CN112229804A - Non-coaxial transmission type ultrafast transient absorption system with temperature field regulation and control function and measurement method - Google Patents
Non-coaxial transmission type ultrafast transient absorption system with temperature field regulation and control function and measurement method Download PDFInfo
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- G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
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- G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
- G01J3/28—Investigating the spectrum
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Abstract
The invention relates to a non-coaxial transmission type transient absorption measurement system with a temperature field regulation function and a method thereof, belonging to the technical field of optical detection. The invention utilizes FPGA technology to synchronize the processes of femtosecond laser emitting laser pulse, chopper modulation laser pulse frequency, fiber spectrometer collection and the like, and the method can effectively improve the real-time reliability of the test result of the measurement system and the signal-to-noise ratio of the system; meanwhile, the transient absorption device and the confocal microscopic imaging and temperature field regulating device are integrated together, so that the transient absorption spectrum information of the microscopic material at different temperatures can be tested, and the relaxation dynamics of the optically-excited carrier of the material at different temperatures can be obtained. The system adopts automatic measurement and has the characteristics of high speed, high efficiency and sensitivity.
Description
Technical Field
The invention belongs to the technical field of optical detection, and particularly relates to a non-coaxial transmission type ultrafast transient absorption system with a temperature field regulation function and a measurement method.
Background
The transient absorption spectrum device is an important scientific instrument for researching dynamic information of a material excited state, and compared with a transient fluorescence spectrum device, the transient absorption spectrum device has the technical advantages that: even if the sample does not emit light, the excited state kinetics of the sample can be researched, so that the sample has a position which is difficult to replace in researching the kinetics of the non-radiative recombination process. The system uses pump light as excitation, a large number of photon-generated carriers are generated in a sample, the carrier distribution in a material is influenced along with the processes of generating band filling, band gap reforming, defect state filling, intersystem crossing and the like, so that the absorption of super-continuum spectrum detection light is influenced, the service life of the carriers in the material, charge energy transfer, multi-body interaction effect, defect capture process and the like can be revealed through processing the absorption and attenuation information of the detection light, and therefore, the system has important application in the fields of materials, physics, chemistry, biology, medicine and the like, and the application fields thereof comprise: (1) the photovoltaic device and the luminescent device based on the optical functional material need excited state kinetic information in a transient absorption spectrum as guidance; (2) excited state physical, lattice relaxation kinetics and chemical reaction kinetics information of the material; (3) research and development of novel nano materials; (4) biophysical and photochemical processes of biological proteins, etc.
The transient absorption spectrum measurement technology is very important and develops rapidly at present, but the following problems exist: (1) only some samples with stronger absorption signals can be selected for the sample to be detected, and the signal of the sample with weaker signal cannot be accurately detected due to the poorer signal-to-noise ratio of the system. (2) The transient absorption spectrum technology based on the ultrafast fiber spectrometer as a spectrum acquisition device does not well process background noise, so that the signal authenticity is seriously influenced. (3) With the emergence of new materials, in order to better explore the application potential of new materials, deep understanding of the physical properties of new materials is needed, and especially, the influence of temperature on the properties of new materials needs to be known before application, so that temperature variation tests are needed to research the properties of materials and provide theoretical experimental guidance for performance optimization. The solution of these problems requires further development of transient absorption measurement technology, increase of temperature field regulation function, and revealing of physical properties of the research material under extreme temperature conditions.
Disclosure of Invention
The invention mainly solves the technical problems of the existing system and provides a novel non-coaxial transmission type synchronous ultrafast transient absorption spectrum measuring system with a temperature field regulation and control function. The system is provided with a temperature changing module, and a sample is placed in a temperature changing cavity, so that the system has a temperature field regulation function, and dynamic information of the sample at different temperatures is obtained. This system uses the fiber optic spectrometer, in order to guarantee the authenticity of the system acquisition signal based on the fiber optic spectrometer, has used the FPGA board to have synchronized processes such as laser emission light pulse, chopper modulation pumping optical frequency and ultrafast fiber optic spectrometer collection for the fiber optic spectrometer can gather the detection light spectral information under two kinds of states in real time: the real-time authenticity of the test result is ensured by the detection light spectrum information under the action of the pump pulse and the detection light spectrum information under the action of the non-pump pulse; meanwhile, 1KHz pulse detection light spectrum information can be well collected, so that the test efficiency is greatly improved, and the test time is reduced; in addition, the modulation frequency of the chopper can be adjusted, so that the frequency of the pump light becomes one half, one quarter or one eighth of the 1KHz frequency of the optical pulse of the original laser, the integration time of weak signals is prolonged, and the signal-to-noise ratio of the system is increased.
