CN205828439U - A kind of complex is the calcium titanium ore bed solaode of presoma - Google Patents
A kind of complex is the calcium titanium ore bed solaode of presoma Download PDFInfo
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- CN205828439U CN205828439U CN201620118084.3U CN201620118084U CN205828439U CN 205828439 U CN205828439 U CN 205828439U CN 201620118084 U CN201620118084 U CN 201620118084U CN 205828439 U CN205828439 U CN 205828439U
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- ore bed
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
Abstract
This utility model relates to the calcium titanium ore bed solaode that a kind of complex is presoma, calcium titanium ore bed solaode is included transparent base layer, transparency conductive electrode, hole transmission layer or electron transfer layer, calcium titanium ore bed, electron transfer layer or hole transmission layer and metal conducting layer successively by top layer to nexine, calcium titanium ore bed includes lead halide complex, lead halide complex is by anhydrous lead halide powder and dimethyl sulfoxide solvent or N, the tetrahydrofuran solution of N solvent dimethylformamide or methylamine mixes mutually so that PbX2Powder is dissolved completely in dimethyl sulfoxide solvent or N, in the tetrahydrofuran solution of N solvent dimethylformamide or methylamine, stands after adding chlorobenzene solvent stirring mixing, and the precipitate obtained after filtering.This utility model reduces CH3NH3PbX3‑nYnCrystal transformation condition, reduces PbX2Impurities left, improves the flatness of thin film, improves the light energy absorption efficiency of calcium titanium ore bed thin film, improves efficiency and the stability of calcium titanium ore bed solaode.
Description
Technical field
This utility model belongs to application of solar, is the calcium titanium ore bed of presoma particularly to a kind of complex
Solaode.
Background technology
Solaode based on perovskite material is a kind of use such as (CH3NH3PbX3-nYn) form compound make
For the solaode of light absorbent, wherein X, Y=Cl, Br, I etc..The basic structure of battery is as it is shown in figure 1, the most successively
It is divided into transparent base layer, transparency conductive electrode, hole/electron transfer layer, calcium titanium ore bed, electrons transport layer, metal electricity
Pole.Wherein Research Emphasis is concerned with calcium titanium ore bed.
The main method of existing formation calcium titanium ore bed is first by anhydrous lead iodide powder (PbI2) it is directly dissolved in N, N-
Dimethylformamide (DMF), heated solution, hereafter the solution dissolved is spin-coated on glass basic surface, forms one layer of PbI2
Thin film, heats this layer film and solvent is volatilized completely；Then PbI will be loaded with2The substrate of glass of thin film is at methylpyridinium iodide ammonium
(MAI) take out after isopropanol (IPA) solution soaks about 30 seconds, rotate drying, drip a certain amount of isopropanol again, get rid of
Dry；Or directly at PbI2Spin coating MAI solution above.Hereafter, thin film is transferred on warm table together with substrate of glass, 70 ~ 100
Degrees Centigrade 10 ~ 120 minutes.MAI will be with PbI in this process2Reaction, changes into (CH not of uniform size3NH3)PbI3
Crystal.Due to PbI2Thickness thicker (generally higher than 200 nanometer), is not easy to MAI and reacts completely, and reaction not exclusively, therefore works as shape
Become (CH3NH3)PbI3After crystal, still have a small amount of PbI2Impurities left in the film, affects property of thin film stable, fall
Low solar absorption efficiency.Additionally, also affect the flatness of thin film, cause the variable thickness of thin film, poor flatness.
Utility model content
Technical problem to be solved in the utility model is, it is provided that a kind of complex is the calcium titanium ore bed sun of presoma
Energy battery, discloses the synthetic technology of a kind of calcium titanium ore bed material, reduces CH3NH3PbX3-nYnCrystal transformation condition, reduces
PbX2Impurities left, improves the flatness of thin film, thus is greatly enhanced the light energy absorption efficiency of calcium titanium ore bed thin film.
