CN107170896A - A kind of perovskite flexible optical detector and preparation method thereof - Google Patents

A kind of perovskite flexible optical detector and preparation method thereof Download PDF

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Publication number
CN107170896A
CN107170896A CN201710295145.2A CN201710295145A CN107170896A CN 107170896 A CN107170896 A CN 107170896A CN 201710295145 A CN201710295145 A CN 201710295145A CN 107170896 A CN107170896 A CN 107170896A
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perovskite
solution
scraper
optical detector
substrate
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CN107170896B (en
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赵奎
李剑波
刘渝城
刘生忠
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Shaanxi Normal University
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    • H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
    • H10K30/10—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising heterojunctions between organic semiconductors and inorganic semiconductors
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Abstract

A kind of perovskite flexible optical detector of the present invention and preparation method thereof, comprises the following steps, step 1, prepares perovskite solution；Step 2, perovskite thin film is prepared by unidirectional doctor blade method on the flexible substrate after cleaning-drying, obtains perovskite fexible film；Step 3, the perovskite fexible film prepared is made annealing treatment；Step 4, gold electrode is deposited on perovskite fexible film after annealing, obtains perovskite flexible optical detector.The film is compared to perovskite thin film prepared by traditional spin-coating method, has crystalline quality high in performance, and crystal boundary is few, and absorption bands is wide, carrier lifetime is long, the advantages of air-stable is good, in technology of preparing, cost is low, simple production process, and energy consumption is low and can mass produce.Perovskite flexible optical detector based on the present invention has very excellent optical detection rate, optical responsivity, Bending Stability and device lifetime.

Description

A kind of perovskite flexible optical detector and preparation method thereof
Technical field
The present invention relates to flexible optical detector, specially a kind of perovskite flexible optical detector and preparation method thereof.
Background technology
Organic and inorganic perovskite in photoelectric field due to wide light absorbs and carrier transport distance, causing huge Big research boom.Photo-detector based on perovskite large size single crystal achieves excellent performance.But large scale perovskite Monocrystalline can not but be prepared using continuous volume to volume technology and prepared by flexible device.Although the light based on perovskite thin film is visited Survey utensil have the advantages that it is lightweight, can large scale prepare and flexible can prepare；But the perovskite nano particle prepared at present is thin There is substantial amounts of crystal boundary and defect in film, cause photo-generated carrier compound serious, limit quantum efficiency and carrier lifetime, into For the bottleneck of the further development of perovskite flexible optical detector.
The content of the invention
For problems of the prior art, the present invention provides a kind of perovskite flexible optical detector and its preparation side Method, the perovskite thin film quality prepared is close to monocrystalline so that the flexible optical detector based on this perovskite thin film has non- Chang Youyi optical detection rate, responsiveness, Bending Stability and device lifetime.
The present invention is to be achieved through the following technical solutions：
A kind of perovskite flexible optical detector preparation method, comprises the following steps,
Step 1, perovskite solution is prepared；
Step 2, perovskite thin film is prepared by doctor blade method on the flexible substrate after cleaning-drying, obtains perovskite soft Property film；
First, the flexible substrate after cleaning-drying is fixed on the working face of thermal station, and at a temperature of 140 DEG C of 80- Preheating 5 minutes；
Secondly, fixed doctor and to adjust scraper and horizontal substrate angle be 30-90 °, between regulation scraper and flexible substrate Slot distances keep fixing；By the way that the slit between perovskite solution filling flexible substrate and scraper is added dropwise；
Finally, under the air or nitrogen environment less than 80% humidity, control thermal station temperature is in 140 DEG C of 80-, with 10- 50mm/min speed unidirectionally moves horizontally scraper, drags perovskite solution film forming on flexible substrate, obtaining fibrous crystal has The perovskite oriented single crystal fiber flexibility film of single crystalline nature, i.e. described perovskite fexible film；
Step 3, the perovskite fexible film prepared is made annealing treatment；
Step 4, gold electrode is deposited on perovskite fexible film after annealing, obtains perovskite flexible optical detector.
It is preferred that, in step 2, slot distances are 50 to 200 μm between scraper and flexible substrate.
It is preferred that, in step 2, volume and the perovskite thin film area relationship of the perovskite solution of the dropwise addition are 3~5 μ L/cm2。
It is preferred that, in step 1, when preparing perovskite solution；
Aggressiveness before organic and inorganic halogen perovskite is added in organic solvent, concentration is between 0.5M to 1.2M；Will be mixed Solution after closing uniformly is placed at 60 DEG C and stirred 2 hours, is subsequently cooled to room temperature and stirs more than four hours；With 0.45 μm of hole The Teflon filtration membrane filtration in footpath obtains perovskite solution for standby；
Wherein, the organic and inorganic halogen perovskite is respectively MAPbI3Or MAPbBr3；Its corresponding preceding aggressiveness difference For MAI and PbI2, and MABr and PbBr2；The mol ratio of corresponding preceding aggressiveness is MAI:PbI2=1:(0.5-1.5), MABr:PbBr2=1:(0.5-1.5)；
Described organic solvent is respectively dimethylformamide, dimethyl sulfoxide (DMSO) or gamma-butyrolacton.
Further, according to different perovskite solution, the thermal station temperature is respectively when using dimethyl formamide solution When 80-120 DEG C, when using dimethyl sulphoxide solution when 110-140 DEG C, when using gamma-butyrolacton solution when 120- 150℃。
It is preferred that, when being annealed in step 3, the perovskite fexible film prepared is placed on 80 DEG C to 150 DEG C thermal station Upper thermal annealing 8-10 minutes.
