CN109509711A - A kind of equipment and its monitoring method of real-time monitoring perovskite thin film quality of forming film - Google Patents
A kind of equipment and its monitoring method of real-time monitoring perovskite thin film quality of forming film Download PDFInfo
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- CN109509711A CN109509711A CN201811623264.7A CN201811623264A CN109509711A CN 109509711 A CN109509711 A CN 109509711A CN 201811623264 A CN201811623264 A CN 201811623264A CN 109509711 A CN109509711 A CN 109509711A
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- 239000010409 thin film Substances 0.000 title claims abstract description 39
- 238000012544 monitoring process Methods 0.000 title claims abstract description 38
- 239000010408 film Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000000758 substrate Substances 0.000 claims abstract description 38
- 238000004458 analytical method Methods 0.000 claims abstract description 35
- 238000001704 evaporation Methods 0.000 claims abstract description 33
- 230000008020 evaporation Effects 0.000 claims abstract description 33
- 238000002441 X-ray diffraction Methods 0.000 claims abstract description 28
- 238000012806 monitoring device Methods 0.000 claims abstract description 22
- 238000004846 x-ray emission Methods 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 238000007789 sealing Methods 0.000 claims description 22
- 238000012360 testing method Methods 0.000 claims description 15
- 238000007740 vapor deposition Methods 0.000 claims description 11
- 238000012545 processing Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000007747 plating Methods 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 3
- 238000010304 firing Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- 239000013078 crystal Substances 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 239000010931 gold Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 150000004820 halides Chemical class 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000004528 spin coating Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 229910052789 astatine Inorganic materials 0.000 description 2
- RYXHOMYVWAEKHL-UHFFFAOYSA-N astatine atom Chemical compound [At] RYXHOMYVWAEKHL-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 2
- 229910052794 bromium Inorganic materials 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910001507 metal halide Inorganic materials 0.000 description 2
- 150000005309 metal halides Chemical class 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- MARUHZGHZWCEQU-UHFFFAOYSA-N 5-phenyl-2h-tetrazole Chemical compound C1=CC=CC=C1C1=NNN=N1 MARUHZGHZWCEQU-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- 229920000144 PEDOT:PSS Polymers 0.000 description 1
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- MCEWYIDBDVPMES-UHFFFAOYSA-N [60]pcbm Chemical compound C123C(C4=C5C6=C7C8=C9C%10=C%11C%12=C%13C%14=C%15C%16=C%17C%18=C(C=%19C=%20C%18=C%18C%16=C%13C%13=C%11C9=C9C7=C(C=%20C9=C%13%18)C(C7=%19)=C96)C6=C%11C%17=C%15C%13=C%15C%14=C%12C%12=C%10C%10=C85)=C9C7=C6C2=C%11C%13=C2C%15=C%12C%10=C4C23C1(CCCC(=O)OC)C1=CC=CC=C1 MCEWYIDBDVPMES-UHFFFAOYSA-N 0.000 description 1
- JTCFNJXQEFODHE-UHFFFAOYSA-N [Ca].[Ti] Chemical compound [Ca].[Ti] JTCFNJXQEFODHE-UHFFFAOYSA-N 0.000 description 1
- KTSFMFGEAAANTF-UHFFFAOYSA-N [Cu].[Se].[Se].[In] Chemical compound [Cu].[Se].[Se].[In] KTSFMFGEAAANTF-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical group [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 1
- 125000003739 carbamimidoyl group Chemical group C(N)(=N)* 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004851 dishwashing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910052699 polonium Inorganic materials 0.000 description 1
- HZEBHPIOVYHPMT-UHFFFAOYSA-N polonium atom Chemical compound [Po] HZEBHPIOVYHPMT-UHFFFAOYSA-N 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical group [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229910052716 thallium Inorganic materials 0.000 description 1
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 238000005019 vapor deposition process Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L22/00—Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
- H01L22/10—Measuring as part of the manufacturing process
- H01L22/12—Measuring as part of the manufacturing process for structural parameters, e.g. thickness, line width, refractive index, temperature, warp, bond strength, defects, optical inspection, electrical measurement of structural dimensions, metallurgic measurement of diffusions
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L22/00—Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
- H01L22/20—Sequence of activities consisting of a plurality of measurements, corrections, marking or sorting steps
- H01L22/26—Acting in response to an ongoing measurement without interruption of processing, e.g. endpoint detection, in-situ thickness measurement
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The present invention 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 present invention also provides a kind of monitoring methods of the equipment of real-time monitoring perovskite thin film quality of forming film.The performance parameter in production process that the present invention passes through monitoring perovskite thin film, controls its reaction process, improves the repeatability of each batch perovskite thin film production.