In order to achieve the above purpose of the invention, the following technical scheme is adopted:
a non-coaxial transmission type novel synchronous ultrafast transient absorption spectrum measuring system with a temperature field regulation function comprises a femtosecond pulse laser, a first full-reflecting mirror, a second full-reflecting mirror, a first spectroscope, a first convex lens, a nonlinear frequency doubling crystal, a second convex lens, a first optical filter, a first Glan Taylor prism, a third full-reflecting mirror, a chopper, a fourth full-reflecting mirror, a stepping motor electric translation table, a hollow retroreflector, a fifth full-reflecting mirror, a first second quarter wave plate, a second Glan Taylor prism, a fourth convex lens, a nonlinear white light generation crystal, a first concave mirror, a first optical filter, a sixth full-reflecting mirror, a long-working-distance objective lens, a temperature-variable cavity, a sample, a fifth convex lens, a third Glan Taylor prism, a sixth convex lens, an optical fiber coupling module, an optical fiber spectrometer, an FPGA plate, a computer, a CCD receiver, a white light source, a third convex lens, a second filter, a third filter, A partition board, a second spectroscope and a third spectroscope. The pulse laser generated along the femtosecond pulse laser sequentially passes through the first total reflection mirror and the second total reflection mirror and is divided into two beams by the first beam splitter, wherein one beam is reflected light, and the other beam is transmitted light; after the reflected light is converged to the nonlinear frequency doubling crystal through the first convex lens, the frequency doubling light collimated by the second convex lens is a parallel light beam which sequentially passes through the first optical filter, the first Glan Taylor prism, the third total reflection mirror, the chopper, the fourth total reflection mirror and the third convex lens to be converged to a sample in the temperature changing cavity, and the pump light transmitted by the sample is blocked by the clapboard; the transmission light is converged to the nonlinear white light generation crystal by the fourth convex lens through the stepping motor electric translation stage, the hollow retroreflector, the fifth total reflection mirror, the first half wave plate and the second Glan Taylor prism to generate a supercontinuum which is used as detection light; the detection light is focused on a sample in the temperature-changing cavity through the long working distance objective lens through the first concave mirror, the first optical filter and the sixth total reflection mirror; the pump light spot and the detection light spot are overlapped at the sample through a sample visualization module;
the detection light penetrates through the sample, then passes through a fifth convex lens, a third Glan Taylor prism and a sixth convex lens, is coupled into the optical fiber by the optical fiber coupling module, and finally is synchronously triggered by the FPGA plate to collect optical signals by the optical fiber spectrometer, the optical fiber spectrometer converts the spectral information into numerical signals, and the computer reads the electrical signals of the spectral information, and the transient absorption spectral information is obtained after processing.
The sample visualization module is composed of a white light source, a movable second spectroscope, a long-working-distance microscope objective, a movable third spectroscope and a CCD detector. In the process of visualizing the sample, the position of the movable second spectroscope is precisely moved, white light emitted by a white light source is guided to sequentially pass through the movable third spectroscope and the microscope objective with long working distance, and the surface of the sample in the temperature-variable cavity is illuminated; after the white light reflected by the surface of the sample is collected by the microscope objective with long working distance, the collected white light reflected by the sample is guided to the CCD detector by the movable third beam splitter to obtain an image of the surface of the sample, and the distance between the sample and the microscope objective with long working distance is adjusted to obtain a clear image of the surface of the sample.
The nonlinear white light generation crystal comprises a sapphire crystal, a calcium fluoride crystal and a YAG crystal, and the laser pulse of 1040nm is focused by a fourth convex lens to excite the nonlinear white light crystal and generate a detection supercontinuum in the range of 350nm to 1200 nm.
The FPGA board is respectively connected with the femtosecond pulse laser and the chopper and is used for controlling the chopper to synchronously modulate the frequency of the pump light, the frequency of the pump light can be modulated into one half, one quarter, one sixth and one eighth of the frequency of the femtosecond pulse laser, and the chopper works in an external trigger mode to improve the detection capability of the system on weak signals.
The FPGA board is respectively connected with the femtosecond laser and the optical fiber spectrometer and is used for controlling the femtosecond pulses emitted by the femtosecond laser to be synchronous with the optical fiber spectrometer and collecting the detection light spectrum information with the pumping light effect and the detection light spectrum information without the pumping light effect.
The first Glan Taylor prism is used for adjusting the polarization state of the pump light, and the second Glan Taylor prism is used for adjusting the polarization state of the probe light and ensuring that the polarization state of the pump light is vertical to that of the probe light. The third Glan Taylor prism adjusts the polarization state of the detection light after penetrating through the sample, and the polarization state of the detection light is perpendicular to the polarization state of the pump light, so that the interference of the pump light on the collection of the spectrum information of the detection light by the ultrafast fiber spectrometer is reduced.
