CN115843186A - SnO modified based on multifunctional polymer 2 All-inorganic CsPbBr 3 Perovskite solar cell and application thereof - Google Patents
SnO modified based on multifunctional polymer 2 All-inorganic CsPbBr 3 Perovskite solar cell and application thereof Download PDFInfo
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Abstract
The invention provides SnO modified based on multifunctional polymer 2 All-inorganic CsPbBr 3 Perovskite solar cell and application thereof, namely SnO modified by polyacrylic acid 2 Preparing an electron transport layer on FTO (fluorine-doped tin oxide) by spin coating after quantum dot solution, coating a PAA (poly (acrylic acid)) layer on the electron transport layer as a pre-buried bottom interface, and forming CsPbBr on the PAA layer by a multi-step spin coating method 3 Layer of CsPbBr 3 And coating a carbon electrode on the surface of the layer to obtain the solar cell. The invention provides for the inhibition of SnO by PAA 2 Quantum dots in solutionThe high-quality electron transmission layer is obtained by the agglomeration phenomenon. The PAA layer can passivate uncoordinated Sn on the surface of the electron transport layer 4+ And CsPbBr 3 Unliganded Pb in the layer 2+ So as to achieve the purpose of compensating thermal strain in situ. The solar cell provided by the invention has high efficiency and good stability, and has practical value and economic value for promoting the industrialization process of the perovskite solar cell.
Description
Technical Field
The invention belongs to the technical field of new materials and new energy, and particularly relates to SnO modified based on multifunctional polymer 2 All-inorganic CsPbBr 3 Perovskite solar cell and application thereof.
Background
Solar energy is one of the main new energy sources, and is naturally burdened with achieving the goal of "carbon peak-to-peak carbon neutralization", in which a solar cell is one of the main ways of directly utilizing solar energy. Through the development of more than 40 years, although the highest certified photoelectric conversion efficiency of the monocrystalline silicon solar cell reaches 26.1%, the monocrystalline silicon rod with the purity of 99.999% is required to be used as a raw material, the cost is high, the manufacturing process is complex, and the perovskite solar cell is widely concerned due to the low manufacturing cost (half of the cost of the monocrystalline silicon cell) and the simple manufacturing process. After only a decade of rapid development, organic-inorganic hybrid perovskite solar cells have been comparable to conventional single crystal silicon cells by virtue of their 25.7% certified photoelectric conversion efficiency.
The organic-inorganic hybrid perovskite solar cell has poor stability under the conditions of humidity, heat, light and oxygen and can not be put into production all the time, and the all-inorganic hybrid perovskite solar cell does not contain easily decomposed organic matters and has stability far higher than that of the organic-inorganic hybrid perovskite solar cell, wherein CsPbBr 3 The perovskite solar cell can stably work for more than 100 days, and CsPbBr 3 The perovskite solar cell adopts a cheap carbon electrode to further reduce the cost, and CsPbBr is adopted by improving the methods of perovskite film preparation process, interface engineering, component engineering, spectral engineering, strain regulation and control and the like 3 The photoelectric conversion efficiency of perovskite solar cells has exceeded 11%.
Tin oxide (SnO) 2 ) By virtue of high electron mobility and high light transmissionThe rate has been widely applied to the preparation of electron transport layers for perovskite solar cells, but SnO in solution due to van der waals interactions between nanoparticles 2 Quantum dots tend to spontaneously form aggregates, precipitating at the bottom of the solution, and SnO 2 The quantum dot surface has a certain amount of hydroxyl groups, and the hydroxyl groups on the surface are easy to separate during annealing to form exposed Sn single bonds, so that defects are generated. Thus, stabilization of SnO in dispersions 2 Quantum dots, reduction of SnO 2 Hydroxyl on the surface of the quantum dot is important for manufacturing a high-quality electron transport layer, promoting electron transport and reducing carrier recombination. In addition, csPbBr is caused 3 The phase transition temperature of the layer is as high as 250 ℃, and residual strain is generated in the process of cooling to room temperature, and the residual strain is CsPbBr 3 The morphology of the layers, the structure of the crystal, the carrier transport at the interface and the photoelectric conversion efficiency and stability of the complete device all have adverse effects. Thus, csPbBr is reduced 3 Residual strain in layers for the manufacture of highly efficient and stable all-inorganic CsPbBr 3 Perovskite solar cells are of critical importance.
Disclosure of Invention
The invention aims to provide SnO modified based on multifunctional polymer 2 All-inorganic CsPbBr 3 Perovskite solar cell and application thereof, and SnO is optimized 2 Electron transport layer and release of CsPbBr 3 The thermal strain in the layer promotes the transmission of carriers and improves the full inorganic CsPbBr 3 Performance of perovskite solar cells.
In order to realize the purpose of the invention, the invention adopts the following technical scheme to realize:
SnO modified based on multifunctional polymer 2 All-inorganic CsPbBr 3 The perovskite solar cell is prepared by the following preparation method:
(1) SnCl 2 And thiourea (CH 4 N 2 S) dissolving in deionized water, stirring, centrifuging, removing precipitate, and filtering to obtain SnO 2 A quantum dot solution;
(2) The SnO in the step (1) 2 Preheating the quantum dot solution;adding polyacrylic acid (PAA) powder into preheated SnO 2 Stirring in quantum dot solution to obtain SnO modified by PAA 2 Solutions of quantum dots, i.e. PAA-SnO 2 A quantum dot solution;
(3) Mixing the PAA-SnO in the step (2) 2 Preheating the quantum dot solution and the FTO conductive glass; preheating PAA-SnO 2 The quantum dot solution is spin-coated on the preheated FTO conductive glass to obtain FTO/PAA-SnO 2 A substrate;
(4) Spin-coating an aqueous PAA solution on the FTO/PAA-SnO described in step (3) 2 Obtaining PAA-SnO modified by single-layer PAA on the substrate 2 An electron transport layer to obtain FTO/PAA-SnO 2 A PAA substrate;
(5) The FTO/PAA-SnO in the step (4) 2 PAA substrate and PbBr 2 Preheating the solution, and adding the preheated PbBr 2 The solution is coated on FTO/PAA-SnO in a spinning way 2 Annealing on PAA substrate to obtain PbBr 2 A film;
(6) PbBr described in step (5) 2 Spin-coating CsBr solution on the film to obtain the CsPbBr modified by PAA 3 A layer;
(7) CsPbBr described in step (6) 3 Coating carbon slurry on the layer, annealing to obtain carbon electrode and obtain fully inorganic CsPbBr 3 Perovskite solar cell.