Description
Technical field
The present invention relates to the technical field of manufacture of solar cells equipment, in particular to a kind of real-time monitoring perovskite thin film
The equipment and its monitoring method of quality of forming film.
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.
Summary of the invention
Technical problem to be solved by the present invention lies in provide a kind of equipment of real-time monitoring perovskite thin film quality of forming film
And its monitoring method, all kinds of performance parameters in production process by monitoring perovskite thin film control its reaction process, improve
The repeatability of each batch perovskite thin film production.
The invention is realized in this way providing 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, the X-ray monitoring data of the X-ray diffraction monitoring device are transmitted to analysis system
Meter systems, the X-ray diffraction monitoring device include sliding rail, angular instrument annulus, X-ray emission device, X-ray reception dress
It sets and pedometer, measurement-recording system, the sliding rail, angular instrument annulus, X-ray emission device and X-ray receives dress
It sets and pedometer is arranged in vacuum sealing cabin, heating perovskite solar cell substrates are provided in the vacuum sealing cabin
Heating device, and be evaporated control system control evaporation source, the sliding rail is fixed in vacuum sealing cabin, described
Angular instrument annulus is slided along sliding rail, and the X-ray emission device and X-ray reception device and pedometer are arranged in angle measurement
On instrument annulus, the X-ray reception device and pedometer are rotated around angular instrument annulus, and the X-ray emission device constantly changes
Incidence angle, the X-ray of transmitting project perovskite solar cell substrates surface generate diffraction, the X-ray reception device and
The data for capturing diffracted ray are transmitted to measurement-recording system by pedometer, which is transmitted to point by the measurement-recording system
Analyse 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.
The invention is realized in this way also providing real-time monitoring perovskite thin film quality of forming film described in above-mentioned one
The monitoring method of equipment, comprising the following steps:
S1, the perovskite solar cell substrates are placed in vacuum sealing cabin, open the evaporation source pair in vacuum sealing cabin
Perovskite solar cell substrates carry out chemical substance vapor deposition processing；
S2, the X-ray diffraction monitoring device and analysis statistical system are opened, the X-ray emission device constantly change into
The x-ray bombardment of firing angle, sending generates X-ray diffraction, the X-ray reception device to perovskite solar cell substrates surface
And pedometer is rotated around angular instrument annulus, receives the corresponding diffracted ray of different angle of diffraction, and by the data of the diffracted ray received
It is transmitted to measurement-recording system, which is transmitted to analysis statistical system by the measurement-recording system, then thus system feedback
In evaporation control system, to adjust other evaporation plating parameters by the evaporation control system, control perovskite thin film react into
Journey；
After processing is completed, communicated band or other modes are from vacuum sealing cabin for S3, perovskite solar cell substrates vapor deposition
It is interior to take out the perovskite solar cell substrates being deposited.
Specifically, in the reaction process of step S2, the testing time and time interval of the X-ray diffraction monitoring device
It is arranged by analysis statistical system.
Compared with prior art, the equipment and its monitoring method of real-time monitoring perovskite thin film quality of forming film of the invention,
Interim or successional X-ray diffraction test is carried out to perovskite solar cell substrates in vapor deposition production process, passes through rank
Section property or the test of successional X-ray diffraction understand ingredient, the crystal structure etc. of perovskite solar cell substrates surface film
Information will analyze data feedback to deposition system by analysis statistical system and automatically adjust evaporation plating parameter, steam to reach control
Reaction process is plated, the repeated purpose of each batch perovskite thin film production is improved.The present invention can be with all kinds of gas evaporation equipment knots
Conjunction prepares perovskite solar battery thin film, in different moments or all kinds of performances of interim monitoring perovskite thin film production process
Parameter makes metal halide and halide vapor fully reacting to control the chemical reaction course of film.
Detailed description of the invention
Fig. 1 is the stereoscopic schematic diagram of one preferred embodiment of equipment of real-time monitoring perovskite thin film quality of forming film of the present invention；
Fig. 2 is the X-ray diffractogram that perovskite solar cell substrates film is tested in the differential responses stage of preparation；
Fig. 3 is the J-V curve of the perovskite solar battery prepared using device and method of the invention.
Specific embodiment
In order to which technical problems, technical solutions and advantages to be solved are more clearly understood, tie below
Accompanying drawings and embodiments are closed, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only
To explain the present invention, it is not intended to limit the present invention.
