CN111175256A - Device for detecting perovskite thin film by photoluminescence and monitoring method thereof - Google Patents
Device for detecting perovskite thin film by photoluminescence and monitoring method thereof Download PDFInfo
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- CN111175256A CN111175256A CN201811342609.1A CN201811342609A CN111175256A CN 111175256 A CN111175256 A CN 111175256A CN 201811342609 A CN201811342609 A CN 201811342609A CN 111175256 A CN111175256 A CN 111175256A
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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
-
- 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
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6402—Atomic fluorescence; Laser induced fluorescence
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- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Biochemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Optics & Photonics (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention relates to a device for detecting a perovskite thin film by utilizing photoluminescence, which comprises a photoluminescence monitoring device and a detection analysis system, wherein the photoluminescence monitoring device comprises a laser source, a telescopic lens, a monochromator, a photomultiplier and a lock-in amplifier, and the telescopic lens and the monochromator are arranged in a vacuum sealed cabin and an evaporation source controlled by an evaporation control system. Laser emitted by the laser source irradiates the surface of a perovskite solar cell substrate in the vacuum sealed cabin, so that the surface perovskite thin film is stimulated to radiate to generate exciting light, the exciting light is conveyed to the detection and analysis system after passing through the telescopic lens, the monochromator, the photomultiplier and the lock-in amplifier in sequence, and the detection and analysis system feeds back the exciting light to the evaporation control system, so that the perovskite thin film is monitored in real time. The invention also provides a method of using the apparatus. The invention controls the reaction process by monitoring the performance parameters in the production process of the perovskite thin film, and improves the repeatability of the production of each batch of perovskite thin film.
Description
Technical Field
The invention relates to the technical field of solar cell production equipment, in particular to equipment for detecting a perovskite thin film by utilizing photoluminescence and a monitoring method thereof.
Background
The solar cell is a photoelectric conversion device, and converts solar energy into electric energy by using the photovoltaic effect of a semiconductor. Solar power generation has been developed to date as the most important renewable energy source in addition to hydroelectric power generation and wind power generation. The semiconductors currently in commercial use include monocrystalline silicon, polycrystalline silicon, amorphous silicon, cadmium telluride, copper indium gallium selenide, and the like, but most of them consume much energy and are expensive.
In recent years, a perovskite solar cell which uses an organic metal halide as a light absorption layer and has a crystal structure of ABX has attracted much attention3A type cuboctahedral structure. The thin-film solar cell prepared by the material has the advantages of simple and convenient process, low production cost, stability and high conversion rate. Since 2009 to date, the photoelectric conversion efficiency has been increased from 3.8% to 23% or more, showing great commercial value.
The forming process of various perovskite solar cell thin films can be divided into two categories: solution processes and gas phase processes. The solution method is simple and convenient to operate, but the film uniformity and repeatability are poor, and the efficiency of the battery is influenced. The gas phase method comprises a double-source co-evaporation method, a gas phase auxiliary solution method, a Chemical Vapor Deposition (CVD) method and the like, wherein the gas phase solution auxiliary method can be used for preparing the perovskite thin film with uniform crystal grains, large crystal grain size and small surface roughness, but the repeatability of each batch needs to be improved.
Disclosure of Invention
The invention aims to solve the technical problem of providing equipment for detecting the perovskite thin film by utilizing photoluminescence and a monitoring method thereof, controlling the reaction process of the perovskite thin film by monitoring various performance parameters in the production process of the perovskite thin film, and improving the repeatability of the production of each batch of perovskite thin film.
The invention is realized in such a way, and provides equipment for detecting a perovskite thin film by utilizing photoluminescence, which comprises a photoluminescence monitoring device and a detection and analysis system, wherein light ray monitoring data of the photoluminescence monitoring device is transmitted to the detection and analysis system, the photoluminescence monitoring device comprises a laser source, a telescopic lens, a monochromator, a photomultiplier and a lock-in amplifier, the telescopic lens and the monochromator are arranged in a vacuum sealed cabin, a heating table for heating the perovskite solar cell substrate and an evaporation source controlled by an evaporation control system are arranged in the vacuum sealed cabin, the laser source is arranged outside the vacuum sealed cabin, laser emitted by the laser source passes through a laser channel and then irradiates the surface of the perovskite solar cell substrate in the vacuum sealed cabin, so that excited radiation of the perovskite thin film deposited on the surface of the perovskite solar cell substrate generates excited excitation light, the excited excitation light is collected by the telescopic lens and enters the monochromator, and then the excited light passes through the The single-color light is decomposed into single-color light, the single-color light is converted into an electric signal through a photomultiplier and then enters a phase-locked amplifier, the electric signal amplified by the phase-locked amplifier is transmitted to a detection and analysis system, and analysis data of the detection and analysis system are fed back to an evaporation control system.
