CN113707817A - Preparation method of inorganic hole transport layer of perovskite solar cell - Google Patents
Preparation method of inorganic hole transport layer of perovskite solar cell Download PDFInfo
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- C23C14/34—Sputtering
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Abstract
The invention relates to a preparation method of an inorganic hole transport layer of a perovskite solar cell, which comprises the following steps: cleaning transparent conductive glass, and then drying the transparent conductive glass in a vacuum drying oven for later use; on transparent conductive glassPreparing an electron transport layer by adopting a spraying method, a thermal evaporation method or an atomic layer deposition method; preparing a perovskite absorption layer on the electron transport layer; the perovskite absorption layer is an ABX3 type perovskite photovoltaic material; preparing p-CuAlO on perovskite absorption layer by magnetron sputtering2A hole transport layer. The invention has the beneficial effects that: the invention adopts p-CuAlO2As hole transport material, p-CuAlO2Has good optical transparency, chemical stability and thermal stability, can be prepared from cheap, easily available and nontoxic elements, and the conductivity of the p-CuAlO2 is as high as 1S/cm. Thus, p-CuAlO is used as an inorganic hole transport layer material instead of Spiro-OMeTAD2Has great development potential.
Description
Technical Field
The invention belongs to the field of photovoltaics, and particularly relates to a preparation method of a perovskite solar cell with an inorganic hole transport layer.
Background
After the perovskite is tried to be applied to the field of photovoltaic power generation for the first time in 2009, the perovskite has great commercial value because of excellent performance, low cost and the possibility of being prepared by a solution method, and is very colorful. In 9 months of 2020, a National Renewable Energy Laboratory (NREL) issues a latest certification device efficiency evolution diagram, and the efficiency of a single perovskite solar cell is innovative and high and reaches 25.5%. Spiro-OMeTAD is the most commonly used HTL in the n-i-p structure battery, but the synthesis process is complex, the price is high, the thermal stability is insufficient, and the large-area application is not facilitated.
Although there have been little progress in the study of hole transport layers for current perovskite cells, there are still some problems, mainly expressed as: 1) the commonly used organic hole transport layer is expensive and has poor stability; 2) the common sol-gel method is not favorable for preparing a large-area perovskite solar cell.
Therefore, it is imperative to find a new material and method for preparing a hole transport layer.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of an inorganic hole transport layer of a perovskite solar cell.
The preparation method of the inorganic hole transport layer of the perovskite solar cell comprises the following steps:
step S1, cleaning the transparent conductive glass, and then drying the transparent conductive glass in a vacuum drying oven for later use;
s2, preparing an electron transport layer on the transparent conductive glass by adopting a spraying method, a thermal evaporation method or an atomic layer deposition method;
step S3, preparing a perovskite absorption layer on the electron transport layer; the perovskite absorption layer is an ABX3 type perovskite photovoltaic material;
step S4, preparing p-CuAlO on the perovskite absorption layer by magnetron sputtering2A hole transport layer.
Preferably, the transparent conductive glass in step S1 is ITO glass or FTO glass; the square resistance of the transparent conductive glass is 10 omega/sq.
Preferably, in step S1, the transparent conductive glass is sequentially cleaned with detergent, deionized water, acetone and ethanol for 10 minutes each time; the drying temperature of the vacuum drying oven is 70 ℃, and the drying time is 30 minutes.
Preferably, the thickness of the electron transport layer in step S2 is 1-300 nm.
Preferably, the thickness of the perovskite absorption layer in step S3 is 50 to 1500 nm.
Preferably, in step S3, a in ABX3 is a monovalent cation, a is at least one of methylamine, formamidine, 5-isopentanoate ammonium or Cs, B is at least one of Sn and Pb, and X is at least one of I, Br or Cl; A. b, X may each be a multi-ion hybrid structure.
Preferably, p-CuAlO is used in step S42The thickness of the hole transport layer is 1-300 nm; preparation of p-CuAlO by magnetron sputtering method2When the cavity is used for transporting the layer, the vacuum degree of the cavity is 1Pa before the magnetron sputtering starts the evaporation.
