CN116973305A - Photogenerated carrier interface transmission rate measurement spectrometer device and method - Google Patents
Photogenerated carrier interface transmission rate measurement spectrometer device and method Download PDFInfo
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
Abstract
The application provides a device and a method for measuring the transmission rate of a photogenerated carrier interface, which are high-efficiency carrier interface transmission rate measuring methods crossing 12 magnitude ranges, and can accurately and rapidly measure the photogenerated carrier interface transmission rate of a substance without damaging the properties of the substance. The photogenerated carrier interface transmission rate measuring device comprises an excitation light source, a light source and a light source, wherein the excitation light source is used for irradiating sample excitation light carriers; placing and fixing a sample to be tested in a sample bin; the monochromator is used for purifying the excited photon-generated carriers; the signal detector detects a photo-generated carrier signal; control system and data output processing system. The application uses a single photon measurement method to detect the transmission rate of the photo-generated carrier interface, and can measure samples added with different transmission layers under the same device system. Meanwhile, the method has the advantages of higher resolution, higher detection speed, capability of obtaining more multidimensional data, low cost, modularization, miniaturization and the like.
Description
Technical Field
The application relates to photogenerated carrier interface transmission rate measurement, in particular to a photogenerated carrier interface transmission rate measurement spectrometer device and a photogenerated carrier interface transmission rate measurement method.
Background
When a material is excited by external single energy (usually light energy) at the time of tstimulation, the material is in an electronic excited state, the retention time depends on the rate of the electronic excited state of the material, and then, when the electronic excited state returns to an electronic ground state, carrier emission is often accompanied, and when tstimulation is defined as a carrier emission time point, deltat=tstimulation-tstimulation is defined, and the physical quantity is proportional to the rate of the excited state of the material.
The above-described basic physicochemical model may be applied to a variety of fields of research, such as: photoelectrocatalysis kinetics, development of dyes and luminescent materials, bioluminescence detection, imaging, photodynamic therapy, detection of environmentally active intermediates (OH free radicals), and the like.
The photo-generated carrier interface transmission rate measurement system is applied in a plurality of applications, and only one example is described in detail. For the novel solar photovoltaic cell with a non-PN junction, a physicochemical model can be described as that in the first step, the photovoltaic material absorbs light energy to generate an electron-hole separation state, in the second step, electrons and holes are respectively diffused to two sides, and in the third step, carriers are transferred to a transmission layer through an interface. Numerous documents (Science, 342,341,2013; science,342,344, 2013.) prove that the carrier transmission speed in the third step determines the photoelectric conversion efficiency of the solar cell, and different transmission layers have great influence on the carrier transmission rate, for example, an organic-inorganic hybrid solar dye cell, and the carrier transmission rate is very low when no transmission layer is added, namely, only 4.5x10 3 And after the addition of a suitable transport layer, the carrier transport rate can reach 7.2×10 10 Spanning seven measurement range orders, it becomes critical how to measure it. The photogenerated carrier interface transmission rate measurement system gives a solution.
The method comprises the steps of firstly exciting a pure photovoltaic material by using short pulse laser, wherein the photovoltaic material with good performance can emit carriers with long speed, the mechanism is simply expressed as that the material absorbs photons to reach an electron-hole separation state, then the material returns to a ground state, meanwhile, along with fluorescence emission, the fluorescence speed directly represents the speed T1 of the electron-hole separation state, after a carrier transmission layer is prepared on the surface of the photovoltaic material, the fluorescence speed T2 of the material is measured again, at the moment, the fluorescence speed T2 is greatly shortened due to the fact that the deactivation path of carrier transmission is increased, and at the moment, K= (1/T2) - (1/T1) is the speed of carrier interface transmission.
In solar cells, the carrier interface transport rate largely determines the efficiency of the cell, whereas solar cells with different transport layers have a large difference in carrier interface transport efficiency from nanoseconds to seconds.
The measurement principle of the photogenerated carrier interface transmission rate measurement system is as follows: first, 4096 channels which exist continuously are defined in a memory, and the time width of each channel is set by software. In the first time channel, the sample is given an excitation of energy, which may be in the form of a number of energies, such as optical, electrical, mechanical, chemical, etc. When measurement starts, an energy source excites a sample, the sample emits light, an instrument sequentially passes through a 1 st channel, a 2 nd channel … … to a last 4096 channels, the number of carriers falling in each channel is measured and used for representing carrier signal strong gambling in a corresponding time period, a curve of carrier intensity resolved along with time is obtained after superposition of multiple measurement results, and information such as carrier velocity and the like is obtained after subsequent fitting treatment. The carrier resolution of the method is single photon, and when the excitation light intensity and the width are reasonably selected, the measurement can be completed within a time scale of seconds to minutes. The shortest time window of the method can be set to 10ns, the total measurement time length can be set to 172000s, and measurement can be carried out across 12 magnitude measuring ranges. Therefore, the method can be used for measuring samples with different transmission layers under the same instrument and the same system, so that systematic errors caused by different measuring ranges and the need of using different instruments for measurement are avoided to the greatest extent, and the application range is very wide.