This utility model is achieved in that the calcium titanium ore bed solaode providing a kind of complex to be presoma, calcium
Titanium ore layer solar cell is included transparent base layer, transparency conductive electrode, hole transmission layer or electronics successively by top layer to nexine
Transport layer, calcium titanium ore bed, electron transfer layer or hole transmission layer and metal conducting layer, calcium titanium ore bed includes lead halide complexation
Thing, calcium titanium ore bed is deposited on hole transmission layer or electron transfer layer formation quasiconductor light-absorption layer.
Further, the material of transparent base layer includes substrate of glass and polyethylene terephthalate (PET) substrate
In at least one.
Further, transparency conductive electrode is deposited on transparent base layer, and the material of transparency conductive electrode includes indium-doped oxygen
Change at least one in stannum (ITO), fluorine doped tin oxide (FTO) and Graphene.
Further, hole transmission layer or electric transmission are deposited upon in transparency conductive electrode, hole transmission layer or electronics
The material of transport layer includes Graphene, PEDOT:PSS, PTAA, CuSCN, CuI, MoOx, V2O5、NiO、spiro-OMeTAD、
PEIE、PEI、ZnO、TiO2, at least one in PCBM.
Further, electron transfer layer or hole transport are deposited upon on calcium titanium ore bed, electron transfer layer or hole transport
The material of layer includes Graphene, PEDOT:PSS, PTAA, CuSCN, CuI, MoOx, V2O5、NiO、spiro-OMeTAD、PEIE、
PEI、ZnO、TiO2, at least one in PCBM.
Further, metallic conduction is deposited upon electron transfer layer or hole transmission layer forms metal electrode.
Compared with prior art, complex of the present utility model is the calcium titanium ore bed solaode of presoma, have with
Lower feature:
1, at calcium titanium ore bed, lead halide complex the thin film formed can directly react with MAI, it is not necessary to heats
Process, under room temperature, just can generate perovskite thin film, energy-conservation, simple flow；
2, lead halide is fully converted into lead halide complex, saves material；
3, to CH3NH3PbX3-nYnThe window considerations that compound converts (includes annealing temperature, annealing time and MAI concentration
Deng) wider, can be at 40 ~ 100 degrees Celsius, 10 minutes ~ 20 hours, MAI concentration 40 ~ 50mg mL-1Window ranges in choosing
Selecting, performance inconsistency is little, and all can keep high efficiency；Compare the problem that condition is harsh, window is little that in background technology, thin film processes,
Adaptability is higher；
4, the calcium titanium ore bed solar battery efficiency utilizing lead halide complex to make is higher, and stability is more preferable.
Accompanying drawing explanation
Fig. 1 is the internal structure schematic diagram of calcium titanium ore bed solaode in prior art；
Fig. 2 is lead halide complex (the i.e. PbI through the present invention2Or PbI (DMSO)2(DMF)) conversion obtains
CH3NH3PbI3 thin film and through traditional PbI2Monomer converts the CH obtained3NH3PbI3 thin film, then experience five kinds of different bars of withdrawing from a secret society or underworld gang
The thin film finally given after part carries out the results contrast schematic diagram of XRD test；
Fig. 3 is lead halide complex (the i.e. PbI through the present invention2Or PbI (DMSO)2(DMF)) conversion obtains
CH3NH3PbI3 thin film and through traditional PbI2Monomer converts the CH obtained3NH3PbI3 thin film carries out transient photoluminescence and measures
The photoluminescence response curve synoptic diagram arrived；
Fig. 4 is that the thin film of Fig. 2 carries out the thin-film light emitting intensity curve schematic diagram that stable state photoluminescence measurement obtains；
Fig. 5 is lead halide complex (the i.e. PbI through the present invention2Or PbI (DMSO)2(DMF)) conversion obtains
CH3NH3PbI3 thin film and through traditional PbI2Monomer converts the CH obtained3NH3Ratio between the surface SEM image of PbI3 thin film
Relatively；
Fig. 6 is PbI2(DMF)/MAI is under different conversion conditions (annealing time, annealing temperature, methylpyridinium iodide ammonium concentration)
Solar absorption efficiency；
Fig. 7 is quasiconductor light-absorption layer PbI2、PbI2And PbI (DMSO)2(DMF) electric energy of calcium titanium ore bed solaode
Absorption efficiency curve synoptic diagram.