Furthermore, the laser channel comprises an optical filter, a reflector and a channel lens, and the laser light enters the laser channel through the optical filter, then is converted and converged by the reflector to change the light path and the channel lens, and then irradiates the surface of the perovskite solar cell substrate.
Further, the telescopic lens is automatically telescopic under the control of the telescopic of the connecting rod.
Further, the testing times and time intervals of the photoluminescence monitoring device are set by a detection and analysis system.
The invention is realized in such a way, and also provides a monitoring method of the equipment for detecting the perovskite thin film by utilizing photoluminescence, which comprises the following steps:
s1, placing the perovskite solar cell substrate in a vacuum sealed cabin, and starting an evaporation source in the vacuum sealed cabin to perform chemical substance evaporation processing on the perovskite solar cell substrate;
s2, starting the photoluminescence monitoring device and the detection and analysis system, wherein laser emitted by the laser source irradiates the surface of a perovskite solar cell substrate after passing through a laser channel, a perovskite material on the surface of the perovskite solar cell can generate fluorescent exciting light after being excited by the laser, the exciting light enters a monochromator through a telescopic lens and is decomposed into monochromatic light, the monochromatic light is converted into an electric signal through a photomultiplier and then enters a phase-locked amplifier, the amplified electric signal is transmitted to the detection and analysis system by the phase-locked amplifier, and the electric signal is analyzed by the system and then fed back to the evaporation control system, so that evaporation parameters are adjusted by the evaporation control system, and the reaction process is controlled;
and S3, taking out the perovskite solar cell substrate from the vacuum sealed cabin through a conveyor belt or other modes after the evaporation processing of the perovskite solar cell substrate is finished.
Specifically, during the reaction of step S2, the number of tests and the time interval of the photoluminescence monitoring device are set by the detection and analysis system.
Compared with the prior art, the invention integrates the photoluminescence detection system into the perovskite solar cell evaporation equipment, utilizes the photoluminescence technology to monitor the film forming process of the perovskite film in real time, collects and converts fluorescent signals generated after the perovskite film is irradiated by laser into electric signals to be transmitted to the detection analysis system, and automatically adjusts the evaporation parameters through the detection analysis system, thereby achieving the purposes of controlling the evaporation reaction process and improving the repeatability of the production of each batch of perovskite film. The invention can be combined with various gas phase evaporation devices to prepare the perovskite solar cell film, and various performance parameters of the perovskite film production process are monitored at different moments or stages, so that the chemical reaction process of the film is controlled, and the metal halide completely reacts with halide steam.
Drawings
FIG. 1 is a perspective view of an apparatus for detecting perovskite thin film by photoluminescence according to a preferred embodiment of the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Taking the solution-assisted vapor phase method as an example to prepare the perovskite thin film, the preparation process comprises the following steps: firstly, one or more metal halides BX are deposited on a glass substrate by using methods of spin coating, blade coating, vacuum deposition and the like2A film.
Secondly, putting the perovskite solar cell substrate prepared in the first step into a metal sealed cabin for evaporation processing, placing one or more evaporation sources below the sealed cabin to evaporate a reactant AX, and evaporating the reactant AX and a metal halide BX on the perovskite solar cell substrate2Carrying out a chemical reaction to generate ABX3And (3) forming a film.
And thirdly, taking out the perovskite solar cell substrate after the evaporation is finished for subsequent processing.
In the first step, B is a divalent metal cation, which can be any one of cations of lead, tin, tungsten, copper, zinc, gallium, germanium, arsenic, selenium, rhodium, palladium, silver, cadmium, indium, antimony, osmium, iridium, platinum, gold, mercury, thallium, bismuth and polonium, and X is any one of anions of iodine, bromine, chlorine and astatine. BX2The thickness of the film is 80 nm-300 nm.
In the second step, A is any one of cesium, rubidium, amine group, amidino group or alkali group, and X is any one of iodine, bromine, chlorine and astatine anion. Prepared perovskite ABX3The thickness of the film is 100nm to 500 nm.
Referring to fig. 1, a preferred embodiment of the apparatus for detecting perovskite thin film by photoluminescence according to the present invention is suitable for manufacturing the perovskite solar cell and other optoelectronic devices. The preferred embodiment of the apparatus for detecting perovskite thin film by using photoluminescence of the invention comprises a photoluminescence monitoring device and a detection and analysis system 1, wherein light ray monitoring data of the photoluminescence monitoring device is transmitted to the detection and analysis system 1. The photoluminescence monitoring device comprises a laser source 2, a telescopic lens 3, a monochromator 4, a photomultiplier 5 and a lock-in amplifier 6.