The design of the time-resolved fluorescence analysis apparatus in the prior patent and paper documents has the following drawbacks:
1. in the patent 'fast fluorescence lifetime imaging method based on a single photon avalanche diode detector' (application No. 201711090809.8), after three time windows are divided, a result is obtained by performing discrete and aliasing multiplexing calculation fitting by using a monte carlo formula, so that the data obtained by fitting may be inaccurate because the divided time windows are too few and more dependent on data fitting.
2. In both the patent 'a time-resolved photon counting imaging system and method' (application No. 201110152839.3) and the patent 'a fluorescence lifetime imaging system and method for photon arrival time and position synchronous measurement' (application No. 201810040971.7), the measurement of the photon arrival position is involved, and the final result is obtained through the position, which can cause the measurement rate to be slow because one-dimensional data is measured more.
3. In the patent "picosecond resolution single photon weak signal measuring device and measuring method" (application number 201910167445.1), picosecond level measurement is performed, and a method of measuring voltages at two ends of a capacitor in real time and recording voltage values is used to measure carrier velocity, and the method is only suitable for measuring a picosecond velocity carrier sample, because when a slow velocity sample is measured, exponentially increasing time is consumed according to the reduction of the carrier velocity of the sample, and the smaller the velocity is, the longer the time required for measurement is.
Disclosure of Invention
The application relates to a photogenerated carrier interface transmission rate measuring system, which uses Einstein photoelectric effect and avalanche effect, and aims to solve the problems of rapidness, convenience, high precision and high time resolution and efficiency in measuring the photogenerated carrier interface transmission rate under a wide time scale. And has the advantages of high sensitivity, light weight, miniaturization, modularization and the like.
In order to achieve the above purpose, the technical scheme of the application is as follows: a photogenerated carrier interface transmission rate measurement spectrometer device, comprising:
the laser is used for emitting monochromatic light to the sample to excite the sample to be tested to generate photogenerated carriers;
the sample bin is used for placing a sample to be tested;
the monochromator is used for eliminating unnecessary signals, collecting photogenerated carriers and purifying the signals;
the signal detection system is used for converting the received purified photo-generated carrier signal into an electric signal and outputting the electric signal to the control system;
the control system is used for outputting signals to control the laser, the sample cell, the monochromator and the signal detection system to work; and counting the data of the purified photogenerated carrier signals and outputting the data to a data output processing system;
the data output processing system is used as a control system upper computer to send instructions to the data output processing system, and the purified photo-generated carrier signal data are subjected to data processing and image visual display;
the exciter, the signal detection system, the control system and the data output processing system are mutually connected; and the laser, the sample bin, the monochromator and the signal detector are connected by an optical component light path.
The laser includes: the light source, the light-emitting control module and the signal connection terminal, wherein the light-emitting control module is connected with the control system and the light source through the signal connection terminal; the light source is any one of an LED lamp tube, a xenon lamp and a halogen tungsten lamp, and is selected according to the required wavelength; a laser light-passing slit is arranged on an emission light path between the light source and the sample; the light-emitting control module is used for receiving a starting signal, controlling the light source to flash according to the set duration and time interval, recording the light-emitting time of the starting signal and sending the light-emitting time to the control system, and changing the output voltage of the starting signal to the light source to change the light intensity.
The sample bin is as follows: the closed bin body with a door at one side is made of aluminum, the inner surface of the bin body is blackened, an attenuation sheet clamping groove and an optical filter clamping groove are embedded in the wall of the bin body, an attenuation sheet and an optical filter are respectively placed in the bin body, and a solid sample tank and a liquid sample tank for containing solid or liquid samples are arranged in the bin body; the outside of the sample bin is covered with shading cloth; the laser outputs monochromatic laser, and the monochromatic laser strikes the sample to generate a photogenerated carrier signal after passing through the attenuation sheet, and the filter sheet filters the unexcited monochromatic light to output the photogenerated carrier signal to the monochromator.
The monochromator includes: two reflective concave lenses and a beam splitting grating; the two reflective concave lenses are respectively arranged on respective base discs, the central shaft of each base disc is connected with the output shaft of the motor, and the motor rotates to drive the reflective concave lenses to rotate; the central shaft of the base disc of the light-splitting grating is connected with the output shaft of the motor, and the motor rotates to drive the light-splitting grating to rotate; the base disc of the light-splitting grating is arranged on the one-dimensional linear motion module; the motor of the one-dimensional linear motion module rotates to drive the light splitting grating to linearly move; each motor or motor rotates according to the control system output instruction so as to drive the two reflective concave lenses to rotate, the beam splitting grating to rotate and move to a set position, so that the first reflective concave lens reflects and gathers carrier signals output by the sample bin to one point on the beam splitting grating for purification and beam splitting, and after purification and beam splitting, the carriers are reflected into a monochromator light-passing slit through the second reflective concave lens and gathered to the signal detection system.
The signal detection system includes: the device comprises a signal receiving module, a photoelectric signal conversion module and a negative voltage converter; the negative voltage converter is used for converting the power supply voltage into a signal receiving module, and the photoelectric signal conversion module needs working negative voltage; the signal receiving module collects carrier signals after required purification and light splitting, and the photoelectric signal conversion module converts the carrier signals into electric signals and outputs the electric signals to the control system.
