CN209344035U - A kind of equipment of real-time monitoring perovskite thin film quality of forming film - Google Patents
A kind of equipment of real-time monitoring perovskite thin film quality of forming film Download PDFInfo
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- CN209344035U CN209344035U CN201822232726.4U CN201822232726U CN209344035U CN 209344035 U CN209344035 U CN 209344035U CN 201822232726 U CN201822232726 U CN 201822232726U CN 209344035 U CN209344035 U CN 209344035U
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Abstract
The utility model relates to a kind of equipment of real-time monitoring perovskite thin film quality of forming film, including X-ray diffraction monitoring device and analysis statistical system, X-ray diffraction monitoring device includes sliding rail, angular instrument annulus, X-ray emission device, X-ray reception device and pedometer, measurement-recording system, the X-ray of X-ray emission device transmitting projects perovskite solar cell substrates surface and generates diffraction, the data for capturing diffracted ray are transmitted to measurement-recording system by X-ray reception device and pedometer, the data are transmitted to analysis statistical system by measurement-recording system, the analysis data feedback of statistical system is analyzed to evaporation control system.The performance parameter in production process that the utility model passes through monitoring perovskite thin film, controls its reaction process, improves the repeatability of each batch perovskite thin film production.
Description
Technical field
The utility model relates to the technical field of manufacture of solar cells equipment, in particular to a kind of real-time monitoring perovskite
The equipment of forming thin film quality.
Background technique
Solar battery is a kind of electrooptical device, is converted solar energy into electrical energy using the photovoltaic effect of semiconductor.
It is developed so far, solar power generation has become the most important renewable energy in addition to hydroelectric generation and wind-power electricity generation.It is current in
Commercialized semiconductor has monocrystalline silicon, polysilicon, amorphous silicon, cadmium telluride, copper indium gallium selenide etc., but energy consumption is high, at high cost mostly.
In recent years, a kind of perovskite solar battery receives significant attention, and this perovskite solar battery is with organic gold
Category halide is light absorbing layer.Perovskite is ABX3The cuboctahedron structure of type.The thin film solar electricity of such material preparation
Pool process is easy, production cost is low, stable and high conversion rate.So far from 2009, photoelectric conversion efficiency is promoted to 22% from 3.8%
More than, it has been higher than commercialized crystal silicon solar batteries and there is biggish cost advantage.
Various perovskite solar battery thin film moulding process can be divided into two major classes: solwution method and vapor phase method.Solwution method behaviour
Make simplicity, but film uniformity, poor repeatability, influences the efficiency of battery.Vapor phase method has double source coevaporation method, gas phase assisted solution
The methods of method, chemical vapor deposition (CVD), wherein it is thick can to prepare uniform crystal grain, big crystal grain size, surface for gas phase solution auxiliary law
The small perovskite thin film of rugosity, but the repeatability of each batch is to be improved.
Utility model content
Technical problem to be solved by the utility model is to provide a kind of real-time monitoring perovskite thin film quality of forming film
Equipment, all kinds of performance parameters in production process by monitoring perovskite thin film, controls its reaction process, improves each batch calcium
The repeatability of titanium ore film production.
The utility model is realized in this way providing a kind of equipment of real-time monitoring perovskite thin film quality of forming film, including X
X ray diffraction monitoring device and analysis statistical system, the X-ray monitoring data of the X-ray diffraction monitoring device are transmitted to point
Analyse statistical system, the X-ray diffraction monitoring device includes that sliding rail, angular instrument annulus, X-ray emission device, X-ray connect
Receiving apparatus and pedometer, measurement-recording system, the sliding rail, angular instrument annulus, X-ray emission device and X-ray connect
Receiving apparatus and pedometer are arranged in vacuum sealing cabin, and heating perovskite solar battery is provided in the vacuum sealing cabin
The heating device of substrate, and it is evaporated the evaporation source of control system control, the sliding rail is fixed in vacuum sealing cabin,
The angular instrument annulus is slided along sliding rail, and the X-ray emission device and X-ray reception device and pedometer setting exist
On angular instrument annulus, the X-ray reception device and pedometer are rotated around angular instrument annulus, and the X-ray emission device is continuous
Change incidence angle, the X-ray of transmitting projects perovskite solar cell substrates surface and generates diffraction, and the X-ray receives dress
It sets and the data for capturing diffracted ray is transmitted to measurement-recording system by pedometer, the measurement-recording system transmits the data
To analysis statistical system, the analysis data feedback for analyzing statistical system to evaporation control system.