Detailed description of the invention
In order to make technical problem to be solved in the utility model, technical scheme and beneficial effect clearer, with
Lower combination drawings and Examples, are further elaborated to this utility model.Should be appreciated that concrete reality described herein
Execute example only in order to explain this utility model, be not used to limit this utility model.
As it is shown in figure 1, the calcium titanium ore bed solaode that a kind of complex of the present utility model is presoma, calcium titanium ore bed
Solaode is included transparent base layer 1, transparency conductive electrode 2, hole transmission layer (or electric transmission successively by top layer to nexine
Layer) 3, calcium titanium ore bed 4, electron transfer layer (or hole transmission layer) 5 and metal conducting layer 6.
Calcium titanium ore bed 4 includes lead halide complex.Lead halide complex is by anhydrous lead halide powder (chemical general formula
PbX2, X is any one in tri-kinds of elements of Cl, I, Br) with dimethyl sulfoxide solvent or DMF solvent,
Or the tetrahydrofuran solvent of methylamine mixes mutually so that PbX2Powder is dissolved completely in dimethyl sulfoxide solvent or N, N-dimethyl
In the tetrahydrofuran solution of formamide solvent or methylamine, stand after adding chlorobenzene solvent stirring mixing, and after filtering
The precipitate arrived.
The material of transparent base layer 1 includes but not limited to substrate of glass and polyethylene terephthalate (PET) substrate
In at least one.Transparency conductive electrode 2 is deposited on transparent base layer 1, and the material of transparency conductive electrode 2 includes but not limited to
At least one in indium doped tin oxide (ITO), fluorine doped tin oxide (FTO) and Graphene.Hole transmission layer (or electron transfer layer) 3
Be deposited in transparency conductive electrode 2, the material of hole transmission layer (or electron transfer layer) 3 include but not limited to Graphene,
PEDOT:PSS、PTAA、CuSCN、CuI、MoOx、V2O5、NiO、spiro-OMeTAD、PEIE、PEI、ZnO、TiO2, in PCBM
At least one；Its deposition process includes but not limited to vacuum vapor deposition method, electron-beam vapor deposition method, magnetron sputtering method, ald
Method, photoetching process, chemical vapour deposition technique, silk screen print method, hydro-thermal method, electrochemical deposition method, spin coating (spin-coating), cutter
Sheet blade coating (blade-coating), bar type coating (bar coating), slit type extrusion pressing type coating (slot-die
Coating), at least one in spraying (spray coating), ink jet printing (ink-jet printing).
Calcium titanium ore bed 4 is deposited on hole transmission layer (or electron transfer layer) 3 formation quasiconductor light-absorption layer.Electron transfer layer
(or hole transmission layer) 5 is deposited on calcium titanium ore bed 4, and the material of electron transfer layer (or hole transmission layer) 5 includes but not limited to
Graphene, PEDOT:PSS, PTAA, CuSCN, CuI, MoOx, V2O5、NiO、spiro-OMeTAD、PEIE、PEI、ZnO、TiO2、
At least one in PCBM；Its deposition process includes but not limited to vacuum vapor deposition method, electron-beam vapor deposition method, magnetron sputtering method, former
Sublayer sedimentation, photoetching process, chemical vapour deposition technique, silk screen print method, hydro-thermal method, electrochemical deposition method, spin coating, blade are scraped
At least one in painting, bar type coating, the coating of slit type extrusion pressing type, spraying, ink jet printing.Metal conducting layer 6 is deposited on electronics
Metal electrode is formed in transport layer (or hole transmission layer) 5.
