CN112186110B - Preparation method of organic-inorganic hybrid perovskite methylamine lead iodide surface in-situ growth organic passivation film - Google Patents
Preparation method of organic-inorganic hybrid perovskite methylamine lead iodide surface in-situ growth organic passivation film Download PDFInfo
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Abstract
The invention discloses a preparation method of an organic-inorganic hybrid perovskite lead methyl iodide surface in-situ growth organic passivation film, which comprises the following steps: a: dissolving methyl amine iodide and lead iodide in anhydrous N, N-dimethylformamide to form a bright yellow solution, adding chlorobenzene to form a white floccule precipitate, placing the white floccule precipitate on a heating table for drying until the white precipitate is completely blackened to obtain methyl amine lead iodide powder; b: dissolving the methylamine lead iodide powder in the HI solution until black precipitates are separated out again from the HI solution, so as to obtain a supersaturated solution for in-situ preparation of the methylamine lead iodide passive film; c: and (D) dropwise adding the supersaturated HI solution obtained in the step (B) into the methylamine lead iodide powder prepared in the step (A), and grinding and illuminating to obtain methylamine lead iodide with an organic passivation film on the surface.
Description
Technical Field
The invention relates to the photovoltaic field, in particular to a preparation method of an organic passive film grown in situ on the surface of organic-inorganic hybrid perovskite methylamine lead iodide.
Background
Some prior art methods prepare a passivation film on the surface of the perovskite to enhance the stability of the perovskite, for example, the stability of the perovskite is enhanced by passivating the surface defects of the perovskite with organic molecules; by reacting in situ with specific inorganic anions, a thin and dense inorganic protective film is formed on the surface of the perovskite.
The prior art has the following problems: 1) Chemical bonds between passivation molecules and the surface of perovskite are weak, so that MAPbI3 is difficult to protect from water and oxygen; 2) Neither chemical bonding nor physical covering can completely cover the perovskite crystals, and perovskite degradation can still occur; 3) Even though the surface protection film and the perovskite have strong chemical bonding force and can well protect the perovskite from external attack, the technical routes are too complex, and the reaction time and the precursor concentration are extremely difficult to control to generate a thin layer with the thickness of less than 5nm so as to maintain effective charge transmission.
In summary, the following problems exist in the prior art: the perovskite is less stable.
Disclosure of Invention
The technical problem to be solved by the invention is how to enhance the stability of perovskite, and therefore, a preparation method of an organic passivation film grown in situ on the surface of methylamine lead iodide is provided, namely, the preparation method of the organic passivation film grown in situ on the surface of organic-inorganic hybrid perovskite methylamine lead iodide.
In order to realize the purpose, the invention adopts the technical scheme that:
a preparation method of an organic-inorganic hybrid perovskite methylamine lead iodide surface in-situ growth organic passivation film is characterized by comprising the following steps:
a: dissolving methyl amine iodide and lead iodide in anhydrous N, N-dimethylformamide to form a bright yellow solution, adding chlorobenzene to form a white floccule precipitate, placing the white floccule precipitate on a heating table for drying until the white precipitate is completely blackened to obtain methyl amine lead iodide powder;
b: dissolving the methylamine lead iodide powder in the HI solution until black precipitates are separated out again from the HI solution, so as to obtain a supersaturated solution for in-situ preparation of the methylamine lead iodide passive film;
c: and (D) dropwise adding the supersaturated solution of the in-situ prepared methylamine lead iodide passive film obtained in the step (B) into the methylamine lead iodide powder prepared in the step (A), grinding, and then illuminating to obtain methylamine lead iodide with an organic passive film on the surface.
Specifically, the molar ratio of the methyl amine iodide to the lead iodide is 1-10.
Specifically, the illumination time is 3 to 6 hours.
Specifically, the drying temperature of the heating table is 60-80 ℃.
Specifically, 1g of methyl amine iodide and 0.5g of lead iodide are mixed, 10mL of N, N-dimethylformamide is added, then 100mL of chlorobenzene is added into the solution to obtain white precipitate, and the white precipitate is placed on a heating table to be dried until the white precipitate is completely blackened to obtain methyl amine lead iodide;
dissolving the methylamine lead iodide powder in 15mL HI solution to obtain supersaturated solution for in-situ preparation of methylamine lead iodide passive film;
and dripping 50 mu L of supersaturated solution for preparing the methylamine lead iodide passive film in situ into 100mg of methylamine lead iodide powder, grinding, and illuminating to obtain methylamine lead iodide with a passive film on the surface.
