CN107591482B - Perovskite solar cell with phase separation structure and preparation method thereof - Google Patents

Perovskite solar cell with phase separation structure and preparation method thereof Download PDF

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CN107591482B
CN107591482B CN201710703841.2A CN201710703841A CN107591482B CN 107591482 B CN107591482 B CN 107591482B CN 201710703841 A CN201710703841 A CN 201710703841A CN 107591482 B CN107591482 B CN 107591482B
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CN107591482A (en
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贾春阳
夏建兴
万中全
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University of Electronic Science and Technology of China
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Abstract

A perovskite solar cell with a phase separation structure and a preparation method thereof belong to the technical field of solar cell preparation. The perovskite solar cell with the phase separation structure comprises a transparent conductive substrate, an electron transmission layer, a perovskite light absorption layer, a phase separation structure of a hole transmission layer and a metal electrode, wherein the electron transmission layer, the perovskite light absorption layer and the hole transmission layer are sequentially formed on the transparent conductive substrate. According to the invention, the mixed solution of the perovskite light absorption material and the hole transmission material is dripped into the area to be deposited on the electron transmission layer, the separation of the light absorption layer and the hole layer is realized through the difference of the hydrophilic and hydrophobic degrees of the two materials under the combined action of the flexible thin film and the thin film layer, so that the phase separation structure of the perovskite light absorption layer and the hole transmission layer is further obtained, the operation is simple and convenient, the cost is low, the generation of impurities between adjacent layers is effectively avoided, the recombination center of the perovskite light absorption material is reduced, and the preparation of a large-area perovskite solar cell is facilitated.

Description

Perovskite solar cell with phase separation structure and preparation method thereof
Technical Field
The invention belongs to the technical field of solar cell preparation, and particularly relates to a perovskite solar cell with a phase separation structure and a preparation method thereof.
Background
The perovskite solar cell is a solar cell taking an organic-inorganic hybrid perovskite material as a light absorption layer, and the perovskite light absorption material has the characteristics of proper light absorption band gap, bipolar carrier transport property, longer carrier diffusion length and the like, so that the perovskite light absorption material has excellent photoelectric conversion performance and is expected to become a new generation of all-solid-state solar cell with high efficiency, low cost and large area.
The perovskite solar cell is generally prepared layer by adopting a spin coating method, an electron transmission layer, a perovskite light absorption layer, a hole transmission layer and the like are prepared by a spin coating and annealing method, and finally a layer of metal electrode is evaporated and plated as a counter electrode. The method is complex to operate and high in cost, impurities are easily generated between adjacent layers in the preparation process, the adhesion of the next layer is not facilitated, and meanwhile, a composite center is introduced, so that the performance of the battery is adversely affected.
Disclosure of Invention
Aiming at the defects in the background technology, the invention provides a novel perovskite solar cell with a phase separation structure and a preparation method thereof, the phase separation structure of a light absorption layer and a hole transmission layer of the perovskite solar cell is obtained through one-step treatment, the operation is simple and convenient, the cost is low, the generation of impurities between adjacent layers is effectively avoided, the recombination center of a perovskite light absorption material is reduced, and the preparation of the perovskite solar cell with a large area is facilitated.
The technical scheme of the invention is as follows:
a perovskite solar cell with a phase separation structure comprises a transparent conductive substrate, an electron transmission layer, a perovskite light absorption layer and a phase separation structure of a hole transmission layer, and metal electrodes, wherein the electron transmission layer, the perovskite light absorption layer and the phase separation structure are sequentially formed on the transparent conductive substrate.