The invention is achieved by the use of SnO 2 Polyacrylic acid (PAA) powder is added into the quantum dot solution, and SnO is regulated and controlled by bonding through carboxyl ligand units on a PAA long chain 2 The distribution of quantum dots in the solution and the film-forming state on FTO after spin-coating annealing, thereby obtaining high-quality uniform SnO 2 An electron transport layer, passivated SnO 2 Defects in the electron transport layer are beneficial to the extraction of charges. By the reaction in SnO 2 Electron transport layer and CsPbBr 3 PAA layer is added between interfaces of the layers to form a pre-buried bottom interface to release CsPbBr 3 Residual strain in the layer and serves to passivate the defects.
CsPbBr 3 The residual strain in the layer is due to CsPbBr 3 The layer has a coefficient of thermal expansion greater than that of SnO 2 Thermal expansion of electron transport layerMuch larger coefficient, so CsPbBr is present at high temperature 3 The expansion volume of the layer is larger, the shrinkage of the substrate is small during cooling, csPbBr 3 The layer shrinks to a greater extent, at which time the substrate blocks CsPbBr 3 Shrinkage of the layer, resulting in CsPbBr 3 The layer is subjected to tensile strain in the in-plane direction, i.e., thermal strain.
On one hand, the pre-buried bottom interface formed by the PAA layer is further passivated SnO through carboxyl ligand units on the PAA long chain 2 Uncoordinated Sn on surface of electron transport layer 4+ On the other hand, csPbBr is passivated 3 Unliganded Pb in the layer 2+ Thus serving as an anchoring function, the anchoring function formed by bonding is just like a 'spring' in CsPbBr 3 Provides a compressive strain to resist CsPbBr during thermal expansion 3 Thermal expansion of the layer and in CsPbBr 3 During the film forming process, the high temperature can lead the PAA part to volatilize to CsPbBr 3 In the layer, the carboxyl group on PAA passes through Pb 2+ Coordinate to further hinder CsPbBr 3 Thermal expansion of the layers, PAA and CsPbBr at the final interface 3 Compressive strain provided by PAA in layers in combination with annealed CsPbBr 3 Tensile strain generated in the layer is offset, the purpose of compensating thermal strain in situ is achieved, after the residual strain of the perovskite thin film is released, larger crystal grains can be formed, carrier recombination is reduced, and the photoelectric conversion efficiency and stability of the device are improved.
Further, snCl in the step (1) 2 And CH 4 N 2 The mol ratio of S is 0.8-1.2 2 The molar concentration of (b) is 0.1 mol/L-0.2 mol/L.
Further, PAA is added into the preheated SnO in the step (2) 2 After the quantum dot solution is adopted, the PAA concentration is 0.5 mg/mL-5 mg/mL.
Further, PAA is added into the preheated SnO in the step (2) 2 After the quantum dot solution, the PAA concentration is 1mg/mL. In the modification of SnO 2 When PAA is used, the optimum concentration of PAA is 1mg/mL.
Further, snO in the step (2) 2 The preheating temperature of the quantum dot solution is 70-90 ℃, and the preheating time is 3-9 minutesThe method comprises the following steps of (1) taking minutes; the stirring temperature after the PAA powder is added is 70-90 ℃, and the stirring time is 5 minutes-1 hour.
Further, in the step (3), PAA-SnO 2 The preheating temperature of the quantum dot solution is 70-90 ℃, and the PAA-SnO 2 The preheating time of the quantum dot solution is 5-30 minutes, the preheating time of the FTO conductive glass is 1-5 minutes, the rotating speed of spin coating is 1000-2000 rpm, and the acceleration is 300-800 rpm/s.
Further, the concentration of the PAA aqueous solution in the step (4) is 0.05 mg/mL-0.5 mg/mL, the rotation speed of spin coating is 4000-6000 rpm, and the acceleration is 2000-3000 rpm/s.
Further, the concentration of the PAA aqueous solution in the step (4) is 0.1mg/mL.
In the invention, PAA is coated on SnO as a single layer 2 For modifying SnO 2 And CsPbBr 3 The interface between the two is modified SnO 2 /CsPbBr 3 The layer at the interface is called the buried interface, since PAA will partially volatilize to CsPbBr during this process 3 So called pre-buried bottom interface. The optimal concentration of single layer PAA is 0.1mg/mL.
Further, in the step (6), a multi-step spin coating method is adopted to spin coat the CsBr solution on the PbBr solution in the step (5) for multiple times 2 On the film.
Further, in the step (6), annealing is performed once every time CsBr solution is spin-coated, wherein the annealing temperature is 240-260 ℃.
The invention also provides the all-inorganic CsPbBr 3 Use of perovskite solar cells for the preparation of cell modules and in power stations.
Further, the fully inorganic CsPbBr 3 The open-circuit voltage of the perovskite solar cell is 1.40-1.75V, and the short-circuit current is 6.5 mA-cm -2 ～9mA·cm -2 The filling factor is 0.70-0.90, and the photoelectric conversion efficiency is 9% -11.5%.
Compared with the prior art, the invention has the advantages and beneficial effects that: the invention prepares SnO modified based on multifunctional polymer 2 All-inorganic CsPbBr 3 Perovskite solar cells by doping in SnO 2 Adding PAA into the quantum dot solution by means of carboxyl ligand units on the PAA long chain and SnO 2 Quantum dot bonding, which in turn can hinder SnO 2 The agglomeration phenomenon of quantum dots in solution and the carboxyl ligand unit on the PAA long chain can consume SnO 2 Hydroxyl on quantum dot, reduction of SnO 2 Uncoordinated Sn in the electron transport layer 4+ (ii) a During the film forming process, since PAA can form strong hydrogen bond with metal oxide, PAA can adhere to FTO and bond with Sn element on the surface of FTO, thereby leading SnO 2 Deposition of quantum dots on FTO to improve SnO 2 The wettability of quantum dots on FTO ensures that SnO is modified after PAA modification 2 The electron transport layer is distributed on the FTO more uniformly; in addition, the weakly acidic PAA can reduce SnO 2 The alkalinity of the quantum dot solution is favorable for improving SnO 2 Stability and charge extraction at the perovskite interface.