The intensity ratio of the reflected light intensity to the transmitted light intensity of the first spectroscope is 8:2, so that the intensity ratio of the pump light and the detection light after light splitting reaches 8: 2. The intensity ratio of the reflected light intensity to the transmitted light intensity of the movable second spectroscope is 5.5. The intensity ratio of the reflected light intensity to the transmitted light intensity of the movable third beam splitter is 5.5.
The temperature changing module comprises a precise three-dimensional adjusting frame, a temperature changing cavity, a temperature control instrument, a liquid nitrogen bottle and a vacuum pump. The precise three-dimensional adjusting frame has an X, Y, Z direction adjusting function, the adjusting precision is 1 mu m, the measuring range is 20cm, and the precise three-dimensional adjusting frame is used for loading a sample temperature changing cavity and adjusting the position. The vacuum pump keeps the vacuum degree of the sample temperature changing cavity. The temperature control instrument is used for adjusting the temperature of the sample in the sample temperature changing cavity, the range of the temperature control instrument is 3.5K to 475K, and the control precision is 0.05K.
The optical fiber coupling system consists of an achromatic convex mirror and a precise five-dimensional adjusting frame.
The step motor electric translation stage and the hollow retroreflector form a time delay line, the step motor electric translation stage is connected with a computer through a USB (universal serial bus) line, the position of the step motor electric translation stage is automatically controlled by using compiled system control software, the difference delta L of the space optical path between the pump light and the probe light is precisely controlled, and the difference delta L of the space optical path between the pump light and the probe light is utilized
And further controls the time delay delta t between the pump light and the probe light. Where c is the speed of light: 3x108m/s. The minimum step length of the precise translation of the stepping motor is 0.1 mu m.
The center wavelength of the femtosecond pulse laser is 1040nm, and the repetition frequency is 1 KHz. By using the combination of the first convex lens, the first frequency doubling crystal and the second convex lens, the center wavelength of the femtosecond pulse laser can be 1040nm and the frequency doubling can be 520nm, and the femtosecond pulse laser can be used as pump light to excite a sample.
The controller of the femtosecond pulse laser is connected with the FPGA board, the controller of the chopper and the fiber spectrometer and is controlled by the computer to realize communication with each other.
The method for measuring the transient absorption spectrum of the sample to be measured by using the non-coaxial transmission type transient absorption measuring system with the temperature field regulation function as claimed in claim 1 is characterized by comprising the following two parts:
a first part: the sample is first placed in a temperature-variable chamber and the sample is fixed. And finally, the vacuum degree in the variable temperature cavity of the vacuum pump is operated to meet the test requirement, and the temperature of the sample is controlled by using the temperature controller to perform transient absorption spectrum test.
A second part: the transient absorption spectrum test of a sample at a specific temperature comprises the following steps:
setting initialization parameters of a stepping motor translation table and an optical fiber spectrometer, wherein the initialization parameters comprise the step motor translation tableAcceleration, step length delta L, and starting time point T of delay line time0And an end time point TeOptical path position Z of pump light and probe light0Etc.; setting working parameters of the fiber spectrometer: initial wavelength (lambda) of the probe spectrum1) And end wavelength (λ)e) Integration time, trigger mode.
Secondly, stable supercontinuum detection light is obtained. Through the cooperative adjustment of the first one-half wave plate and the second Glan Taylor mirror, the adjustment of the aspects of the beam size, the light intensity, the polarization direction and the like is carried out on the laser before the laser enters the nonlinear white light generation crystal, so that the nonlinear white light crystal generates a stable and smooth supercontinuum under the excitation of base frequency light of 1040 nm.
And thirdly, adjusting the efficiency of the detection light coupling optical fiber after the sample is penetrated. And precisely adjusting the optical fiber coupling frame to enable the intensity of the supercontinuum displayed in the computer control software to be strongest.
And fourthly, adjusting the coincidence degree of the pump light spot and the detection light spot on the sample. The working point of the translation table of the stepping motor is set to be Z1And satisfy Z1Greater than Z0The detection function in the control program is turned off. Clicking an optimization function, precisely adjusting a knob of X, Y of the fourth all-mirror, observing the change of the intensity of the transient absorption spectrum displayed by the computer control software, and optimizing the position of a pump light spot on a sample at X, Y until the intensity of the transient absorption spectrum displayed by the computer control software is maximum (-delta T/T).