The preparation method of the inorganic hole transport layer is applied to the preparation of the perovskite solar cell and comprises the following steps:
step S1, cleaning the transparent conductive glass, and then drying the transparent conductive glass in a vacuum drying oven for later use;
s2, preparing an electron transport layer on the transparent conductive glass by adopting a spraying method, a thermal evaporation method or an atomic layer deposition method;
step S3, preparing a perovskite absorption layer on the electron transport layer; the perovskite absorption layer is an ABX3 type perovskite photovoltaic material;
step S4, preparing p-CuAlO on the perovskite absorption layer by magnetron sputtering2A hole transport layer;
step S5, adding p-CuAlO2And preparing an electrode layer on the hole transport layer.
Preferably, in step S5, the electrode layer is made of one of Al, Ag, Au, Mo, Cr and C, and the thickness of the electrode layer is 80-120 nm.
Preferably, the electrode layer is made of Ag in step S5, and p-CuAlO is plated on the electrode layer by thermal evaporation plating at step S52And coating a film on the hole transport layer to obtain the Ag electrode.
The invention has the beneficial effects that:
the invention adopts p-CuAlO2As hole transport material, p-CuAlO2Has good optical transparency, chemical stability and thermal stability, can be prepared from cheap, easily available and nontoxic elements, and the conductivity of the p-CuAlO2 is as high as 1S/cm. Thus, p-CuAlO is used as an inorganic hole transport layer material instead of Spiro-OMeTAD2Has great development potential.
The hole transport layer prepared by the magnetron sputtering technology is more compact and has better electrical property, and the stability of the perovskite solar cell can be improved. In the large-area perovskite battery, the film forming quality is improved. The efficiency is within acceptable limits at moderate losses because the cell area can be increased. An electron transport layer, a perovskite absorption layer, a hole transport layer and a metal anode electrode are sequentially prepared on the cleaned transparent conductive glass (FTO, ITO or transparent metal electrode).
The electron transport layer and the hole transport layer are made of inorganic materials, so that the stability of the whole perovskite solar cell is ensured. The invention optimizes the p-CuAlO by adjusting the magnetron sputtering process2And (5) forming the thin film, thereby obtaining the high-performance perovskite battery device. Furthermore, the battery stability can be comprehensively improved on the premise of ensuring the battery efficiency.
Drawings
FIG. 1 shows CuAlO2The structure of the cell is shown as a schematic diagram of a hole transport layer.
Description of reference numerals: the solar cell comprises an electrode layer 1, a p-CuAlO2 hole transport layer 2, a perovskite absorption layer 3, an electron transport layer 4 and transparent conductive glass 5.
Detailed Description
The present invention will be further described with reference to the following examples. The following examples are set forth merely to aid in the understanding of the invention. It should be noted that, for a person skilled in the art, several modifications can be made to the invention without departing from the principle of the invention, and these modifications and modifications also fall within the protection scope of the claims of the present invention.
At the same time, in order to prepare p-CuAlO in large area2Precise control of film morphology and crystalline quality is critical to device performance. The uniformly covered and smooth thin film of the transfer layer can reduce the recombination loss of charges. The invention adopts a magnetron sputtering method to prepare p-CuAlO2The film has the following advantages that (1) any substance can be sputtered; whether metal, semiconductor, insulator, compound, and mixture, and whether bulk or particulate matter, as long as it is solid, can be used as a target material, and the composition of matter can be adjusted by the target making process. (2) The adhesion between the sputtering film and the substrate is good; evaporating atoms due to the energy ratio of the sputtered atomsThe energy of the sputtering target is 1 to 2 orders of magnitude, so that the high-energy particles are deposited on the substrate to perform energy conversion, high heat energy is generated, and the adhesive force between the sputtered atoms and the substrate is enhanced. (3) High density of sputtered film, less pinholes, less pollution and high purity of film. (4) The controllability and the repeatability of the film are good. (5) Sputter coating can deposit thin films of uniform thickness over a large area.