The control system includes: the power supply is used for supplying power to the laser, the monochromator, the signal detector, the control system, the main control module for receiving and transmitting command signals and the digital display screen for displaying working voltage; the main control module is used for controlling the power supply to start and stop so as to control the laser, the monochromator, the signal detector to work and record the time of each time of lighting of the laser, outputting an instruction to adjust the working voltage of the laser to change the light intensity of output laser, outputting the instruction to a motor and each motor in the monochromator, enabling the positions of two reflecting concave lenses and the grating to be changed to realize the purification of photogenerated carriers, receiving and recording the output signals of the signal detection system, processing and analyzing the output signals, and outputting the processed signals to the data output processing system.
The data output processing system includes: front-end visual graphic operation interface and data processing background carried on computer; the front-end visual graphic operating system is used for inputting various parameters of the instrument required to be regulated during measurement through man-machine interaction and visually displaying graphic data; and deconvoluting data acquired by the data processing background control system, and performing fitting operation to obtain a photo-generated carrier map.
A photogenerated carrier interface transmission rate measuring method comprises the following steps:
1) According to the sample to be measured, replacing a sample pool in which the sample is placed, and covering a shading cloth to isolate an external light source; according to the sample to be tested, replacing the required excitation light source, the attenuation sheet and the optical filter;
2) Inputting instrument operation parameters through a front-end visual graphical operation interface: excitation wavelength, monochromator purification wavelength;
3) Starting a control system to perform a measurement flow, lighting a lamp tube in a laser, flashing, emitting photons into a sample cell, exciting a sample to be tested to generate photo-generated carriers, transmitting the photo-generated carriers to a monochromator through an interface, enabling a first reflection concave lens to reflect and collect carrier signals to one point on a beam splitting grating for purification and beam splitting, enabling the purified and split carriers to be reflected into a monochromator light-transmitting slit through a second reflection concave lens, and collecting the carriers to a signal detector; the signal detector converts the collected photo-generated carrier signals into electric signals and outputs the electric signals to the control system;
4) The data output processing system counts the photo-generated carrier electric signals of the sample measured in the lighting time of the excitation light source, fits the photo-generated carrier electric signals to obtain carrier interface transmission rate data, and then converts the carrier interface transmission rate data into a visual pattern to be displayed on the front end interface.
The measurement flow of the control system comprises the following steps:
a. outputting a control signal to the laser according to the operation parameters, and adjusting the excitation wavelength of the output laser;
b. outputting a control signal to the monochromator according to the operation parameters, and controlling each motor or motor in the monochromator to rotate so as to drive the two reflective concave lenses to rotate or the beam splitter grating to rotate or move to a set position;
c. outputting instructions to control the start and stop of each power supply so as to control the operation of the laser, the monochromator and the signal detection system, and recording the time of each time of the laser;
d. and the control system counts and outputs the photo-generated carrier electric signals of the sample measured in the lighting time of the excitation light source to the signal output processing system.
In the process of measuring the flow by the control system, when the light intensity of the output laser needs to be changed, the control system is realized in the following two modes:
1) The size of the light-passing slit of the laser is changed to adjust the light-passing amount so as to change the light intensity;
2) Changing the output voltage of the light-emitting control module realizes changing the light intensity.
The application has the following beneficial effects and advantages:
1. according to the application, 4096 time channels are divided, the number of carriers falling in each time channel is collected, the carrier intensity in the corresponding time is calculated, a curve of the carrier intensity relative to time resolution is made, and the carrier velocity is fitted.
2. The method can measure samples with carrier rates of different time scales by setting different time channel lengths, and can measure the carrier rates from nanosecond level to second level across 12 magnitude measuring ranges. And the time taken to measure samples at different time scale rates is substantially the same, the measurement can be accomplished in a time scale of seconds to minutes when the excitation light intensity and width are reasonably selected.
3. Meanwhile, the application can measure the same system sample with the same instrument, which only changes the transmission layer but has carrier interface transmission rate with a plurality of orders of magnitude difference, thereby avoiding the systematic error caused by using different instruments to the greatest extent
4. Compared with the rapid fluorescence lifetime imaging method based on a single photon avalanche diode detector, the method disclosed by the application is used for directly measuring the photon number in each channel to obtain a curve of carrier intensity resolved with time in the patent of application number 201711090809.8.
5. Compared with the system and the method for fluorescence lifetime imaging, which are named as 'a time resolution photon counting imaging system and method', application number 201110152839.3 and the patent 'photon arrival time and position synchronous measurement', the application only relates to the measurement of the number of photon arrival at different times and obtains final data in the patent of application number 201810040971.7. While other patents are hardly concerned with single photon measurement methods.
6. Compared with a measurement device and a measurement method for picosecond resolution single photon weak signals, the method disclosed by the application uses a patent with application number 201910167445.1 to define 4096 time channels, a curve of carrier intensity resolved along with time is obtained according to the number of photons in each time channel, and required data is obtained according to subsequent fitting. The method can obtain data spanning 12 magnitude ranges from nanoseconds, and the measurement time consumed in measuring data of different magnitudes is a fixed value and cannot increase along with the increase of the speed.
