CN111435709A - Method for improving stability of perovskite thin film - Google Patents

Method for improving stability of perovskite thin film Download PDF

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CN111435709A
CN111435709A CN202010136324.3A CN202010136324A CN111435709A CN 111435709 A CN111435709 A CN 111435709A CN 202010136324 A CN202010136324 A CN 202010136324A CN 111435709 A CN111435709 A CN 111435709A
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不公告发明人
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Hangzhou Microquanta Semiconductor Corp ltd
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Abstract

The invention relates to a method for improving the stability of a perovskite thin film, which comprises the following steps: placing a substrate with a perovskite film on the surface in a reaction cavity, and repeatedly cleaning the reaction cavity by using inert gas; introducing hydrogen sulfide gas into the reaction cavity to react with perovskite film molecules to generate a sulfide layer on the surface of the perovskite film; and after the reaction is finished, repeatedly cleaning the reaction cavity by using inert gas, inflating to normal pressure, and taking out the substrate after the reaction cavity is cooled. The invention changes the chemical composition of the surface and the crystal boundary of the perovskite material and inhibits the degradation of the perovskite by generating the nano-scale lead sulfide layer on the crystal boundary and the surface of the perovskite film material, thereby improving the performance of the perovskite film material and prolonging the stability of the perovskite film material.

Description

Method for improving stability of perovskite thin film
Technical Field
The invention belongs to the technical field of perovskite solar cell preparation, and particularly relates to a method for improving the stability of a perovskite thin film.
Background
Generally, the perovskite material used in high efficiency solar cells is an inorganic-organic ABX3A mold type hybrid structure. Wherein A is mainly methylamino (CH)3NH3 +) Formamidino (CH (NH)2)2 +) Monovalent organic cation and K+、Rb+、Cs+One or more of monovalent inorganic cations are contained at any ratio, and B is mainly divalent lead ion (Pb)2+) X is predominantly a halogen anion (Cl)-，Br-，I-). Research shows that the perovskite materialThe degradation of the material mainly starts from the surface and the grain boundary, which are caused by the fact that the perovskite material has a large number of defects on the surface and the grain boundary, the defects have high reactivity, and under the factors of water, oxygen, light and the like, the perovskite material is easy to chemically react to cause the degradation of the perovskite material from outside to inside. In order to improve the stability of perovskite, it is common practice to passivate the surface of perovskite, to reduce the concentration of active defects, and to inhibit the reactivity of defect sites, for example, in patent publication CN 109686843A. There have also been some studies on the effect of improving the stability of perovskite by embedding a water oxygen barrier layer, such as patent publication No. CN 105161623A.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for improving the stability of a perovskite thin film, which changes the chemical composition of the surface and the grain boundary of the perovskite material and inhibits the degradation of perovskite by generating a nano-scale lead sulfide layer on the grain boundary and the surface of the perovskite thin film material, thereby improving the performance of the perovskite thin film material and prolonging the stability of the perovskite thin film material.
The invention is realized by providing a method for improving the stability of a perovskite thin film, which comprises the following steps:
placing a substrate with a perovskite film on the surface in a reaction cavity, and repeatedly cleaning the reaction cavity by using inert gas;
secondly, introducing hydrogen sulfide gas into the reaction cavity to react with perovskite film molecules to generate a sulfide layer on the surface of the perovskite film;
and step three, after the reaction is finished, repeatedly cleaning the reaction cavity by using inert gas, inflating to normal pressure, and taking out the substrate after the reaction cavity is cooled.
Further, the inert gas includes argon or nitrogen.
Further, in the first step and the third step, the step of repeatedly cleaning the reaction chamber with the inert gas means that the reaction chamber is vacuumized, the inert gas is filled again, and the operations of air suction and air inflation are repeatedly performed for many times, so that the reaction chamber is purified.
Further, in the second step, the volume ratio of the introduced hydrogen sulfide gas is 0.1-10%, and the temperature of the reaction cavity is not more than 300 ℃.