The invention is achieved by the use of SnO 2 Electron transport layer and CsPbBr 3 PAA is added between the interfaces of the layers to form a pre-buried bottom interface for releasing CsPbBr 3 Residual strain in the layer, carboxyl ligand units on the PAA long chain can passivate SnO on the one hand 2 Uncoordinated Sn on surface of electron transport layer 4+ On the other hand, csPbBr can be passivated 3 Unliganded Pb in the layer 2+ And, at a phase transition temperature of 250 ℃, a portion of PAA is volatilized to CsPbBr 3 In the layer, csPbBr is further released 3 Residual strain of layer and passivated CsPbBr 3 Pb in the layer 2+ The strain relief and defect passivation described above help to form large-grained CsPbBr 3 The defect state density is reduced, the non-radiative recombination of carriers is reduced, the transmission of the carriers at an interface is promoted, and the battery performance is obviously improved.
SnO prepared by PAA modification 2 The electron transport layer is more uniform, and the crystallization quality is higher; csPbBr 3 The maximum grain size of the layer can reach 3.08 mu m, and the assembled fully inorganic CsPbBr 3 The device structure of the perovskite solar cell is FTO/PAA-SnO 2 /PAA/CsPbBr 3 Carbon electrode due to extraction of carriersThe photoelectric conversion efficiency of the whole device can reach 10.83 percent due to high and carrier recombination reduction, the open-circuit voltage can reach 1.674V, the initial photoelectric conversion efficiency of the device can still be maintained by more than 90 percent under the condition of 80 percent of humidity or in a thermal environment of 80 ℃ for more than 120 days, the stability is good, and the method has important practical value and economic value for promoting the industrialization process of the perovskite solar cell.
Drawings
FIG. 1 is a SnO proposed by the present invention 2 Quantum dot solution and PAA-SnO 2 The preparation process and the film forming process of the quantum dot solution are shown schematically.
FIG. 2 shows SnO prepared by the present invention 2 HRTEM and surface SEM images of the electron transport layer; wherein a and b are SnO 2 And PAA-SnO 2 HRTEM image of (A); c. d and e are FTO and SnO 2 And PAA-SnO 2 Surface SEM image of (d).
FIG. 3 shows PAA-SnO prepared by the present invention 2 Surface SEM image of (1), PAA addition concentration is 2mg/mL.
FIG. 4 shows SnO prepared by the present invention with different PAA addition concentrations 2 AFM images of electron transport layers.
FIG. 5 is a diagram of SnO prepared by the present invention 2 And PAA-SnO 2 Cross-sectional SEM image of (a).
FIG. 6 shows SnO prepared by the present invention 2 An XRD pattern and an FTIR pattern of the electron transport layer; wherein a is SnO 2 And PAA-SnO 2 XRD pattern of (a); b is SnO 2 And PAA-SnO 2 FTIR chart of (1).
FIG. 7 shows SnO prepared by the present invention 2 And PAA-SnO 2 XPS plots of (c); wherein a is an XPS chart of Sn 3 d; b is an XPS plot of O1 s; c and d are SnO 2 And PAA-SnO 2 XPS graph of oxygen partial peak.
FIG. 8 shows SnO prepared by the present invention 2 And PAA-SnO 2 UPS graphs and device energy level graphs; wherein a is a secondary electron cut-off edge binding energy diagram; b is an initial binding energy diagram; c and d are SnO 2 And PAA-SnO 2 The Tauc bandgap diagram of (1); e is an energy level diagram of the charge transfer process in the PAA modified perovskite solar cell.
FIG. 9 shows SnO prepared by the present invention with different PAA addition concentrations 2 A light transmittance map and a conductivity map of the electron transport layer; wherein a is a light transmittance diagram, and b is a conductivity diagram.
FIG. 10 shows the volatilization of a portion of PAA in a PAA layer proposed by the present invention to CsPbBr 3 Schematic illustration of the passivation of defects in a layer.
FIG. 11 shows the PAA layer as an embedded bottom interface to passivate SnO 2 Electron transport layer and CsPbBr 3 Schematic of the interface between layers.
Fig. 12 is a schematic diagram of PAA layer in situ compensating thermal strain according to the present invention.
FIG. 13 shows the preparation of CsPbBr under PAA modification 3 XRD patterns and calculated patterns of strain experienced.
FIG. 14 shows CsPbBr in different PAA monolayers 3 GIXRD patterns of the layers and
a residual strain map; wherein, the graphs a, b, d and e are CsPbBr under different single-layer PAA addition concentrations 3 The GIXRD pattern, c, f pattern of the layer is the residual strain profile.
FIG. 15 shows CsPbBr prepared according to the present invention 3 XPS plot of the layer; wherein a is an XPS diagram of Sn 3 d; b is an XPS map of Pb 4 f.
FIG. 16 shows PbBr prepared by the present invention 2 Surface SEM of thin film, csPbBr 3 Surface SEM and CsPbBr of layer 3 Cross-section SEM of the layer; wherein a, b and c are not modified by PAA; d. e and f are modified by PAA.
FIG. 17 shows the PAA-modified CsPbBr prepared by the present invention 3 Light absorbance pattern of the layer.
FIG. 18 shows the fully inorganic CsPbBr under PAA modification prepared by the present invention 3 The complete device architecture of the perovskite solar cell.
FIG. 19 shows the total inorganic CsPbBr under PAA modification prepared by the present invention 3 A device performance characterization map of the perovskite solar cell; wherein a is a J-V curveThe graph b is an external quantum efficiency graph, the graph c is a steady state output graph, the graph d is a steady state photoluminescence graph, the graph e is a time-resolved photoluminescence graph, the graph f is a Mott-Schottky graph, the graph g is a space charge limiting current graph, the graph h is a dark state J-V graph, and the graph i is an impedance graph.