It is specifically described below and of the present utility model a kind of prepares calcium titanium ore bed solaode that complex is presoma
Method, including following key step:
The first step: dissolve, synthesize complex,
Under conditions of 25 degrees Celsius of room temperatures and normal atmosphere, in air ambient, by anhydrous lead iodide powder (chemistry
Formula PbI2) it is 5 mg PbI with dimethyl sulfoxide solvent (be called for short DMSO) according to proportioning2The ratio mixing of corresponding 15mL DMSO, stirs
Mix 5 ~ 10 minutes so that PbI2Powder is dissolved completely in DMSO solvent, obtains solution A.
Second step: obtain novel lead halide complex solid,
Under conditions of 25 degrees Celsius of room temperatures and normal atmosphere, in air ambient, by chlorobenzene solvent (be called for short CB) with
The solution A obtained in the first step mixes according to volume ratio CB:A=2:1, stirs 1 ~ 2 minute, stands 5 ~ 10 minutes, produces and separates out network
Compound solid P, through filter paper filtering, obtains separating out complex solid P；Separate out complex solid P and be PbI2Halogen with DMSO
Change lead complex, separate out complex solid P and be denoted as again PbI2 (DMSO)。
3rd step: make to separate out the complex solid P calcium titanium ore bed solaode as calcium titanium ore bed,
1) surface is selected to be coated with the substrate of glass (transparent base layer) of indium doped tin oxide (ITO) electrode as calcium titanium ore bed too
The transparency conductive electrode of sun energy battery, the sheet resistance of ITO is not higher than 15 ohm；
2) depositing PEDOT:PSS with spin-coating method in transparency conductive electrode, spin coating process is: room temperature, atmospheric pressure environment,
The PEDOT:PSS that can complete to cover substrate surface amount is dripped in substrate surface, starts to rotate with 4000 revs/min rapidly, rotation
Stop after turning 30 seconds, then warm table is transferred in substrate, heat 10 minutes at a temperature of 140 degree；
3) on PEDOT:PSS layer, deposition separates out complex solid P.Whole process is carried out in pure nitrogen gas environment, environment
Air pressure is an atmospheric pressure, and ambient temperature is 25 degrees Celsius of room temperatures, and its detailed process is:
1. precipitation complex solid P is dissolved in DMF solvent (being called for short DMF), stirs 5 minutes, obtain
Solution B, the concentration of solution B is 1 mol/L；
2. methylpyridinium iodide ammonium (MAI) is dissolved in isopropanol solvent according to the mass/volume ratio of 60mg/mL and (is called for short
IPA) solution C is formed；
3. solution B is heated to 70 degrees Celsius and keeps being stirred continuously；
4. take the solution B being heated to 70 degrees Celsius in right amount, be the most uniformly spin-coated on the PEDOT:PSS that step 2 has been formed
The surface of layer, spin coating rotating speed 3000 revs/min, continue 30 seconds, the amount smeared is determined by the size of concrete sample, forms thickness
The complete thin film of 500 nanometers；
5. smearing on the thin film that solution B is formed again with the rotating speed spin coating solution C of 3000 revs/min so that molten within 30 seconds
Solvent in liquid C volatilizees substantially, and solute retains；Then, the thin film having smeared solution B and C is heated 120 under 100 degrees Celsius
Minute, form quasiconductor light-absorption layer；
4) depositing electron transfer layer on quasiconductor light-absorption layer, the material of use is a kind of fullerene derivate, is referred to as
PCBM and zinc oxide (being called for short ZnO).Concrete grammar is: PCBM is dissolved in chlorobenzene solvent according to the amount of 20mg/mL, is heated to
60 degrees Celsius make PCBM be completely dissolved, and are then titrated on aforementioned film (calcium titanium ore bed) by solution, with the speed of 2000 revs/min
Spin coating 45 seconds；Then the ZnO particle (20mg/m) being scattered in ethanol is spun on according to the speed of 4000 revs/min and is painted with
The film surface of PCBM, spin coating duration 30 seconds；
5) 4) depositing metal conductive layer in structure formed in step, selected material is gold.It is embodied as step
Suddenly: aforementioned sample is transferred into hot evaporation in instrument, and utilizes temperature control console regulation transparent substrates to need when heat is deposited with
Temperature.Open vacuum pump, open reel servo mechanism, treat that vacuum is higher than 1 × 10-4After Pa, it is deposited with 100 nanometers with hot vapour deposition method
Gold.