Drawings
FIG. 1 is a block diagram of the system components of the present application.
FIG. 2 is a block diagram of a laser, sample compartment, monochromator, signal detector in the instrument.
Fig. 3 is a block diagram of a control system in an instrument.
Fig. 4 is a chart of the photo-generated carrier interface transmission rate of two samples of the cimetidine cesium lead iodine solar cell without the addition of the transmission layer according to the present application, and v is the fitted carrier lifetime transmission rate.
Fig. 5 is a graph of the photo-generated carrier interface transmission rate spectrum of two samples of the solar cell of cesium lead iodide added with PCBM transmission layer according to the present application, v is the fitted carrier lifetime transmission rate.
In the figure, 201 is a laser control system, 202 is a lamp tube, 203 is an attenuation sheet, 204 is a sample cell, 205 is an optical filter, 206 is a concave mirror moving motor No. two, 207 is a concave mirror, 208 is a concave mirror, 209 is a concave mirror moving motor No. one, 210 is a monochromatic grating, 211 is a grating moving motor, 212 is a signal receiving device, 213 is a negative voltage converter, 214 is an electric signal conversion device, 301 is an excitation light source power supply fan, 302 is an excitation light source power supply, 303 is an operating voltage digital display system, 304 is a control system power supply fan, 305 is a monochromator motor power supply, 306 is a monochromator motor power supply fan, 307 is a signal detector power supply fan, 308 is a signal detector power supply, 309 is a control system, and 310 is a control system power supply.
Detailed Description
In order to make the objects, features and advantages of the embodiments of the present application more obvious and understandable, the technical solutions of the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is apparent that the described embodiments are only some embodiments of the present application, not all embodiments of the present application.
The application relates to a photogenerated carrier interface transmission rate system, which uses Einstein photoelectric effect and avalanche effect, and aims to solve the problems of rapidness, convenience, high precision and high time resolution and high efficiency in measuring photogenerated carriers under an ultrafast time scale.
A high-precision modularized photogenerated carrier interface transmission rate measurement system comprises an excitation light source, a sample bin, a monochromator, a signal detector, a control system and a data output processing system.
The excitation light source is used for emitting high-purity monochromatic laser, and the inside of the excitation light source comprises a laser light source and a light-emitting control module. The lamp tube, xenon lamp and halogen tungsten lamp are mutually replaceable laser light source components, and the wavelength is selected according to the requirement. A laser light-passing slit is arranged on an emission light path between the light source and the sample, and the light-passing slit is as follows: the two aluminum sheets (the surfaces of which are subjected to blackening treatment) are arranged in parallel and are connected through screws, reverse threads are arranged on the screws, one end of each screw is connected with a miniature motor, and the motor drives the screws to rotate, so that the distance between the two aluminum sheets is adjusted, and the light quantity entering the light-passing slit is changed. The luminous control module is connected with the control system and the lamp tube through electric signals, and the lamp tube is connected with the sample bin through optical signals. After the photogenerated carrier interface transmission rate measurement system is started, different excitation light sources (in the embodiment, the LED light sources are adopted) are replaced according to the property of the sample to be measured, and fixing is carried out. And the size of the laser light-passing slit is adjusted to change the light-passing amount and then the incident light intensity by controlling the electric motor to rotate the metal sheet through the input parameters. The control system then turns on the excitation light source power supply 302, and after the measurement is started, the light emission control module controls the light source to flash in an ultrafast time scale, records the time of each flash, and sends the time to the control system. After the light source is lightened each time, the emitted photons enter the sample bin to excite the sample to be tested, and the photo-generated carriers are generated.
The sample bin is used for placing and fixing a sample, and internally comprises a solid powder sample tank or a liquid sample tank which can be replaced according to the property of the sample, a filter which can be replaced according to the wavelength of the excitation light source and a shading cloth. The internal sample cell is interconnected with an excitation light source and a monochromator by optical signals. After the picosecond single photon-generated carrier measuring system is started, a filter plate is selected according to the wavelength of the selected excitation light, the filter plate is placed into a groove at the joint of the sample bin and the wall of the monochromator inner bin, and the thickness of the groove is adjusted and fixed by using a screw. Photons are emitted from the excitation light source into the sample cell, exciting the sample in the sample cell, generating photogenerated carriers. Meanwhile, the filter filters out photons incident from the excitation light source, and influences of the incident light are eliminated. The photo-generated carriers generated by the sample are collected and enter a monochromator. The sample bin is a fully-closed metal aluminum plate, chemical blackening is carried out in the sample bin, and the shading cloth is used for shading the joint of each part of the sample bin, so that the influence of external photons and noise is discharged as much as possible.