FIG. 20 shows the total inorganic CsPbBr under PAA modification prepared by the present invention 3 A long-term stability diagram of the perovskite solar cell under the conditions that the humidity is 80% and the temperature is room temperature; in the figure, a is a stability chart of photoelectric conversion efficiency, b is a stability chart of open-circuit voltage, c is a stability chart of short-circuit current density, and d is a stability chart of filling factor.
FIG. 21 shows the total inorganic CsPbBr under PAA modification prepared by the present invention 3 A long-term stability diagram of the perovskite solar cell under the conditions that the humidity is 0% and the temperature is 80 ℃; in the figure, a is a stability chart of photoelectric conversion efficiency, b is a stability chart of open-circuit voltage, c is a stability chart of short-circuit current density, and d is a stability chart of filling factor.
Detailed Description
The technical solution of the present invention will be described in further detail with reference to the following embodiments.
Example 1 preparation of PAA-modified all-inorganic CsPbBr 3 Perovskite solar cell
This example provides a PAA-modification-based fully inorganic CsPbBr 3 A perovskite solar cell, obtainable by the following preparation method:
(1) 853mg of SnCl 2 And 338mg of thiourea (CH) 4 N 2 S) is dissolved in 30mL deionized water, the solution is placed on a magnetic stirrer and stirred at room temperature for 36h at high speed, then a high-speed centrifuge is used for centrifuging to remove precipitates, and a PTFE filter membrane is used for filtering to obtain yellow transparent SnO 2 A quantum dot solution;
(2) 10mL of SnO was sampled 2 Preheating the quantum dot solution in a beaker at 80 ℃ for 5min, adding polyacrylic acid (PAA) powder with different amounts into SnO 2 Stirring the quantum dot solution at high speed for 15min to respectively obtain PAA-SnO with the PAA concentrations of 0mg/mL, 0.5mg/mL, 1mg/mL and 2mg/mL 2 A quantum dot solution;
(3) Cleaning the FTO conductive glass by using an ultrasonic cleaning machine, and then deeply cleaning by using a plasma cleaning machine; then mixing the PAA-SnO in (2) 2 The quantum dot solution and FTO conductive glass are placed on a heating table at the temperature of 80 ℃ for preheating, and PAA-SnO 2 Preheating time of the quantum dot solution is 15min, and preheating time of the FTO conductive glass is 3min; preheating PAA-SnO 2 The quantum dot solution is spin-coated on the preheated FTO conductive glass at the rotating speed of 1500rpm, the acceleration of 500rpm/s and the spin-coating time of 30s, and the FTO/PAA-SnO is obtained after annealing 2 A substrate;
(4) Preheating 10mL of deionized water in a beaker at 80 ℃ for 10min, adding different amounts of PAA powder into the preheated deionized water, and stirring at high speed for 15min to obtain PAA aqueous solutions with the concentrations of PAA of 0mg/mL, 0.05mg/mL, 0.1mg/mL, 0.2mg/mL and 0.3mg/mL respectively; spin coating aqueous PAA solution to FTO/PAA-SnO 2 On the substrate, the rotation speed is 5000rpm, the acceleration is 2500rpm/s, the spin coating time is 30s, and the FTO/PAA-SnO is obtained after annealing at 80 ℃ for 15min 2 A PAA substrate;
(5) 734mg of PbBr were taken 2 Heating to fully dissolve in 2mL of DMF at 90 ℃ to obtain 1mol/L of PbBr 2 A solution; mixing the FTO/PAA-SnO mentioned in (4) 2 Preheating a PAA substrate for 5min on a heating table at 90 ℃ 2 Preheating the solution on a heating table at 90 ℃ for 15min, and preheating the preheated PbBr 2 The solution is coated on FTO/PAA-SnO in a spinning way 2 On the PAA substrate, the rotating speed is 2000rpm, the acceleration is 1000rpm/s, and the time is 30s; annealing on a heating table at 90 ℃ for 30min after the spin coating is finished, and volatilizing DMF to obtain PbBr 2 A film;
(6) 149mg of CsBr is dissolved in 10mL of anhydrous methanol, and ultrasonic treatment is carried out for 30min to obtain 0.07mol/L CsBr solution; spin-coating CsBr solution on PbBr in (5) for multiple times by multi-step spin-coating method 2 On the film, the rotating speed is 2000rpm, the acceleration is 1000rpm/s, the time is 30s, annealing is carried out on a heating table at 250 ℃ for 5min after each spin coating, and the steps are repeated for 6-8 times until uniform yellow CsPbBr is formed 3 A perovskite thin film;
(7) The carbon slurry is coated on CsPbBr by blade coating method 3 Thin perovskiteAnnealing on a film for 15min on a heating table at 90 ℃ to obtain complete all-inorganic CsPbBr 3 Perovskite solar cell, PAA modified fully inorganic CsPbBr 3 The device structure of the perovskite solar cell is FTO/PAA-SnO 2 /PAA/CsPbBr 3 A carbon electrode.
Example 2 PAA modified SnO 2 Performance characterization of electron transport layers
1. By in SnO 2 By adding PAA into the quantum dot solution, snO can be reduced by virtue of carboxyl ligand units on a PAA long chain 2 Agglomeration of quantum dots and SnO 2 Hydroxyl on the surface of the quantum dot, and PAA can guide SnO in the film forming process 2 The quantum dots are distributed on the FTO to obtain uniform and continuous SnO 2 The electron transport layer is schematically shown in FIG. 1.