The feature of above-mentioned preparation method is:
1、PbI2(DMF) thin film can directly react with MAI, it is not necessary to carries out heat treated, just can generate under room temperature
Perovskite thin film, energy-conservation, simple flow.
2、PbI2(U) CH can be fully converted into3NH3PbI3, improve and convert the CH obtained3NH3PbI3Quality, simultaneously
Can also save material.Refer to shown in Fig. 2, (a), (b), (c) in Fig. 2 is by PbI respectively2、PbI2And PbI (DMSO)2
(DMF) convert and finally give after certain annealing (room temperature, 70 ° of C, 80 ° of C, 90 ° of C or 100 ° of C)
CH3NH3PbI3The XRD test result of thin film.In the XRD signal obtained under all annealing conditions of (a), on the left of main peak, i.e.
2 θ=12.5 degree, can be clearly seen that a peak-to-peak signal, and that the peak of this position is corresponding is PbI2Crystal, explanation
CH3NH3PbI3Thin film has PbI2Residual.Above-mentioned signal is not then had in any XRD curve of (b) and (c).This illustrates PbI2
(U) CH can be fully converted into3NH3PbI3, there is no PbI2Remain in CH3NH3PbI3In thin film, improve what conversion obtained
CH3NH3PbI3Quality, simultaneously can also reduce PbI2Consumption.
3、CH3NH3PbI3Membrane quality promotes, and the defect within thin film is less, and the thin film carriers life-span improves 10 times.
Support in data refer to shown in Fig. 3, and Fig. 3 is to PbI2、PbI2And PbI (DMSO)2(DMF) CH obtained is converted3NH3PbI3
It is corresponding that thin film carries out the luminescence generated by light that transient photoluminescence measurement obtains, the most corresponding different carrier lifetime.Carrier
Life-span is the longest, and in thin film is described, defect concentration is the least, and film quality is the highest.From the three of Fig. 3 curves it can be seen that by PbI2
(DMSO) CH obtained is converted3NH3PbI3Thin film internal flaw is minimum, calculates through models fitting, by PbI2(DMSO) convert
The CH arrived3NH3PbI3The thin film carriers life-span is by PbI2Monomer converts the CH obtained3NH3PbI310 times, therefore its electric charge
Mobility is the highest.
4、CH3NH3PbI3Membrane quality promotes, and the internal non-radiation type of thin film is compound to be significantly reduced.Support in data please be joined
According to shown in Fig. 4, Fig. 4 is to PbI2、PbI2And PbI (DMSO)2(DMF) CH obtained is converted3NH3PbI3Thin film carries out steady-state light
The thin-film light emitting intensity that photoluminescence measurement obtains, it can be seen that by PbI2The luminous intensity of the thin film prepared is minimum, by PbI2
(DMSO)zThe luminous intensity of the thin film prepared is the highest, is PbI225 times of peak of curve.
5, the CH formed3NH3PbI3Thin film is the most smooth.Refer to shown in Fig. 5, (a), (b), (c) are quasiconductor light-absorption layers
PbI2、PbI2And PbI (DMSO)2(DMF) CH obtained is converted3NH3PbI3Film surface top view, (d), (e), (f) are section views
Figure；Wherein figure (a) and figure (d) are the thin film utilizing traditional method to prepare, it can clearly be seen that there is overshooting shape structure on surface.