However, sputter coating also has some disadvantages: the sputtering equipment is complex, a high-pressure device is needed, the sputtering deposition rate is low, the substrate temperature is high, and the sputtering equipment is easily influenced by impurity gases. Therefore, the invention optimizes the p-CuAlO by adjusting the magnetron sputtering process2And (5) forming the thin film, thereby obtaining the high-performance perovskite battery device.
Example one
The first embodiment of the application provides a CuAlO as shown in FIG. 12The preparation method of the perovskite battery used as the hole transport layer comprises the following steps:
step S1, cleaning the transparent conductive glass 5(ITO glass or FTO glass) by using a detergent, deionized water, acetone and ethanol in sequence, and cleaning for 10 minutes each time; then drying the transparent conductive glass 5 in a vacuum drying oven at 70 ℃ for 30 minutes for later use;
step S2, preparing an electron transport layer 4 with the thickness of 1-300 nm on the transparent conductive glass 5 by adopting a spin coating method, a spraying method, a thermal evaporation method or an atomic layer deposition method;
the precursor solution of spin coating is SnO2The concentration of the aqueous solution is 3-12 mg/mL, and the rotating speed is 3000-5000 rpm;
TiO prepared by thermal evaporation method, atomic layer deposition method and other methods2、ZnO、PCBM、C60And the like. By spraying with TiO2For example, 5% titanium acetylacetonate in isopropanol is sprayed onto a 500 ℃ transparent conductive glass substrate at a speed of 0.5mL/min, the spraying thickness is 10-50 nm, and after the spraying is finished, the substrate is continuously annealed at the temperature for 10-30 minutes and then cooled to room temperature; thermal evaporation method with C60For example, C60Powder of
At a speed of less than 8 x 10-6Evaporating 5-20 nm on transparent conductive glass at room temperature under the pressure of a torr; atomic layer deposition with SnO2For example, tetra (dimethylamino) tin is used as a tin source, water or ozone is used as an oxygen source, 5-20 nm SnO is atomically deposited at 150-300 DEG C2The film is on the transparent conductive glass.
S3, preparing an ABX3 type perovskite absorption layer 3 with the thickness of 50-1500 nm on the electron transmission layer 4; the perovskite absorption layer 3 is an ABX3 type perovskite photovoltaic material; a is univalent cation, A is at least one of methylamine, formamidine, 5-iso-ammonium valerate or Cs, B is at least one of Sn and Pb, and X is at least one of I, Br or Cl;
step S4, preparing 1-300 nm thick p-CuAlO on the perovskite absorption layer 3 by magnetron sputtering2A hole transport layer;
step S5, using thermal evaporation coating machine to form p-CuAlO2And coating a film on the hole transport layer to obtain an electrode layer 1 with the thickness of 80-120 nm, wherein the material of the electrode layer 1 is one of Al, Ag, Au, Mo, Cr and C.
Example two
1) Preparing an electron transport layer (TiO) with the thickness of 1-300 nm on a conductive substrate of an ITO (indium tin oxide), FTO (fluorine-doped tin oxide), ATO (antimony tin oxide) or transparent metal electrode in sequence2、SnO2、ZnO、PCBM、C60、Nb2O5、SrTiO3ICBA, ICTA) and perovskite thin film (ABX) with thickness of 50-1500 nm3Wherein A is MA (methylamine), FA (formamidine), 5-AVA (5-isopentanoate ammonium), or CS, and combinations thereof, B is Sn, Pb, and combinations thereof, and X is I, Br or Cl, and combinations thereof).
2) Preparation of p-CuAlO by magnetron sputtering coating equipment2A hole transport layer. Before starting sputtering, the vacuum degree of the chamber was controlled to 1 Pa. Setting Ar: o is2The gas flow ratio is 1:4, 2:3, 3:2, 4: 1. When the Ar gas is too large, the Ar gas is changed into residual gas because of not colliding with the target, and the residual gas and target atoms are deposited on a substrate together, so that the compactness of a formed film is deteriorated, and the electric leakage phenomenon is caused; and too small an Ar gas cannot sustain plasma. O is2Excessive gas can oxidize Cu+Ion to Cu2+Shadow capable of showingThe efficiency of its hole transport; and O is2Too little gas affects the film quality. Preferably, Ar: o is2The gas flow ratio was 4: 1. The sputtering power is 80W, and the sputtering time is controlled so that the film thickness is 20 nm.
