white light source 10 sequentially passes through a first lens 11, a second beam splitter prism 12 and a second beam splitter prism 7, then reaches a back focal plane of a microscope objective 8, is focused by the microscope objective 8 and then irradiates the near end of an optical fiber bundle 25 arranged on a sample rod, has the same path as the path of the pulse light reflected by the end face, and finally reaches the target surface of an image acquisition device 15 after passing through the microscope objective 8, the first beam splitter prism 7, the second beam splitter prism 12 and the second lens 13; when only a white light source is used for illumination, the proximal end of the optical fiber bundle 25 mounted on the sample rod is adjusted in the z direction to enable the end face to be clearly imaged on the target surface of the image acquisition device 15 (as shown in fig. 3 (a)), then femtosecond pulse light is focused on the proximal end of the optical fiber bundle, the proximal end of the optical fiber bundle 25 mounted on the sample rod is adjusted in the xy direction, and a corresponding reflection intensity image is recorded in real time through the image acquisition device 15 (as shown in fig. 3 (b)), so that the pulse light is coupled into a single fiber core of the optical fiber bundle (as shown in an insert drawing of fig. 3 (b)), and the single fiber core coupled into the pulse light is equivalent to a point light source after the distal end of the. In order to achieve focusing of a spot of size less than 2 μm on the sample-holding jig 22, the beam after exiting at the distal end of the fiber passes through a beam splitter composed of a second small-caliber lens 24 (diameter: 6.25mm, focal length: 15mm, numerical aperture: 0.21) and a first small-caliber lens 23 (diameter: 6.25mm, focal length: 7.5mm, numerical aperture: 0.42) according to the parameters of the fiber bundle 25 mounted on the sample rod used (core diameter: about 3.5 μm and numerical aperture: about 0.35): 1, 4f scaling system. In the present embodiment, when the guaranteed numerical aperture of the first small-caliber lens 23 is not smaller than the numerical aperture of the used optical fiber and the laser utilization efficiency is maximized, according to the commercially available small-caliber lens, 2: the 4f scaling system of 1 achieves a focused spot size of less than 2 μm. . When the front end 21 of the sample shaft 9 and the sample-carrying jig 22 were not mounted, the focused light spot generated could be observed by the auxiliary optical imaging system 20 (as shown in FIG. 4 (a)) and the spot size could be measured to be 1.6 μm (as shown in FIG. 4 (b)) based on the intensity distribution of the focused light spot in the horizontal direction. The proximal end of the fiber bundle 25 mounted on the sample rod is adjusted in the xy direction to couple the pulse light into different fiber cores, and the pulse light is emitted from the corresponding fiber cores at the distal end of the fiber bundle, so that the scanning of the focused light spot on the sample surface can be realized, the scanning can be recorded by the auxiliary optical imaging system 20 (as shown in fig. 5), and the accurate scanning of the focused light spot can be realized by the piezoelectric ceramic tube 26.
In addition, the commercial autocorrelator can also be used for representing the pulse width of the focused light spot, when the femtosecond pulse light is directly coupled into a single fiber core without a dispersion compensation element, the pulse width of the pulse light emitted from the far end of the optical fiber bundle is measured to be 1.96ps (as shown in fig. 6 (a)), and when the pulse light which is reversely broadened by the dispersion compensation element is coupled into the single fiber core, the pulse width is measured to be 300fs (as shown in fig. 6 (b)) when the pulse light output power is 3 mW.
Further, a front end 21 and a sample bearing clamp 22 are mounted on a sample rod 9, a tungsten needle point coated with quantum dots is selected as the sample bearing clamp 22, the front end 21 is adjusted to focus the compensated pulsed light on the tungsten needle point, an excited fluorescent signal is focused through a first small-caliber lens 23 and a second small-caliber lens 24 and then coupled into an optical fiber bundle mounted on the sample rod, a signal emitted from the near end of the optical fiber bundle is collected through a microscope objective 8, then is reflected through a first light splitting prism 7 and a second light splitting prism 12 in sequence, is reflected through a third turning reflector 14 and then irradiates onto an optical filter 16, and finally is coupled into a spectrometer through multimode optical fibers to detect and record the fluorescent signal. According to the fluorescence signal intensity recorded by the spectrometer, the emergent pulse light is just focused on the quantum dots by adjusting the near end of the optical fiber bundle, the piezoelectric ceramic tube 26 and the differential micrometer head 27, the collected fluorescence signal is strongest at the moment (as shown in fig. 7 (a)), and then the fluorescence signal enters the time-dependent single photon counter 19 after being focused by the lens by adjusting the turnover reflecting mirror in the spectrometer, so that the fluorescence life detection is realized (as shown in fig. 7 (b)).
Example 2
This example illustrates the method of using a transmission electron microscope sample rod system in accordance with the present invention.