Furthermore, the perovskite thin film contains a molecular structural formula ABX3Wherein A is methylamino (CH)3NH3 +) Or formamidinyl (CH (NH)2)2 +) A monovalent organic cation, or K+、Rb+、Cs+At least one of monovalent inorganic cations, B being lead ion (Pb)2+) Or stannous ion (Sn)2+) A divalent main cation, X is Cl-、Br-、I-Any one of monovalent halide anions, or thiocyanate (SCN)-) Or acetate ion (CH)3COO-) A monovalent anion.
Further, B also comprises a divalent doping cation, wherein the divalent doping cation comprises at least one of boron, silicon, germanium, arsenic, antimony, beryllium, magnesium, calcium, strontium, barium, aluminum, indium, gallium, thallium, bismuth, lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, scandium, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc, yttrium, zirconium, niobium, molybdenum, ruthenium, rhodium, palladium, silver, cadmium, hafnium, tantalum, tungsten, rhenium, osmium, iridium, platinum and gold ions, and the divalent doping cation and a divalent main cation (Pb, Pb) are mixed2+Or Sn2+) The ratio of the mole percentages of (a) does not exceed 5%.
Specifically, the method for improving the stability of the perovskite thin film comprises the following steps:
step 11, preparing ITO/SnO2/CH3NH3PbI3Placing the substrate in a reaction chamber, and vacuumizing the reaction chamber to 1 × 10-4Pa, filling high-purity nitrogen to the pressure of 10Pa in the cavity, and repeating the operations of air suction and air filling for three times to purify the reaction cavity;
step 12, introducing a mixed gas of hydrogen sulfide and nitrogen with the volume fraction of 0.6% into a reaction cavity, keeping the pressure in the cavity at 50Pa and the temperature at 90 ℃, and reacting the hydrogen sulfide with perovskite film molecules to generate a sulfide layer on the surface of the perovskite film for 2 min;
step 13, after the reaction is finished, vacuumizing the reaction cavity to 1 × 10-2Pa, and filling high-purity nitrogen to the pressure of 1 × 10 in the cavity4And Pa, repeating the operations of air suction and air inflation for three times, finally refilling air until the reaction cavity recovers to normal pressure, opening the reaction cavity after the reaction cavity is cooled, and taking out the substrate after the reaction is finished.
Specifically, the method for improving the stability of the perovskite thin film comprises the following steps:
step 21, preparing the ITO/PTAA/Cs0.05FA0.80MA0.15Pb(I0.85br0.15)3The substrate is placed in a reaction cavity, the reaction cavity is vacuumized to 10Pa, and high-purity nitrogen is charged until the pressure in the cavity is 10 DEG5Pa, repeatedly performing air suction and inflation operations for four times to purify the reaction cavity;
step 22, introducing mixed gas of hydrogen sulfide and nitrogen with the temperature of 150 ℃ and the volume fraction of 5% into the reaction cavity at the rate of 10 ml/min, so that a sulfide layer is generated on the surface of the perovskite film after the hydrogen sulfide reacts with the perovskite film molecules, and the reaction time is 10 s;
step 23, after the reaction is finished, vacuumizing the reaction cavity to 10Pa, and filling high-purity nitrogen to the pressure of 1 × 10 in the cavity5And Pa, repeating the operations of air suction and air inflation for four times in sequence, finally re-inflating until the reaction cavity recovers to normal pressure, opening the reaction cavity after the reaction cavity is cooled, and taking out the substrate after the reaction is finished.
Compared with the prior art, the method for improving the stability of the perovskite thin film has the advantages that hydrogen sulfide gas is introduced into the reaction cavity through the substrate with the perovskite thin film on the surface, so that the lead sulfide layer with the nanometer thickness is generated on the surface and the grain boundary of the perovskite thin film after the hydrogen sulfide reacts with perovskite thin film molecules, the chemical composition on the surface and the grain boundary of the perovskite thin film is changed, the effect of passivating the surface defects of the perovskite thin film is achieved, the degradation of the perovskite thin film material is inhibited, in addition, the generated sulfide layer has excellent water-oxygen stability, and the stability of the perovskite thin film material is greatly improved.
