CN108461635A - A kind of method and its application of boron compound surface modification perovskite thin film - Google Patents
A kind of method and its application of boron compound surface modification perovskite thin film Download PDFInfo
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Abstract
The invention discloses a kind of method and its application of boron compound surface modification perovskite thin film, it is effectively passivated the iodide ion not being coordinated in perovskite thin film by being introduced into boron element, reduce defect state density, the photoelectric properties of perovskite thin film are improved, and then realize the perovskite solar cell device of efficient stable.The solar cell device that perovskite light-absorption layer is modified through joining boron compound obtains higher photoelectric conversion efficiency, and preparation method is easy and the production cycle is shorter while with good stability.
Description
Technical field
Present invention relates particularly to a kind of method and its application of boron compound modifying interface perovskite thin film, belong to light
Sulfate ferroelectric functional material and device arts.
Background technology
It is increasing to the demand of the energy with the continuous development of human society.Develop renewable, environmentally friendly energy
Source (such as wind energy, water energy, solar energy) is imperative.It is to solve currently faced energy shortage and ring to make full use of solar energy
One of effective ways of vital conjunctures such as border pollution.Photovoltaic generation is prior development direction.It is traditional based on silicon semiconductor at present
There are production cost height, energy consumptions for the photovoltaic technology of technique greatly, easily causes the shortcomings of environmental pollution, and researcher always searches for
The novel photovoltaic technology of " high performance-price ratio " solar cell may be implemented.Perovskite solar cell is due to its low cost and height
The features such as efficiency, receives the extensive concern of academia and industrial quarters, and device photoelectric transfer efficiency is rapid from 3.8% in 2009
Rise to the 22.1% of current certification.
Perovskite material refers to having and CaTiO3A kind of organic-inorganic hybrid material of same crystal structure, chemistry are logical
Formula ABX3.Such material has cheap, absorption coefficient of light height, band gap can with inorganic and organic semiconducting materials advantages
It adjusts, the advantages that carrier mobility is high.Perovskite thin film is processed usually using solution and is prepared, and the film of acquisition has polycrystallinity
With the characteristic of ionic crystals.In this film, the ligancy of crystal boundary or grain surface ion with the ligancy of body phase ion not
Together, crystal boundary or grain surface is caused to be made of the excessive cation in part or anion.This surface characteristic is inevitably made
At the structural disorder and crystal defect of perovskite thin film, and then reduce the photoelectric properties of film.Many researchers have by introducing
Machine or inorganic material carry out modifying interface to perovskite thin film, reduce film defects state, obtain the perovskite of efficient stable too
Positive energy battery.
Invention content
The purpose of the present invention is to provide a kind of method and its application of boron compound surface modification perovskite thin film, lead to
It crosses to perovskite thin film surface modification, reduces the film defects density of states, improve film photoelectric performance, and then realize efficient stable
Perovskite solar cell device.
Method provided by the invention to perovskite thin film surface modification is connection boron compound solution that will be containing B-B keys
It is supported on perovskite thin film surface, then 50-100 DEG C of annealing, obtains the perovskite thin film of connection boron compound modification.
It is ABX that chemical general formula, which can be selected, in above-mentioned perovskite active layer material3Material, wherein A be CH3NH3 +(MA+),
NH2CH=NH2 +(FA+), C4H9NH3 +, Cs+, Ru+, K+One or more of mixing；B is Pb2+、Sn2+、Ge2+、Sb3+、Bi3+、
Ag+At least one of；X is Cl-, Br-, I-One or more of mixing.
Above-mentioned boron compound can be selected from the following compound containing B-B keys：C12H24B2O4、C10H20B2O4、
C12H8B2O4、 B2(OH)4、C8H24B2N4Deng.Its compound formula is represented by B2(XY)4, wherein X can be N, O or Si element,
Y can be hydrogen (Hp, p is positive integer) or alkyl (CmHn, m, n are positive integer).