The monochromator is used for purifying photo-generated carriers generated by exciting a sample, and comprises an electric motor, a monochromic grating, two reflecting concave lenses and a slit. The single-color grating is connected with the electric motor in a physical mode, and the electric motor is connected with the control system and the electric signal. The two reflective concave lenses are respectively arranged on respective base discs, the central shaft of each base disc is connected with the output shaft of the motor, and the motor rotates to drive the reflective concave lenses to rotate; the central shaft of the base disc of the light-splitting grating is connected with the output shaft of the motor, and the motor rotates to drive the light-splitting grating to rotate; the base disc of the light-splitting grating is arranged on the one-dimensional linear motion module; the motor of the one-dimensional linear motion module rotates to drive the light splitting grating to linearly move. After the picosecond single photon generation carrier measuring system is started, the control system starts the electric motor to change the positions of the monochromatic grating and the reflection concave lens according to the property of the measured sample, so that the required photon generation carrier can be purified. After the excited photon-generated carriers of the sample are injected from the sample pool, the excited photon-generated carriers are collected by the first reflecting concave lens, reflected to the monochromatic grating and purified by the monochromatic grating, and the purified photon-generated carriers are collected by the second reflecting concave lens, reflected to the light-passing slit of the monochromator and gathered into the signal detector. The intensity of the emitted carrier signal can be adjusted by adjusting the size of the light-passing slit of the monochromator.
The signal detector is used for detecting the photo-generated carriers excited by the sample to be detected and purified by the monochromator, converting the photo-generated carriers into electric signals and transmitting the electric signals into the control system, and the control system internally comprises a signal receiving device, an electric signal conversion device and a negative voltage converter. The signal receiving device, the electric signal conversion device and the negative voltage converter are connected by electric signals, the signal receiving device is connected with the monochromator by optical signals, and the electric signal conversion device is connected with the control system by electric signals. After the photogenerated carrier interface transmission rate measuring system is started, the negative voltage converter is started to change the input voltage into negative voltage, so that the signal detector can normally operate. The purified photon-generated carriers are injected from the monochromator and collected by the optical signal receiving device, the received optical signals are converted into electric signals by the electric signal conversion device, and the obtained electric signals are transmitted into the control system through the signal connection terminal.
The control system is a main core control device and is used for controlling the operation of the whole photogenerated carrier interface transmission rate measuring system, and the control system comprises a main control module, a main control module power supply system, an excitation light source power supply system, a monochromator mechanical transmission device power supply system, a signal detector power supply system, a cooling fan independently equipped by each power supply system and a working voltage digital display screen. The internal components and other components are connected by electric signals. After the photo-generated carrier interface transmission rate measuring system is started, each power supply and a fan system thereof are started to provide working power for each component. Meanwhile, according to the properties of the sample, the control system controls an electric motor in the monochromator component to start and drive the first reflecting concave mirror, the second reflecting concave mirror and the monochromatic grating on the linear module to change positions. And the time of each lighting of the excitation light source is recorded, the excitation light source is stored and compared with the photo-generated carrier electric signal of the measured sample received and transmitted by the signal detector, and a group of measurement data is generated and transmitted into the data output processing system through the signal connection terminal.
The data output processing system is a visual system and is used for visualizing the input control system, the visual data output and the post-processing system, and the data output processing system comprises a graphic visual control system, a graphic visual data output system and a graphic visual data processing system. After the photogenerated carrier interface transmission rate measuring system is started, various data indexes (such as laser excitation wavelength) of a sample are input into the graphic visualization control system, and each component of the photogenerated carrier interface transmission rate measuring system is controlled to prepare before measurement. After the control system transmits a group of light source starting time and photo-generated carrier measurement signals, the graphic visual data output system outputs the light source starting time and photo-generated carrier measurement signals into a visual map, and the graphic visual data processing system performs further data processing according to sample properties and requirements. For example, a two-dimensional variable map of time versus photogenerated carrier intensity is made.
The problem to be solved in this embodiment is to excite the photo-generated carriers of 9-fluorenone in the sample to be measured, collect the photo-generated carriers with specific wavelengths, and determine the interface transmission rate of the photo-generated carriers according to the number of the collected carriers in different time intervals. Fig. 1 shows a connection manner between each component and each component included in the embodiment of the device for detecting photo-generated carriers of a sample, which includes an excitation light source, a sample chamber, a monochromator, a signal detector, a control system and a data output processing system. The data output processing system is connected with the control system, the control system is connected with the signal detector, the excitation light source and the monochromator, and the sample bin is connected with the monochromator and the excitation light source.
Fig. 2 shows the specific structure of the excitation light source, the sample chamber, the monochromator, and the signal detector, and the connection and installation modes of the excitation light source, the sample chamber, the monochromator and the signal detector. The excitation light source comprises a laser control system 201 and a lamp tube 202, wherein the lamp tube 202 can be replaced according to the requirements (an LED lamp tube is adopted in the embodiment) according to the measured sample properties, namely the difference of carrier excitation wavelength and emission wavelength, and the emitted excitation light wavelength is changed; the excitation light power can be adjusted within a certain range by changing the power supply voltage according to the requirement, and the working voltage can be adjusted to be between 14mv and 16mv on the premise of ensuring the stability of the light source. The sample bin comprises an attenuation sheet 203 mounting groove, a sample pool 204 and an optical filter 205, wherein the attenuation sheet mounting groove can be used for mounting optical filters with different light transmittance according to the properties such as sample stability and the like and the excitation light source power; the sample cell can be replaced by a solid sample cell and a liquid sample cell respectively according to the fact that the sample is liquid, solid and the like; a vacuum system can be added into the sample bin according to the detection requirement of the sample, and the sample is measured under the vacuum system; the optical filter can be flexibly selected according to the wavelength difference of the incident laser and the carrier generated by the excitation of the sample. The monochromator comprises a first concave mirror 208, a first concave mirror motion motor 209, a monochromator grating 210, a monochromator grating motion motor 211, a second concave mirror 207, and a second concave mirror motor 206. The first concave reflecting mirror and the second concave reflecting mirror can rotate to a certain extent through a photon-generated carrier moving motor below the first concave reflecting mirror and the second concave reflecting mirror according to incident photon-generated carrier wavelength generated by the sample; the monochromatic grating can rotate and move through the monochromatic grating motor below the monochromatic grating with different wavelengths of photo-generated carriers. The signal detector comprises 212 optical signal receiving means, 213 negative voltage converting means, 214 optical-electrical signal converting means.