Drawings
FIG. 1 is a SEM illustration of a perovskite thin film of example 1 of the method of improving the stability of a perovskite thin film of the present invention;
FIG. 2 is a schematic current density-voltage curve for a device prepared in example 2 of the method of improving the stability of a perovskite thin film according to the present invention;
FIG. 3 is a graphical representation of the air stability curve for a device prepared in example 2 of the method of improving the stability of a perovskite thin film of the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The preferred embodiment of the method for improving the stability of the perovskite thin film comprises the following steps:
placing a substrate with a perovskite film on the surface in a reaction cavity, and repeatedly cleaning the reaction cavity by using inert gas.
And step two, introducing hydrogen sulfide gas into the reaction cavity to react with perovskite film molecules to generate a nano sulfide layer on the surface of the perovskite film.
And step three, after the reaction is finished, repeatedly cleaning the reaction cavity by using inert gas, removing hydrogen sulfide and other residues in the reaction cavity, inflating to normal pressure, and taking out the substrate with the perovskite film on the surface after the reaction cavity is cooled.
Specifically, the inert gas includes argon or nitrogen.
Specifically, in the first step and the third step, the step of repeatedly cleaning the reaction chamber with the inert gas means that the reaction chamber is vacuumized, the inert gas is filled again, and the operations of air suction and air inflation are repeatedly performed for many times to purify the reaction chamber.
Specifically, in the second step, the volume ratio of the introduced hydrogen sulfide gas is 0.1-10%, and the temperature of the reaction cavity is not more than 300 ℃.
Specifically, the perovskite thin film contains a molecular structural formula ABX3Wherein A is methylamino (CH)3NH3 +) Or formamidinyl (CH (NH)2)2 +) A monovalent organic cation, or K+、Rb+、Cs+At least one of monovalent inorganic cations, B being lead ion (Pb)2+) Or stannous ion (Sn)2+) A divalent main cation, X is Cl-、Br-、I-Any one of monovalent halide anions, or thiocyanate (SCN)-) Or acetate ion (CH)3COO-) A monovalent anion.
Wherein B also comprises divalent doping cations, the divalent doping cations comprise at least one of boron, silicon, germanium, arsenic, antimony, beryllium, magnesium, calcium, strontium, barium, aluminum, indium, gallium, thallium, bismuth, lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, scandium, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc, yttrium, zirconium, niobium, molybdenum, ruthenium, rhodium, palladium, silver, cadmium, hafnium, tantalum, tungsten, rhenium, osmium, iridium, platinum and gold ions, wherein the divalent doping cations are mixed with divalent main cations (Pb, iridium, platinum and gold ions)2+Or Sn2+) The ratio of the mole percentages of (a) does not exceed 5%.
The method of improving the stability of perovskite thin film according to the present invention will be further described with reference to the following specific examples.
Example 1
The first embodiment of the method for improving the stability of the perovskite thin film comprises the following steps:
step 11, depositing electronic transmission material SnO on the surface of the transparent conductive glass Indium Tin Oxide (ITO) in sequence2And perovskite material CH3NH3PbI3Then the ITO/SnO layer is formed2/CH3NH3PbI3Placing the substrate in a reaction chamber, and vacuumizing the reaction chamber to 1 × 10-4And Pa, filling high-purity nitrogen to the pressure of 10Pa in the cavity, and repeating the operations of air suction and air filling for three times to purify the reaction cavity. And step 12, introducing a mixed gas of hydrogen sulfide and nitrogen with the volume fraction of 0.6% into a reaction cavity, keeping the pressure in the cavity at 50Pa and the temperature at 90 ℃, reacting the hydrogen sulfide with perovskite film molecules, and generating a sulfide layer on the surface of the perovskite film for 2 min.