Further, the phase separation structure of the perovskite light absorption layer and the hole transport layer is obtained by adopting the following steps: a. adhering a flexible film with the thickness of 0.005-0.05 mm to the peripheral edge of an electron transmission layer formed on a transparent conductive substrate to form a region to be deposited; b. dripping 10-50 mu L/cm on the area to be deposited obtained in the step a2A mixed solution of a perovskite light-absorbing layer material and a hole-transporting material; the concentration of the perovskite light absorption layer material in the mixed solution is 0.2-0.9 mmol/mL, and the concentration of the hole transport material is 10-55 mg/mL; c, covering a thin film layer on the transparent conductive substrate dropwise added with the mixed solution in the step b to enable the thin film layer to be tightly attached to the mixed solution, standing for 1-5 min, placing on a heating table, heating for 15-60 s at the temperature of 90-240 ℃, removing the covered thin film layer, and heating for 10-30 min at the temperature of 80-100 ℃ to obtain the phase separation structure of the perovskite light absorption layer and the hole transmission layer.
A preparation method of a perovskite solar cell with a phase separation structure comprises the following steps:
step 1, preparing an electron transport layer on a substrate;
step 2, adhering a flexible film with the thickness of 0.005-0.05 mm to the peripheral edge of the electron transmission layer obtained in the step 1 to form a region to be deposited;
step 3, dripping 10-50 mu L/cm on the area to be deposited obtained in the step 22A mixed solution of a perovskite light-absorbing layer material and a hole-transporting material; the calcium and the titanium in the mixed solutionThe concentration of the material of the ore light absorption layer is 0.2-0.9 mmol/mL, and the concentration of the material of the hole transmission layer is 10-55 mg/mL;
step 4, covering a thin film layer on the substrate dropwise added with the mixed solution in the step 3 to enable the thin film layer to be tightly attached to the mixed solution, standing for 1-5 min, placing the substrate on a heating table, heating for 15-60 s at the temperature of 90-240 ℃, removing the covered thin film layer, and heating for 10-30 min at the temperature of 80-100 ℃ to obtain a phase separation structure of the perovskite light absorption layer and the hole transmission layer;
and 5, preparing a metal electrode on the phase separation structure of the perovskite light absorption layer and the hole transmission layer obtained in the step 4 to be used as a counter electrode, and thus obtaining the perovskite solar cell with the phase separation structure.
Further, a step of modifying the surface of the electron transport layer treated in the step 2 can be added before the treatment in the step 3; the modification treatment method comprises the methods of ultraviolet-ozone, plasma, surface deposition of substances for changing hydrophilicity and hydrophobicity, or soaking in a solution for changing the hydrophilicity and hydrophobicity of the surface, and the like, wherein the substances for changing the hydrophilicity and hydrophobicity of the surface are PEI (polyethyleneimine), glycine, alanine, serine, and the like.
Further, the substrate in step 1 is a transparent conductive substrate such as FTO glass, ITO glass, AZO (aluminum-doped zinc oxide transparent conductive glass), flexible ITO, PET (polyethylene terephthalate), PEN (polyethylene naphthalate), or the like.
Further, the electron transport layer material in the step 1 is TiO2、ZnO、SnO2Or Zn2SnO4And the like, and the preparation method is prepared by ALD (atomic layer deposition), spin coating, dip coating, and the like.
Further, a mesoporous supporting layer can be prepared on the electron transport layer in the step 1, and a mesoporous material of the mesoporous supporting layer is TiO2、ZnO、SiO2、Al2O3、SiTiO3、ZrO2Or Zn2SnO4And the like.
Further, in step 2, the flexible film is Polyimide (PI), Polytetrafluoroethylene (PTFE), Polyethylene (PE), polyvinyl chloride (PVC), polyethylene terephthalate (PET), polypropylene (PP), Polystyrene (PS), or the like.
Further, the mixed solution in step 3 is a mixed solution of a perovskite light absorption layer material and a hole transport material; wherein the chemical formula of the perovskite light absorption layer material is ABmX3-m，A＝CH3NH3、C4H9NH3、 NH2＝CHNH2Or Cs and the like, B is Pb, Sn and the like, and X is Cl, Br, I and the like; the hole transport material is Spiro-OMeTAD, PTAA (poly [ bis (4-phenyl) (2,4, 6-trimethylphenyl) amine]) P3HT (poly-3-hexylthiophene), PEDOT: PSS (poly-3, 4-ethylenedioxythiophene/polystyrene sulfonate) or NPB (N, N '-diphenyl-N, N' -di (1-naphthyl) -1,1 '-biphenyl-4, 4' -diamine), etc.
