CN118251022B - Inverse type wide-bandgap perovskite solar cell and preparation method thereof - Google Patents
Inverse type wide-bandgap perovskite solar cell and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an inverse type wide-bandgap perovskite solar cell and a preparation method thereof, wherein the inverse type wide-bandgap perovskite solar cell comprises a hole transmission layer, a perovskite film layer and an electron transmission layer which are sequentially stacked from a substrate to an electrode layer, the perovskite film layer generates electron-hole pairs under illumination, electrons are extracted and led out by the electron transmission layer, and holes are extracted and led out by the hole transmission layer; the hole transport layer is arranged on the substrate, the perovskite film layer is deposited on the hole transport layer, the perovskite film layer is a component for forming perovskite ABX 3, and the hole transport layer material at least comprises a compound I. The perovskite solar cell adopts the compound I with cyano groups and electron withdrawing groups as the hole transport layer material, so that the connection effect between the perovskite film layer and the hole transport layer is enhanced, the defect between the perovskite film layer and the hole transport layer is effectively passivated, and the efficiency and the stability of the perovskite solar cell are improved.
Description
Technical Field
The invention relates to an inverse type wide-bandgap perovskite solar cell and a preparation method thereof, and belongs to the field of photovoltaics.
Background
Perovskite solar cells are of great interest because of their high power conversion efficiency and low manufacturing costs. The theoretical efficiency limit of the single junction perovskite solar cell is about 33%, and the recording efficiency of the laboratory is 26.1% at present, so that the efficiency is more difficult to further improve. Compared with a single-junction battery, the theoretical efficiency of the laminated battery reaches about 45%, and the laminated battery has absolute efficiency advantages. The wide band gap perovskite solar cell can be matched with various narrow band gap bottom cells (such as a silicon cell, a copper indium gallium selenide cell, an organic cell and the like) to form a laminated cell, so that the wide band gap perovskite solar cell has a great application prospect. In order to realize a high-efficiency perovskite laminated cell, the preparation of a wide-band-gap perovskite solar cell is particularly important. Among perovskite solar cell structures, the inverted structure (p-i-n) perovskite solar cell has a simpler device structure, lower preparation temperature and preparation cost compared with the positive structure (n-i-p), and is suitable for the development of industrialization. Currently, the development of efficiency for wide bandgap inverted perovskite cells lags behind conventional bandgap inverted perovskite cells, one of the reasons being that hole transport materials used as wide bandgap cells are typically adapted to conventional bandgap cells, where mismatched energy levels often occur. The unmatched energy levels can form larger potential energy difference at the interface to prevent the extraction and transmission of carriers, thereby reducing the efficiency of the battery.
For the inverted wide band gap perovskite solar cell, a proper hole transport material is designed, the recombination of carriers at the interface is reduced, the extraction of carriers at the hole interface is accelerated, the efficiency and stability of the inverted wide band gap cell and the stacked cell are improved, the industrialization of the perovskite solar cell is facilitated, and the method has great significance for the development of the whole photovoltaic industry.
Disclosure of Invention
In order to reduce the recombination of carriers at an interface and accelerate the extraction of carriers at a hole interface, the invention provides an inverse type wide-bandgap perovskite solar cell, which adopts organic-inorganic hybridized lead-based perovskite as a cell light absorption material and adopts a compound with cyano groups and electron withdrawing groups as a hole transport layer material, so that the connection effect between a perovskite film layer and the hole transport layer is enhanced, the defects between the perovskite film layer and the hole transport layer are effectively passivated, and the efficiency and the stability of the perovskite solar cell are improved.
The technical scheme adopted by the invention is as follows: an inverse wide-bandgap perovskite solar cell comprises a hole transmission layer, a perovskite film layer and an electron transmission layer which are sequentially stacked from a substrate to an electrode layer, wherein the perovskite film layer generates electron-hole pairs, electrons are guided out by the electron transmission layer, and holes are guided out by the hole transmission layer; the hole transport layer is arranged on the substrate, the hole transport layer is made of a compound CN-4PA-PX (R1, R2), the compound I is provided with cyano groups, phosphonic acid groups and electron withdrawing groups R1, R2, the perovskite film layer is deposited on the hole transport layer, the perovskite film layer is made of a component of perovskite ABX 3, wherein A site is an organic-inorganic cation, namely part of A site is an organic ion, and part of A site is an inorganic ion; the B site is lead ion; the X position is halogen. Preferably, the substrate is a transparent conductive substrate. According to the perovskite solar cell, CN-4PA-PX (R1, R2) is adopted as a hole transmission material of the cell, phosphonic acid groups in the material can be anchored with transparent electrode oxide, cyano groups can be passivated and anchored with the surface of perovskite and defects, so that molecules can effectively form a molecular bridge between perovskite and a transparent electrode, and the extraction process of photo-generated holes is accelerated. In addition, the molecule has proper energy level arrangement for the wide band gap perovskite, so that the energy barrier difference after the interface is formed between the conventional hole transport material and the wide band gap perovskite film layer is reduced, the extraction and migration of carriers are further accelerated, and the efficiency and stability of the perovskite solar cell are improved.
The structural formula of the compound I in the hole transport layer material isR1 and R2 in the structural formula are identical or different in structure and can be selected from one or two of halogen groups, alkyl groups, alkoxy groups, halogenated alkyl groups, halogenated alkoxy groups, nitro groups and sulfonic groups, preferably halogen groups, wherein R1 and R2 serve as electron withdrawing groups to change the delocalization space of electrons, so that the mismatch of HOMO energy levels between the perovskite film layer material and the hole transport layer material is reduced, and holes can be effectively extracted. In the invention, R1 and R2 and cyano are in meta position of benzene ring.