Step 13, after the reaction is finished, vacuumizing the reaction cavity to 1 × 10-2Pa, and filling high-purity nitrogen to the pressure of 1 × 10 in the cavity4And Pa, repeating the operations of air suction and air inflation for three times, finally refilling air until the reaction cavity recovers to normal pressure, opening the reaction cavity after the reaction cavity is cooled, and taking out the substrate after the reaction is finished.
And observing the surface of the obtained substrate by an electron microscope to obtain a schematic micro-morphology of the perovskite thin film on the surface of the substrate as shown in figure 1. As can be seen from the figure, the perovskite thin film processed by the method of the invention is uniform and compact, the surface of the crystal grain is smooth, and the structure is clear.
Example 2
The second embodiment of the method for improving the stability of the perovskite thin film comprises the following steps:
step 21, depositing hole transport material poly [ bis (4-phenyl) (2,4, 6-trimethylphenyl) amine on the surface of the light-transmitting conductive glass fluorine-doped tin oxide (FTO) in sequence](PTAA) and perovskite Material Cs0.05FA0.80MA0.15Pb(I0.85br0.15)3Then will have FTO/PTAA/Cs0.05FA0.80MA0.15Pb(I0.85br0.15)3The substrate is placed in a reaction cavity, the reaction cavity is vacuumized to 10Pa, and high-purity nitrogen is charged until the pressure in the cavity is 10 DEG5And Pa, repeatedly performing air suction and air inflation operation for four times to purify the reaction cavity.
And step 22, introducing mixed gas of hydrogen sulfide and nitrogen with the temperature of 150 ℃ and the volume fraction of 5% into the reaction cavity at the rate of 10 ml/min, so that a sulfide layer is generated on the surface of the perovskite film after the hydrogen sulfide reacts with the perovskite film molecules, and the reaction time is 10 s.
Step 23, after the reaction is finished, vacuumizing the reaction cavity to 10Pa, and filling high-purity nitrogen to the pressure of 1 × 10 in the cavity5And Pa, repeating the operations of air suction and air inflation for four times in sequence, finally re-inflating until the reaction cavity recovers to normal pressure, opening the reaction cavity after the reaction cavity is cooled, and taking out the substrate after the reaction is finished.
And (4) continuously processing the substrate obtained in the step (23), and sequentially depositing C60, BCP and Ag on the surface of the perovskite film to finish the preparation of the solar photovoltaic cell device. Then, the prepared device was subjected to a performance test to obtain a current density-voltage curve, as shown in fig. 2, and the prepared device had almost no hysteresis. The stability curve of the device in air is shown in fig. 3, revealing that the perovskite cell after hydrogen sulfide treatment has better stability in air. After 1000 hours of air exposure, the hydrogen sulfide treated perovskite cells maintained an initial photoelectric conversion efficiency of 93%, whereas the perovskite cells not treated with hydrogen sulfide had a decay in photoelectric conversion efficiency to 31% of the initial value.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (8)

1. A method of improving the stability of a perovskite thin film, comprising the steps of:
placing a substrate with a perovskite film on the surface in a reaction cavity, and repeatedly cleaning the reaction cavity by using inert gas;
secondly, introducing hydrogen sulfide gas into the reaction cavity to react with perovskite film molecules to generate a sulfide layer on the surface of the perovskite film;
and step three, after the reaction is finished, repeatedly cleaning the reaction cavity by using inert gas, inflating to normal pressure, and taking out the substrate after the reaction cavity is cooled.
2. The method of improving the stability of a perovskite thin film as claimed in claim 1, wherein the inert gas comprises argon or nitrogen.
3. The method for improving the stability of a perovskite thin film as claimed in claim 1, wherein in the first step and the third step, the step of repeatedly cleaning the reaction chamber with the inert gas means that the reaction chamber is vacuumized, the inert gas is refilled, and the operations of air suction and air inflation are repeatedly performed for a plurality of times to purify the reaction chamber.