Testing transient absorption spectrum-delta T/T (lambda) at set temperature1,λ2,…,λe；t1,t2,…te). Starting the test function, moving the step motor electric translation table to the initial position set in the step II, and collecting the delay time t at the position0Lower transient spectral information- Δ T/T (λ)1,λ2,…,λe；t0) And displaying and storing the data in the computer control program. Then the step length delta L set in the step II is taken as the moving amount delta L of the electric translation table of the stepping motor moving to the next position, and the computer control program automatically updates the electric translation table of the stepping motorMoving the translation stage to obtain a new delay time t1＝t0+ 2. delta.L/c, and t is collected1Time-delayed transient dynamics information- Δ T/T (λ)1,λ2,…,λe；t1). The computer control program automatically updates the position of the electric translation table of the stepping motor by the step length delta L set in the step II to obtain new delay time ti(i＝0,1,2,3,4,5,6,…,te) Up to ti＝teEnding the collection and saving the test data-delta T/T (lambda)1,λ2,…,λe；t1,t2,…te)。
Processing transient absorption spectrum data. The transient absorption spectrum acquired by the step (c) is a two-dimensional intensity distribution diagram-delta T/T (lambda)1,λ2,…,λe；t1,t2,…te) At a wavelength λiAs abscissa, time delay tiIs the ordinate. Kinetics for a certain wavelength- Δ T/T (λ)i；t1,t2,…te) The lifetime of each relaxation process can be found using exponential fitting. The fitting formula is
Wherein n is the number of fitting indexes, aiHas a lifetime of tauiThe weight of the component.
The invention has the advantages that: firstly, a pumping light and detection light non-coaxial type excitation sample scheme is adopted, the detection light spectrum range collected by the optical fiber spectrometer is ensured not to be influenced by the pumping light, and the defect that the spectrum discontinuity is generated due to the influence of the pumping light on the detection light spectrum range collected by the spectrometer in the pumping light and detection light coaxial type excitation sample scheme is avoided; secondly, the system is provided with a temperature changing cavity, and a sample is placed in the temperature changing cavity, so that the dynamic information of the sample at different temperatures can be obtained; in addition, the system adopts the optical fiber spectrometer, and the FPGA board is used for synchronizing the processes of transmitting light pulses by the femtosecond pulse laser, modulating the frequency of the pump light by the chopper, collecting by the optical fiber spectrometer and the like, so that the optical fiber spectrometer can collect the spectrum information of the detection light in two states in real time: the detection light spectrum information under the action of the pump pulse and the detection light spectrum information under the action of the non-pump pulse guarantee the real-time authenticity of the test result, and meanwhile, the 1KHz pulse detection light spectrum information can be well collected, so that the test efficiency is greatly improved, and the test time is shortened; in addition, the modulation frequency of the chopper can be adjusted, so that the frequency of the pump light becomes one half, one quarter, one eighth and the like of the 1KHz frequency of the optical pulse of the original laser, the integration time of weak signals is increased, and the signal-to-noise ratio of the system is improved.
Drawings
Fig. 1 is a schematic diagram of the optical path of the present invention.
Fig. 2 is a schematic diagram of a temperature changing chamber in a conventional temperature changing apparatus.
FIG. 3 is a transient absorption spectrum of a sample of material in a temperature changing chamber of a temperature changing apparatus at different temperatures. FIG. 3 (left) is a graph of transient absorption spectrum at 275K temperature, and FIG. 3 (right) is information of relaxation kinetics at a wavelength of 617 nm.
FIG. 4 is a graph of single-layer WS at room temperature in a temperature changing apparatus2Transient absorption spectrum of the sample.
FIG. 5 is an operating interface of the automation control software of the non-coaxial transmission-type ultrafast transient absorption system with temperature field regulation function.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
As shown in fig. 1, one pulsed laser beam generated by a femtosecond pulse laser 1 passes through a first holomirror 2 and a second holomirror 3, and is then split into two pulsed light beams by a first beam splitter 4: one of the beams is reflected light, and the other beam is transmitted light. After the reflected light is converged to the nonlinear frequency doubling crystal 6 through the first convex lens 5, the frequency doubling light collimated by the second convex lens 7 is a parallel light beam, the parallel light beam passes through the first optical filter 8, the first Glan Taylor prism 9, the third holophote 10, the chopper 11 and the fourth holophote 12 and is converged to the sample 25 in the temperature changing cavity 24 through the third convex lens 36, and the pump light emitted after transmitting the sample is blocked by the clapboard 37. The light transmitted by the first spectroscope 4 passes through a time delay line (a stepping motor electric translation stage 13, a hollow retroreflector 14), a fifth total reflection mirror 15, a first half wave plate 16 and a second Glan Taylor prism 17, and is converged to a nonlinear white light generation crystal 19 by a fourth convex lens 18 to generate a supercontinuum as detection light. Then, the supercontinuum detection light is focused on a sample 25 in a temperature-changing cavity 24 through a first concave mirror 20, a first optical filter 21 and a sixth total reflection mirror 22 and a long working distance objective lens 23, and the fourth total reflection mirror 12 is adjusted to enable the pump light spot and the detection light spot to coincide at the sample 25. After the supercontinuum detection light penetrates through a sample 25, the detection light is coupled into an optical fiber 30 through a fifth convex lens 26, a third Glan Taylor prism 27 and a sixth convex lens 28 through an optical fiber coupling module 29, an FPGA (field programmable gate array) board 32 synchronously triggers an optical fiber spectrometer 31 to collect optical signals, the optical fiber spectrometer 31 converts spectral information into numerical signals, and a computer 33 reads electric signals of the spectral information to obtain transient absorption spectral information.