The laser source 2 includes, but is not limited to, a he — ne laser, an ar ion laser, a nitrogen molecule laser, a ruby laser, a semiconductor laser, and the like.
The telescopic lens 3 is used for collecting exciting light such as fluorescence emitted after the perovskite thin film material is irradiated by the exciting light and converging the exciting light on the monochromator. Because the fixed lens can shield AX evaporant from depositing on the surface of the perovskite solar cell substrate in the evaporation process, the lens is designed into a telescopic form of a connecting rod, can be extended only when collecting emitted light and is positioned at the edge of the inner wall of an evaporation chamber when not collecting light.
The monochromator 4 is used for decomposing a broadband of exciting light emitted by the perovskite thin film after being irradiated by laser into a single chromatogram so as to obtain a specific fluorescence spectrum of the perovskite thin film.
The photomultiplier 5 is used for converting a weak optical signal received by the monochromator into an electric signal and then transmitting the electric signal to the phase-locked amplifier.
The phase-locked amplifier 6 is used for amplifying the electric signal transmitted by the photomultiplier tube, and then the electric signal can be recorded and analyzed by the detection and analysis system.
The telescopic lens 3 and the monochromator 4 are arranged in a vacuum sealed cabin 7, and a heating table 9 for heating the perovskite solar cell substrate 8 is arranged in the vacuum sealed cabin 7. A perovskite solar cell substrate 8 and an evaporation source 10 controlled by an evaporation control system are placed on the lower portion of the heating stage 9. In the present embodiment, a plurality of evaporation sources 10 are provided in the vacuum sealed chamber 7.
The laser source 2 is arranged outside the vacuum-tight capsule 7. Laser emitted by the laser source 2 passes through the laser channel 11 and then irradiates the surface of the perovskite solar cell substrate 8 in the vacuum sealed cabin 7, so that the perovskite thin film deposited on the surface of the perovskite solar cell substrate 8 is stimulated to radiate to generate exciting light, and the exciting light is collected by the telescopic lens 3 and enters the monochromator 4 to be decomposed into monochromatic light. The monochromatic light is converted into an electric signal by a photomultiplier 5 and enters a phase-locked amplifier 6 for amplification. The electric signal data amplified by the lock-in amplifier 6 is transmitted to the detection and analysis system 1. The analysis data of the detection and analysis system 1 is fed back to an evaporation control system (not shown in the figure), so that evaporation parameters are adjusted by the evaporation control system to control the reaction process.
The laser channel 11 includes a mirror 12, a channel lens 13, and a filter 14. The laser light enters the laser channel 11 through the optical filter 14, then is converted and converged through the reflector 12 and the channel lens 13, and then is irradiated onto the surface of the perovskite solar cell substrate 8.
The channel lens 13 is used for collecting laser emitted by the laser source and irradiating the laser to the surface of the perovskite solar cell substrate in the form of single beam with a specific wavelength.
The telescopic lens 3 is automatically telescopic under the control of the telescopic of the connecting rod.
The real-time monitoring device of the present invention may be used in conjunction or alone in various vaporization systems for manufacturing perovskite cells, as well as in combination with other testing methods. The number of tests and the time interval of the photoluminescence monitoring device are set by the detection and analysis system 1.
A layer of metal halide BX is prepared on the surface of the perovskite solar cell substrate in advance2Then feeding into a vapor deposition chamber, and heating and evaporating the reactant AX to react with BX2Reaction to form perovskite ABX3. In the process, the perovskite thin film is gradually formed, the material components and the crystal structure of the perovskite thin film are changed from time to time, and the material corresponding to each reaction time has the intrinsic spectral response property, so that the surface of the perovskite solar cell substrate can be irradiated at a specific time through a photoluminescence technical means to generate exciting light, and the exciting light is collected, converted, processed and analyzed to feed back information to an evaporation control system, so that the purposes of monitoring the reaction process and regulating and controlling evaporation parameters are achieved.
The invention also provides a monitoring method of the equipment for detecting the perovskite thin film by utilizing photoluminescence, which comprises the following steps:
s1, placing the perovskite solar cell substrate 8 in a vacuum sealed cabin 7, and starting an evaporation source 10 in the vacuum sealed cabin 7 to carry out chemical substance evaporation processing on the perovskite solar cell substrate 8.
S2, open photoluminescence monitoring devices and detection and analysis system 1, the laser that laser source 2 sent shines perovskite solar cell substrate 8 surface behind laser channel 11, makes the perovskite film of deposit on perovskite solar cell substrate 8 surface produce the excitation light of fluorescence class after the stimulated radiation, and the excitation light passes through telescopic lens 3 and gets into monochromator 4, monochromator 4 gets into photomultiplier 5 after decomposing the excitation light that the perovskite film produced into the monochromatic light of specific wavelength in real time, and photomultiplier 5 converts monochromatic light signal into the signal of telecommunication and transmits to detection and analysis system 1 after receiving the amplification through lock-in amplifier 6, again from this system analysis back feedback in evaporation control system, thereby pass through evaporation control system adjusts the coating by vaporization parameter, control reaction process.