It is preferred that, in step 2, described flexible substrate is flexible PET film.
A kind of perovskite flexible optical detector, is prepared by preparation method of the present invention.
Compared with prior art, the present invention has following beneficial technique effect：
The monocrystalline perovskite orientation that perovskite thin film in the perovskite photo-detector of the present invention is prepared for unidirectional doctor blade method Fibrous crystal.The film is compared to perovskite thin film prepared by traditional spin-coating method, has crystalline quality high in performance, crystal boundary Few, absorption bands is wide, and carrier lifetime is long, the advantages of air-stable is good, and in technology of preparing, cost is low, production technology letter Single, energy consumption is low and can mass produce.Perovskite flexible optical detector based on the present invention has very excellent optical detection Rate, optical responsivity, Bending Stability and device lifetime.
Brief description of the drawings
Fig. 1 is the perovskite oriented single crystal fiber flexibility film scanning electron microscope that described in present example prepared by method.
Fig. 2 a are the transmission electron microscope of perovskite oriented single crystal fiber flexibility film prepared by method described in present example Electron diffraction diagram.
Fig. 2 b be present example described in method prepare perovskite oriented single crystal fiber flexibility film wide-angle plunder into Penetrate x-ray diffraction pattern.
Fig. 3 a are the UV absorption of perovskite oriented single crystal fiber flexibility film prepared by method described in present example Spectrogram；Object of reference is used as using perovskite nanometer particle film prepared by common spin-coating method.
Fig. 3 b are the time resolution of perovskite oriented single crystal fiber flexibility film prepared by method described in present example Luminescence generated by light spectrogram；Object of reference is used as using perovskite nanometer particle film prepared by common spin-coating method.
Fig. 4 a are that the perovskite oriented single crystal fiber flexibility photo-detector that described in present example prepared by method exists The photoresponse of 560nm wavelength；Object of reference is used as using perovskite nanometer particle film prepared by common spin-coating method.
Fig. 4 b are that the perovskite oriented single crystal fiber flexibility photo-detector that described in present example prepared by method exists The optical detection rate of 560nm wavelength；Object of reference is used as using perovskite nanometer particle film prepared by common spin-coating method.
Fig. 5 a are the bending of perovskite oriented single crystal fiber flexibility photo-detector prepared by method described in present example Test.
Fig. 5 b are the air of perovskite oriented single crystal fiber flexibility photo-detector prepared by method described in present example Middle life test.
Embodiment
With reference to specific embodiment, the present invention is described in further detail, and described is explanation of the invention Rather than limit.
A kind of preparation method of the broadband flexible optical detector of perovskite of the present invention, comprises the following steps：
Step 1, the regular flexible substrate of high-quality ethylene glycol terephthalate (PET) is chosen, respectively in acetone, second In alcohol, isopropanol be cleaned by ultrasonic 15 minutes, then with nitrogen drying be put into oxygen plasma handle 5 minutes it is stand-by；
Step 2, by before organic and inorganic halogen perovskite aggressiveness add organic solvent in, concentration 0.5M to 1.2M it Between.Solution is placed at 60 DEG C and stirred 2 hours, room temperature is subsequently cooled to and is stirred overnight.Solution is using preceding with 0.45 μm of aperture Polytetrafluoroethylene (PTFE) (PTFE) filtering membrane filtration.Wherein, the organic and inorganic halogen perovskite is respectively MAPbI3With MAPbBr3.Its preceding aggressiveness is respectively MAI and PbI2, and MABr and PbBr2.The mol ratio of preceding aggressiveness is MAI:PbI2= 1:(0.5- 1.5), MABr:PbBr2=1:(0.5-1.5).The organic solvent of the perovskite is its good solvent, respectively two NMF (DMF), gamma-butyrolacton (GBL) and dimethyl sulfoxide (DMSO) (DMSO).
Step 3, the PET substrates cleaned up are fixed in smooth thermal station, and preheat at a temperature of 80-140 DEG C 5 Minute.Fixed doctor and to adjust scraper and horizontal substrate angle be 30-90 °.Slot distances are between regulation scraper and substrate 50-200μm.Take the slit between a certain amount of perovskite solution filling substrate and scraper.With the unidirectional water of 1-50mm/min speed The dynamic scraper of translation, drags perovskite solution film forming on PET substrates.Wherein, the blade coating environment is the sky less than 80% humidity Gas or nitrogen environment；Different, 80-100 DEG C when the thermal station temperature is respectively DMF solution, DMSO according to SOLUTION PROPERTIES 120-140 DEG C during 110-130 DEG C and GBL solution during solution；The volume and perovskite of the perovskite solution of the dropwise addition Film size relation is：3~5 μ L/cm2, according to the perovskite fexible film size to be prepared, the calcium titanium of respective volume is added dropwise Mineral solution.
Step 4, stop after blade coating, transfer perovskite fexible film to thermal annealing 8- in 100 DEG C of thermal station 10 minutes.It is made Standby perovskite thin film is by SEM pattern test, it is observed that height-oriented fibrous crystal, such as Fig. 1 a With shown in Fig. 1 b；Tested by transmission electron microscope and wide-angle glancing incidence X-ray diffraction crystal structure, it may be determined that fiber Crystalline substance has single crystalline nature, as shown in Figure 2 a and 2 b；Tested, can observed by ultra-violet absorption spectrum film optical absorption property There are broader light absorbs than Conventional nano particle film to oriented single crystal fiber membrane, as shown in Figure 3 a；Passage time point Photoluminescence spectra photo-generated carrier life test is distinguished, it is observed that the life-span ratio of oriented single crystal fiber membrane carriers Conventional nano particle film is longer, as shown in Figure 3 b.Wherein, the thermal annealing environment be less than 80% humidity air or Nitrogen environment.