As shown in fig. 1, the sample visualization module is composed of a white light source 35, a movable second spectroscope 38, a long-working-distance microscope objective 23, a movable third spectroscope 39 and a CCD detector 34. In the process of sample visualization, the position of the movable second spectroscope 38 is precisely moved, white light emitted by the white light source 35 is guided to sequentially pass through the movable third spectroscope 39 and the microscope objective 23 with long working distance, and the surface of the sample 25 in the temperature-variable cavity 24 is illuminated; after the white light reflected by the surface of the sample 25 is collected by the microscope objective 23 with long working distance, the collected white light reflected by the sample is guided to the CCD detector 34 by the movable third beam splitter 39, an image of the surface of the sample 25 is obtained, and the distance between the sample 25 and the microscope objective 23 with long working distance is adjusted to obtain a clear image of the surface of the sample.
As shown in fig. 1, the femtosecond pulse laser 1 emits a light pulse signal and simultaneously outputs a digital pulse signal, the digital pulse signal is input to the FPGA board 32 for logic processing, the processed digital signal is output to trigger the chopper 11 to synchronously modulate the frequency of the pump light, the frequency of the pump light can be modulated into one half, one quarter or one eighth of the frequency of the femtosecond laser according to the test requirement, the integration time of the fiber spectrometer is increased, and the detection capability of the system on weak signals is improved.
As shown in fig. 1, the femtosecond pulse laser 1 emits a light pulse signal and simultaneously outputs a digital pulse signal, the digital pulse signal is input to the FPGA board 32 for logic processing, and the processed digital signal is output to trigger the fiber spectrometer 30 to synchronously acquire probe light spectrum information, so as to obtain probe light spectrum information under the action of a pump pulse and probe light spectrum information under the action of no pump pulse.
As shown in fig. 1, the quality of the white light produced by the nonlinear white light generating crystal directly determines the reliability of the measurement data in the transient absorption spectroscopy test. The first and second quarter-wave plates 16 and 17 are used to adjust the beam size, light intensity, polarization direction, etc. of the laser light before entering the nonlinear white light generating crystal, so that the YAG crystal can generate stable and smooth super-continuum spectrum under the excitation of 1040nm fundamental frequency light, and therefore, the YAG crystal is preferably used as the nonlinear white light generating crystal.
As shown in FIG. 1, the femtosecond laser 1 generates femtosecond pulse laser with an output center wavelength of 1040nm and a repetition frequency of 1KHz, and the laser pulse center wavelength after frequency multiplication becomes 520 nm.
As shown in FIG. 1, a time delay line is composed of a stepping motor electric translation stage 13 and a hollow retroreflector 14, the hollow retroreflector 14 is used for keeping incident light and emergent light parallel, and finally, the precise movement is carried out according to the setting requirement under the control of an automatic control program of a computer 33.
As shown in fig. 1, for the first beam splitter 4, the transient absorption spectrum acquisition needs to be achieved by pumping and detecting two short pulse beams, so that the laser generated from the same femtosecond pulse laser needs to be split into two beams. In the system, a first spectroscope 4 with a pump detection energy ratio of 8:2 is empirically selected, so that the intensity ratio of the pump light and the detection light after light splitting reaches 8: 2. The main function of the spectroscope is to make the light intensity of the pump light far stronger than that of the detection light, so that when the sample is excited, the excitation of the detection light to the sample can be ignored, and only the excitation of the pump light to the sample is considered. To observe the test sample, the splitting ratio of the second beam splitter 34 to the third beam splitter 33 was 5: 5.
The method for measuring the transient absorption spectrum of the sample to be measured by using the non-coaxial transmission type transient absorption measurement system with the temperature varying test function as claimed in claim 1, is characterized by comprising the following two parts:
a first part: the sample is first placed in a temperature-variable chamber and the sample is fixed. And finally, the vacuum degree in the variable temperature cavity of the vacuum pump is operated to meet the test requirement, and the temperature of the sample is controlled by using the temperature controller to perform transient absorption spectrum test.