Figure (b) and figure (e) are to utilize PbI2(DMF) thin film obtained, surface is the most homogeneous, smooth.Figure (c) and figure (f) are to utilize PbI2
(DMSO) thin film obtained, surface is the most homogeneous, smooth.
6, to CH3NH3PbI3The window considerations converted (includes annealing time, annealing temperature and methylpyridinium iodide ammonium concentration
(MAI concentration)) wider, can be at 40 ~ 100 degrees Celsius, 10 minutes ~ 20 hours, the window of MAI concentration 40mg/mL ~ 50mg/mL
Selecting in the range of Kou, performance inconsistency is little, and all can keep high efficiency；Compare thin film treatment conditions harshness, window in background technology
Little problem, adaptability is higher.Refer to shown in Fig. 6, (a) is to obtain under the conditions of the different annealing times of 15 ~ 120 minutes
Battery efficiency curve；B () is the battery efficiency curve obtained under the conditions of the different annealing temperature of 70 ~ 100 degrees Celsius；C () is
The battery efficiency curve obtained under the different MAI concentration levels of 40mg/mL ~ 50mg/mL.
7, calcium titanium ore bed solar battery efficiency is higher, and stability is more preferable.Refer to shown in Fig. 7.
List below is shown that hole transport strata triaryl amine of the present utility model, and (poly-triaryamine is called for short
PTAA) with the Contrast on effect (PTAA VS Pedot:PSS VS CuSCN VS CuI) of other hole transport layer material:
| HTL | Short circuit current | Open-circuit voltage | Fill factor, curve factor | Transformation efficiency |
| PTAA | 19.4 | 1.10 | 79.9% | 17.0% |
| PEDOT:PSS | 17.4 | 1.03 | 75.9% | 13.6% |
| CuSCN | 15.5 | 1.06 | 63.2% | 10.5% |
| CuI | 14.5 | 1.03 | 61.4% | 9.17% |
The foregoing is only preferred embodiment of the present utility model, not in order to limit this utility model, all at this
Any amendment, equivalent and the improvement etc. made within the spirit of utility model and principle, should be included in this utility model
Protection domain within.
Claims (6)
1. complex is a calcium titanium ore bed solaode for presoma, and described calcium titanium ore bed solaode is by top layer inwards
Layer includes transparent base layer, transparency conductive electrode, hole transmission layer or electron transfer layer, calcium titanium ore bed, electron transfer layer successively
Or hole transmission layer and metal conducting layer, it is characterised in that described calcium titanium ore bed includes lead halide complex, described perovskite
It is deposited upon on hole transmission layer or electron transfer layer formation quasiconductor light-absorption layer.
2. complex as claimed in claim 1 is the calcium titanium ore bed solaode of presoma, it is characterised in that described transparent
The material of basal layer includes at least one in substrate of glass and PET substrate.
3. complex as claimed in claim 1 is the calcium titanium ore bed solaode of presoma, it is characterised in that described transparent
Conductive electrode is deposited on transparent base layer, the material of described transparency conductive electrode include indium doped tin oxide, fluorine doped tin oxide and
At least one in Graphene.
4. complex as claimed in claim 1 is the calcium titanium ore bed solaode of presoma, it is characterised in that described hole
Transport layer or electric transmission are deposited upon in transparency conductive electrode.
5. complex as claimed in claim 1 is the calcium titanium ore bed solaode of presoma, it is characterised in that described electronics
Transport layer or hole transport are deposited upon on calcium titanium ore bed.
6. complex as claimed in claim 1 is the calcium titanium ore bed solaode of presoma, it is characterised in that described metal
Conductive layer deposition forms metal electrode on electron transfer layer or hole transmission layer.
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