Step 5, the perovskite fexible film that thermal annealing is finished is transferred in vaporization chamber, is aided with mask and carries out gold electrode Evaporation.Perovskite thin film effective dimensions is 40 μm wide, 1mm length between gold electrode.Gold electrode 300nm is thick.Illumination effective area is 2.7×10-7m2。
Step 6, visible ray is configured on Keithley2400SourceMeter instrument platforms interval in 480nm to 750nm The LASER Light Source of different-waveband, adjusts laser output waveband and power output (0.08 to 0.5mw/cm respectively2), test calcium titanium Ore deposit flexible optical detector detectivity and response, as shown in figures 4 a and 4b.
Step 7, respectively by freshly prepared perovskite flexible optical detector by the crooked test stability of 1000 times, As shown in Figure 5 a, the device lifetime after and being exposed 48 hours in the air ambient of 50-70% humidity, as shown in Figure 5 b.
The present invention prepares the flexible optical detector that perovskite is orientated fibrous crystal using doctor blade method.The perovskite of the present invention The preparation method of photo-detector takes full advantage of the blade coating printing technology of low cost, simple production process, and energy consumption is low and can be big Scale Growth.Prepared perovskite thin film crystalline quality is high, and crystal boundary is few, and absorption bands is wide, and carrier lifetime is long, and air is steady Set.Perovskite flexible optical detector based on the present invention has very excellent optical detection rate, optical responsivity, bending stable Property and device lifetime.
Embodiment 1
The best embodiment of the present invention is by 1.0M MAPbI3Preceding aggressiveness MAI and PbI2With 1:1 mol ratio is added to In dimethylformamide (DMF) solvent, solution is placed at 60 DEG C and stirred 2 hours, room temperature is subsequently cooled to and is stirred overnight. Solution filters membrane filtration using the preceding polytetrafluoroethylene (PTFE) (PTFE) with 0.45 μm of aperture.
By the PET substrates (3 × 3cm cleaned up2) be fixed in smooth thermal station, and preheat 5 at a temperature of 100 DEG C Minute.Fixed doctor simultaneously adjusts scraper and horizontal sextant angle for 50 °.It is 100 μm to adjust slot distances between scraper and substrate.Take 40μL MAI:PbI2DMF solution filling substrate and scraper between slit.Unidirectionally moved horizontally with 10mm/min speed Scraper drags perovskite solution film forming on substrate.
Stop after blade coating, transfer perovskite fexible film to thermal annealing in 100 DEG C of thermal station 10 minutes.Prepared calcium titanium Ore deposit film is tested by pattern and crystal structure, and life test in photoresponse, detectivity, Bending Stability and air.
Embodiment 2
By 0.5M MAPbI3Preceding aggressiveness MAI and PbI2With 1:1 mol ratio is added to dimethylformamide (DMF) solvent In, solution is placed at 60 DEG C and stirred 2 hours, room temperature is subsequently cooled to and is stirred overnight.Solution is using preceding with 0.45 μm of aperture Polytetrafluoroethylene (PTFE) (PTFE) filtering membrane filtration.
By the PET substrates (3 × 3cm cleaned up2) be fixed in smooth thermal station, and 5 points of the preheating at a temperature of 80 DEG C Clock.Fixed doctor simultaneously adjusts scraper and horizontal sextant angle for 50 °.It is 50 μm to adjust slot distances between scraper and substrate.Take 40 μ L MAI:PbI2DMF solution filling substrate and scraper between slit.Scraper is unidirectionally moved horizontally with 10mm/min speed to drag Dynamic perovskite solution film forming on substrate.
Stop after blade coating, transfer perovskite fexible film to thermal annealing in 100 DEG C of thermal station 10 minutes.Other steps and reality Apply example 1 identical.
Embodiment 3
By 1.2M MAPbI3Preceding aggressiveness MAI and PbI2With 1:1 mol ratio is added to dimethylformamide (DMF) solvent In, solution is placed at 60 DEG C and stirred 2 hours, room temperature is subsequently cooled to and is stirred overnight.Solution is using preceding with 0.45 μm of aperture Polytetrafluoroethylene (PTFE) (PTFE) filtering membrane filtration.
By the PET substrates (3 × 3cm cleaned up2) be fixed in smooth thermal station, and 5 points of the preheating at a temperature of 90 DEG C Clock.Fixed doctor simultaneously adjusts scraper and horizontal sextant angle for 50 °.It is 100 μm to adjust slot distances between scraper and substrate.Take 40 μ L MAI:PbI2DMF solution filling substrate and scraper between slit.Scraper is unidirectionally moved horizontally with 1mm/min speed Drag perovskite solution film forming on substrate.
Stop after blade coating, transfer perovskite fexible film to thermal annealing in 80 DEG C of thermal station 10 minutes.Other steps are with implementing Example 1 is identical.
Embodiment 4
By 1.0M MAPbI3Preceding aggressiveness MAI and PbI2With 1:It is molten that 0.8 mol ratio is added to dimethylformamide (DMF) In agent, solution is placed at 60 DEG C and stirred 2 hours, room temperature is subsequently cooled to and is stirred overnight.Solution is using preceding with 0.45 μm of hole Polytetrafluoroethylene (PTFE) (PTFE) the filtering membrane filtration in footpath.