Fig. 3 shows a control system in this embodiment, which includes an excitation light source power supply fan 301, an excitation light source power supply 302, a working voltage digital display system 303, a control system power supply fan 304, a monochromator motor power supply 305, a monochromator motor power supply fan 306, a signal detector power supply fan 307, a signal detector power supply 308, a control system 309, and a control system power supply 310.
Fig. 4 and 5 are graphs of photo-generated carrier interface transport rates measured for two samples with different transport layers according to one embodiment of the application, v being the fitted carrier lifetime transport rate. FIG. 4 is a graph of the photo-generated carrier interface transport rate of a lead-iodine solar cell with no transport layer added, fitted to a rate of 5.1X10 3 . FIG. 5 is a graph of the photo-generated carrier interface transport rate of a cesium lead-iodine solar cell with PCBM transport layer added, fitted with a rate of 6.2 to 6.2×10 11 . It can be seen that the rates differ by eight orders of magnitude, and the application can directly measure the two samples without changing fittings and settings, avoiding systematic errors to the greatest possible extent.
The steps for measuring the sample to be measured are as follows.
(1) The sample compartment is opened and replaced with a solid sample cell or a liquid sample cell 204 depending on the nature of the sample to be tested. In the case of a solid sample, the sample was ground to a powder and sandwiched between two pieces of quartz glass, the sample size was about 1 square centimeter and the sample thickness was about 0.5 millimeters. The prepared sample quartz glass was then placed in solid sample Chi Kacao, ensuring that the sample carrying portion was aligned with the incident laser light path, and secured using a snap fit. If the sample is a liquid sample, the sample is injected into a quartz cuvette with the diameter of 10mm by 10mm, the absorbance of the sample is ensured to be between 0.2 and 0.8, and the specific numerical value is determined according to the quantum yield. The quartz cuvette with the sample is then added to a dedicated liquid sample cell 204 and it is ensured that the cuvette is clean and free of contamination.
(2) According to the property of the sample, namely the maximum excitation wavelength, the required excitation light source 202 is replaced, after the replacement is finished, the optical filter with the corresponding wavelength is added into the clamping groove of the optical filter 205 according to the replaced excitation light source, and the optical filter is fixed by using a hasp. And corresponding attenuation sheets are placed according to the property of the excitation light source and added into the clamping grooves of the attenuation sheets 203, and are fixed by using buckles. The sample compartment was closed and further optically shielded by adding black mask.
(3) The control system power supply 310, the control system switch, the data output processing system power supply, the excitation light source power supply 302, the monochromator motor power supply 305, and the signal detector power supply 308 are sequentially turned on. And then opening a graphical page of the data output processing system, inputting corresponding excitation wavelength according to the sample property, and transmitting wavelength data into control software. At this time, the data output processing system transmits corresponding signals and commands to the control system 309, and the control system outputs signals to the first concave mirror moving motor 209, the second concave mirror motor 206, the single-color grating moving motor 211 and the one-dimensional linear module according to the input signals, and the first concave mirror 208, the second concave mirror 207 and the single-color grating 210 are operated by these motors to reach the corresponding positions.
(4) After the optical path is moved to the corresponding position, a signal is output in the data output processing system, the signal is transmitted to the control system 309, the control system transmits a command to the laser control system 201, and the laser control system 201 lights the lamp tube 202 to perform the first test run. Observing the signal intensity and the signal obtaining time obtained in the data output processing system, if the signal is too strong or too weak, the quantum yield of the sample is too high or too low, the number of generated carriers is too high or too low, the obtained signal is distorted, or the finally obtained data is not accurate enough. At this time, the signal detector power supply 308 should be turned off by the data output processing system, and the excitation light source power supply 302 should be turned off, so as to ensure that the working voltage digital display system 303 displays an indication of 0. And then the shading cloth is uncovered, the cover plate of the sample bin is opened, the attenuation sheet with stronger or weaker attenuation is replaced, the previous steps are repeated for testing, the acquired data intensity is ensured to be in a proper intensity interval, and accurate data can be acquired.