As a preferable scheme, in the structural formula of the compound I, R1 and R2 are-Cl or-Br, or R1 is-Cl, R2 is-CF 3, and the structural formula of the compound I is as follows:、、。
as a preferred embodiment, compound one is prepared by the following method:
(1) Raw materials were obtained as the compounds dican-PX (R1, R2) and 1, 4-dibromobutane.
(2) The compound II and 1, 4-dibromobutane are reacted under the action of strong alkali and phase transfer catalyst to graft the long chain of the 1, 4-dibromobutane onto the compound II, so as to obtain a compound III, the concentration of strong alkali, preferably KOH or NaOH, in the reaction solution is about 8-12 mol/L,
The first reaction is preferably carried out at 60-80 ℃, so that the reaction progress is facilitated to be promoted, the reaction is more thorough, the reaction temperature is preferably 65 ℃, the reaction time is preferably 10-14 h, and the yield of the compound III can reach more than 90%.
(3) The compound III is reacted under the action of a catalyst to obtain phosphonate, the phosphonate is placed in a mixed solution of SiBr (CH 3)3 and dioxane for reaction to obtain silicon phosphonate, the silicon phosphonate is hydrolyzed to obtain the compound I, preferably the compound III is reacted under the action of a Pt catalyst to obtain the phosphonate, the reaction temperature is preferably 150-170 ℃, more preferably 160 ℃ and the reaction time is 0-28 h, preferably the phosphonic acid ester reacts at room temperature to obtain the phosphonic acid silicon ester, and the phosphonic acid silicon ester is hydrolyzed into a compound I, preferably methanol and water, in the presence of alcohol and water.
The thickness of the hole transport layer affects the carrier transport efficiency, and as a preferred scheme, the thickness of the hole transport layer is 2-10 nm, preferably 4-8 nm, and more preferably 5-6 nm.
The perovskite film layer material comprises a component a and a component b, wherein the component a is one component or a combination of multiple components of lead iodide, lead bromide and lead chloride, and the component b is one component or a combination of multiple components of cesium iodide, rubidium iodide, formamidine iodine, formamidine bromine, formamidine chlorine, methyl amine iodine, methyl amine bromine, methyl amine chlorine, cesium chloride and cesium bromide.
The electron transport layer material is at least one of tin oxide, titanium oxide, zinc oxide, fullerene and fullerene derivative material, preferably fullerene and fullerene derivative material.
The invention also provides a preparation method of the inverse type wide-bandgap perovskite solar cell, which comprises the following steps:
S01, acquiring a substrate;
s02 preparation of hole transport layer:
(1) Dissolving a hole transport layer material in an organic solvent to prepare a solution with the concentration of 0.2-2.5 mg/mL, wherein the hole transport layer material is CN-4PA-PX (R1, R2);
(2) Coating a hole transport layer material solution on a substrate;
(3) Annealing a substrate coated with a hole transport layer material, forming the hole transport layer on the substrate;
s03, preparing a perovskite film layer: coating perovskite film layer materials on the hole transport layer;
s04, preparing an electron transport layer: and coating an electron transport layer material on the perovskite film layer.
As a preferred method for preparing the perovskite film layer, the method comprises the following steps: (1) Mixing one or more components of lead iodide, lead bromide and lead chloride with one or more components of cesium iodide, rubidium iodide, formamidine iodine, formamidine bromine, formamidine chlorine, methyl amine iodine, methyl amine bromine, methyl amine chlorine, cesium chloride and cesium bromide to form a mixed solution, and depositing the mixed solution on the hole transport layer; (2) adding an antisolvent dropwise into the mixture to form a film; (3) Heating and annealing after forming a wet film, evaporating residual solvent and promoting the crystallization of the perovskite film layer; (4) And (3) carrying out post-treatment on the film formed by annealing crystallization, and drying by adopting a heating or vacuum mode. The perovskite film layer material obtained by the preparation method has strong bonding strength with the hole transport layer, and the valence band top of the obtained material is higher than the HOMO energy level of the hole transport material, so that holes are favorably transferred from the perovskite film layer to the hole layer.
As a preferred mode, the electron transport layer is deposited on the perovskite film layer, and the material of the electron transport layer is at least one of tin oxide, titanium oxide, zinc oxide, fullerene (C 60) and fullerene derivative material.
As a preferred mode, the electron transport layer is prepared by vacuum deposition or solution deposition; the vacuum deposition is preferred, and the deposition mode not only can obtain a compact and uniform film layer, but also can form an interface with good contact, thereby improving the electron transmission efficiency.
As a preferred mode, the electron transport layer is prepared by evaporating the C 60 material on the perovskite film layer by means of thermal evaporation.
As a preferable mode, a hole blocking layer is arranged between the electron transport layer and the electrode layer, and the hole blocking layer material is 2, 9-dimethyl-4, 7-diphenyl-1, 10-phenanthroline (BCP). Still more preferably, the hole blocking layer is vapor-deposited on the electron transport layer by thermal vapor deposition.
The invention has the technical effects that: according to the invention, an organic-inorganic hybridized lead type material is adopted as a perovskite film layer material, CN-4PA-PX (R1, R2) containing cyano groups is adopted as a hole transport layer material, so that on one hand, the connection strength between the perovskite film layer and the hole transport layer is effectively enhanced, the defects of the perovskite film layer are passivated, on the other hand, the cyano groups serve as high-efficiency Lewis bases, and paired electrons can be provided for common defects such as unpaired Pb 2+ on the bottom surface, so that the effect of passivating the defects is achieved, and the efficiency and stability of the reverse wide band gap battery are further improved.