By the PET substrates (3 × 3cm cleaned up2) be fixed in smooth thermal station, and preheat 5 at a temperature of 100 DEG C Minute.Fixed doctor simultaneously adjusts scraper and horizontal sextant angle for 60 °.It is 100 μm to adjust slot distances between scraper and substrate.Take 40μL MAI:PbI2DMF solution filling substrate and scraper between slit.Unidirectionally moved horizontally with 10mm/min speed Scraper drags perovskite solution film forming on substrate.
Stop after blade coating, transfer perovskite fexible film to thermal annealing in 100 DEG C of thermal station 10 minutes.Other steps and reality Apply example 1 identical.
Embodiment 5
By 1.0M MAPbI3Preceding aggressiveness MAI and PbI2With 1:It is molten that 1.2 mol ratios are added to dimethylformamide (DMF) In agent, solution is placed at 60 DEG C and stirred 2 hours, room temperature is subsequently cooled to and is stirred overnight.Solution is using preceding with 0.45 μm of hole Polytetrafluoroethylene (PTFE) (PTFE) the filtering membrane filtration in footpath.
By the PET substrates (3 × 3cm cleaned up2) be fixed in smooth thermal station, and preheat 5 at a temperature of 110 DEG C Minute.Fixed doctor simultaneously adjusts scraper and horizontal sextant angle for 90 °.It is 120 μm to adjust slot distances between scraper and substrate.Take 40μL MAI:PbI2DMF solution filling substrate and scraper between slit.Unidirectionally moved horizontally with 30mm/min speed Scraper drags perovskite solution film forming on substrate.
Stop after blade coating, transfer perovskite fexible film to thermal annealing in 100 DEG C of thermal station 10 minutes.Other steps and reality Apply example 1 identical.
Embodiment 6
By 1.2M MAPbI3Preceding aggressiveness MAI and PbI2With 1:1 mol ratio is added to dimethyl sulfoxide (DMSO) (DMSO) solvent In, solution is placed at 60 DEG C and stirred 2 hours, room temperature is subsequently cooled to and is stirred overnight.Solution is using preceding with 0.45 μm of aperture Polytetrafluoroethylene (PTFE) (PTFE) filtering membrane filtration.
By the PET substrates (3 × 3cm cleaned up2) be fixed in smooth thermal station, and preheat 5 at a temperature of 110 DEG C Minute.Fixed doctor simultaneously adjusts scraper and horizontal sextant angle for 50 °.It is 50 μm to adjust slot distances between scraper and substrate.Take 40 μL MAI:PbI2DMF solution filling substrate and scraper between slit.Unidirectionally moved horizontally and scraped with 50mm/min speed Knife drags perovskite solution film forming on substrate.
Stop after blade coating, transfer perovskite fexible film to thermal annealing in 100 DEG C of thermal station 10 minutes.Other steps and reality Apply example 1 identical.
Embodiment 7
By 1.0M MAPbI3Preceding aggressiveness MAI and PbI2With 1:0.5 mol ratio is added to dimethyl sulfoxide (DMSO) (DMSO) solvent In, solution is placed at 60 DEG C and stirred 2 hours, room temperature is subsequently cooled to and is stirred overnight.Solution is using preceding with 0.45 μm of aperture Polytetrafluoroethylene (PTFE) (PTFE) filtering membrane filtration.
By the PET substrates (3 × 3cm cleaned up2) be fixed in smooth thermal station, and preheat 5 at a temperature of 120 DEG C Minute.Fixed doctor simultaneously adjusts scraper and horizontal sextant angle for 50 °.It is 100 μm to adjust slot distances between scraper and substrate.Take 40μL MAI:PbI2DMF solution filling substrate and scraper between slit.Unidirectionally moved horizontally with 10mm/min speed Scraper drags perovskite solution film forming on substrate.
Stop after blade coating, transfer perovskite fexible film to thermal annealing in 100 DEG C of thermal station 10 minutes.Other steps and reality Apply example 1 identical.
Embodiment 8
By 1.0M MAPbI3Preceding aggressiveness MAI and PbI2With 1:0.8 mol ratio is added to dimethyl sulfoxide (DMSO) (DMSO) solvent In, solution is placed at 60 DEG C and stirred 2 hours, room temperature is subsequently cooled to and is stirred overnight.Solution is using preceding with 0.45 μm of aperture Polytetrafluoroethylene (PTFE) (PTFE) filtering membrane filtration.
By the PET substrates (3 × 10cm cleaned up2) be fixed in smooth thermal station, and preheat 5 at a temperature of 130 DEG C Minute.Fixed doctor simultaneously adjusts scraper and horizontal sextant angle for 50 °.It is 200 μm to adjust slot distances between scraper and substrate.Take 40μL MAI:PbI2DMF solution filling substrate and scraper between slit.Unidirectionally moved horizontally with 10mm/min speed Scraper drags perovskite solution film forming on substrate.
Stop after blade coating, transfer perovskite fexible film to thermal annealing in 100 DEG C of thermal station 10 minutes.Other steps and reality Apply example 1 identical.
Embodiment 9
By 1.0M MAPbI3Preceding aggressiveness MAI and PbI2With 1:1.5 mol ratios are added to dimethyl sulfoxide (DMSO) (DMSO) solvent In, solution is placed at 60 DEG C and stirred 2 hours, room temperature is subsequently cooled to and is stirred overnight.Solution is using preceding with 0.45 μm of aperture Polytetrafluoroethylene (PTFE) (PTFE) filtering membrane filtration.