4. The method for improving the stability of the perovskite thin film as claimed in claim 1, wherein in the second step, the volume ratio of the introduced hydrogen sulfide gas is 0.1-10%, and the temperature of the reaction cavity is not more than 300 ℃.
5. The method of improving the stability of a perovskite thin film as claimed in claim 1, wherein the perovskite thin film contains a compound having a molecular structural formula ABX3Wherein A is a methylamino or formamidino monovalent organic cation, or K is+、Rb+、Cs+At least one of monovalent inorganic cations, B is lead ion or stannous ion divalent main cation, and X is Cl-、Br-、I-Any one of monovalent halide anions, or thiocyanate or acetate monovalent anion.
6. The method of improving the stability of a perovskite thin film as defined in claim 5, wherein B further comprises a divalent dopant cation comprising at least one of boron, silicon, germanium, arsenic, antimony, beryllium, magnesium, calcium, strontium, barium, aluminum, indium, gallium, thallium, bismuth, lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, scandium, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc, yttrium, zirconium, niobium, molybdenum, ruthenium, rhodium, palladium, silver, cadmium, hafnium, tantalum, tungsten, rhenium, osmium, iridium, platinum, gold ions, wherein the molar percentage of the divalent dopant cation to the divalent host cation is not more than 5%.
7. The method of improving the stability of a perovskite thin film as claimed in claim 1, comprising the steps of:
step 11, preparing ITO/SnO2/CH3NH3PbI3Placing the substrate in a reaction chamber, and vacuumizing the reaction chamber to 1 × 10-4Pa, filling high-purity nitrogen to the pressure of 10Pa in the cavity, and repeating the operations of air suction and air filling for three times to purify the reaction cavity;
step 12, introducing a mixed gas of hydrogen sulfide and nitrogen with the volume fraction of 0.6% into a reaction cavity, keeping the pressure in the cavity at 50Pa and the temperature at 90 ℃, and reacting the hydrogen sulfide with perovskite film molecules to generate a sulfide layer on the surface of the perovskite film for 2 min;
step 13, after the reaction is finished, vacuumizing the reaction cavity to 1 × 10-2Pa, and filling high-purity nitrogen to the pressure of 1 × 10 in the cavity4And Pa, repeating the operations of air suction and air inflation for three times, finally refilling air until the reaction cavity recovers to normal pressure, opening the reaction cavity after the reaction cavity is cooled, and taking out the substrate after the reaction is finished.
8. The method of improving the stability of a perovskite thin film as claimed in claim 1, comprising the steps of:
step 21, preparing the ITO/PTAA/Cs0.05FA0.80MA0.15Pb(I0.85br0.15)3The substrate is placed in a reaction cavity, the reaction cavity is vacuumized to 10Pa, and high-purity nitrogen is charged until the pressure in the cavity is 10 DEG5Pa, repeatedly performing air suction and inflation operations for four times to purify the reaction cavity;
step 22, introducing mixed gas of hydrogen sulfide and nitrogen with the temperature of 150 ℃ and the volume fraction of 5% into the reaction cavity at the rate of 10 ml/min, so that a sulfide layer is generated on the surface of the perovskite film after the hydrogen sulfide reacts with the perovskite film molecules, and the reaction time is 10 s;
step 23, after the reaction is finished, vacuumizing the reaction cavity to 10Pa, and filling high-purity nitrogen to the pressure of 1 × 10 in the cavity5And Pa, repeating the operations of air suction and air inflation for four times in sequence, finally re-inflating until the reaction cavity recovers to normal pressure, opening the reaction cavity after the reaction cavity is cooled, and taking out the substrate after the reaction is finished.
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CN105602560A (en) * 2016-02-01 2016-05-25 南京理工大学 Method for synthetizing high-stability metal halide perovskite/lead sulfide heterostructure nanocrystals
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115074667A (en) * 2022-07-01 2022-09-20 郑州大学 High-mobility p-type SrHfS 3 Film and preparation method thereof

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