3) Preparing metal electrode on the prepared battery with hole transmission layer by vacuum thermal evaporation coating machine, wherein before evaporation coating, the vacuum degree of the cavity is lower than 4X 10-6Pa, regulating the current and voltage range of the power supply, and controlling the evaporation speed of the film to be
Controlling the evaporation time to ensure that the thickness of the film is 80 nm-100 nm. And obtaining the perovskite solar cell with the halide modified anode electrode.
EXAMPLE III
1) Preparing an electron transport layer (TiO) with the thickness of 1-300 nm on a conductive substrate of an ITO (indium tin oxide), FTO (fluorine-doped tin oxide), ATO (antimony tin oxide) or transparent metal electrode in sequence2、SnO2、ZnO、PCBM、C60、Nb2O5、SrTiO3ICBA, ICTA) and perovskite thin film (ABX) with thickness of 50-1500 nm3Wherein A is MA (methylamine), FA (formamidine), 5-AVA (5-isopentanoate ammonium), or CS, and combinations thereof, B is Sn, Pb, and combinations thereof, and X is I, Br or Cl, and combinations thereof).
2) Preparation of p-CuAlO by magnetron sputtering coating equipment2A hole transport layer. Before sputtering, the working vacuum degree of the cavity is set to be 1Pa, 2Pa and 3 Pa. The change of the working gas pressure is changed by controlling the inflow amount of the gas. Namely, less gas is introduced in unit time, and the air pressure in the sputtering chamber is low; the gas is introduced more, and the gas pressure of the sputtering chamber is higher. This means that the probability of collision between sputtered particles with low gas pressure and gas molecules is small, the mean free path of the sputtered particles is large, the kinetic energy when reaching the substrate is also large, and the deposition rate of the film is fast; the collision probability of air pressure high sputtering particles and gas molecules is large, and the average self of the sputtering particlesThe distance from the bottom to the substrate is small, the kinetic energy when the film reaches the substrate is small, and the deposition rate of the film is slow. Therefore, the change of the working air pressure can affect the growth condition of the film. Setting Ar: o is2The gas flow ratio was 4: 1. The sputtering power was 80W. The film thickness was 20nm by controlling the sputtering time.
3) Preparing metal electrode on the prepared battery with hole transmission layer by vacuum thermal evaporation coating machine, wherein before evaporation coating, the vacuum degree of the cavity is lower than 4X 10-6Pa, regulating the current and voltage range of the power supply, and controlling the evaporation speed of the film to be
Controlling the evaporation time to ensure that the thickness of the film is 80 nm-100 nm. And obtaining the perovskite solar cell with the halide modified anode electrode.
Example four:
1) preparing an electron transport layer (TiO) with the thickness of 1-300 nm on a conductive substrate of an ITO (indium tin oxide), FTO (fluorine-doped tin oxide), ATO (antimony tin oxide) or transparent metal electrode in sequence2、SnO2、ZnO、PCBM、C60、Nb2O5、SrTiO3ICBA, ICTA) and perovskite thin film (ABX) with thickness of 50-1500 nm3Wherein A is MA (methylamine), FA (formamidine), 5-AVA (5-isopentanoate ammonium), or CS, and combinations thereof, B is Sn, Pb, and combinations thereof, and X is I, Br or Cl, and combinations thereof).
2) Preparation of p-CuAlO by magnetron sputtering coating equipment2A hole transport layer. Before sputtering, the working vacuum degree of the cavity is set to be 1pa, Ar: o is2The gas flow ratio is 4: 1. the sputtering power was 60W, 80W and 100W. When the sputtering power is too high, the target is easily broken, and the deposition rate is too high, which reduces the film formation quality of the thin film. However, if the sputtering power is too low, the target cannot be sputtered normally, and the film-forming conductivity is too low. The film thickness was 20nm by controlling the sputtering time.