In the invention, a halogen group, an alkyl group, an alkoxy group, a halogenated alkyl group, a halogenated alkoxy group, a nitro group or a sulfonic acid group is adopted in the cavity transmission layer material CN-4PA-PX (R1, R2) as an electron-withdrawing group to change the delocalization space of electrons, so that the HOMO energy level of the cavity transmission layer material is reduced, and the position which is more matched with the perovskite film layer material is achieved. Therefore, the introduction of the material can further reduce the potential energy difference between the HOMO of the hole transport layer and the valence band of the wide-bandgap perovskite film layer, and accelerate the extraction and transmission of photo-generated holes at the interface.
In the invention, the electron-withdrawing group and the cyano group are in meta position of the benzene ring, which is beneficial to strengthening the connection strength between the hole transport layer material and the perovskite film layer material and strengthening the transport performance of holes on the interface.
Drawings
FIG. 1 is a schematic diagram of a perovskite solar cell of the present invention;
Fig. 2 is a graph of current versus voltage for the cells of example 1 and comparative example 1;
Fig. 3 is a graph of current versus voltage for the cells of example 2 and comparative example 2;
FIG. 4 is a graph of normalized efficiency of the cells of example 2 and comparative example 2 under light conditions;
fig. 5 normalized efficiency plots for the cells of example 3 and comparative example 3 under heated conditions.
Detailed Description
The invention will be explained in further detail below with reference to the drawings and the specific embodiments, but it should be understood that the scope of protection of the invention is not limited to the specific embodiments.
The perovskite solar cell is an inverse wide-bandgap perovskite solar cell, and the film structure is shown in figure 1 and comprises a substrate 1, a hole transport layer 2, a perovskite film layer 3, an electron transport layer 4 and an electrode layer 5 which are sequentially arranged.
Example 1
The preparation method of the inverted wide-band-gap perovskite solar cell in the embodiment comprises the following steps:
S01 acquisition substrate
An ITO (indium tin oxide) glass substrate is adopted as a substrate, the ITO glass substrate is firstly ultrasonically cleaned in deionized water for 30 minutes, then ultrasonically cleaned in acetone for 30 minutes, finally ultrasonically cleaned in isopropyl alcohol (IPA) for 30 minutes, then dried by a nitrogen gun, and then treated in an ultraviolet ozone processor for 30 minutes for standby.
S02 preparation of hole transport layer
(1) Preparation of the hole-transporting layer material (this step may be performed in a preparation stage before the perovskite solar cell is prepared, ready for use)
In this embodiment, the hollow transmission layer is made of CN-4PA-PX (Cl, cl) and has the structural formula: The preparation method of the hole transport layer material comprises the following steps:
a. The obtained raw materials CN-PX (Cl, cl) and 1, 4-dibromobutane, wherein the CN-PX (Cl, cl) has the structural formula: ；
b. Reacting CN-PX (Cl, cl) with 1, 4-dibromobutane under the action of a strong alkali phase transfer catalyst to enable the 1, 4-dibromobutane to be grafted on the CN-PX (Cl, cl) to obtain CN-4Br-PX (Cl, cl), namely The strong alkali environment is realized by KOH with the concentration of 8mol/L in the reaction liquid, the reaction temperature is 65 ℃, and the reaction time is 12 hours;
；
c. The product CN-4Br-PX (Cl, cl) obtained in the reaction 1-1 is reacted for 24 hours under the condition of 160 ℃ under the action of a Pt catalyst to obtain phosphonate, then the phosphonate is reacted for 12 hours under the action of SiBr (CH 3)3 and dioxane) at room temperature to obtain silicon phosphonate, and the silicon phosphonate is hydrolyzed under the action of methanol and water at room temperature to obtain a hole transport layer material CN-4PA-PX (Cl, cl), namely 。
(2) 0.5Mg of CN-4PA-PX (Cl, cl) was mixed with 1mL of ethanol solution to obtain 0.5mg/mL of CN-4PA-PX (Cl, cl) solution, which was filtered to remove large particulate matters using a 0.45 μm filter core, and the filtered solution was ready for use.
(3) The filtered solution was spin-coated onto ITO glass at a spin-coating rate of 3200rpm for 30 seconds.
(4) Annealing at 100deg.C for 13min to obtain a hole transport layer with a thickness of about 5 nm.
S03 preparation of perovskite film layer
(1) Preparing perovskite film layer solution:
a. PbI 2 (lead iodide), FAI (formamidine iodine), pbBr 2 (lead bromide) and FABr (formamidine bromine) are dissolved in a mixed solution of N, N-Dimethylformamide (DMF) and dimethyl sulfoxide (DMSO) in a molar ratio of 0.75:0.75:0.25:0.25 to form a solution I, wherein the volume ratio of DMF to DMSO is 4:1, and the concentration of Pb 2+ in the solution I is 1.5mol/L;
b. Adding methylamine chloride (MACl) additive into the first solution to form a solution with MACl mass fraction of 31.5%;
c. heating the solution to 70 ℃ and stirring for 60min to completely dissolve;
d. the solution was filtered using a 0.22 μm filter to remove large particulate matter from the solution and the solution was filtered for use.