Further, the solvent of the mixed solution in the step 3 is one of N, N-Dimethylformamide (DMF), N-Dimethylacetamide (DMA), dimethyl sulfoxide (DMSO), and gamma-butyrolactone (GBL), or a mixed solvent of Chlorobenzene (CB) and one of the above solvents, or a mixed solvent of Toluene (TL) and one of the above solvents.
Further, in the step 4, the film layer is a flexible film or a hard film, the thickness of the film layer is 0.005-0.05 mm, and the material is Polyimide (PI), Polytetrafluoroethylene (PTFE), Polyethylene (PE), polyvinyl chloride (PVC), polyethylene terephthalate (PET), polypropylene (PP), Polystyrene (PS), or the like.
Further, the metal electrode in step 5 is gold, silver, carbon, aluminum, or the like.
The invention has the beneficial effects that:
according to the invention, the mixed solution of the perovskite light absorption material and the hole transmission material is dripped into the area to be deposited on the electron transmission layer, the separation of the light absorption layer and the hole layer is realized through the difference of the hydrophilic and hydrophobic degrees of the two materials under the combined action of the flexible thin film and the thin film layer, so that the phase separation structure of the perovskite light absorption layer and the hole transmission layer is further obtained, the operation is simple and convenient, the cost is low, the generation of impurities between adjacent layers is effectively avoided, the recombination center of the perovskite light absorption material is reduced, and the preparation of a large-area perovskite solar cell is facilitated.
Drawings
FIG. 1 is a schematic structural diagram of a perovskite solar cell having a phase separation structure provided by the present invention; a transparent conductive substrate 1, an electron transport layer 2, a phase separation structure 3 of a perovskite light absorption layer and a hole transport layer, and a metal electrode 4 are arranged from bottom to top in sequence, wherein ● represents a hole transport material,
Figure DEST_PATH_GDA0001427911910000031
represents a perovskite light absorbing material;
FIG. 2 is a process for preparing a phase separated structure of a perovskite light absorbing layer and a hole transporting layer according to the present invention; b, adhering a flexible film to the peripheral edge of the electron transport layer to form a region to be deposited, c, dripping a mixed solution of a perovskite light absorption layer material and a hole transport material in the formed region to be deposited and covering the thin film layer, d, placing the device structure obtained in the step c on a heating table for heating, and e, removing the covered thin film layer and heating to form a perovskite light absorption layer and hole transport layer phase separation structure;
FIG. 3 is an enlarged view of step c of FIG. 2;
FIG. 4 is an I-V curve of a perovskite solar cell having a phase separation structure obtained by an embodiment of the present invention;
FIG. 5 shows an example of FTO/TiO in accordance with the present invention2Sectional SEM topography of phase separation structure.
Detailed Description
The technical scheme of the invention is detailed below by combining the accompanying drawings and the embodiment.
As shown in fig. 1, the structural diagram of the perovskite solar cell with a phase separation structure provided by the present invention is shown; the transparent conductive substrate 1, the electron transport layer 2, the perovskite light absorption layer and the phase separation structure 3 of the hole transport layer and the metal electrode 4 are arranged from bottom to top in sequence.