By the PET substrates (3 × 3cm cleaned up2) be fixed in smooth thermal station, and preheat 5 at a temperature of 140 DEG C Minute.Fixed doctor simultaneously adjusts scraper and horizontal sextant angle for 30 °.It is 150 μm to adjust slot distances between scraper and substrate.Take 40μL MAI:PbI2DMF solution filling substrate and scraper between slit.Unidirectionally moved horizontally with 30mm/min speed Scraper drags perovskite solution film forming on substrate.
Stop after blade coating, transfer perovskite fexible film to thermal annealing in 100 DEG C of thermal station 10 minutes.Other steps and reality Apply example 1 identical.
Embodiment 10
By 1.5M MAPbI3Preceding aggressiveness MAI and PbI2With 1:1 mol ratio is added in gamma-butyrolacton (GBL) solvent, Solution is placed at 60 DEG C and stirred 2 hours, room temperature is subsequently cooled to and is stirred overnight.Solution is using preceding with 0.45 μm of aperture Polytetrafluoroethylene (PTFE) (PTFE) filters membrane filtration.
By the PET substrates (3 × 3cm cleaned up2) be fixed in smooth thermal station, and preheat 5 at a temperature of 120 DEG C Minute.Fixed doctor simultaneously adjusts scraper and horizontal sextant angle for 90 °.It is 100 μm to adjust slot distances between scraper and substrate.Take 40μL MAI:PbI2DMF solution filling substrate and scraper between slit.Unidirectionally moved horizontally with 30mm/min speed Scraper drags perovskite solution film forming on substrate.
Stop after blade coating, transfer perovskite fexible film to thermal annealing in 80 DEG C of thermal station 10 minutes.Other steps are with implementing Example 1 is identical.
Embodiment 11
By 1.0M MAPbI3Preceding aggressiveness MAI and PbI2With 1:1 mol ratio is added in gamma-butyrolacton (GBL) solvent, Solution is placed at 60 DEG C and stirred 2 hours, room temperature is subsequently cooled to and is stirred overnight.Solution is using preceding with 0.45 μm of aperture Polytetrafluoroethylene (PTFE) (PTFE) filters membrane filtration.
By the PET substrates (3 × 3cm cleaned up2) be fixed in smooth thermal station, and preheat 5 at a temperature of 130 DEG C Minute.Fixed doctor simultaneously adjusts scraper and horizontal sextant angle for 50 °.It is 100 μm to adjust slot distances between scraper and substrate.Take 40μL MAI:PbI2DMF solution filling substrate and scraper between slit.Unidirectionally moved horizontally and scraped with 1mm/min speed Knife drags perovskite solution film forming on substrate.
Stop after blade coating, transfer perovskite fexible film to thermal annealing in 100 DEG C of thermal station 10 minutes.Other steps and reality Apply example 1 identical.
Embodiment 12
By 1.2M MAPbI3Preceding aggressiveness MAI and PbI2With 1:1 mol ratio is added in gamma-butyrolacton (GBL) solvent, Solution is placed at 60 DEG C and stirred 2 hours, room temperature is subsequently cooled to and is stirred overnight.Solution is using preceding with 0.45 μm of aperture Polytetrafluoroethylene (PTFE) (PTFE) filters membrane filtration.
By the PET substrates (3 × 3cm cleaned up2) be fixed in smooth thermal station, and preheat 5 at a temperature of 150 DEG C Minute.Fixed doctor simultaneously adjusts scraper and horizontal sextant angle for 50 °.It is 100 μm to adjust slot distances between scraper and substrate.Take 40μL MAI:PbI2DMF solution filling substrate and scraper between slit.Unidirectionally moved horizontally with 30mm/min speed Scraper drags perovskite solution film forming on substrate.
Stop after blade coating, transfer perovskite fexible film to thermal annealing in 100 DEG C of thermal station 10 minutes.Other steps and reality Apply example 1 identical.
Embodiment 13
By 1.0M MAPbI3Preceding aggressiveness MAI and PbI2With 1:1 mol ratio is added to dimethylformamide (DMF) solvent In, solution is placed at 60 DEG C and stirred 2 hours, room temperature is subsequently cooled to and is stirred overnight.Solution is using preceding with 0.45 μm of aperture Polytetrafluoroethylene (PTFE) (PTFE) filtering membrane filtration.
By the PET substrates (3 × 3cm cleaned up2) be fixed in smooth thermal station, and preheat 5 at a temperature of 100 DEG C Minute.Fixed doctor simultaneously adjusts scraper and horizontal sextant angle for 60 °.It is 100 μm to adjust slot distances between scraper and substrate.Take 40μL MAI:PbI2DMF solution filling substrate and scraper between slit.Unidirectionally moved horizontally and scraped with 5mm/min speed Knife drags perovskite solution film forming on substrate.
Stop after blade coating, transfer perovskite fexible film to thermal annealing in 80 DEG C of thermal station 10 minutes.Other steps are with implementing Example 1 is identical.
Embodiment 14
By 1.0M MAPbI3Preceding aggressiveness MAI and PbI2With 1:1 mol ratio is added to dimethylformamide (DMF) solvent In, solution is placed at 60 DEG C and stirred 2 hours, room temperature is subsequently cooled to and is stirred overnight.Solution is using preceding with 0.45 μm of aperture Polytetrafluoroethylene (PTFE) (PTFE) filtering membrane filtration.
By the PET substrates (3 × 3cm cleaned up2) be fixed in smooth thermal station, and preheat 5 at a temperature of 100 DEG C Minute.Fixed doctor simultaneously adjusts scraper and horizontal sextant angle for 50 °.It is 100 μm to adjust slot distances between scraper and substrate.Take 40μL MAI:PbI2DMF solution filling substrate and scraper between slit.Unidirectionally moved horizontally with 20mm/min speed Scraper drags perovskite solution film forming on substrate.