(2) And (3) spin-coating the perovskite film layer solution on the hole transport layer, wherein the spin-coating speed is 4000rpm, and when the spin-coating is 15s, dropwise adding 0.5mL of anti-solvent chlorobenzene on the film layer, and then continuing spin-coating for 40s.
(3) And (3) annealing the substrate in air at 145 ℃ for 20 minutes after spin coating, and controlling the humidity to be 20-30%.
S04 preparation of an Electron transport layer
And evaporating the C 60 material by using a vacuum evaporation device in a thermal evaporation mode to form a 25nm electron transport layer on the perovskite film layer, wherein the evaporation vacuum degree is below 7 x 10 -4 Pa.
S05, preparing a hole blocking layer:
And evaporating the 2, 9-dimethyl-4, 7-diphenyl-1, 10-phenanthroline (BCP) material by using vacuum evaporation equipment in a thermal evaporation mode to form an 8nm hole blocking layer on the electron transport layer, wherein the evaporation vacuum degree is below 7 x 10 -4 Pa.
Preparation of an S06 electrode layer:
Using a vacuum deposition apparatus, 150nm copper (Cu) was deposited on the surface of BCP by a thermal deposition method as an electrode, and the deposition vacuum was 7×10 -4 Pa or less.
Comparative example 1
The difference from example 1 is that: the preparation method of the inverse type wide band gap perovskite solar cell in the embodiment adopts PTAA (poly [ bis (4-phenyl) (2, 4, 6-trimethylphenyl) amine ]) as a hole transport layer material, and comprises the following steps:
S01 acquisition substrate
An ITO glass substrate is adopted as a substrate, the ITO glass substrate is firstly ultrasonically cleaned in deionized water for 30 minutes, then ultrasonically cleaned in acetone for 30 minutes, finally ultrasonically cleaned in isopropyl alcohol (IPA) for 30 minutes, then dried by a nitrogen gun, and then treated in an ultraviolet ozone processor for 30 minutes for standby.
S02 preparation of hole transport layer
(1) Mixing 2mg of PTAA with 1mL of ethanol solution to obtain 2mg/mL of PTAA solution, filtering to remove large particulate matters by using a filter core with the thickness of 0.45 mu m, and reserving the filtered solution;
(2) Spin-coating the filtered solution on ITO glass at a spin-coating speed of 3200rpm for 30s;
(3) Annealing at 100℃for 13min gave a hole transport layer of about 5nm thickness.
S03 preparation of perovskite film layer
(1) Preparing perovskite film layer solution:
a. PbI 2,FAI,PbBr2, FABr is dissolved in a mixed solution of N, N-Dimethylformamide (DMF) and dimethyl sulfoxide (DMSO) in a molar ratio of 0.75:0.75:0.25:0.25 to form a solution I, wherein the volume ratio of DMF to DMSO is 4:1, and the concentration of Pb 2+ in the solution I is 1.5mol/L;
b. adding MACl additives to the solution to form a solution with MACl mass fraction of 31.5%;
c. heating the solution to 70 ℃ and stirring for 60min to completely dissolve;
d. the solution was filtered using a 0.22 μm filter to remove large particulate matter from the solution and the solution was filtered for use.
(2) And (3) spin-coating the perovskite film layer solution on the hole transport layer, wherein the spin-coating speed is 4000rpm, and when the spin-coating is 15s, dropwise adding 0.5mL of anti-solvent chlorobenzene on the film layer, and then continuing spin-coating for 40s.
(3) And after spin coating, annealing in air at 145 ℃ for 20min, and controlling the humidity to be 20-30%.
S04 preparation of an Electron transport layer
And evaporating the C 60 material by using a vacuum evaporation device in a thermal evaporation mode to form a 25nm electron transport layer on the perovskite film layer, wherein the evaporation vacuum degree is below 7 x 10 -4 Pa.
S05, preparing a hole blocking layer:
And evaporating the BCP material by using a vacuum evaporation device in a thermal evaporation mode to form an 8nm hole blocking layer on the electron transport layer, wherein the evaporation vacuum degree is below 7 x 10 -4 Pa.
Preparation of an S06 electrode:
Using a vacuum deposition apparatus, 150nm copper (Cu) was deposited on the surface of BCP by a thermal deposition method as an electrode, and the deposition vacuum was 7×10 -4 Pa or less.
The current and voltage of the perovskite solar cell obtained in example 1 and comparative example 1 were monitored and plotted as a graph, and as shown in fig. 2, the perovskite solar cell using CN-4PA-PX (Cl, cl) as the hole transport layer material exhibited higher open circuit voltage and fill factor, mainly derived from suppressed non-radiative recombination and enhanced transport characteristics, with a conversion efficiency improved by 1.88% over the absolute efficiency of the perovskite solar cell using PTAA as the hole transport layer material, as shown in table 1 in particular.
Table 1 example 1 and comparative example 1 perovskite solar cell photovoltaic parameters
| Conditions (conditions) | Open circuit voltage (V) | Short-circuit current (mA/cm 2) | Fill factor (%) | Conversion efficiency (%) |
| Example 1 | 1.167 | 22.05 | 79.18 | 20.38 |
| Comparative example 1 | 1.139 | 21.98 | 73.87 | 18.50 |
。
Example 2
The preparation method of the inverted wide-bandgap perovskite solar cell comprises the following steps:
S01 acquisition substrate
The ITO glass substrate was first ultrasonically cleaned in deionized water for 30 minutes, then in acetone for 30 minutes, finally in isopropyl alcohol (IPA) for 30 minutes, then blow-dried with a nitrogen gun, and treated in an ultraviolet ozone treater for 30 minutes for use.