Further, the testing time of the X-ray diffraction monitoring device and time interval are arranged by analysis statistical system.
Compared with prior art, the equipment of the real-time monitoring perovskite thin film quality of forming film of the utility model gives birth to vapor deposition
Perovskite solar cell substrates carry out interim or successional X-ray diffraction test during production, by stage or even
The X-ray diffraction test of continuous property understands the information such as ingredient, the crystal structure of perovskite solar cell substrates surface film, passes through
Analyze statistical system will analyze data feedback to deposition system automatically adjust evaporation plating parameter, thus reach control vapor deposition react into
Journey improves the repeated purpose of each batch perovskite thin film production.The utility model can be made in conjunction with all kinds of gas evaporation equipment
Standby perovskite solar battery thin film, in different moments or all kinds of performances ginseng of interim monitoring perovskite thin film production process
Number, to control the chemical reaction course of film, makes metal halide and halide vapor fully reacting.
Detailed description of the invention
Fig. 1 is the three-dimensional signal of one preferred embodiment of equipment of the utility model real-time monitoring perovskite thin film quality of forming film
Figure;
Fig. 2 is the X-ray diffraction that perovskite solar cell substrates film is tested in the differential responses stage of preparation
Figure;
Fig. 3 is the J-V curve of the perovskite solar battery prepared using the device and method of the utility model.
Specific embodiment
In order to which technical problem to be solved in the utility model, technical solution and beneficial effect is more clearly understood, with
Lower combination accompanying drawings and embodiments, the present invention will be further described in detail.It should be appreciated that specific reality described herein
It applies example to be only used to explain the utility model, is not used to limit the utility model.
Illustrate the production method of existing perovskite solar battery thin film first.
The first step is depositing one or more gold using the methods of spin coating, blade coating, vacuum deposition first on the glass substrate
Belong to halide BX2Film.
Perovskite solar cell substrates made of the first step are put into metal sealing cabin and carry out vapor deposition processing by second step,
It is placed on one or more evaporation source evaporation reactant AX, evaporation reactant AX and perovskite solar cell substrates in sealed compartment
Metal halide BX2Reaction generates ABX3Type perovskite thin film.
Perovskite solar cell substrates, which are taken out, after the completion of third step, vapor deposition carries out following process.
In the first step, B is divalent metal, can for lead, tin, tungsten, copper, zinc, gallium, germanium, arsenic, selenium, rhodium, palladium, silver,
Cadmium, indium, antimony, osmium, iridium, platinum, gold, mercury, thallium, bismuth, any one cation in polonium, X be iodine, bromine, chlorine, in astatine any one yin from
Son.BX2Film thickness is in 80nm ~ 300nm.
In second step, A is arbitrary a kind of cation in caesium, rubidium, amido, amidino groups or alkali family, X be iodine, bromine, chlorine,
Any one anion in astatine.The perovskite ABX of preparation3Type film thickness is 100nm ~ 500nm.
It please refers to shown in Fig. 1, the preferred embodiment of the equipment of the utility model real-time monitoring perovskite thin film quality of forming film,
Suitable for preparing perovskite solar battery and other photoelectric devices above-mentioned.Because X-ray diffraction test can be appreciated that material
All there is specific X-ray diffraction peak in the information such as ingredient, crystal structure, each substance, thus can analysis detection by X-ray diffraction
The information such as ingredient, crystal structure of different phase perovskite thin film in the film vapor deposition reaction process of perovskite solar battery,
Make it possible the optimal evaporation condition of Exploring Analysis.The XRD spectra that can also be obtained by known XRD spectrum and real-time testing
Comparison understands the extent of reaction of this stage perovskite thin film, and by the information feedback after analysis in vapor deposition control system, to control
Reaction process processed or other evaporation plating parameters.