Stop after blade coating, transfer perovskite fexible film to thermal annealing in 150 DEG C of thermal station 10 minutes.Other steps and reality Apply example 1 identical.
Embodiment 15
By 1.0M MAPbI3Preceding aggressiveness MAI and PbI2With 1:1 mol ratio is added to dimethylformamide (DMF) solvent In, solution is placed at 60 DEG C and stirred 2 hours, room temperature is subsequently cooled to and is stirred overnight.Solution is using preceding with 0.45 μm of aperture Polytetrafluoroethylene (PTFE) (PTFE) filtering membrane filtration.
By the PET substrates (3 × 3cm cleaned up2) be fixed in smooth thermal station, and preheat 5 at a temperature of 100 DEG C Minute.Fixed doctor simultaneously adjusts scraper and horizontal sextant angle for 50 °.It is 100 μm to adjust slot distances between scraper and substrate.Take 40μL MAI:PbI2DMF solution filling substrate and scraper between slit.Unidirectionally moved horizontally with 30mm/min speed Scraper drags perovskite solution film forming on substrate.
Stop after blade coating, transfer perovskite fexible film to thermal annealing in 100 DEG C of thermal station 5 minutes.Other steps are with implementing Example 1 is identical.
Embodiment 16
By 1.0M MAPbBr3Preceding aggressiveness MABr and PbBr2With 1:It is molten that 1 mol ratio is added to dimethylformamide (DMF) In agent, solution is placed at 60 DEG C and stirred 2 hours, room temperature is subsequently cooled to and is stirred overnight.Solution is using preceding with 0.45 μm of hole Polytetrafluoroethylene (PTFE) (PTFE) the filtering membrane filtration in footpath.
By the PET substrates (3 × 3cm cleaned up2) be fixed in smooth thermal station, and 5 points of the preheating at a temperature of 80 DEG C Clock.Fixed doctor simultaneously adjusts scraper and horizontal sextant angle for 50 °.It is 150 μm to adjust slot distances between scraper and substrate.Take 40 μ L MAI:PbI2DMF solution filling substrate and scraper between slit.Scraper is unidirectionally moved horizontally with 50mm/min speed Drag perovskite solution film forming on substrate.
Stop after blade coating, transfer perovskite fexible film to thermal annealing in 100 DEG C of thermal station 10 minutes.Other steps and reality Apply example 1 identical.
Embodiment 17
By 1.0M MAPbBr3Preceding aggressiveness MABr and PbBr2With 1:1.2 mol ratios are added to dimethylformamide (DMF) In solvent, solution is placed at 60 DEG C and stirred 2 hours, room temperature is subsequently cooled to and is stirred overnight.Solution is using preceding with 0.45 μm Polytetrafluoroethylene (PTFE) (PTFE) the filtering membrane filtration in aperture.
By the PET substrates (3 × 3cm cleaned up2) be fixed in smooth thermal station, and preheat 5 at a temperature of 100 DEG C Minute.Fixed doctor simultaneously adjusts scraper and horizontal sextant angle for 50 °.It is 100 μm to adjust slot distances between scraper and substrate.Take 40μL MAI:PbI2DMF solution filling substrate and scraper between slit.Unidirectionally moved horizontally and scraped with 5mm/min speed Knife drags perovskite solution film forming on substrate.
Stop after blade coating, transfer perovskite fexible film to thermal annealing in 150 DEG C of thermal station 10 minutes.Other steps and reality Apply example 1 identical.
Embodiment 18
By 1.0M MAPbBr3Preceding aggressiveness MABr and PbBr2With 1:0.8 mol ratio is added to dimethylformamide (DMF) In solvent, solution is placed at 60 DEG C and stirred 2 hours, room temperature is subsequently cooled to and is stirred overnight.Solution is using preceding with 0.45 μm Polytetrafluoroethylene (PTFE) (PTFE) the filtering membrane filtration in aperture.
By the PET substrates (3 × 3cm cleaned up2) be fixed in smooth thermal station, and preheat 5 at a temperature of 100 DEG C Minute.Fixed doctor simultaneously adjusts scraper and horizontal sextant angle for 50 °.It is 50 μm to adjust slot distances between scraper and substrate.Take 40 μL MAI:PbI2DMF solution filling substrate and scraper between slit.Scraper is unidirectionally moved horizontally with 5mm/min speed Drag perovskite solution film forming on substrate.
Stop after blade coating, transfer perovskite fexible film to thermal annealing in 150 DEG C of thermal station 10 minutes.Other steps and reality Apply example 1 identical.
Embodiment 19
By 1.0M MAPbBr3Preceding aggressiveness MABr and PbBr2With 1:It is molten that 1 mol ratio is added to dimethyl sulfoxide (DMSO) (DMSO) In agent, solution is placed at 60 DEG C and stirred 2 hours, room temperature is subsequently cooled to and is stirred overnight.Solution is using preceding with 0.45 μm of hole Polytetrafluoroethylene (PTFE) (PTFE) the filtering membrane filtration in footpath.
By the PET substrates (3 × 3cm cleaned up2) be fixed in smooth thermal station, and preheat 5 at a temperature of 110 DEG C Minute.Fixed doctor simultaneously adjusts scraper and horizontal sextant angle for 50 °.It is 100 μm to adjust slot distances between scraper and substrate.Take 40μL MAI:PbI2DMF solution filling substrate and scraper between slit.Unidirectionally moved horizontally and scraped with 5mm/min speed Knife drags perovskite solution film forming on substrate.