S02 preparation of hole transport layer
(1) Preparation of the hole-transporting layer material (this step may be performed in a preparation stage before the perovskite solar cell is prepared, ready for use)
The hollow transmission layer material in this embodiment includes CN-4PA-PX (Br, br), and the structural formula is: The preparation method of the hole transport layer material comprises the following steps:
a. The structural formulas of the obtained raw materials CN-PX (Br, br) and 1, 4-dibromobutane, and CN-PX (Br, br) are as follows: ；
b. The CN-PX (Br, br) and the 1, 4-dibromobutane are reacted for 1-2 under the action of strong alkali and a phase transfer catalyst, so that the 1, 4-dibromobutane is grafted on the CN-PX (Br, br) to obtain the CN-4Br-PX (Br, br), and the strong alkali environment is realized by NaOH with the concentration of 10mol/L in the reaction liquid, namely The reaction temperature is 70 ℃ and the reaction time is 12 hours;
；
c. The product CN-4Br-PX (Br, br) obtained in the reaction 1-2 is reacted for 20 hours under the action of a Pt catalyst at 150 ℃ to obtain phosphonate, then the phosphonate is reacted for 12 hours under the action of SiBr (CH 3)3 and dioxane) at room temperature to obtain silicon phosphonate, and the silicon phosphonate is hydrolyzed under the action of methanol and water at room temperature to obtain a hole transport layer material CN-4PA-PX (Br, br), namely 。
(2) 20Mg of NiO x powder was mixed with 1mL of deionized water, stirred at room temperature for 1 hour, and the large particles in the solution were removed by filtration using a 0.45 μm filter core, and a NiO x solution was obtained after filtration for use.
(3) 0.6Mg of CN-4Br-PX (Br, br) was mixed with 1mL of isopropyl alcohol (IPA), and after dissolution by stirring, the mixture was filtered through a 0.45 μm filter to obtain a CN-4PA-PX (Br, br) solution for use.
(4) The filtered NiO x solution was spin coated onto the UV treated ITO substrate at a spin rate of 3000rpm for 30s followed by annealing at 130℃for 30min.
(5) After the film was cooled, a solution of CN-4PA-PX (Br, br) was spin-coated on the substrate of NiO x at 4000rpm for 30s, followed by annealing at 100℃for 10min to obtain a hole transport layer having a thickness of about 7 nm.
S03 preparation of perovskite film layer
(1) The perovskite film layer material is dissolved in a solvent to obtain a perovskite film layer solution, the perovskite film layer material is 22.0mg of cesium iodide, 29.2mg of methylamine bromide, 230.5mg of formamidine iodine, 548.6mg of lead iodide and 187.5mg of lead bromide, the solvent is 1mL of a mixed solution of DMF and DMSO, the volume ratio of DMF to DMSO is 6:1, the solution is heated to 60 ℃ and stirred for 1 hour to enable the solution to be fully dissolved, a filter core of 0.22 mu m is used for filtering, and the filtered solution is reserved.
(2) And (3) spin-coating the prepared perovskite film layer solution on the hole transport layer, wherein the spin-coating speed is 4000rpm, the spin-coating time is 40s, and when the spin-coating is 19s, 0.4mL of anti-solvent chlorobenzene is dropwise added on the film layer, and then annealing is carried out for 20min at 100 ℃, and cooling is carried out for later use.
S04 preparation of an Electron transport layer
And evaporating the C 60 material by using a vacuum evaporation device in a thermal evaporation mode to form a 25nm electron transport layer on the perovskite film layer, wherein the evaporation vacuum degree is below 7 x 10 -4 Pa.
S05 preparation of hole blocking layer
And evaporating the BCP material by using a vacuum evaporation device in a thermal evaporation mode to form an 8nm hole blocking layer (BCP film layer) on the electron transport layer, wherein the evaporation vacuum degree is below 7 x 10 -4 Pa.
S06 preparation of electrode layer
And (3) using a vacuum evaporation device, and evaporating 120nm silver (Ag) on the surface of the BCP film layer by using a thermal evaporation mode to serve as an electrode, wherein the evaporation vacuum degree is below 7 x 10 -4 Pa.
Comparative example 2
The difference from example 2 was only that the hole transport layer material was MeO-2PACz ([ 2- (3, 6-dimethoxy-9H-carbazol-9-yl) ethyl ] phosphonic acid).
The preparation method of the inverted wide-bandgap perovskite solar cell comprises the following steps:
S01 acquisition substrate
The ITO glass substrate was first ultrasonically cleaned in deionized water for 30 minutes, then in acetone for 30 minutes, finally in isopropyl alcohol (IPA) for 30 minutes, then blow-dried with a nitrogen gun, and treated in an ultraviolet ozone treater for 30 minutes for use.
S02 preparation of hole transport layer
(1) 20Mg of NiO x powder was mixed with 1mL of deionized water, stirred at room temperature for 1 hour, and the large particles in the solution were removed by filtration using a 0.45 μm filter core, and a NiO x solution was obtained after filtration for use.
(2) 0.6Mg of MeO-2PACz was mixed with 1mL of IPA, dissolved with stirring, and filtered through a 0.45 μm filter to obtain a MeO-2PACz solution for use.
(3) The filtered NiO x solution was spin coated onto the UV treated ITO substrate at a spin rate of 3000rpm for 30s followed by annealing at 130℃for 30min.
(4) After the film was cooled, a MeO-2PACz solution was spin-coated on the substrate of NiO x at 4000rpm for 30s, followed by annealing at 100℃for 10min to obtain a hole transport layer having a thickness of about 7 nm.