Connection boron compound is dissolved in solvent and is configured to connection boron compound solution, the solvent is selected from：Isopropanol, positive fourth
The organic solvents such as alcohol, chlorobenzene, toluene, methyl phenyl ethers anisole, hexamethylene.The concentration of the boron compound solution is preferably 0.5~
20mg/mL.It is with the concrete operations that boron compound modifies perovskite thin film are joined：Under oxygen-free atmosphere, connection boronation is closed
Object solution is coated to perovskite thin film surface, then in 50~100 DEG C of annealings, the annealing time is preferably 5~
30min.The oxygen-free atmosphere is typically chosen in N2, the inert atmospheres such as Ar.In some embodiments of the invention, using N2Protection
The aqueous isopropanol of the connection boron compound of 0.5~10 mg/mL concentration is surface modified perovskite thin film under atmosphere.
The present invention also provides a kind of perovskite solar cells, including transparent substrates, and layer successively over the substrate
Folded transparent electrode, electron transfer layer, perovskite light-absorption layer, hole transmission layer and top electrode, which is characterized in that the calcium titanium
The interface that mine light-absorption layer is contacted with hole transmission layer is modified by connection boron compound.
In above-mentioned perovskite solar cell, the transparent materials such as glass, flexiplast may be used in the transparent substrates.
Transparent electrode material can be tin oxide (FTO), nano silver wire, graphene or the carbon nanometer of tin indium oxide (ITO), Fluorin doped
Pipe.Frequently with ITO electro-conductive glass, FTO electro-conductive glass, nano silver wire modified conducting glass, graphene modified electro-conductive glass and carbon
It is a kind of as transparent substrates and transparent electrode in nanotube layer modified conducting glass.
In above-mentioned perovskite solar cell, metal oxide electron transport layer may be selected in the electron transfer layer, including
TiO2、 SnO2, any one or more material such as ZnO, MgO.
In above-mentioned perovskite solar cell, the perovskite light-absorption layer the surface that it is contacted with hole transmission layer be by
Join boron compound modification.The modification is effectively passivated the iodide ion not being coordinated in perovskite thin film by being introduced into boron element, drop
The low defect density of states improves the photoelectric properties of perovskite thin film.
In above-mentioned perovskite solar cell, organic and inorganic material, organic material can be used in the hole transmission layer
Including but not limited to：Spiro-OMeTAD、PEDOT:Organic P-type semiconductor material such as PSS, TPD, PTAA, P3HT, PCPDTBT
Material；Inorganic material includes but not limited to：NixO、V2O5、CuI、MoO3Etc. inorganic p-type semiconductor material.Common appropriate bis- (trifluoros
Methane) sulfimide lithium salts and 4- tert .-butylpyridines (4-tBP) adulterate organic cavity transmission layer.
In above-mentioned perovskite solar cell, the metals such as Au, Ag can be used in the top electrode.
Invention further provides the preparation methods of above-mentioned perovskite solar cell, include the following steps：
1) transparent substrates and transparent electrode are provided；
2) electron transfer layer is prepared on the transparent electrodes；
3) perovskite light-absorption layer is prepared on the electron transport layer, and connection boron compound is carried out to perovskite extinction layer surface and is repaiied
Decorations；
4) hole transmission layer is prepared on the perovskite light-absorption layer of connection boronation modified；
5) top electrode is prepared on the hole transport layer.
Above-mentioned steps 1) in, transparent electrode is cleaned and dried and carries out ultraviolet and/or ozone treatment.
Above-mentioned steps 3) to perovskite light-absorption layer carry out connection boron compound modifying interface method be：Under oxygen-free atmosphere,
By the connection boron compound solution loadings containing B-B keys in perovskite extinction layer surface；It is transferred at 50-100 DEG C of annealing of warm table
Reason obtains the perovskite light-absorption layer of connection boron compound modification.
In the above method, dissolves solvent used in the boron compound and be selected from：Isopropanol, n-butanol, chlorobenzene, first
The organic solvents such as benzene, methyl phenyl ethers anisole, hexamethylene.Frequently with the aqueous isopropanol of the connection boron compound of 0.5-20mg/mL concentration.
Above-mentioned steps 5) method that vacuum thermal evaporation can be used prepares metallic top electrode.For rationally utilize cell area and
Convenient test controls top electrode shape frequently with different shape template.
Compared to the method for existing modifying interface perovskite thin film, the present invention is using connection boron compound to perovskite thin film
It is post-processed, boron element is introduced into the iodide ion that can be effectively passivated and be not coordinated in perovskite thin film, and it is close to reduce defect state
Degree, improves the photoelectric properties of perovskite thin film.Modifying interface is carried out to perovskite thin film using connection boron compound, in perovskite
It still belongs to the first time in the research field of solar cell.The device prepared based on the method obtains higher photoelectric conversion efficiency
(21%, referring to Fig. 3), preparation method is easy and the production cycle is shorter while also with good stability.