From FIG. 1, snO can be seen 2 After preparation of the quantum dot solution, snO 2 Quantum dots are prone to agglomeration and SnO 2 The surface of the quantum dot has hydroxyl, and SnO is caused by separation of the hydroxyl in the annealing process 2 Oxygen vacancy occurs in the alloy, so that uncoordinated Sn occurs 4 + By the use of SnO 2 Adding PAA into the quantum dot solution by virtue of a carboxyl ligand unit on a PAA long chain and SnO 2 Quantum dot bonding, which in turn can hinder SnO 2 The agglomeration phenomenon of quantum dots in solution and the carboxyl ligand unit on the PAA long chain can consume SnO 2 Hydroxyl on quantum dot, reduction of SnO 2 Uncoordinated Sn on surface of electron transport layer 4+ (ii) a During the film forming process, since PAA can form strong hydrogen bond with metal oxide, PAA is easy to adhere on FTO and bond with Sn element on the surface of FTO, thereby leading SnO 2 Deposition of quantum dots to enhance SnO 2 The wettability of quantum dots on FTO ensures that SnO modified by PAA 2 The electron transport layer is uniformly distributed on the FTO; in addition, the weakly acidic PAA can reduce SnO 2 The alkalinity of the quantum dot solution is favorable for improving SnO 2 Stability and charge extraction at the perovskite interface.
2. Separately testing whether or not SnO with PAA was added 2 HRTEM image of quantum dot solution, and FTO, snO 2 And PAA-SnO 2 As shown in fig. 2.
It can be seen from the graphs a and b in FIG. 2 that SnO with or without PAA added 2 The interplanar spacing of the quantum dots on the (110) plane is 0.335nm, which indicates that PAA is not doped into SnO 2 Internal, still rutile SnO 2 And the modification of PAA makes the interplanar spacing more obvious, which shows that PAA-SnO 2 (PAA-SnO 2 The adding concentration of the medium PAA is 1 mg/mL) has better crystallization performance; from the c diagram of fig. 2, it can be seen that the FTO surface is a rugged surface with a certain roughness; snO can be seen from d diagram of FIG. 2 2 After the quantum dots are covered on the FTO, the roughness of the substrate is reduced, the substrate is smoother, but quantum dot clusters can be seen, and the SnO is proved 2 The agglomeration phenomenon of quantum dots; from the e plot of FIG. 2, it can be seen that PAA-SnO 2 The roughness of the substrate is also reduced after the quantum dots are covered on the FTO, but quantum dot clusters are not obvious, which shows that the SnO is subjected to the addition of PAA 2 The dispersion of the quantum dots plays a positive role.
3. SEM images of the surface when PAA addition concentration was too high were tested, as shown in figure 3.
As can be seen from FIG. 3, when the PAA is added at a concentration of 2mg/mL, the concentration at SnO 2 SnO distributed in a chain form can be seen on the surface of the electron transport layer 2 The quantum dots may be caused by that when the concentration of the PAA is too high, carboxyl groups among the PAA are connected through hydrogen bonds, so that a plurality of parallel PAA long chains are formed, and the quality and the roughness of the film are influenced.
4. Separately testing SnO at different PAA addition concentrations 2 AFM view of the electron transport layer, as shown in FIG. 4.
The adding concentration of PAA is 0mg/mL, 0.5mg/mL, 1mg/mL and 2mg/mL respectively; as can be seen from FIG. 4, the SnO was not modified with PAA 2 The root mean square roughness of the electron transport layer is the largest, the value is 16.3nm, and SnO is realized at the PAA adding concentration of 1mg/mL 2 The root mean square roughness of the electron transport layer is the smallest, the value is 14.5nm, and SnO is realized at the PAA adding concentration of 2mg/mL 2 The increase in the root mean square roughness of the electron transport layer is due to the phenomenon described in fig. 3.
5. Respectively measureSnO tried to be added with PAA 2 A cross-sectional SEM image of the electron transport layer is shown in fig. 5.
As can be seen from FIG. 5, snO without PAA addition 2 The quantum dots are not uniformly distributed on the FTO, and SnO is not seen at some bulges 2 Distribution of quantum dots, snO modified by 1mg/mL PAA 2 The quantum dots are uniformly distributed on the FTO, and are smooth and complete.
6. Separately testing whether or not SnO with PAA was added 2 An XRD pattern and fourier transform infrared spectroscopy (FTIR) pattern of the electron transport layer are shown in fig. 6.
As can be seen from a diagram of FIG. 6, snO with no PAA addition 2 The peak position of XRD of the electron transport layer and SnO added with 1mg/mL PAA 2 The peak position of the electron transport layer was the same, again demonstrating that PAA was not incorporated into SnO 2 In the method, only the modification effect is achieved, and in addition, snO with 1mg/mL PAA is added 2 The peak intensity of the electron transport layer is higher, which shows that SnO is modified by 1mg/mL PAA 2 The crystallization property of (b) is better, which corresponds to the clear interplanar spacing of the (110) plane in the b diagram of fig. 2; from the b diagram of fig. 6, it can be seen that the main C = O peak and Sn-O peak are from 1694 to 1691cm respectively -1 And 604 to 614cm -1 This phenomenon indicates the presence of PAA and is associated with SnO 2 The reaction takes place, bringing the tin oxide into closer alignment.
7. SnO testing whether PAA is added or not 2 XPS diagram of electron transport layer, as shown in fig. 7.
As can be seen from panel a of FIG. 7, for 1mg/mL PAA modified SnO 2 Increase in binding energy of the electron transport layer, sn 3d indicates that PAA and SnO 2 Chemical interaction occurs between the electron transport layers, and oxygen vacancies are filled after coordination with Sn; FIG. 7 panel b shows 1mg/mL PAA modified SnO 2 The peak intensity of the O1s peak of the electron transport layer increased, indicating SnO 2 The oxygen content in the electron transport layer increases, again demonstrating the presence of PAA; the c, d diagrams in FIG. 7 show that the O1s peak can be divided into two peaks, wherein the peak with low binding energy comes from SnO 2 Lattice oxygen (O) of Sn ) While the peak of high binding energy belongs to vacancy oxygen (O) OH ) From the ratio of oxygen partial peaks, it can be seen that 1mg/mL PAA is repairedDecorated SnO 2 The electron transport layer ratio is smaller, again indicating that the presence of PAA passivates oxygen vacancy defects.
8. Separately testing whether or not SnO with PAA was added 2 A UPS diagram of an electron transport layer as shown in fig. 8.