Stop after blade coating, transfer perovskite fexible film to thermal annealing in 150 DEG C of thermal station 10 minutes.Other steps and reality Apply example 1 identical.
Embodiment 20
By 1.0M MAPbBr3Preceding aggressiveness MABr and PbBr2With 1:It is molten that 1 mol ratio is added to dimethyl sulfoxide (DMSO) (DMSO) In agent, solution is placed at 60 DEG C and stirred 2 hours, room temperature is subsequently cooled to and is stirred overnight.Solution is using preceding with 0.45 μm of hole Polytetrafluoroethylene (PTFE) (PTFE) the filtering membrane filtration in footpath.
By the PET substrates (3 × 3cm cleaned up2) be fixed in smooth thermal station, and preheat 5 at a temperature of 120 DEG C Minute.Fixed doctor simultaneously adjusts scraper and horizontal sextant angle for 50 °.It is 100 μm to adjust slot distances between scraper and substrate.Take 40μL MAI:PbI2DMF solution filling substrate and scraper between slit.Unidirectionally moved horizontally and scraped with 5mm/min speed Knife drags perovskite solution film forming on substrate.
Stop after blade coating, transfer perovskite fexible film to thermal annealing in 100 DEG C of thermal station 10 minutes.Other steps and reality Apply example 1 identical.
Embodiment 21
By 1.0M MAPbBr3Preceding aggressiveness MABr and PbBr2With 1:It is molten that 1 mol ratio is added to dimethyl sulfoxide (DMSO) (DMSO) In agent, solution is placed at 60 DEG C and stirred 2 hours, room temperature is subsequently cooled to and is stirred overnight.Solution is using preceding with 0.45 μm of hole Polytetrafluoroethylene (PTFE) (PTFE) the filtering membrane filtration in footpath.
By the PET substrates (2 × 10cm cleaned up2) be fixed in smooth thermal station, and preheat 5 at a temperature of 140 DEG C Minute.Fixed doctor simultaneously adjusts scraper and horizontal sextant angle for 50 °.It is 100 μm to adjust slot distances between scraper and substrate.Take 40μL MAI:PbI2DMF solution filling substrate and scraper between slit.Unidirectionally moved horizontally and scraped with 5mm/min speed Knife drags perovskite solution film forming on substrate.
Stop after blade coating, transfer perovskite fexible film to thermal annealing in 80 DEG C of thermal station 10 minutes.Other steps are with implementing Example 1 is identical.
Embodiment 22
By 0.8M MAPbBr3Preceding aggressiveness MABr and PbBr2With 1:1 mol ratio is added to gamma-butyrolacton (GBL) solvent In, solution is placed at 60 DEG C and stirred 2 hours, room temperature is subsequently cooled to and is stirred overnight.Solution is using preceding with 0.45 μm of aperture Polytetrafluoroethylene (PTFE) (PTFE) filtering membrane filtration.
By the PET substrates (3 × 3cm cleaned up2) be fixed in smooth thermal station, and preheat 5 at a temperature of 120 DEG C Minute.Fixed doctor simultaneously adjusts scraper and horizontal sextant angle for 50 °.It is 100 μm to adjust slot distances between scraper and substrate.Take 40μL MAI:PbI2DMF solution filling substrate and scraper between slit.Unidirectionally moved horizontally and scraped with 5mm/min speed Knife drags perovskite solution film forming on substrate.
Stop after blade coating, transfer perovskite fexible film to thermal annealing in 150 DEG C of thermal station 10 minutes.Other steps and reality Apply example 1 identical.
Embodiment 23
By 1.2M MAPbBr3Preceding aggressiveness MABr and PbBr2With 1:1 mol ratio is added to gamma-butyrolacton (GBL) solvent In, solution is placed at 60 DEG C and stirred 2 hours, room temperature is subsequently cooled to and is stirred overnight.Solution is using preceding with 0.45 μm of aperture Polytetrafluoroethylene (PTFE) (PTFE) filtering membrane filtration.
By the PET substrates (3 × 3cm cleaned up2) be fixed in smooth thermal station, and preheat 5 at a temperature of 130 DEG C Minute.Fixed doctor simultaneously adjusts scraper and horizontal sextant angle for 90 °.It is 200 μm to adjust slot distances between scraper and substrate.Take 40μL MAI:PbI2DMF solution filling substrate and scraper between slit.Unidirectionally moved horizontally and scraped with 5mm/min speed Knife drags perovskite solution film forming on substrate.
Stop after blade coating, transfer perovskite fexible film to thermal annealing in 100 DEG C of thermal station 10 minutes.Other steps and reality Apply example 1 identical.
Embodiment 24
By 0.8M MAPbBr3Preceding aggressiveness MABr and PbBr2With 1:1 mol ratio is added to gamma-butyrolacton (GBL) solvent In, solution is placed at 60 DEG C and stirred 2 hours, room temperature is subsequently cooled to and is stirred overnight.Solution is using preceding with 0.45 μm of aperture Polytetrafluoroethylene (PTFE) (PTFE) filtering membrane filtration.
By the PET substrates (3 × 3cm cleaned up2) be fixed in smooth thermal station, and preheat 5 at a temperature of 150 DEG C Minute.Fixed doctor simultaneously adjusts scraper and horizontal sextant angle for 50 °.It is 100 μm to adjust slot distances between scraper and substrate.Take 40μL MAI:PbI2DMF solution filling substrate and scraper between slit.Unidirectionally moved horizontally with 50mm/min speed Scraper drags perovskite solution film forming on substrate.