A second part: the transient absorption spectrum test of a sample at a specific temperature comprises the following steps:
hardware interconnection communication in the non-coaxial transmission type transient absorption measurement system with the temperature field regulation function is achieved. According to the measurement requirement, the controller of the femtosecond pulse laser is connected with the FPGA board, the controller of the chopper and the fiber spectrometer, and the communication between the FPGA board, the chopper controller and the fiber spectrometer is realized under the control of the computer.
And secondly, setting and initializing parameters of the stepping motor translation table and the optical fiber spectrometer in a control program. Setting the acceleration, step length delta L and the starting time point T of the time of a delay line of a translation stage of a stepping motor0And an end time point TeOptical path position Z of pump light and probe light0Etc.; setting working parameters of the fiber spectrometer: initial wavelength (lambda) of the probe spectrum1) And end wavelength (λ)e) Integration time, trigger mode.
And thirdly, obtaining stable supercontinuum detection light. Through the cooperative adjustment of the first one-half wave plate and the second Glan Taylor mirror, the adjustment of the aspects of the beam size, the light intensity, the polarization direction and the like is carried out on the laser before the laser enters the nonlinear white light generation crystal, so that the nonlinear white light crystal can generate a stable and smooth supercontinuum under the excitation of base frequency light of 1040 nm. And clicking a detection function in the control program to monitor the range and stability of the super-continuum spectrum in real time.
Adjusting the efficiency of the probe light after transmitting the sample to be coupled with the optical fiber. And precisely adjusting the optical fiber coupling frame to enable the intensity of the supercontinuum displayed in the computer control software to be strongest.
Regulating the coincidence degree of the pump light spot and the detection light spot on the sample. The working point of the translation table of the stepping motor is set to be Z1And satisfy Z1Greater than Z0The detection function in the control program is turned off. Clicking an optimization function, precisely adjusting a knob of X, Y of the fourth holophote, observing the change of the intensity of the transient absorption spectrum displayed by the computer control software, and optimizing the position of a pump light spot on a sample at X, Y until the intensity (-delta T/T) of the transient absorption spectrum displayed by the computer control software is maximum, thereby canceling the optimization function.
Sixthly, testing the transient absorption spectrum-delta T/T (lambda) at the set temperature1,λ2,…,λe；t1,t2,…te). Starting the test function, moving the step motor electric translation stage to the set initial position, and collecting the delay time t at the position0Lower transient spectral information- Δ T/T (λ)1,λ2,…,λe；t0) And displaying and storing the data in the computer control program. Then the step length delta L set in the step II is taken as the moving amount delta L of the electric translation table of the stepping motor moving to the next position, the position of the electric translation table of the stepping motor is automatically updated in the computer control program, and the new delay time t is obtained1＝t0+ 2. delta.L/c, and t is collected1Time-delayed transient dynamics information- Δ T/T (λ)1,λ2,…,λe；t1). The computer control program automatically updates the position of the electric translation table of the stepping motor by the step length delta L set in the step II to obtain new delay time ti(i＝0,1,2,3,4,5,6,…,te) Up to ti＝teEnding the collection and saving the test data-delta T/T (lambda)1,λ2,…,λe；t1,t2,…te)。
And (9) processing transient absorption spectrum data. The transient absorption spectrum acquired by the step (c) is a two-dimensional intensity distribution diagram-delta T/T (lambda)1,λ2,…,λe；t1,t2,…te) At a wavelength λiAs abscissa, time delay tiIs the ordinate. Kinetics for a certain wavelength- Δ T/T (λ)i；t1,t2,…te) The lifetime of each relaxation process can be found using exponential fitting. The fitting formula is
Wherein n is the number of fitting indexes, aiHas a lifetime of tauiThe weight of the component.