Examples
A preparation method of a perovskite solar cell with a phase separation structure specifically comprises the following steps:
step 1, selecting FTO glass with the size of 1.95cm x 1.95cm as a substrate, sequentially cleaning by using a cleaning agent, a saturated ethanol solution of KOH, deionized water, acetone, deionized water, ethanol and deionized water, blow-drying by using nitrogen, and then treating for 30min under ultraviolet-ozone for later use;
step 2, adding 35uL 2M HCl into 2.53mL ethanol, and uniformly mixing to obtain a solution A; adding 369uL titanium isopropoxide into 2.53mL of ethanol, and uniformly mixing to obtain a solution B; slowly dripping the solution A into the solution B in the stirring process of the solution B, and continuously stirring for 2 hours to obtain clear TiO2Precursor liquid C;
step 3, dripping TiO obtained in the step 2 on the FTO glass treated in the step 12The precursor solution C is rotated at 2000r for 50s, heated on a heating table at 150 ℃ for 15min, and finally annealed at 500 ℃ for 30min to obtain TiO2An electron transport layer;
step 4, 276.6mg of PbI2，95.4mg CH3NH3I and 25mg of spiro-OMeTAD are added into 1mL of N, N-Dimethylformamide (DMF) and stirred for 12h to obtain a solution D;
step 5, TiO obtained in step 32Attaching a polyimide film with the width of 0.5cm and the thickness of 0.05mm to the peripheral edge of the electron transmission layer, and then treating for 15min under the ultraviolet-ozone condition to form a region to be deposited;
step 6, dripping 20uL of solution D into the area to be deposited formed in the step 5, covering a polyethylene film (PE) with the thickness of 0.01mm on the surface of the area to be deposited to enable the polyethylene film to be tightly attached to the solution, standing for 3min, placing the area on a heating table, heating for 35s at the temperature of 100 ℃, uncovering the covered polyethylene film according to a certain angle, and heating for 20min at the temperature of 100 ℃ to obtain a phase separation structure of a perovskite light absorption layer and a hole transmission layer;
and 7, evaporating gold with the thickness of 80nm on the surface of the thin film obtained in the step 6 to be used as a counter electrode, and thus obtaining the perovskite solar cell with the phase separation structure.
FIG. 4 is an I-V curve of a perovskite solar cell obtained in accordance with an embodiment of the present invention; the perovskite solar cell obtained in the example isAM1.5，100mW/cm2The xenon lamp is obtained by adopting a three-electrode method for testing, wherein the scanning voltage is 0-1.2V, and the scanning speed is 100 mV/s. As can be seen from fig. 4, the perovskite solar cell obtained by the embodiment of the invention obtains an efficiency of 3.12% without doping the hole transport layer Spiro-OMeTAD; wherein the short-circuit current is 5.88mA/cm2The open circuit voltage was 0.79V and the fill factor was 0.67.
FIG. 5 shows an example of FTO/TiO in accordance with the present invention2Sectional SEM topography of phase separation structure; as can be seen from fig. 5, the thickness of the phase-separated structure of the perovskite light absorption layer and the hole transport layer prepared in the example is about 290nm, wherein the continuous amorphous layer with the uppermost layer of about 80nm is a region rich in spiro-OMeTAD material, the region with the shaped crystal grains thereunder is a region rich in perovskite material, and the thickness of the region rich in perovskite material is only one third of that of the perovskite layer prepared by the conventional layer-by-layer method.

Claims (9)

1. A perovskite solar cell with a phase separation structure comprises a transparent conductive substrate, an electron transmission layer, a perovskite light absorption layer, a phase separation structure of a hole transmission layer and a metal electrode, wherein the electron transmission layer, the perovskite light absorption layer and the phase separation structure of the hole transmission layer are sequentially formed on the transparent conductive substrate; the phase separation structure of the perovskite light absorption layer and the hole transmission layer is obtained by adopting the following steps: a. adhering a flexible film with the thickness of 0.005-0.05 mm to the peripheral edge of an electron transmission layer formed on a transparent conductive substrate to form a region to be deposited; b. dripping 10-50 mu L/cm on the area to be deposited obtained in the step a2A mixed solution of a perovskite light-absorbing layer material and a hole-transporting material; the concentration of the perovskite light absorption layer material in the mixed solution is 0.2-0.9 mmol/mL, and the concentration of the hole transport material is 10-55 mg/mL; c. and c, covering a thin film layer on the transparent conductive substrate dropwise added with the mixed solution in the step b, standing for 1-5 min, placing on a heating table, heating for 15-60 s at the temperature of 90-240 ℃, removing the covered thin film layer, and heating for 10-30 min at the temperature of 80-100 ℃ to obtain the phase separation structure of the perovskite light absorption layer and the hole transmission layer.