(5) After the actual measurement is entered, the data output processing system inputs signals to the control system 309, the control system 309 controls the signal detector power supply 308 which is turned off before being turned on, excites the light source power supply 302, and outputs signals to the laser control system 201, which controls the lighting tube 202 to emit high-purity excitation light. The excitation light passes through the attenuator 205, filters out a large number of photons, attenuates the intensity of the incident light, and reaches the sample cell 204. The excitation light excites the sample to be measured in the sample cell 204, causing it to excite carriers. The carriers excited by the sample and the unabsorbed excitation light pass through the filter 206, wherein the excitation photons are absorbed by the filter 206 and cannot pass through the filter, and the carriers excited by the sample can successfully pass through the filter and enter the monochromator.
(6) After entering the monochromator, the carriers firstly reach the first concave reflecting mirror 208, are collected by the first concave reflecting mirror and reflected to the monochromatic grating 210, are purified by the monochromatic grating, and independently reflect the carriers with required wavelengths to the second concave reflecting mirror 207 according to the properties of the sample, and are collected by the second concave reflecting mirror and reflected to the signal detector.
(7) After the signal receiving device receives the signal 212, the collected carrier signal is transmitted to the electric signal conversion device 214, the electric signal conversion device 214 converts the carrier signal into an electric signal, the converted electric signal is transmitted to the control system 309, the control system 309 collects the sample signal and then transmits the sample signal to the data output processing system, the data output system performs graphical presentation, and the final data is obtained by fitting, so as to obtain a data map (fig. 4).
In a word, the photogenerated carrier interface transmission rate system described by the application can be easily measured by only adjusting the gear of the time scale in the graphic interface when facing samples with different or even extremely different carrier rates. The measurable range is from nanosecond level to hundreds of milliseconds, and the measuring is carried out by spanning 12 magnitude ranges, so that the measuring is very convenient and quick. Meanwhile, the photo-generated carrier interface transmission rate measurement system on the market is large in size, difficult to debug and transport, and the operation system is complex in interface, numerous in parameters and difficult to rapidly start. The picosecond single photon generation carrier interface transmission rate measurement system has the characteristics of modularization and portability, and a person can be easily disassembled, transported, installed, debugged and easily tested through simple education. And the measured data can be subjected to post-processing processes such as fitting by using a self-contained graphical interface, and other software is not required to be additionally used for data processing. Finally, the obtained data file is in a common form, can be opened at any place, does not encrypt data of a certain photogenerated carrier rate interface transmission measurement system on the market, can be referred and opened only by installing special software, and is convenient for data transmission and use.
Example embodiments have been disclosed herein, and although specific terms are employed, they are used and are to be interpreted in a generic and descriptive sense only and not for purpose of limitation. In some cases, as will be apparent to one of ordinary skill in the art at the time of filing of the present application, features, characteristics, and/or elements described with respect to one particular embodiment may be used alone or in combination with features, characteristics, and/or elements described with respect to other embodiments unless explicitly indicated otherwise. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the application as set forth in the appended claims.
Claims (10)
1. A photogenerated carrier interface transmission rate measurement spectrometer device, comprising:
the laser is used for emitting monochromatic light to the sample to excite the sample to be tested to generate photogenerated carriers;
the sample bin is used for placing a sample to be tested;
the monochromator is used for eliminating unnecessary signals, collecting photogenerated carriers and purifying the signals;
the signal detection system is used for converting the received purified photo-generated carrier signal into an electric signal and outputting the electric signal to the control system;
the control system is used for outputting signals to control the laser, the sample cell, the monochromator and the signal detection system to work; and counting the data of the purified photogenerated carrier signals and outputting the data to a data output processing system;
the data output processing system is used as a control system upper computer to send instructions to the data output processing system, and the purified photo-generated carrier signal data are subjected to data processing and image visual display;
the exciter, the signal detection system, the control system and the data output processing system are mutually connected; and the laser, the sample bin, the monochromator and the signal detector are connected by an optical component light path.
2. A photogenerated carrier interface transmission rate measurement spectrometer device according to claim 1, wherein said laser comprises: the light source, the light-emitting control module and the signal connection terminal, wherein the light-emitting control module is connected with the control system and the light source through the signal connection terminal; the light source is any one of an LED lamp tube, a xenon lamp and a halogen tungsten lamp, and is selected according to the required wavelength; a laser light-passing slit is arranged on an emission light path between the light source and the sample; the light-emitting control module is used for receiving a starting signal, controlling the light source to flash according to the set duration and time interval, recording the light-emitting time of the starting signal and sending the light-emitting time to the control system, and changing the output voltage of the starting signal to the light source to change the light intensity.
3. The photogenerated carrier interface transmission rate measurement spectrometer device according to claim 1, wherein the sample compartment is: the closed bin body with a door at one side is made of aluminum, the inner surface of the bin body is blackened, an attenuation sheet clamping groove and an optical filter clamping groove are embedded in the wall of the bin body, an attenuation sheet and an optical filter are respectively placed in the bin body, and a solid sample tank and a liquid sample tank for containing solid or liquid samples are arranged in the bin body; the outside of the sample bin is covered with shading cloth; the laser outputs monochromatic laser, and the monochromatic laser strikes the sample to generate a photogenerated carrier signal after passing through the attenuation sheet, and the filter sheet filters the unexcited monochromatic light to output the photogenerated carrier signal to the monochromator.