Claims (9)
1. A non-coaxial transmission type transient absorption measurement system with a temperature field regulation and control function is characterized in that: the device comprises a femtosecond pulse laser (1), a first total reflection mirror (2), a second total reflection mirror (3), a first spectroscope (4), a first convex lens (5), a nonlinear frequency doubling crystal (6), a second convex lens (7), a first optical filter (8), a first Glan-Taylor prism (9), a third total reflection mirror (10), a chopper (11), a fourth total reflection mirror (12), a stepping motor electric translation table (13), a hollow retroreflector (14), a fifth total reflection mirror (15), a first one-half wave plate (16), a second Glan-Taylor prism (17), a fourth convex lens (18), a nonlinear white light generation crystal (19), a first concave mirror (20), a first optical filter (21), a sixth total reflection mirror (22), a long working distance objective (23), a variable temperature cavity (24), a sample (25), a fifth convex lens (26), a third Glan-Taylor prism (27), The device comprises a sixth convex lens (28), an optical fiber coupling module (29), an optical fiber (30), an optical fiber spectrometer (31), an FPGA (32) board, a computer (33), a CCD receiver (34), a white light source (35), a third convex lens (36), a partition plate (37), a second beam splitter (38) and a third beam splitter (39);
pulse laser generated along the femtosecond pulse laser (1) sequentially passes through the first total reflection mirror (2) and the second total reflection mirror (3) and is divided into two beams by the first beam splitter (4), wherein one beam is reflected light, and the other beam is transmitted light; after the reflected light is converged to a nonlinear frequency doubling crystal (6) through a first convex lens (5), the frequency doubling light collimated by a second convex lens (7) is a parallel light beam which sequentially passes through a first optical filter (8), a first Glan Taylor prism (9), a third total reflection mirror (10), a chopper (11), a fourth total reflection mirror (12) and a sample (25) in a temperature changing cavity (24) through a third convex lens (36), and the pump light transmitted by the sample is blocked by a clapboard (37); the transmission light is converged to a nonlinear white light generation crystal (19) by a fourth convex lens (18) through a stepping motor electric translation table (13), a hollow retroreflector (14), a fifth total reflection mirror (15), a first half wave plate (16) and a second Glan Taylor prism (17) to generate a supercontinuum which is used as detection light; the detection light is focused on a sample (25) in a temperature-variable cavity (24) through a long working distance objective lens (23) through a first concave mirror (20), a first optical filter (21) and a sixth total reflection mirror (22); the pumping light spot and the detection light spot are overlapped at the sample (25) through a sample visualization module;
the detection light penetrates through a sample (25), then is coupled into an optical fiber (30) through a fifth convex lens (26), a third Glan Taylor prism (27) and a sixth convex lens (28) through an optical fiber coupling module (29), finally an optical fiber spectrometer (31) is synchronously triggered by an FPGA (field programmable gate array) board (32) to collect optical signals, the optical fiber spectrometer (31) converts spectral information into numerical signals, a computer (33) reads electric signals of the spectral information, and transient absorption spectral information is obtained through processing.
2. The non-coaxial transmission type transient absorption measurement system with the temperature field regulation function as claimed in claim 1, wherein: the sample visualization module is composed of a white light source (35), a movable second spectroscope (38), a long-working-distance microscope objective (23), a movable third spectroscope (39) and a CCD detector (34), wherein in the sample visualization process, the position of the second spectroscope (38) can be moved, white light emitted by the white light source (35) is guided to sequentially pass through the movable third spectroscope (39) and the long-working-distance microscope objective (23), and the sample (25) in the temperature-variable cavity (24) is illuminated; after the white light reflected by the surface of the sample (25) is collected by the microscope objective (23) with long working distance, the third spectroscope (39) can be moved to guide the collected white light reflected by the sample to the CCD detector (34) to obtain an image of the surface of the sample, and the distance between the sample (25) and the microscope objective (23) with long working distance is adjusted to obtain a clear image of the surface of the sample.
3. The non-coaxial transmission type transient absorption measurement system with the temperature field regulation function as claimed in claim 1, wherein: the nonlinear white light generation crystal (19) is sapphire, calcium fluoride or YAG crystal, and can generate supercontinuum detection light in the range of 340nm-1200nm based on 1040nm laser pulse.
4. The non-coaxial transmission type transient absorption measurement system with the temperature field regulation function as claimed in claim 1, wherein: the center wavelength of an output light pulse of the femtosecond laser generated by the femtosecond pulse laser (1) is 1040nm, the repetition frequency is 1KHz, and the center wavelength of the light pulse after passing through the nonlinear frequency doubling crystal (6) is changed into 520nm, and the repetition frequency is 1 KHz.
5. The non-coaxial transmission type transient absorption measurement system with the temperature field regulation function as claimed in claim 1, wherein: the system adopts an external trigger mode, realizes communication of the connection by using the FPGA board (32), realizes time sequence control, and synchronizes the process of transmitting light pulses by the femtosecond pulse laser (1) and the process of collecting spectrum information of detection light by the optical fiber spectrometer (31).
6. The non-coaxial transmission type transient absorption measurement system with the temperature field regulation function as claimed in claim 1, wherein: the chopper (11) adopts an external trigger mode, the FPGA board (32) is used for connecting the femtosecond pulse laser (1) and the chopper (11) to realize communication, the chopper (11) can synchronously reduce the frequency of pump light to one half, one quarter or one eighth of the frequency of detection light, and meanwhile, the integration time of the optical fiber spectrometer (31) for collecting spectrum is increased to realize weak signal enhanced detection.