2. A preparation method of a perovskite solar cell with a phase separation structure comprises the following steps:
step 1, preparing an electron transport layer on a substrate;
step 2, adhering a flexible film with the thickness of 0.005-0.05 mm to the peripheral edge of the electron transmission layer obtained in the step 1 to form a region to be deposited;
step 3, dripping 10-50 mu L/cm on the area to be deposited obtained in the step 22A mixed solution of a perovskite light-absorbing layer material and a hole-transporting material; the concentration of the perovskite light absorption layer material in the mixed solution is 0.2-0.9 mmol/mL, and the concentration of the hole transport material is 10-55 mg/mL;
step 4, covering a thin film layer on the substrate dropwise added with the mixed solution in the step 3, standing for 1-5 min, placing the substrate on a heating table, heating for 15-60 s at the temperature of 90-240 ℃, removing the covered thin film layer, and heating for 10-30 min at the temperature of 80-100 ℃ to obtain a phase separation structure of the perovskite light absorption layer and the hole transmission layer;
and 5, preparing a metal electrode on the phase separation structure of the perovskite light absorption layer and the hole transmission layer obtained in the step 4 to be used as a counter electrode, and thus obtaining the perovskite solar cell with the phase separation structure.
3. The method for producing a perovskite solar cell having a phase separation structure as claimed in claim 2, wherein a step of modifying the surface of the electron transport layer treated in the step 2 is added before the treatment in the step 3.
4. The method for preparing a perovskite solar cell with a phase separation structure according to claim 2, wherein the substrate of step 1 is FTO glass, ITO glass, AZO, flexible ITO, PET or PEN.
5. The method for preparing a perovskite solar cell having a phase separation structure as claimed in claim 2, wherein the electron transport layer material of step 1 is TiO2、ZnO、SnO2Or Zn2SnO4To adoptThe material is prepared by an atomic layer deposition, spin coating or dipping and pulling method; the electron transport layer is also prepared from TiO2、ZnO、SiO2、Al2O3、SiTiO3、ZrO2Or Zn2SnO4The mesoporous support layer.
6. The method for preparing a perovskite solar cell with a phase separation structure as claimed in claim 2, wherein the flexible film in step 2 is polyimide, polytetrafluoroethylene, polyethylene, polyvinyl chloride, polyethylene terephthalate, polypropylene or polystyrene.
7. The method for manufacturing a perovskite solar cell having a phase separation structure as claimed in claim 2, wherein the mixed solution of the perovskite light absorption layer material and the hole transport material in the step 3 is a mixed solution; wherein the chemical formula of the perovskite light absorption layer material is ABmX3-m，A＝CH3NH3、C4H9NH3、NH2＝CHNH2Or Cs, B is Pb or Sn, X is Cl, Br or I; the hole transport material is Spiro-OMeTAD, PTAA, P3HT, PEDOT PSS or NPB.
8. The method according to claim 2, wherein the solvent of the mixed solution in step 3 is one of N, N-dimethylformamide, N-dimethylacetamide, dimethylsulfoxide, and γ -butyrolactone, or a mixed solvent of chlorobenzene and one of the above solvents, or a mixed solvent of toluene and one of the above solvents.
9. The method according to claim 2, wherein the thin film layer in step 4 is a flexible thin film or a hard thin film, the thickness of the thin film is 0.005-0.05 mm, and the thin film layer is made of polyimide, polytetrafluoroethylene, polyethylene, polyvinyl chloride, polyethylene terephthalate, polypropylene or polystyrene.
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