S03 preparation of perovskite film layer
(1) Dissolving a perovskite film layer material in a solvent to obtain a perovskite film layer solution, wherein the perovskite film layer material comprises 22.0mg of cesium iodide, 29.2mg of methylamine bromide, 230.5mg of formamidine iodine, 548.6mg of lead iodide and 187.5mg of lead bromide; in a mixed solution of DMF and DMSO with a solvent of 1mL, the volume ratio of DMF to DMSO was 6:1, the solution was heated to 60℃and stirred for 1 hour to dissolve thoroughly, and the solution was filtered using a 0.22 μm filter cartridge and the filtered solution was ready for use.
(2) And (3) spin-coating the prepared perovskite film layer solution on the hole transport layer, wherein the spin-coating speed is 4000rpm, the spin-coating time is 40s, and when the spin-coating is 19s, 0.4mL of anti-solvent chlorobenzene is dropwise added on the film layer, and then annealing is carried out for 20min at 100 ℃, and cooling is carried out for later use.
S04 preparation of an Electron transport layer
And evaporating the C 60 material by using a vacuum evaporation device in a thermal evaporation mode to form a 25nm electron transport layer on the perovskite film layer, wherein the evaporation vacuum degree is below 7 x 10 -4 Pa.
S05 preparation of hole blocking layer
And evaporating the BCP material by using a vacuum evaporation device in a thermal evaporation mode to form an 8nm hole blocking layer (BCP film layer) on the electron transport layer, wherein the evaporation vacuum degree is below 7 x 10 -4 Pa.
S06 preparation of electrode layer
And (3) using a vacuum evaporation device, and evaporating 120nm silver (Ag) on the surface of the BCP film layer by using a thermal evaporation mode to serve as an electrode, wherein the evaporation vacuum degree is below 7 x 10 -4 Pa.
In test example 2, the cell photoelectric parameters using NiOx+CN-4PA-PX (Br, br) as the hole transport layer material and the cell photoelectric parameters using NiOx+MeO-2PACz as the hole transport layer material in the comparative example are obviously superior to those of the comparative example in terms of open-circuit voltage, short-circuit current, filling factor and cell conversion efficiency, and the filling factor and conversion efficiency are respectively improved by 3.56% and 1.23%, as shown in Table 2.
Table 2 example 2 and comparative example 2 perovskite solar cell photoelectric parameters
| Conditions (conditions) | Open circuit voltage (V) | Short-circuit current (mA/cm 2) | Fill factor (%) | Conversion efficiency (%) |
| Example 2 | 1.161 | 20.93 | 78.09 | 18.98 |
| Comparative example 2 | 1.134 | 21.00 | 74.53 | 17.75 |
The voltage-dependent change curve of the battery current using NiOx+CN-4PA-PX (Br, br) as the hole transport layer material in test example 2 was comparable to the voltage-dependent change curve of the battery current using NiOx+MeO-2PACz as the hole transport layer material in comparative example 2, as shown in FIG. 3, but the open circuit voltage example 2 was significantly higher than comparative example 2, and it was found that the passivation performance of the example was excellent.
Under the illumination condition, as shown in fig. 4, the illumination stability of the batteries in comparative example 2 and comparative example 2 shows that the normalization efficiency of the battery in example 2 is still about 0.9 after 550 hours of illumination, while the battery efficiency in comparative example 2 is drastically reduced with the increase of illumination time, and is reduced to less than 0.8 after 550 hours.
Example 3
The preparation method of the inverted wide-bandgap perovskite solar cell comprises the following steps:
S01 acquisition substrate
The ITO glass is used as a substrate, the substrate is firstly ultrasonically cleaned in deionized water for 30 minutes, then in acetone for 30 minutes, finally in isopropyl alcohol (IPA) for 30 minutes, then dried by a nitrogen gun, and then treated in an ultraviolet ozone processor for 30 minutes for standby.
S02 preparation of hole transport layer
(1) Preparation of the hole-transporting layer material (this step may be performed in a preparation stage before the perovskite solar cell is prepared, ready for use)
In this embodiment, the hollow transmission layer is made of CN-4PA-PX (Br, CF 3), and the structural formula is: The preparation method of the hole transport layer material comprises the following steps:
a. The obtained raw materials CN-PX (Br, CF 3) and 1, 4-dibromobutane, the structural formula of CN-PX (Br, CF 3) is as follows: ；
b. Reacting CN-PX (Br, br) with 1, 4-dibromobutane under the action of strong alkali and phase transfer catalyst for 1-3, grafting 1, 4-dibromobutane onto CN-PX (Br, CF 3) to obtain CN-4Br-PX (Br, CF 3), namely The strong alkali environment is realized by KOH with the concentration of 11mol/L, the reaction temperature is 65 ℃, and the reaction time is 12 hours;
；
c. The product CN-4Br-PX (Br, CF 3) obtained in the reaction 1-3 is reacted for 20 hours under the action of Pt catalyst at 150 ℃ to obtain phosphonate, then the phosphonate is reacted for 12 hours under the action of SiBr (CH 3)3 and dioxane) at room temperature to obtain silicon phosphonate, and the silicon phosphonate is hydrolyzed under the action of methanol and water at room temperature to obtain a hole transport layer material CN-4PA-PX (Br, CF 3), namely 。
(2) 0.55Mg of CN-4PA-PX (Br, CF 3) was mixed with 1mL of ethanol solution and the large particulate matter was removed by filtration using a 0.45 μm filter cartridge, and the filtered solution was ready for use.