7. The non-coaxial transmission type transient absorption measurement system with the temperature field regulation function as claimed in claim 1, wherein: the first Glan Taylor prism (9) is used for adjusting the polarization state of the pump light, and the second Glan Taylor prism (17) is used for adjusting the polarization state of the probe light and ensuring that the polarization state of the pump light and the polarization state of the probe light are perpendicular to each other. The third Glan Taylor prism (27) adjusts the polarization state of the detection light after penetrating through the sample, and the polarization state is vertical to the polarization state of the pump light, so that the interference of the pump light on the spectrum information of the detection light collected by the fiber spectrometer (31) is reduced.
8. The non-coaxial transmission type transient absorption measurement system with the temperature field regulation function as claimed in claim 1, wherein: the controller of the femtosecond pulse laser (1) is connected with the FPGA board (32), the controller of the chopper (11) and the optical fiber spectrometer (31) and is controlled by the computer (33) to realize communication with each other.
9. The method for measuring the transient absorption spectrum of a sample to be measured by using the non-coaxial transmission type transient absorption measuring system with the temperature field regulation function as claimed in any one of claims 1 to 8 is characterized by comprising the following two parts:
a first part: firstly, placing a sample (25) in a temperature-variable cavity (24), fixing the sample, then operating a vacuum pump to ensure that the vacuum degree in the temperature-variable cavity (24) meets the test requirement, and finally utilizing a temperature controller to realize the temperature control of the sample and carrying out transient absorption spectrum test;
a second part: the transient absorption spectrum test of a sample at a specific temperature comprises the following steps:
setting initialization parameters of a stepping motor translation table (13) and an optical fiber spectrometer (31), wherein the initialization parameters comprise acceleration, step length delta L and initial time point T of delay line time of the stepping motor translation table (13)0And an end time point TeOptical path position Z of pump light and probe light0Etc.; setting the working parameters of the fiber spectrometer (31): initial wavelength (lambda) of the probe spectrum1) And end wavelength (λ)e) Integration time, trigger mode;
obtaining stable supercontinuum detection light: the laser which is incident to the nonlinear white light generation crystal (19) is adjusted in the aspects of beam size, light intensity, polarization direction and the like through cooperatively adjusting the first half wave plate (16) and the second Glan Taylor mirror (17), so that the nonlinear white light generation crystal (19) can generate a stable and smooth supercontinuum under the excitation of 1040nm fundamental frequency light;
regulating the efficiency of coupling the detection light into the optical fiber after the detection light penetrates through the sample (25): precisely adjusting the optical fiber coupling frame to enable the intensity of the supercontinuum displayed in the computer control software to be strongest;
adjusting the coincidence degree of the pump light spot and the detection light spot on the sample: the working point of a translation table (13) of the stepping motor is set to be Z1And satisfy Z1Greater than Z0Closing the detection function in the control program, clicking the optimization function, precisely adjusting a knob of X, Y of the fourth all-mirror (36) and observing the change of the intensity of the transient absorption spectrum displayed by the control software of the computer (33), and precisely optimizing the position of a pump light spot X, Y on the sample (25) until the intensity (-Delta T/T) of the transient absorption spectrum displayed by the control software of the computer (33) is maximum;
testing transient absorption spectrum-delta T/T (lambda) at set temperature1,λ2,…,λe；t1,t2,…te): starting a test function, moving the electric translation table (13) of the stepping motor to the set initial position in the step II, and acquiring the delay time t at the position0Lower transient spectral information- Δ T/T (λ)1,λ2,…,λe；t0) And displayed and stored in the computer (33) control program. Then, the step length delta L set in the step II is taken as the moving amount delta L of the electric translation table (13) of the stepping motor moving to the next position, the position of the electric translation table (13) of the stepping motor is automatically updated in the control program of the computer (33), and new delay time t is obtained1＝t0+ 2. delta.L/c, and t is collected1Time-delayed transient dynamics information- Δ T/T (λ)1,λ2,…,λe；t1). Will automatically update the stepper motor with the step length delta L set in the step twoMoving the translation stage position (13) to obtain a new delay time ti(i＝0,1,2,3,4,5,6,…,te) Up to ti＝teEnding the collection and saving the test data-delta T/T (lambda)1,λ2,…,λe；t1,t2,…te)。
Processing transient absorption spectrum data: the transient absorption spectrum acquired by the step (c) is a two-dimensional intensity distribution diagram-delta T/T (lambda)1,λ2,…,λe；t1,t2,…te) At a wavelength λiAs abscissa, time delay tiIs the ordinate. Relaxation kinetics for transient absorption at a certain wavelength- Δ T/T (λ)i；t1,t2,…te) Using multi-exponential fitting, the lifetime of each relaxation process can be obtained. The fitting formula is
Wherein n is the number of fitting indexes, aiHas a lifetime of tauiThe weight of the component.
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