4. A photogenerated carrier interface transmission rate measurement spectrometer device according to claim 1, wherein the monochromator comprises: two reflective concave lenses and a beam splitting grating; the two reflective concave lenses are respectively arranged on respective base discs, the central shaft of each base disc is connected with the output shaft of the motor, and the motor rotates to drive the reflective concave lenses to rotate; the central shaft of the base disc of the light-splitting grating is connected with the output shaft of the motor, and the motor rotates to drive the light-splitting grating to rotate; the base disc of the light-splitting grating is arranged on the one-dimensional linear motion module; the motor of the one-dimensional linear motion module rotates to drive the light splitting grating to linearly move; each motor or motor rotates according to the control system output instruction so as to drive the two reflective concave lenses to rotate, the beam splitting grating to rotate and move to a set position, so that the first reflective concave lens reflects and gathers carrier signals output by the sample bin to one point on the beam splitting grating for purification and beam splitting, and after purification and beam splitting, the carriers are reflected into a monochromator light-passing slit through the second reflective concave lens and gathered to the signal detection system.
5. A photogenerated carrier interface transmission rate measurement spectrometer device according to claim 1, wherein the signal detection system comprises: the device comprises a signal receiving module, a photoelectric signal conversion module and a negative voltage converter; the negative voltage converter is used for converting the power supply voltage into a signal receiving module, and the photoelectric signal conversion module needs working negative voltage; the signal receiving module collects carrier signals after required purification and light splitting, and the photoelectric signal conversion module converts the carrier signals into electric signals and outputs the electric signals to the control system.
6. A photogenerated carrier interface transmission rate measurement spectrometer device according to claim 1, wherein the control system comprises: the power supply is used for supplying power to the laser, the monochromator, the signal detector, the control system, the main control module for receiving and transmitting command signals and the digital display screen for displaying working voltage; the main control module is used for controlling the power supply to start and stop so as to control the laser, the monochromator, the signal detector to work and record the time of each time of lighting of the laser, outputting an instruction to adjust the working voltage of the laser to change the light intensity of output laser, outputting the instruction to a motor and each motor in the monochromator, enabling the positions of two reflecting concave lenses and the grating to be changed to realize the purification of photogenerated carriers, receiving and recording the output signals of the signal detection system, processing and analyzing the output signals, and outputting the processed signals to the data output processing system.
7. A photogenerated carrier interface transmission rate measurement spectrometer device according to claim 1, wherein the data output processing system comprises: front-end visual graphic operation interface and data processing background carried on computer; the front-end visual graphic operating system is used for inputting various parameters of the instrument required to be regulated during measurement through man-machine interaction and visually displaying graphic data; and deconvoluting data acquired by the data processing background control system, and performing fitting operation to obtain a photo-generated carrier map.
8. The method for measuring the transmission rate of the photogenerated carrier interface is characterized by comprising the following steps of:
1) According to the sample to be measured, replacing a sample pool in which the sample is placed, and covering a shading cloth to isolate an external light source; according to the sample to be tested, replacing the required excitation light source, the attenuation sheet and the optical filter;
2) Inputting instrument operation parameters through a front-end visual graphical operation interface: excitation wavelength, monochromator purification wavelength;
3) Starting a control system to perform a measurement flow, lighting a lamp tube in a laser, flashing, emitting photons into a sample cell, exciting a sample to be tested to generate photo-generated carriers, transmitting the photo-generated carriers to a monochromator through an interface, enabling a first reflection concave lens to reflect and collect carrier signals to one point on a beam splitting grating for purification and beam splitting, enabling the purified and split carriers to be reflected into a monochromator light-transmitting slit through a second reflection concave lens, and collecting the carriers to a signal detector; the signal detector converts the collected photo-generated carrier signals into electric signals and outputs the electric signals to the control system;
4) The data output processing system counts the photo-generated carrier electric signals of the sample measured in the lighting time of the excitation light source, fits the photo-generated carrier electric signals to obtain carrier interface transmission rate data, and then converts the carrier interface transmission rate data into a visual pattern to be displayed on the front end interface.
9. The method for measuring a transmission rate of a photogenerated carrier interface according to claim 8, wherein the measurement procedure of the control system includes:
a. outputting a control signal to the laser according to the operation parameters, and adjusting the excitation wavelength of the output laser;
b. outputting a control signal to the monochromator according to the operation parameters, and controlling each motor or motor in the monochromator to rotate so as to drive the two reflective concave lenses to rotate or the beam splitter grating to rotate or move to a set position;
c. outputting instructions to control the start and stop of each power supply so as to control the operation of the laser, the monochromator and the signal detection system, and recording the time of each time of the laser;
d. and the control system counts and outputs the photo-generated carrier electric signals of the sample measured in the lighting time of the excitation light source to the signal output processing system.
10. The method for measuring the transmission rate of the photogenerated carrier interface according to claim 8, wherein the control system performs the measurement process by changing the light intensity of the output laser in two ways:
1) The size of the light-passing slit of the laser is changed to adjust the light-passing amount so as to change the light intensity;
2) Changing the output voltage of the light-emitting control module realizes changing the light intensity.
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