Description of the drawings
Fig. 1 is that connection boron compound modifies front and back calcium titanium in the embodiment 1 observed using scanning electron microscope (SEM)
Mine film surface appearance figure, wherein before the boron compound modification of (a) connection, after (b) joining boron compound modification.
Fig. 2 is that the transient state of the front and back perovskite thin film of connection boron compound modification in the embodiment 1 using spectrometer test is glimmering
Light spectrum.
Fig. 3 is the J-V curves of the perovskite solar cell prepared in embodiment 1.
Fig. 4 is to modify lacking for front and back perovskite thin film using connection boron compound in dark-state current-voltage testing example 1
Fall into state characterization.
Specific implementation mode
Below in conjunction with specific embodiment to the specific steps of the present invention with principle is further is annotated, but the present invention is simultaneously
It is not limited to following embodiment.
Embodiment 1
The first step uses deionized water, acetone, optical glass detergent, deionized water, isopropanol to be cleaned by ultrasonic successively
ITO glass substrates (15 Ω/), in baking oven after 60 DEG C of dry 4h, in the SnO of a concentration of 5wt% of the surfaces ITO spin coating2Nanometer
Brilliant material, wherein solvent for use are distilled water.Spin coating rotating speed is 3000rpm, spin-coating time 20s, acceleration 2000rpm/
s.Then by 150 DEG C of substrate, 30 minutes heating anneals.
Second step, by SnO2Film substrate is transferred to N2The perovskite precursor liquid of 1.3M is supported on SnO by atmosphere glove box2
On film, spin coating rotating speed is 6000rpm, spin-coating time 30s, acceleration 2000rpm/s.The formula of perovskite precursor liquid
For：1.09M iodate carbonamidine, the lead iodide of 1.15M, the bromination methylamine of 0.20M, 0.20M lead bromide, be dissolved in DMF and
DMSO(V:V=4:1) in the mixed solvent.Spin coating terminates film being transferred to 100 DEG C of the thermal station film forming of heating 60 minutes.
Third walks, and the C of 5mg/mL is loaded on perovskite thin film after the cooling period12H24B2O4Aqueous isopropanol, spin coating turn
Speed is 5000rpm, spin-coating time 30s, acceleration 2000rpm/s.It is transferred at thermal station 100 DEG C of heating annealing in 10 minutes
Reason.C12H24B2O4The SEM of perovskite thin film before and after the processing is shown in Fig. 1, it can be seen that before and after the processing, perovskite thin film surface shape
Too big change does not occur for looks.C12H24B2O4The transient state fluorescence spectrum of perovskite thin film before and after the processing is shown in Fig. 2, it can be seen that
C12H24B2O4The perovskite thin film of processing has the decay life time of bigger, illustrates to obtain higher-quality perovskite thin film.
4th step, the chlorobenzene solution of the Spiro-OMeTAD of spin coating 72.3mg/mL on the perovskite thin film after modification, and
Contain lithium salts 17.5 microlitres (520mg/mL is dissolved in acetonitrile) and 28.8 microlitres of 4-tBP in every milliliter of solution.Spin coating turns
Speed is 4000rpm, spin-coating time 25s.The gold of 80nm thickness is deposited after film forming as metallic top electrode.Such cell photoelectric
Transfer efficiency can reach 21% (see Fig. 3).Fig. 4 is to utilize dark-state current-voltage test characterization perovskite thin film defect state density
Collection of illustrative plates, it can be seen from the figure that connection boron processing perovskite thin film have smaller trap filling region starting voltage (VTFL),
Illustrate that the perovskite thin film for joining boron processing has smaller defect state density.
Embodiment 2
In third step, the C of 5mg/mL is loaded on perovskite thin film after the cooling period10H20B2O4Aqueous isopropanol, spin coating
Rotating speed is 5000rpm, spin-coating time 30s, acceleration 2000rpm/s.The heating 10 minutes of 100 DEG C of thermal station is transferred to anneal
Processing.The preparation method is the same as that of Example 1 for remaining step.This perovskite-like solar cell photoelectric transfer efficiency is reachable~and 21%.