The preferred embodiment of the equipment of the utility model real-time monitoring perovskite thin film quality of forming film, including X-ray diffraction
Monitoring device and analysis statistical system 1, the X-ray monitoring data of the X-ray diffraction monitoring device are transmitted to analysis statistics
System 1.
The X-ray diffraction monitoring device includes that sliding rail 2, angular instrument annulus 3, X-ray emission device 4, X-ray connect
Receiving apparatus and pedometer 5 and measurement-recording system 6.The sliding rail 2, angular instrument annulus 3, X-ray emission device 4 and
X-ray reception device and pedometer 5 are arranged in vacuum sealing cabin 7.
Be provided in the vacuum sealing cabin 7 heating perovskite solar cell substrates 8 heating device 9, and by
The evaporation source 10 of evaporation control system control.In the present embodiment, multiple evaporation sources 10 are provided in the vacuum sealing cabin 7.
The sliding rail 2 is fixed in vacuum sealing cabin 7, and the angular instrument annulus 3 is slided along sliding rail 2, the X
Radiation-emitting device 4 and X-ray reception device and pedometer 5 are arranged on angular instrument annulus 3, the X-ray reception device
And pedometer 5 is rotated around angular instrument annulus 3.
When X-ray diffraction monitoring device is tested, the angular instrument annulus 3 slides into calcium along sliding rail 2
At titanium ore solar cell substrates 8, the X-ray emission device 4 and X-ray reception device and pedometer 5 start to work into
Row measurement.After to be tested, the angular instrument annulus 3 is removed from perovskite solar cell substrates 8 along sliding rail 2,
8 vapor deposition process of perovskite solar cell substrates is not influenced.In test process, the X-ray emission device 4 constantly changes incident
Angle θ, the X-ray reception device and pedometer 5 are rotated around angular instrument annulus 3, and it is strong to receive the corresponding diffraction of 2 θ of different angle of diffraction
Degree.
The X-ray that the X-ray emission device 4 emits projects 8 surface of perovskite solar cell substrates and generates diffraction,
5 data for capturing diffracted ray of the X-ray reception device and pedometer are transmitted to measurement-recording system 6.The measurement note
The data are transmitted to analysis statistical system 1 by recording system 6.The analysis data feedback of the analysis statistical system 1 is to evaporation control
System (not shown).
The X-ray reception device and pedometer 5 monitor the X by 8 surface of perovskite solar cell substrates in real time
The diffracted ray of ray simultaneously by 6 reception of measurement-recording system handle after is transmitted to analysis statistical system 1, then thus system feedback in
Evaporation control system controls reaction process to adjust other evaporation plating parameters by the evaporation control system.
The real-time watch device of the utility model can be in the vapo(u)rization system of various manufacture perovskite batteries collectively or individually
It uses, can also be used in combination with other test methods.The testing time and time interval of the X-ray diffraction monitoring device are by dividing
Statistical system 1 is analysed to be arranged.
Combined with specific embodiments below come illustrate the utility model real-time monitoring perovskite thin film quality of forming film equipment.
Embodiment 1
A kind of device and method progress perovskite of the real-time monitoring perovskite thin film quality of forming film using the utility model
The preparation process of the solar film battery of film forming, comprising the following steps:
(1) by the ito glass plate of 2.5 × 2.5cm successively through dish washing liquid, deionized water, acetone, each cleaning of isopropanol ultrasound
30min, then use N210min is handled through UV O-zone after drying.
(2) spin coating PEDOT:PSS, 90 DEG C ~ 150 DEG C drying 5min ~ 20min, is prepared hole transmission layer.