And S3, taking out the perovskite solar cell substrate 8 from the vacuum sealed cabin 7 through a conveyor belt or other modes after the evaporation processing is finished.
Specifically, in the reaction process of step S2, the number of tests and the time interval of the photoluminescence monitoring device are set by the detection and analysis system 1.
Since the photoluminescence spectrum is closely related to the electronic structure, defect state, impurities, and the like of the semiconductor material, the properties of the perovskite thin film crystal can be intuitively understood. In the vapor deposition reaction process for manufacturing the perovskite solar cell, the invention can utilize photoluminescence spectra of perovskite thin films at different reaction stages to know the change of the photoelectric properties of the perovskite thin films at different reaction stages, and analyze and judge the optimal vapor deposition conditions; the reaction process or evaporation parameters of the perovskite thin film can be controlled by comparing the known photoluminescence spectrum with the real-time test result, and the property difference of each batch of perovskite thin film can also be judged.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (6)
1. The equipment for detecting the perovskite thin film by utilizing photoluminescence is characterized by comprising a photoluminescence monitoring device and a detection and analysis system, wherein light monitoring data of the photoluminescence monitoring device is transmitted to the detection and analysis system, the photoluminescence monitoring device comprises a laser source, a telescopic lens, a monochromator, a photomultiplier and a lock-in amplifier, the telescopic lens and the monochromator are arranged in a vacuum sealed cabin, a heating table for heating the perovskite solar cell substrate and an evaporation source controlled by an evaporation control system are arranged in the vacuum sealed cabin, the laser source is arranged outside the vacuum sealed cabin, laser emitted by the laser source passes through a laser channel and then irradiates the surface of the perovskite solar cell substrate in the vacuum sealed cabin, so that the perovskite thin film deposited on the surface of the perovskite solar cell substrate generates exciting light after being stimulated and radiated, the device comprises a phase-locked amplifier, a detection and analysis system, a telescopic lens, a photoelectric multiplier tube, a phase-locked amplifier, an evaporation control system and a control system.
2. The apparatus for detecting perovskite thin film by photoluminescence as claimed in claim 1, wherein the laser channel comprises an optical filter, a reflector and a channel lens, and the laser light enters the laser channel through the optical filter, then is converted and converged by the reflector to change the optical path and the channel lens, and then is irradiated onto the surface of the perovskite solar cell substrate.
3. The apparatus for perovskite thin film detection using photoluminescence as defined in claim 1, wherein the telescopic lens is automatically telescopic by controlling the telescopic of the connecting rod.
4. The apparatus for perovskite thin film detection using photoluminescence as defined in claim 1, wherein the number and time intervals of the tests of the photoluminescence monitoring device are set by a detection analysis system.
5. A method for monitoring an apparatus for perovskite thin film detection using photoluminescence as defined in any one of claims 1 to 4, comprising the steps of:
s1, placing the perovskite solar cell substrate in a vacuum sealed cabin, and starting an evaporation source in the vacuum sealed cabin to perform chemical substance evaporation processing on the perovskite solar cell substrate;
s2, starting the photoluminescence monitoring device and the detection and analysis system, wherein laser emitted by the laser source irradiates the surface of the perovskite solar cell substrate after passing through a laser channel, so that excited radiation is generated on the perovskite thin film deposited on the surface of the perovskite solar cell substrate, the excited light enters the monochromator through the telescopic lens and is decomposed into monochromatic light, the monochromatic light enters the phase-locked amplifier through the photomultiplier, the phase-locked amplifier transmits an amplified electric signal to the detection and analysis system, and the amplified electric signal is analyzed by the phase-locked amplifier and then fed back to the evaporation control system, so that evaporation parameters are adjusted by the evaporation control system, and the reaction process is controlled;
and S3, taking out the perovskite solar cell substrate from the vacuum sealed cabin through a conveyor belt or other modes after the evaporation processing of the perovskite solar cell substrate is finished.
6. The method for monitoring an apparatus for perovskite thin film detection using photoluminescence as defined in claim 5, wherein the number and time interval of tests of said photoluminescence monitoring device are set by a detection analysis system during the reaction of step S2.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115597501A (en) * | 2022-09-30 | 2023-01-13 | 中山吉联光电科技有限公司（Cn） | High-precision wide-spectrum optical film thickness online monitoring system |
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