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 real-time monitoring perovskite thin film quality of forming film of the present invention, is applicable in
In preparing perovskite solar battery and other photoelectric devices above-mentioned.Because X-ray diffraction test can be appreciated that material ingredient,
All there is specific X-ray diffraction peak in the information such as crystal structure, each substance, thus can analysis detection calcium titanium by X-ray diffraction
The information such as ingredient, crystal structure of different phase perovskite thin film, make to visit in the film vapor deposition reaction process of mine solar battery
Rope is analyzed optimal evaporation condition and is possibly realized.The XRD spectra pair that can also be obtained by known XRD spectrum and real-time testing
Than the extent of reaction of this stage perovskite thin film being understood, and by the information feedback after analysis in vapor deposition control system, to control
Reaction process or other evaporation plating parameters.
The preferred embodiment of the equipment of real-time monitoring perovskite thin film quality of forming film of the present invention, 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 statistical 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.
Real-time watch device of the invention can collectively or individually use in the vapo(u)rization system of various manufacture perovskite batteries,
It can also be used in combination with other test methods.The testing time and time interval of the X-ray diffraction monitoring device are united by analysis
Meter systems 1 are arranged.
The present invention also provides the monitoring sides of the equipment of real-time monitoring perovskite thin film quality of forming film described in above-mentioned one
Method, comprising the following steps:
S1, the perovskite solar cell substrates 8 are placed in vacuum sealing cabin 7, open the evaporation source in vacuum sealing cabin 7
10 pairs of perovskite solar cell substrates 8 carry out chemical substance vapor deposition processing.
S2, the X-ray diffraction monitoring device and analysis statistical system 1 are opened, the X-ray emission device 4 is constantly
Change the x-ray bombardment that incidence angle θ issues and generate diffraction to 8 surface of perovskite solar cell substrates, the X-ray receives dress
It sets and the diffracted ray data received is transmitted to measurement-recording system 6 by pedometer 5, the measurement-recording system 6 is by the data
It is transmitted to analysis statistical system 1, then thus system feedback is in evaporation control system, to adjust by the evaporation control system
Other evaporation plating parameters control perovskite thin film reaction process；
After processing is completed, communicated band or other modes are from vacuum sealing cabin for S3, the perovskite solar cell substrates 8 vapor deposition
The perovskite solar cell substrates 8 being deposited are taken out in 7.
Specifically, in the reaction process of step S2, the testing time and time interval of the X-ray diffraction monitoring device
It is arranged by analysis statistical system 1.
Combined with specific embodiments below come illustrate real-time monitoring perovskite thin film quality of forming film of the invention equipment and its
Monitoring method.Example 1
A kind of device and method using real-time monitoring perovskite thin film quality of forming film of the invention carry out perovskite film forming too
The preparation process of positive energy hull cell, 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 the calcium using equipment and its monitoring method preparation of real-time monitoring perovskite thin film quality of forming film of the invention
The J-V curve of titanium ore solar battery, as can be seen from the figure PCE is up to 16.47%.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (4)
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.
3. a kind of monitoring method of the equipment of real-time monitoring perovskite thin film quality of forming film as claimed in claim 1 or 2, special
Sign is, comprising the following steps:
S1, the perovskite solar cell substrates are placed in vacuum sealing cabin, open the evaporation source pair in vacuum sealing cabin
Perovskite solar cell substrates carry out chemical substance vapor deposition processing；
S2, the X-ray diffraction monitoring device and analysis statistical system are opened, the X-ray emission device constantly change into
The x-ray bombardment that firing angle issues generates X-ray diffraction, the X-ray reception device to perovskite solar cell substrates surface
And pedometer is rotated around angular instrument annulus, receives the corresponding diffracted ray of different angle of diffraction；And by the data of the diffracted ray received
It is transmitted to measurement-recording system, which is transmitted to analysis statistical system by the measurement-recording system, then thus system feedback
In evaporation control system, to adjust other evaporation plating parameters by the evaporation control system, control perovskite thin film react into
Journey；
After processing is completed, communicated band or other modes are from vacuum sealing cabin for S3, perovskite solar cell substrates vapor deposition
It is interior to take out the perovskite solar cell substrates being deposited.
4. the monitoring method of the equipment of real-time monitoring perovskite thin film quality of forming film as claimed in claim 3, which is characterized in that
In the reaction process of step S2, the testing time and time interval of the X-ray diffraction monitoring device are by analysis statistical system
Setting.
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| CN112748218A (en) * | 2020-12-20 | 2021-05-04 | 浙江大学 | On-line real-time monitoring system for preparing perovskite semiconductor photoelectric device |
| CN117637545A (en) * | 2023-11-30 | 2024-03-01 | 重庆大学 | Preparation method and preparation system of semi-automatic perovskite solar cell for laboratory |
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