3) In alreadyPreparing metal electrode on the prepared cell with hole transmission layer by vacuum thermal evaporation coating machine, wherein before evaporation coating, the vacuum degree of the cavity is lower than 4 × 10-6Pa, regulating the current and voltage range of the power supply, and controlling the evaporation speed of the film to be
Controlling the evaporation time to ensure that the thickness of the film is 80 nm-100 nm. And obtaining the perovskite solar cell with the halide modified anode electrode.
Example five:
1) preparing an electron transport layer (TiO) with the thickness of 1-300 nm on a conductive substrate of an ITO (indium tin oxide), FTO (fluorine-doped tin oxide), ATO (antimony tin oxide) or transparent metal electrode in sequence2、SnO2、ZnO、PCBM、C60、Nb2O5、SrTiO3ICBA, ICTA) and perovskite thin film (ABX) with thickness of 50-1500 nm3Wherein A is MA (methylamine), FA (formamidine), 5-AVA (5-isopentanoate ammonium), or CS, and combinations thereof, B is Sn, Pb, and combinations thereof, and X is I, Br or Cl, and combinations thereof).
2) Preparation of p-CuAlO by magnetron sputtering coating equipment2A hole transport layer. Before sputtering, setting the working vacuum degree of a cavity to be 1Pa, Ar: o is2The gas flow ratio was 4: 1. The sputtering power was 80W. The thickness of the film is 10nm, 20nm, 50nm, 100nm, 200nm, 300nm and 400nm by controlling the sputtering time. The thickness of the film has great influence on the performances of the conductivity, the light transmittance, the carrier transmission efficiency and the like of the film, and the proper thickness control can ensure that the performance of the perovskite solar cell device is optimal.
3) Preparing metal electrode on the prepared battery with hole transmission layer by vacuum thermal evaporation coating machine, wherein before evaporation coating, the vacuum degree of the cavity is lower than 4X 10-6Pa, regulating the current and voltage range of the power supply, and controlling the evaporation speed of the film to be
Controlling the evaporation time to ensure that the thickness of the film is 80 nm-100 nm. And obtaining the perovskite solar cell with the halide modified anode electrode.
Comparative example:
1) preparing an electron transport layer (TiO) with the thickness of 1-300 nm on a conductive substrate of an ITO (indium tin oxide), FTO (fluorine-doped tin oxide), ATO (antimony tin oxide) or transparent metal electrode in sequence2、SnO2、ZnO、PCBM、C60、Nb2O5、SrTiO3ICBA, ICTA) and perovskite thin film (ABX) with thickness of 50-1500 nm3Wherein A is MA (methylamine), FA (formamidine), 5-AVA (5-isopentanoate ammonium) or CS and combinations thereof, B is Sn, Pb, and combinations thereof, and X is I, Br or Cl and combinations thereof).
2) Preparing a hole transport layer (spiro-OMeTAD, NiO) with the thickness of 1-300 nm on the perovskite absorption layerx、CuI、CuSCN、PEDOT:PSS、Graphene oxide、Cu2O、CuO、P3HT、VOx)。
3) And preparing an Ag electrode on the hole transport layer by using vacuum thermal evaporation coating. Before starting evaporation, the vacuum degree of the cavity is lower than 4 multiplied by 10-6Pa, regulating the current and voltage range of the power supply, and controlling the evaporation speed of the film to be
Controlling the evaporation time to make the thickness of the metal silver electrode be 80-300 nm. And obtaining the perovskite solar cell.
And (4) conclusion:
the cells in the comparative example and the second to fifth examples were subjected to a current-voltage test under simulated sunlight, and as a result, it was found that p-CuAlO was produced using a magnetron sputtering coating apparatus2A hole transport layer. Before sputtering, setting the working vacuum degree of a cavity to be 1Pa, Ar: o is2The gas flow ratio was 4: 1. The sputtering power was 80W. By controlling the sputtering time, the performance of the device is optimal when the thickness of the film is 20 nm. The invention utilizes p-CuAlO2As perovskite solar cellsThe hole transport layer has not only good optical transparency, chemical stability and thermal stability, but also can be made of cheap, easily available and non-toxic elements, compared to the currently most commonly used Spiro-OMeTAD materials. Its conductivity can also be up to 1S/cm. The invention prepares the p-CuAlO by a magnetron sputtering method2The film overcomes the defect of difficult film formation on a large area by a sol-gel method under the adverse effect of proper loss of the efficiency of the perovskite solar cell, and can be prepared into a thickness of 10cm2The above large-area battery is extremely important for its industrial and commercial significance.