(3) The filtered hole transport layer solution was spin-coated on an ITO substrate at 3500rpm for 30s, followed by annealing at 100deg.C for 10min to obtain a hole transport layer about 6nm thick.
S03 preparation of perovskite film layer
(1) PbI 2,FAI,PbBr2, FABr is dissolved in a mixed solution of N, N-Dimethylformamide (DMF) and N-methylpyrrolidone (NMP) in a molar ratio of 0.75:0.75:0.25:0.25 to form a solution I, wherein the volume ratio of DMF to NMP is 7.5:1, and the Pb 2+ concentration in the solution I is 1.75mol/L;
(2) Adding MACl additives to the solution to form a solution with MACl mass fraction of 30%;
(3) Heating the solution to 70 ℃ and stirring for 60min to completely dissolve;
(4) Filtering the solution by using a filter element with the diameter of 0.22 mu m, removing large particulate matters in the solution, and filtering the solution for later use;
(5) Spin-coating the filtered solution on the hole transport layer at a spin-coating speed of 4500rpm for 40s, dropwise adding 0.5mL of anti-solvent chlorobenzene on the film layer at the spin-coating time of 25s, and then annealing for 20min at 140 ℃ in air with the humidity controlled at 30-40%, thereby obtaining the perovskite film layer.
S04 preparation of an Electron transport layer
[6,6] -Phenyl-C61-butyric acid methyl ester (PCBM) was dissolved in chlorobenzene at a concentration of 20mg/mL, and stirred at room temperature for 2 hours to dissolve, thereby obtaining a PCBM solution.
PCBM solution was spin coated onto the perovskite film layer at 3000rpm for 60 seconds.
S05 preparation of hole blocking layer
BCP was dissolved in isopropyl alcohol at a concentration of 0.2mg/mL and stirred at room temperature for 2 hours to obtain a BCP solution.
The BCP solution was spin coated on PCBM film at 4000rpm for 60 seconds.
S06 preparation of electrode layer
120Nm silver (Ag) is evaporated on the surface of BCP by using a vacuum evaporation device as an electrode, and the vacuum degree is controlled below 7 x10 -4 Pa.
Comparative example 3
The only difference from example 3 is that the hole transport layer material was different, the preparation method used was:
S01 acquisition substrate
The ITO glass is used as a substrate, the substrate is firstly ultrasonically cleaned in deionized water for 30 minutes, then in acetone for 30 minutes, finally in isopropyl alcohol (IPA) for 30 minutes, then dried by a nitrogen gun, and then treated in an ultraviolet ozone processor for 30 minutes for standby.
S02 preparation of hole transport layer
0.55Mg of Me-4PACz ((4- (3, 6-dimethyl-9H-carbazol-9-yl) butyl) phosphonic acid) was mixed with 1mL of ethanol solution and the large particulate matter was removed by filtration using a 0.45 μm filter cartridge, and the filtered solution was ready for use.
The filtered hole transport layer solution was spin-coated on an ITO substrate at a spin-coating rate of 3500rpm for a spin-coating time of 30s, followed by annealing at 100℃for 10min to obtain a hole transport layer of about 6nm.
S03 preparation of perovskite film layer
(1) PbI 2,FAI,PbBr2, FABr is dissolved in a mixed solution of N, N-Dimethylformamide (DMF) and N-methylpyrrolidone (NMP) in a molar ratio of 0.75:0.75:0.25:0.25, wherein the volume ratio of DMF to NMP is 7.5:1, and the Pb 2+ concentration in the obtained solution is 1.75mol/L;
(2) Adding MACl additives to the solution to form a solution with MACl mass fraction of 30%;
(3) Heating the solution to 70 ℃ and stirring for 60min to completely dissolve;
(4) Filtering the solution by using a filter element with the diameter of 0.22 mu m, removing large particulate matters in the solution, and filtering the solution for later use;
(5) Spin-coating the prepared perovskite film layer solution on a hole transport layer, wherein the spin-coating speed is 4500rpm, the spin-coating time is 40s, dropwise adding 0.5mL of anti-solvent chlorobenzene on the film layer when spin-coating is 25s, then annealing for 20min at 140 ℃ in air, controlling the humidity to be 30-40%, and cooling to obtain the perovskite film layer.
S04 preparation of an Electron transport layer
(1) Dissolving [6,6] -phenyl-C61-methyl butyrate (PCBM) in chlorobenzene with the concentration of 20mg/mL, stirring at room temperature for 2 hours to obtain PCBM solution;
(2) PCBM solution was spin coated onto the perovskite film layer at 3000rpm for 60 seconds.
S05 preparation of hole blocking layer
(1) BCP is dissolved in isopropanol with the concentration of 0.2mg/mL, and stirred at room temperature for 2 hours to be dissolved, so as to obtain BCP solution;
(2) The BCP solution was spin coated on PCBM film at 4000rpm for 60 seconds.
S06 preparation of electrode layer
120Nm silver (Ag) is evaporated on the surface of BCP by using a vacuum evaporation device as an electrode, and the vacuum degree is controlled below 7 x10 -4 Pa.
The batteries of example 3 and comparative example 3 were tested for thermal stability, and the batteries of example 3 and comparative example 3 were placed in a glove box environment at 85 ℃ to test the normalized efficiencies of both, and as shown in fig. 5, the normalized efficiencies of the batteries of example 3 and comparative example 3 were reduced with the increase of time, the variation trend difference of both in the initial stage was not obvious, the battery variation in example 3 was gradually smoothed after 200 hours, and the battery of comparative example 3 still maintained the original dropping rate, and the stability of the battery of example 3 under the high temperature environment was significantly better than that of comparative example 3.