As can be seen from the a-plot of FIG. 8, different SnO values were calculated by measuring the energy of the cut-off edge 2 The Fermi level of the electron transport layer is increased from-4.76 to-4.51 eV after being modified by 1mg/mL of PAA; from the b plot of FIG. 8, it can be seen that SnO can be determined by measuring the onset energy 2 The valence band of the electron transport layer is increased from 3.52 to 3.64eV after being modified by 1mg/mL PAA; from the c and d plots of FIG. 8, different SnO values can be calculated 2 The band gap value of the electron transport layer, calculated as described above, finally determined that the conduction band increased from-4.48 to-4.36 eV after 1mg/mL of PAA modification, indicating that electrons are more easily transported from CsPbBr 3 Layer transition to SnO 2 An electron transport layer, effectively inhibits CsPbBr 3 Electrons in the layers accumulate, thereby reducing recombination losses and increasing voltage output; the detailed energy level diagram is shown in e diagram of fig. 8.
9. Separately testing SnO at different PAA addition concentrations 2 The light transmittance and conductivity maps of the electron transport layer are shown in fig. 9.
As can be seen from the a diagram of FIG. 9, snO when the concentration of PAA is 1mg/mL 2 The electron transport layer has the highest transmittance to light, which allows CsPbBr 3 The layer makes efficient use of incident photons; thus, as can be seen from graph b of FIG. 9, by recording FTO/SnO 2 Or (PAA-SnO) 2 ) The I-V curve shows that SnO is at 1mg/mL 2 The slope of the electron transport layer is the largest, so SnO at 1mg/mL 2 The electron transport layer has the largest conductivity, and the result shows that the modified oxygen vacancy of PAA is improved, so that PAA-SnO 2 Has good charge extraction capability and higher conductivity.
Example 3 PAA layer in situ Compensation CsPbBr 3 Characterization of layer thermal strain
1. By the reaction in SnO 2 Coating a PAA layer on the electron transport layer to form an embedded bottom interface, and annealing the embedded bottom interface at high temperatureDuring the fire, a part of PAA volatilizes to CsPbBr 3 In the layer, thereby regulating CsPbBr 3 The layer formation is schematically illustrated in fig. 10.
As can be seen from FIG. 10, the PAA layer is sandwiched between SnO and serves as an embedded bottom interface 2 Electron transport layer and PbBr 2 Between films, due to CsPbBr 3 The phase transition temperature of the single-layer PAA is up to 250 ℃, while the boiling point of the PAA is only 116 ℃, so that part of the PAA in the single-layer PAA is volatilized to CsPbBr within 5min of annealing 3 Layer, thereby regulating CsPbBr 3 Formation of a layer, after cooling to room temperature, a PAA-modified CsPbBr was formed 3 And (3) a layer.
2. A pre-embedded bottom interface is formed through the PAA layer, and CsPbBr is passivated 3 Defects at the layer interface and volatilization to CsPbBr 3 PAA in the layer further modifies CsPbBr 3 The schematic diagram of the vacancy defect inside the layer is shown in fig. 11.
As can be seen in FIG. 11, in one aspect, snO 2 The single Sn bond formed after the hydroxyl is separated when annealing exists on the surface of the electron transport layer, and the carboxyl ligand unit on the single-layer PAA long chain can passivate SnO 2 Uncoordinated Sn on surface of electron transport layer 4+ On the other hand, csPbBr can be passivated 3 Unliganded Pb in the layer 2+ The PAA layer reduces the recombination of current carriers at the interface by passivating vacancy defects at the interface and enhances SnO 2 Electron transport layer and CsPbBr 3 The bonding energy between the layers; further volatilize to CsPbBr 3 PAA in the layer further modifies CsPbBr 3 Vacancy defects within the layer, which is advantageous for obtaining high quality large grained CsPbBr 3 。
3. Releasing CsPbBr by forming pre-buried bottom interface through PAA layer 3 Residual strain in the layer, forming CsPbBr in a low strain state 3 Layer, schematic as in figure 12.
As can be seen from FIG. 12, csPbBr 3 The residual strain in the layer is due to CsPbBr 3 The layer has a coefficient of thermal expansion greater than that of SnO 2 The electron transport layer has a much higher coefficient of thermal expansion, so CsPbBr is present at high temperatures 3 The expansion volume of the layer is larger, and the shrinkage degree of the substrate is small when cooling and shrinking,CsPbBr 3 the layer shrinks to a greater extent, at which time the substrate blocks CsPbBr 3 Shrinkage of the layer, resulting in CsPbBr 3 The layer is subjected to a tensile strain in the in-plane direction, i.e. a thermal strain; the pre-buried bottom interface formed by the PAA layer passes through the carboxyl ligand unit on the PAA long chain and SnO 2 Uncoordinated Sn on surface of electron transport layer 4+ To CsPbBr on the other hand 3 Unliganded Pb in the layer 2+ Connected to act as an anchor, this anchoring by bonding acting like a "spring" in CsPbBr 3 Provides a compressive strain to resist CsPbBr during thermal expansion 3 Thermal expansion of the layer, and in CsPbBr 3 During the film forming process, the high temperature can lead the PAA part to volatilize to CsPbBr 3 In the layer, the carboxyl group on PAA passes through Pb 2+ Coordinate to further hinder CsPbBr 3 Thermal expansion of the layers, finally PAA and CsPbBr at the interface 3 Compressive strain provided by PAA in layer in combination with CsPbBr after annealing 3 The tensile strain produced in the layer is cancelled out, achieving the purpose of compensating the thermal strain in situ.
4. CsPbBr for separately testing whether PAA was added 3 XRD pattern of the layer, csPbBr was calculated by Williamson-Hall equation 3 The strain of the layer is shown in fig. 13.
As can be seen from the graph a in FIG. 13, the pre-buried bottom interface of PAA of 0.1mg/mL can improve CsPbBr 3 The crystalline strength of the layer, without the appearance of a hetero-peak, csPbBr was calculated by Williamson-Hall equation from the data in the XRD pattern 3 Strain value of layer, csPbBr after modification of PAA 3 The strain of the layer is only 0.00178.