Claims (10)
1. A preparation method of an inorganic hole transport layer of a perovskite solar cell is characterized by comprising the following steps:
step S1, cleaning the transparent conductive glass (5), and then drying the transparent conductive glass (5) in a vacuum drying oven for later use;
s2, preparing an electron transport layer (4) on the transparent conductive glass (5) by adopting a spraying method, a thermal evaporation method or an atomic layer deposition method;
step S3, preparing a perovskite absorption layer (3) on the electron transport layer (4); the perovskite absorption layer (3) is an ABX3 type perovskite photovoltaic material;
step S4, preparing p-CuAlO on the perovskite absorption layer (3) by utilizing magnetron sputtering2A hole transport layer.
2. The method of preparing an inorganic hole transport layer of a perovskite solar cell according to claim 1, characterized in that: in the step S1, the transparent conductive glass (5) is ITO glass or FTO glass; the sheet resistance of the transparent conductive glass (5) is 10 omega/sq.
3. The method of preparing an inorganic hole transport layer of a perovskite solar cell according to claim 1, characterized in that: in the step S1, the transparent conductive glass (5) is cleaned by sequentially utilizing a detergent, deionized water, acetone and ethanol for 10 minutes each time; the drying temperature of the vacuum drying oven is 70 ℃, and the drying time is 30 minutes.
4. The method of preparing an inorganic hole transport layer of a perovskite solar cell according to claim 1, characterized in that: in step S2, the thickness of the electron transport layer (4) is 1-300 nm.
5. The method of preparing an inorganic hole transport layer of a perovskite solar cell according to claim 1, characterized in that: in the step S3, the thickness of the perovskite absorption layer (3) is 50-1500 nm.
6. The method of preparing an inorganic hole transport layer of a perovskite solar cell according to claim 1, characterized in that: in step S3, A in ABX3 is a monovalent cation, A is at least one of methylamine, formamidine, 5-iso-ammonium valerate or Cs, B is at least one of Sn and Pb, and X is at least one of I, Br or Cl.
7. The method of preparing an inorganic hole transport layer of a perovskite solar cell according to claim 1, characterized in that: P-CuAlO in step S42The thickness of the hole transport layer is 1-300 nm; preparation of p-CuAlO by magnetron sputtering method2When the cavity is used for transporting the layer, the vacuum degree of the cavity is 1Pa before the magnetron sputtering starts the evaporation.
8. Use of a process for the preparation of an inorganic hole transport layer according to claim 1 in the preparation of a perovskite solar cell, comprising the steps of:
step S1, cleaning the transparent conductive glass (5), and then drying the transparent conductive glass (5) in a vacuum drying oven for later use;
s2, preparing an electron transport layer (4) on the transparent conductive glass (5) by adopting a spraying method, a thermal evaporation method or an atomic layer deposition method;
step S3, preparing a perovskite absorption layer (3) on the electron transport layer (4); the perovskite absorption layer (3) is an ABX3 type perovskite photovoltaic material;
step S4, preparing p-CuAlO on the perovskite absorption layer (3) by utilizing magnetron sputtering2A hole transport layer;
step S5, adding p-CuAlO2And preparing an electrode layer (1) on the hole transport layer.
9. Use of the method of manufacturing an inorganic hole transport layer according to claim 8 in the manufacture of a perovskite solar cell, characterized in that: in the step S5, the electrode layer (1) is made of one of Al, Ag, Au, Mo, Cr and C, and the thickness of the electrode layer (1) is 80-120 nm.
10. Use of the method of manufacturing an inorganic hole transport layer according to claim 8 in the manufacture of a perovskite solar cell, characterized in that: in step S5, the electrode layer (1) is made of Ag, and in step S5, a thermal evaporation coating machine is used for coating p-CuAlO2And coating a film on the hole transport layer to obtain the Ag electrode.
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