The foregoing has shown and described the basic principles and features of the invention and the advantages of the inventive patent. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the foregoing description is only illustrative of one or more embodiments of the invention, and that various changes and modifications may be made therein without departing from the spirit and scope of the invention as defined in the following claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. An inverse wide bandgap perovskite solar cell, characterized by: the perovskite type solar cell comprises a hole transmission layer, a perovskite film layer and an electron transmission layer which are sequentially laminated from a substrate to an electrode layer, wherein the perovskite film layer generates electron-hole pairs under illumination, electrons are extracted and led out by the electron transmission layer, and holes are extracted and led out by the hole transmission layer; the hole transport layer is arranged on a substrate, the perovskite film layer is deposited on the hole transport layer, the perovskite film layer is a component for forming perovskite ABX 3, wherein A is an organic-inorganic cation, B is a lead ion, X is halogen, the hole transport layer material at least comprises a compound I, and the structural formula of the compound I is as follows:
；
Wherein R1 and R2 are the same or different, and R1 and R2 are one or two selected from halogen groups, alkyl groups, alkoxy groups, halogenated alkyl groups, halogenated alkoxy groups, nitro groups and sulfonic acid groups.
2. The inverted wide bandgap perovskite solar cell of claim 1, wherein: in the first compound, R1 and R2 are-Cl or R1 is-Br, R2 is-CF 3 or R1 and R2 are-Br, and the structural formula of the first compound is one of the following:
、、。
3. The inverted wide bandgap perovskite solar cell of claim 1, wherein: the preparation method of the compound I comprises the following steps:
(1) Obtaining a raw material, wherein the raw material comprises CN-PX (R1, R2) and 1, 4-dibromobutane, and the CN-PX (R1, R2) has the structural formula:
；
(2) Reacting CN-PX (R1, R2) with 1, 4-dibromobutane to enable long chains of the 1, 4-dibromobutane to be grafted to the CN-PX (R1, R2) to obtain CN-4Br-PX (R1, R2), wherein the CN-4Br-PX (R1, R2) has the structural formula:
，
；
(3) Phosphonating CN-4Br-PX (R1, R2) to obtain the compound I.
4. An inverted wide bandgap perovskite solar cell according to claim 3, wherein: the phosphonating in the step (3) specifically comprises the following steps:
a. CN-4Br-PX (R1, R2) generates phosphonate under the action of a catalyst;
b. Adding SiBr (mixed solution of CH 3)3 and dioxane) into the phosphonate, and reacting the phosphonate, the SiBr (CH 3)3 and dioxane) to generate silicon phosphonate;
c. the silicon phosphonate is hydrolyzed in the presence of alcohol and water to obtain the compound one.
5. The inverted wide bandgap perovskite solar cell of claim 1, wherein: the thickness of the hole transport layer is 2-10 nm.
6. The inverted wide bandgap perovskite solar cell of claim 1, wherein: the perovskite film layer material comprises a component a and a component b, wherein the component a is one component or a combination of multiple components of lead iodide, lead bromide and lead chloride, and the component b is one component or a combination of multiple components of cesium iodide, rubidium iodide, formamidine iodine, formamidine bromine, formamidine chlorine, methyl amine iodine, methyl amine bromine, methyl amine chlorine, cesium chloride and cesium bromide.
7. The inverted wide bandgap perovskite solar cell of claim 1, wherein: the electron transport layer material is at least one of tin oxide, titanium oxide, zinc oxide, fullerene and fullerene derivative material.
8. The preparation method of the inverted wide-bandgap perovskite solar cell is characterized by comprising the following steps of: the method comprises the following steps:
S01, acquiring a substrate;
s02, disposing a hole transport layer on the substrate: the hole transport layer material comprises a compound I with the structural formula of Wherein R1 and R2 are the same or different, and R1 and R2 are one or two selected from halogen groups, alkyl groups, alkoxy groups, halogenated alkyl groups, halogenated alkoxy groups, nitro groups and sulfonic groups;
s03, arranging a perovskite film layer on the hole transport layer;
s04, arranging an electron transport layer on the perovskite film layer;
and S05, arranging an electrode layer on the electron transmission layer to obtain the inverse type wide-bandgap perovskite solar cell.
9. The method of manufacturing a reverse-type wide bandgap perovskite solar cell as claimed in claim 8, wherein: the preparation method of the hole transport layer comprises the following steps:
(1) Dissolving a first compound in an organic solvent to prepare a solution of 0.2-2.5 mg/mL;
(2) Coating the prepared solution of the compound I on a substrate;
(3) And (3) placing the substrate coated with the hole transport layer material at 90-110 ℃ for annealing for 10-30 min, and forming the hole transport layer on the substrate.
10. The method of manufacturing a reverse-type wide bandgap perovskite solar cell as claimed in claim 8, wherein: the preparation method of the compound I comprises the following steps:
a. obtaining a raw material, wherein the raw material comprises a compound of CN-PX (R1, R2) and 1, 4-dibromobutane, and the structural formula of the CN-PX (R1, R2) is as follows:
；
b. CN-PX (R1, R2) reacts with 1, 4-dibromobutane to make long chain of 1, 4-dibromobutane grafted to CN-PX (R1, R2) to obtain compound III,
；
C. phosphonating the third compound to obtain the first compound.
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