5. Respectively testing CsPbBr under different PAA layer adding concentrations 3 GIXRD pattern of the layers, and the residual strain distribution obtained from GIXRD (2 theta data as
As a function of) as shown in fig. 14.
The adding concentration of the PAA layer is respectively 0mol/L, 0.05mol/L, 0.1mol/L and 0.2mol/L; as can be seen from the graphs a, b, d and e of FIG. 14, the peaks all move to the left with increasing grazing incidence angleThis indicates that the film is tensile strained in the in-plane direction, and as the PAA layer addition concentration increases, the peak shift corresponding to the large grazing incidence angle decreases, which indicates that PAA releases CsPbBr 3 The residual strain of the layer and the peak intensity increased significantly when the PAA layer was added at a concentration of 0.1mol/L, indicating CsPbBr at this addition concentration 3 The best crystallization properties of the layer; the graphs c and f in FIG. 14 show that 2 θ data is used as
The function of (c) can calculate CsPbBr 3 The layer residual strain, the greater the slope, the greater the residual strain, and it was found that the slope was the smallest at a concentration of 0.1mol/L for the PAA layer, i.e., the tensile strain experienced by the film was the smallest at a concentration of 0.1mol/L for the PAA layer.
6. SnO testing whether PAA layer is added or not 2 Electron transport layer and CsPbBr 3 XPS map of the layer, as shown in fig. 15.
As can be seen from panel a of FIG. 15, modified SnO was coated with a 0.1mg/mL PAA layer 2 The combination energy of Sn 3d of the electron transport layer is obviously increased, which shows that the PAA layer and SnO 2 The electron transport layer is chemically interacted with the uncoordinated Sn 4+ The interaction further fills the oxygen vacancy; csPbBr grown on 0.1mg/mL PAA layer 3 The Pb 4f of the layer shifts to higher binding energies, indicating that the PAA layer is associated with CsPbBr 3 The layers also chemically interact with each other, i.e. with unliganded Pb 2+ (ii) interaction; the above XPS conclusion provides evidence for the schematic diagram 11.
7. Separately testing whether PbBr of PAA layer is added 2 Thin film and CsPbBr 3 SEM image of the layer, as shown in fig. 16.
A, d PbBr from FIG. 16 2 As can be seen from the surface SEM image of the film, 0.1mg/mL of PAA layer is aligned with PbBr 2 The influence of pores in the film is not great, but PbBr 2 There is a certain increase in the grain size, which is CsPbBr 3 The large crystal grains lay a foundation; 0.1mg/mL PAA layer modified CsPbBr 3 Larger grain size of the layer CsPbBr 3 The maximum grain size of the layer can reach 3.08 μm, which does not depart from the strain relief and defects of PAAPassivation; csPbBr 3 The cross-sectional SEM images of the layers also show that the above conclusions are met.
8. CsPbBr to test whether PAA is added or not 3 The light absorbance of the layer is plotted as shown in fig. 17.
As can be seen from FIG. 17, csPbBr with large grains was modified with a 0.1mg/mL PAA layer 3 The light absorption of the layer is higher, which undoubtedly facilitates CsPbBr 3 The layer efficiently utilizes incident photons.
Example 4 PAA-modified all-inorganic CsPbBr 3 Performance testing of perovskite solar cells
1. PAA-modified all-inorganic CsPbBr prepared in example 1 3 The device structure of the perovskite solar cell is FTO/PAA-SnO 2 /PAA/CsPbBr 3 A/carbon electrode as shown in FIG. 18.
2. Respectively testing the photoelectric performance and CsPbBr of the full device added with PAA 3 The photoluminescence spectrum of the layer is shown in figure 19.
As can be seen from the graph a in FIG. 19, the photoelectric conversion efficiency of the whole device without PAA modification is only 8.13%, and 1mg/mL of PAA modified SnO 2 The photoelectric conversion efficiency is greatly improved after the electron transport layer is formed, the photoelectric conversion efficiency is 10.36 percent, and when the single-layer PAA of 0.1mg/mL passivates CsPbBr 3 The photoelectric conversion efficiency is further improved to 10.83% after the layer defects and strain relief, which is benefited by high-quality SnO 2 Electron transport layer and CsPbBr with large grains 3 A layer.
As can be seen from panel b of FIG. 19 (there are two PAA modifications in the present invention, one is that PAA only modifies SnO 2 (1 mg/mL) with PAA-SnO 2 Expressed as the second is modified SnO 2 (1 mg/mL) and PAA-SnO as a monolayer of PAA (0.1 mg/mL) 2 Represented by/PAA), the external quantum efficiency of the total device modified by two PAAs is higher, which indicates that the integral current density of the total device is also higher, and PAA-SnO 2 The integrated current density of the total device under the PAA condition is 7.89mA cm -2 This is compared with the PAA-SnO in the J-V curve 2 7.93mA cm under the conditions of/PAA -2 The current densities of (a) and (b) are matched.
As can be seen from the c diagram of FIG. 19, the steady-state output performance of the full device after PAA modification is better and the attenuation is lower, no matter that the PAA only modifies SnO 2 Or PAA modified SnO 2 And the effect of the single layer is better than that of the PAA group without adding.
As can be seen from d plot of FIG. 19, the PAA layer modifies CsPbBr 3 After layering, the reduction in PL intensity indicates that PAA effectively inhibits carrier recombination, improving charge transport, and the blue shift of the PL peak also demonstrates a reduction in device internal defects, inhibiting carrier recombination.
As can be seen from the e plot of FIG. 19, the lifetime of TRPL spectrum of PAA-modified device is shorter, and the average lifetime of 1.99ns of unmodified device is reduced to PAA-SnO 2 1.22ns under the conditions of/PAA, which indicates CsPbBr 3 Electrons generated by the layer can be extracted to SnO more quickly 2 In the electron transport layer, thereby relieving SnO 2 Electron transport layer and CsPbBr 3 Non-radiative recombination between layers; as can be seen from the f-plot of FIG. 19, the built-in electric field (V) derived from the C-V plot according to the C-V plot converted by the Mott-Schottky equation bi ) Increased after PAA modification, which also confirmed that electrons were transferred to SnO 2 The electron transport layer, rather than being trapped by defects, undergoes non-radiative recombination.