The specific implementation steps are as follows:
step 1: the horizontal polarized light emitted by the femtosecond laser is firstly converted into quasi-parallel light by the beam expanding collimator 2;
step 2: generating negative group velocity dispersion by the quasi-parallel femtosecond pulse light obtained in the step (1) through a grating pair;
and step 3: focusing the pulse light which is widened due to the negative group velocity dispersion obtained in the step (2) on the near end of the optical fiber bundle arranged in the sample rod through a microscope objective 8;
and 4, step 4: irradiating the whole end face of the near end of the optical fiber bundle by a white light source 10 through a lens and a microscope objective 8;
and 5: adjusting the near end of the optical fiber bundle in the z direction, and imaging the white light reflected in the step (4) to an image acquisition device;
step 6: adjusting the near end of the optical fiber bundle in the xy direction by means of the end surface reflection image of the optical fiber bundle obtained in the step 5, and coupling the pulse light focused in the step 3 into a certain single fiber core of the optical fiber bundle;
and 7: and (3) pulsed light which is coupled into the corresponding step 6 and is emitted from the other end of the single fiber core is respectively emitted through 2 consisting of a second small-caliber lens 24 and a first small-caliber lens 23 with focal lengths of 15mm and 7.5 mm: 1, focusing a 4f zooming system on a tungsten needle point with quantum dots on the surface;
and 8: repeating the step 6 or adjusting the pulsed light to focus on the position of the tungsten needle tip through the piezoelectric ceramic tube, and simultaneously measuring the two-photon fluorescence intensity of the quantum dot in real time by using a spectrometer to optimize the position of a focused light spot;
and step 9: adjusting the focusing light spots of the optimized focusing pulse light obtained in the step 8 in the z direction of a differential micrometer head 28, measuring the fluorescence intensity in real time by using a spectrometer 17, and repeating the step 8 to enable the spectral intensity to reach the maximum;
step 10: the optimized spectra are introduced into a time-dependent single photon counter 19 to measure the ultrafast fluorescence lifetime.
Although the present invention has been described to a certain extent, it is apparent that appropriate changes in the respective conditions may be made without departing from the spirit and scope of the present invention. It is to be understood that the invention is not limited to the described embodiments, but is to be accorded the scope consistent with the claims, including equivalents of each element described.

Claims (10)

1. A tem sample rod system capable of ultrafast time resolved spectroscopy, the tem sample rod system comprising: the system comprises a laser, a beam expanding collimator, a first turnover reflector, a dispersion compensation element, a second turnover reflector, a first light splitting prism, a microscope objective, a sample rod provided with an optical fiber and a 4f zooming system, a light source, a first lens, a second light splitting prism, a second lens, a third turnover reflector, an image acquisition device, an optical filter, a spectrometer, a third lens, a time-dependent single photon counter and an auxiliary optical imaging system;
the 4f zooming system consists of two small-caliber lenses.
2. The system of claim 1, wherein the aperture of the small-aperture lens of the 4f zoom system is 2mm to 8mm, preferably 5mm to 6.25 mm.
3. The system of claim 1 or 2, wherein the laser is a femtosecond laser;
preferably, the laser is selected from a solid femtosecond laser or a fiber femtosecond laser;
most preferably, the laser is a solid state femtosecond laser.
4. The system of any one of claims 1 to 3, wherein the optical fiber in the sample rod with the optical fiber and 4f zoom system installed is a single mode or few mode fiber at the operating wavelength;
preferably, the optical fiber is a fiber bundle consisting of single mode or few mode fibers.
5. The system according to any one of claims 1 to 4, wherein the dispersion compensating element is selected from one or more of: grating pair, prism pair, chirp reflector, programmable phase compensation system and acousto-optic programmable dispersion filter; preferably a grating pair.
6. The system of any one of claims 1 to 5, wherein the sample rod with the fiber and 4f zoom system mounted thereto further comprises:
the near end of the optical fiber is fixed on the three-dimensional displacement table;
a front end;
a sample-carrying clamp;
the piezoelectric ceramic tube is used for accurately adjusting the position of a focusing light spot in a plane perpendicular to the light propagation direction;
a centering device; and
and a differential micrometer head.
7. The system of claim 6, wherein the sample support fixture is selected from one or more of: a tungsten needle tip, a gold needle tip, and a micro-grid placed obliquely;
preferably a tungsten tip.
8. The system according to any one of claims 1 to 7, wherein the sample rod with the optical fiber and 4f zoom system mounted thereon emits focused pulsed light.
9. The system of any one of claims 1 to 8, wherein the light source is selected from a white light source or a light emitting diode.
10. A transmission electron microscope comprising a transmission electron microscope sample rod system with ultrafast time resolved spectroscopy capability according to any one of claims 1 to 9.
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