(3) by PbI2It is dissolved in DMF, concentration 1M, 70 DEG C of stirring 2h obtain PbI in the spin coating of the upper layer PEDOT:PSS2It is thin
Film, 70 DEG C ~ 100 DEG C annealing 5min ~ 60min.
(4) PbI will be deposited with2The substrate of film is put into vacuum sealing cabin, opens evaporation source and evaporates MAI.
(5) it opens X-ray diffraction monitoring device and analysis statistical system, X-ray emission device constantly changes incidence angle θ
The x-ray bombardment of sending generates diffraction to perovskite solar cell substrates surface, the X-ray reception device and pedometer around
The rotation of angular instrument annulus receives the corresponding diffracted ray of different angle of diffraction, and the data of the diffracted ray received is transmitted to measurement
Record system, is arranged test interval in testing and analysis system, and test angle range is 10o -60o。
(6) reaction terminate, the perovskite solar cell substrates prepared are taken out out of vacuum sealing cabin, perovskite too
It is positive to deposit electron transfer layer PCBM on cell substrate.
(7) evaporation metal conductive layer Au electrode, obtains solar battery.
Fig. 2 is the X of the perovskite thin film of differential responses stage test of the perovskite solar cell substrates film in preparation
X ray diffration pattern x, with the progress of reaction, PbI2Characteristic peak gradually weaken, the characteristic peak of perovskite gradually increases, until reaction
Terminate, PbI2Characteristic peak completely disappear.
Fig. 3 is to be prepared using the equipment and its monitoring method of the real-time monitoring perovskite thin film quality of forming film of the utility model
Perovskite solar battery J-V curve, as can be seen from the figure PCE is up to 16.47%.
The above is only the preferred embodiment of the utility model only, is not intended to limit the utility model, all at this
Made any modifications, equivalent replacements, and improvements etc., should be included in the utility model within the spirit and principle of utility model
Protection scope within.
Claims (2)
1. a kind of equipment of real-time monitoring perovskite thin film quality of forming film, which is characterized in that including X-ray diffraction monitoring device with
And analysis statistical system, the X-ray monitoring data of the X-ray diffraction monitoring device are transmitted to analysis statistical system, the X is penetrated
Line diffraction monitoring device includes sliding rail, angular instrument annulus, X-ray emission device, X-ray reception device and pedometer, survey
Measure record system, the sliding rail, angular instrument annulus, X-ray emission device and X-ray reception device and pedometer setting
In vacuum sealing cabin, the heating device of heating perovskite solar cell substrates is provided in the vacuum sealing cabin, with
And it is evaporated the evaporation source of control system control, the sliding rail is fixed in vacuum sealing cabin, angular instrument annulus edge
Sliding rail sliding, the X-ray emission device and X-ray reception device and pedometer are arranged on angular instrument annulus, institute
It states X-ray reception device and pedometer to rotate around angular instrument annulus, the X-ray emission device constantly changes incidence angle, emits
X-ray project perovskite solar cell substrates surface and generate diffraction, the X-ray reception device and pedometer are capturing
Data to diffracted ray are transmitted to measurement-recording system, which is transmitted to analysis statistical system by the measurement-recording system,
The analysis data feedback of the analysis statistical system is to evaporation control system.
2. the equipment of real-time monitoring perovskite thin film quality of forming film as described in claim 1, which is characterized in that the X-ray
The testing time and time interval of diffraction monitoring device are arranged by analysis statistical system.
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Cited By (1)
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CN109509711A (en) * | 2018-12-28 | 2019-03-22 | 杭州纤纳光电科技有限公司 | A kind of equipment and its monitoring method of real-time monitoring perovskite thin film quality of forming film |
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CN109509711A (en) * | 2018-12-28 | 2019-03-22 | 杭州纤纳光电科技有限公司 | A kind of equipment and its monitoring method of real-time monitoring perovskite thin film quality of forming film |
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