Embodiment 3
In third step, the C of 5mg/mL is loaded on perovskite thin film after the cooling period12H8B2O4Aqueous isopropanol, spin coating turn
Speed is 5000rpm, spin-coating time 30s, acceleration 2000rpm/s.It is transferred at thermal station 100 DEG C of heating annealing in 10 minutes
Reason.The preparation method is the same as that of Example 1 for remaining step.This perovskite-like solar cell photoelectric transfer efficiency is reachable~and 20%.
Embodiment 4
In third step, the B of 5mg/mL is loaded on perovskite thin film after the cooling period2(OH)4Aqueous isopropanol, spin coating turn
Speed is 5000rpm, spin-coating time 30s, acceleration 2000rpm/s.It is transferred at thermal station 100 DEG C of heating annealing in 10 minutes
Reason.The preparation method is the same as that of Example 1 for remaining step.This perovskite-like solar cell photoelectric transfer efficiency is reachable~and 20%.
Embodiment 5
In third step, the C of 5mg/mL is loaded on perovskite thin film after the cooling period8H24B2N4Aqueous isopropanol, spin coating turn
Speed is 5000rpm, spin-coating time 30s, acceleration 2000rpm/s.It is transferred at thermal station 100 DEG C of heating annealing in 10 minutes
Reason.The preparation method is the same as that of Example 1 for remaining step.This perovskite-like solar cell photoelectric transfer efficiency is reachable~and 20%.
Claims (10)
1. a kind of method being surface modified to perovskite thin film, by the connection boron compound solution loadings containing B-B keys in calcium
Titanium ore film surface obtains the perovskite thin film of connection boron compound modification then in 50-100 DEG C of annealing.
2. the method as described in claim 1, which is characterized in that the chemical general formula of the boron compound is B2(XY)4, wherein X
It is N, O or Si, Y represents HpOr CmHn, m, n, p are positive integer.
3. method as claimed in claim 2, which is characterized in that the boron compound is selected from the following chemical combination containing B-B keys
It is one or more in object：C12H24B2O4、C10H20B2O4、C12H8B2O4、B2(OH)4And C8H24B2N4。
4. the method as described in claim 1, which is characterized in that connection boron compound is dissolved in organic solvent and is configured to connection boron
Connection boron compound solution is coated to perovskite thin film surface, then in 50~100 DEG C by compound solution under oxygen-free atmosphere
Annealing.
5. method as claimed in claim 4, which is characterized in that a concentration of 0.5~20mg/ of the boron compound solution
mL；The annealing time is 5~30min.
6. a kind of perovskite solar cell, including transparent substrates, and stack gradually over the substrate transparent electrode, electronics
Transport layer, perovskite light-absorption layer, hole transmission layer and top electrode, which is characterized in that the perovskite light-absorption layer and hole transport
The interface of layer contact is modified by connection boron compound.
7. perovskite solar cell as claimed in claim 6, which is characterized in that the chemical general formula of the boron compound is
B2(XY)4, wherein X is N, O or Si, and Y represents HpOr CmHn, m, n, p are positive integer.
8. perovskite solar cell as claimed in claim 7, which is characterized in that the boron compound be selected from it is following containing
It is one or more in the compound of B-B keys：C12H24B2O4、C10H20B2O4、C12H8B2O4、B2(OH)4And C8H24B2N4。
9. the preparation method of any perovskite solar cell of claim 6~8, includes the following steps：
1) transparent substrates and transparent electrode are provided；
2) electron transfer layer is prepared on the transparent electrodes；
3) perovskite light-absorption layer is prepared on the electron transport layer, and connection boron compound modification is carried out to perovskite extinction layer surface；
4) hole transmission layer is prepared on the perovskite light-absorption layer of connection boronation modified；
5) top electrode is prepared on the hole transport layer.
10. preparation method as claimed in claim 9, which is characterized in that step 3) carries out connection boronation to perovskite light-absorption layer and closes
The method of object modifying interface is：Under oxygen-free atmosphere, by the connection boron compound solution loadings containing B-B keys in perovskite light-absorption layer
Surface；50~100 DEG C of annealings of warm table are transferred to, the perovskite light-absorption layer of connection boron compound modification is obtained.
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