Stop after blade coating, transfer perovskite fexible film to thermal annealing in 120 DEG C of thermal station 10 minutes.Other steps and reality Apply example 1 identical.

Claims (8)

1. a kind of perovskite flexible optical detector preparation method, it is characterised in that comprise the following steps,
Step 1, perovskite solution is prepared；
Step 2, perovskite thin film is prepared by doctor blade method on the flexible substrate after cleaning-drying, obtains perovskite flexible thin Film；
First, the flexible substrate after cleaning-drying is fixed on the working face of thermal station, and preheats at a temperature of 80-140 DEG C 5 Minute；
Secondly, fixed doctor and to adjust scraper and horizontal substrate angle be 30-90 °, slit between regulation scraper and flexible substrate Distance keeps fixing；By the way that the slit between perovskite solution filling flexible substrate and scraper is added dropwise；
Finally, under the air or nitrogen environment less than 80% humidity, control thermal station temperature is at 80-140 DEG C, with 10-50mm/ Min speed unidirectionally moves horizontally scraper, drags perovskite solution film forming on flexible substrate, obtain fibrous crystal have it is monocrystalline The perovskite oriented single crystal fiber flexibility film of matter, i.e. described perovskite fexible film；
Step 3, the perovskite fexible film prepared is made annealing treatment；
Step 4, gold electrode is deposited on perovskite fexible film after annealing, obtains perovskite flexible optical detector.
2. a kind of perovskite flexible optical detector preparation method according to claim 1, it is characterised in that in step 2, scrape Slot distances are 50 to 200 μm between knife and flexible substrate.
3. a kind of perovskite flexible optical detector preparation method according to claim 1, it is characterised in that in step 2, institute The volume and perovskite thin film area relationship for stating the perovskite solution of dropwise addition are 3~5 μ L/cm2。
4. a kind of perovskite flexible optical detector preparation method according to claim 1, it is characterised in that in step 1, system During standby perovskite solution；
Aggressiveness before organic and inorganic halogen perovskite is added in organic solvent, concentration is between 0.5M to 1.2M；Will be well mixed Solution afterwards is placed at 60 DEG C and stirred 2 hours, is subsequently cooled to room temperature and stirs more than four hours；With poly- the four of 0.45 μm of aperture PVF filter membrane is filtrated to get perovskite solution for standby；
Wherein, the organic and inorganic halogen perovskite is respectively MAPbI3Or MAPbBr3；Its corresponding preceding aggressiveness is respectively MAI And PbI2, and MABr and PbBr2；The mol ratio of corresponding preceding aggressiveness is MAI:PbI2=1:(0.5-1.5), MABr: PbBr2=1:(0.5-1.5)；
Described organic solvent is respectively dimethylformamide, dimethyl sulfoxide (DMSO) or gamma-butyrolacton.
5. a kind of perovskite flexible optical detector preparation method according to claim 4, it is characterised in that according to different Perovskite solution, the thermal station temperature is respectively 80-120 DEG C when using dimethyl formamide solution, when using dimethyl 110-140 DEG C during sulfoxide solution, 120-150 DEG C when using gamma-butyrolacton solution.
6. a kind of perovskite flexible optical detector preparation method according to claim 1, it is characterised in that moved back in step 3 When fiery, the perovskite fexible film prepared is placed on thermal annealing 8-10 minutes in 80 DEG C to 150 DEG C thermal station.
7. a kind of perovskite flexible optical detector preparation method according to claim 1, it is characterised in that in step 2, institute The flexible substrate stated is flexible PET film.
8. a kind of perovskite flexible optical detector, it is characterised in that as the preparation method system described in claim 1-7 any one It is standby to obtain.
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CN108321297A (en) * 2018-02-05 2018-07-24 湖南纳昇印刷电子科技有限公司 A kind of flexible perovskite photodetector and preparation method of printing
CN109166970A (en) * 2018-08-14 2019-01-08 陕西师范大学 A kind of perovskite device and preparation method thereof
CN109888113A (en) * 2019-03-25 2019-06-14 苏州协鑫纳米科技有限公司 Calcium titanium ore bed and preparation method thereof, perovskite solar battery
CN110620178A (en) * 2018-06-19 2019-12-27 湖北万度光能有限责任公司 Preparation method of perovskite solar cell
CN112614946A (en) * 2020-12-16 2021-04-06 同济大学 Flexible perovskite photoelectric detector with pyramid structure and preparation thereof
CN112614945A (en) * 2020-12-16 2021-04-06 同济大学 Micro-nano single crystal flexible photoelectric detector with groove array structure and preparation thereof

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108321297A (en) * 2018-02-05 2018-07-24 湖南纳昇印刷电子科技有限公司 A kind of flexible perovskite photodetector and preparation method of printing
CN110620178A (en) * 2018-06-19 2019-12-27 湖北万度光能有限责任公司 Preparation method of perovskite solar cell
CN109166970A (en) * 2018-08-14 2019-01-08 陕西师范大学 A kind of perovskite device and preparation method thereof
CN109166970B (en) * 2018-08-14 2022-03-29 陕西师范大学 Perovskite device and preparation method thereof
CN109888113A (en) * 2019-03-25 2019-06-14 苏州协鑫纳米科技有限公司 Calcium titanium ore bed and preparation method thereof, perovskite solar battery
CN112614946A (en) * 2020-12-16 2021-04-06 同济大学 Flexible perovskite photoelectric detector with pyramid structure and preparation thereof
CN112614945A (en) * 2020-12-16 2021-04-06 同济大学 Micro-nano single crystal flexible photoelectric detector with groove array structure and preparation thereof

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