As can be seen from the g plot of FIG. 19, after PAA modification, the trap filling limits the voltage (V) TFL ) Directly indicates CsPbBr 3 The defect state density of the layer is decreased and the electron mobility is improved, which is consistent with the results of the TRPL analysis of the e-diagram of fig. 19. As can be seen from the h plot of fig. 19, the leakage current of the full device after PAA modification is smaller due to the i plot of fig. 19, the composite resistance of the full device after PAA modification increases.
3. The devices were tested for long-term stability at room temperature with PAA added, respectively, and the results are shown in fig. 20.
As can be seen from FIG. 20, 1mg/mL PAA modified SnO was added at room temperature with humidity of 80% 2 And the stability of the full device modified by 0.1mg/mL monolayer PAA is obviously higher than that of the full device without PAA modification, which is mainly attributed to that the filling factor is more stable after PAA modificationAfter 120 days, the PAA modified full device still maintains more than 80% of the initial photoelectric conversion efficiency.
4. The PAA added full devices were tested for long term stability at sustained high temperatures, respectively, and the results are shown in fig. 21.
As can be seen from FIG. 21, in an environment with a temperature of 80 ℃ and a humidity of 0%, 1mg/mL of PAA-modified SnO 2 And the stability of the full device modified by 0.1mg/mL monolayer PAA is also higher than that of the full device without PAA modification, and the initial photoelectric conversion efficiency of the PAA-modified full device is still maintained to be more than 80% after 120 days.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions.
Claims (10)
1. SnO modified based on multifunctional polymer 2 All-inorganic CsPbBr 3 A perovskite solar cell is characterized by being prepared by the following preparation method:
(1) SnCl 2 Dissolving thiourea in deionized water, stirring, centrifuging, removing precipitate, and filtering to obtain SnO 2 A quantum dot solution;
(2) SnO in the step (1) 2 Preheating the quantum dot solution; adding polyacrylic acid powder into preheated SnO 2 Stirring in quantum dot solution to obtain SnO modified by PAA 2 Solutions of quantum dots, i.e. PAA-SnO 2 A quantum dot solution;
(3) Mixing the PAA-SnO in the step (2) 2 Preheating the quantum dot solution and the FTO conductive glass; preheating PAA-SnO 2 The quantum dot solution is coated on the preheated FTO conductive glass in a spin mode to obtain FTO/PAA-SnO 2 A substrate;
(4) Spin coating PAA aqueous solution on the stepThe FTO/PAA-SnO mentioned in step (3) 2 Obtaining PAA-SnO modified by single-layer PAA on the substrate 2 An electron transport layer to obtain FTO/PAA-SnO 2 A PAA substrate;
(5) The FTO/PAA-SnO in the step (4) 2 PAA substrate and PbBr 2 Preheating the solution, and adding the preheated PbBr 2 Solution spin coating on FTO/PAA-SnO 2 Annealing on PAA substrate to obtain PbBr 2 A film;
(6) PbBr described in step (5) 2 Spin-coating CsBr solution on the film to obtain the CsPbBr modified by PAA 3 A layer;
(7) CsPbBr described in step (6) 3 Coating carbon slurry on the layer, annealing to obtain carbon electrode and obtain fully inorganic CsPbBr 3 A perovskite solar cell.
2. The all-inorganic CsPbBr of claim 1 3 A perovskite solar cell characterized by: snCl in the step (1) 2 And CH 4 N 2 The mol ratio of S is 0.8-1.2 2 The molar concentration of (b) is 0.1 mol/L-0.2 mol/L.
3. The all-inorganic CsPbBr of claim 1 3 A perovskite solar cell characterized by: in the step (2), PAA is added into the preheated SnO 2 After the quantum dot solution is adopted, the PAA concentration is 0.5 mg/mL-5 mg/mL.
4. The all-inorganic CsPbBr of claim 3 3 A perovskite solar cell characterized by: snO in the step (2) 2 The preheating temperature of the quantum dot solution is 70-90 ℃, and the preheating time is 3-9 minutes; the stirring temperature after the PAA powder is added is 70-90 ℃, and the stirring time is 5 minutes-1 hour.
5. The all-inorganic CsPbBr of claim 1 3 A perovskite solar cell characterized by: in the step (3), PAA-SnO 2 The preheating temperature of the quantum dot solution is 70-90 DEG C，PAA-SnO 2 The preheating time of the quantum dot solution is 5-30 minutes, the preheating time of the FTO conductive glass is 1-5 minutes, the rotating speed of spin coating is 1000-2000 rpm, and the acceleration is 300-800 rpm/s.
6. The all-inorganic CsPbBr of claim 1 3 A perovskite solar cell characterized by: in the step (4), the concentration of the PAA aqueous solution is 0.05 mg/mL-0.5 mg/mL, the rotation speed of spin coating is 4000-6000 rpm, and the acceleration is 2000-3000 rpm/s.
7. The all-inorganic CsPbBr of claim 1 3 The perovskite solar cell is characterized in that a CsBr solution is repeatedly spin-coated on PbBr in the step (5) by adopting a multi-step spin coating method in the step (6) 2 On the film.
8. The all-inorganic CsPbBr of claim 7 3 The perovskite solar cell is characterized in that annealing is carried out once every time CsBr solution is spin-coated in the step (6), and the annealing temperature is 240-260 ℃.
9. The all-inorganic CsPbBr of any one of claims 1 to 8 3 Perovskite solar cells are used for the production of cell modules and in power stations.
10. The all-inorganic CsPbBr of claim 9 3 Use of perovskite solar cells for the preparation of cell modules and for power stations, characterized in that the all-inorganic CsPbBr is used 3 The open-circuit voltage of the perovskite solar cell is 1.40-1.75V, and the short-circuit current is 6.5 mA-cm -2 ～9mA·cm -2 The filling factor is 0.70-0.90, and the photoelectric conversion efficiency is 9% -11.5%.
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