Specifically, 60 mu L of supersaturated solution for preparing the methylamine lead iodide passive film in situ is dripped into 200mg of methylamine lead iodide powder, and after grinding, illumination is carried out for 3h to obtain methylamine lead iodide with a passive film on the surface.
Specifically, 70 mu L of supersaturated solution for preparing the methylamine lead iodide passive film in situ is dripped into 300mg of methylamine lead iodide powder, and the methylamine lead iodide powder with the passive film on the surface is obtained by illumination for 3h after grinding.
Specifically, 80 μ L of the supersaturated solution for in-situ preparation of the methylamine lead iodide passivation film is dripped into 400mg of methylamine lead iodide powder, and after grinding, illumination is carried out for 3h to obtain methylamine lead iodide with a passivation film on the surface.
Specifically, 90 mu L of supersaturated solution for preparing the methylamine lead iodide passive film in situ is dripped into 500mg of methylamine lead iodide powder, and after grinding, illumination is carried out for 3h to obtain methylamine lead iodide with a passive film on the surface.
The beneficial effects of the invention are: according to the invention, a compact and continuous protective film is grown in situ on the surface of the methylamine lead iodide through a simple technical means, so that the stability of the methylamine lead iodide is effectively improved.
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FIG. 1 is a flow chart of a preparation method of an organic passive film grown in situ on the surface of organic-inorganic hybrid perovskite methylamine lead iodide
FIG. 2 is a comparison XRD pattern of 0 day and 28 days of exposure to air of methylamine lead iodide with and without protective film prepared in example 1;
Detailed Description
The invention provides a preparation method of an organic-inorganic hybrid perovskite lead methyl amine iodide surface in-situ growth organic passivation film, which comprises the following overall flow:
(1) Dissolving methyl amine iodide and lead iodide in anhydrous N, N-dimethylformamide according to a molar ratio of 1-10 to form a bright yellow solution, adding chlorobenzene, wherein the volume ratio of the bright yellow solution to the chlorobenzene is 5 to form a white flocculent precipitate, placing the white flocculent precipitate on a heating table for drying at the drying temperature of 60-80 ℃ until the white precipitate is completely blackened to obtain methyl amine lead iodide powder;
(2) Dissolving the methylamine lead iodide powder prepared in the step (1) in 2-6mL of HI solution until black precipitates are separated out again from the HI solution, so as to obtain a supersaturated solution for preparing the methylamine lead iodide passive film in situ;
(3) And (3) dropwise adding 10-60mL of supersaturated solution for preparing the methylamine lead iodide passivation film in situ obtained in the step (2) into the methylamine lead iodide powder prepared in the step (1), grinding, and then illuminating for 3-6h to obtain the methylamine lead iodide with the organic passivation film on the surface.
The present invention will be further described with reference to the following examples, but is not limited thereto.
Example 1:
(1) 1g of methyl amine iodide was weighed and mixed with 0.5g of lead iodide, and 10mL of N, N-dimethylformamide was added, and then 100mL of chlorobenzene was added to the solution to obtain a white precipitate. Placing the obtained white precipitate on a heating table for drying at the drying temperature of 70 ℃ until the white precipitate is completely blackened to obtain methylamine lead iodide;
(2) Dissolving the methylamine lead iodide black powder prepared in the step 1 in 15mL of HI solution;
(3) And (3) dropwise adding 50 mu L of the supersaturated HI solution prepared in the step (2) into 100mg of the methylamine lead iodide powder prepared in the step (1), quickly grinding, and illuminating for 3h to obtain methylamine lead iodide with a passivation film on the surface.
As shown in fig. 2, after methylamine lead iodide without protective film and methylamine lead iodide with protective film are exposed in air for 28 days, XRD contrast graph shows that methylamine lead iodide without protective film is seriously degraded after being exposed in air for 28 days; and after the methylamine lead iodide containing the protective film is exposed in the air for 28 days, the structure is not changed. It can be seen that the stability of methylamine lead iodide containing a protective film is significantly increased.
Example 2:
(1) 1g of methyliodiamide was weighed and mixed with 0.5g of lead iodide, and 10mL of N, N-dimethylformamide was added, and then 100mL of chlorobenzene was added to the solution to obtain a white precipitate. Placing the obtained white precipitate on a heating table for drying at the drying temperature of 70 ℃ until the white precipitate is completely blackened to obtain methylamine lead iodide;
(2) The methylamine lead iodide saturated HI solution was prepared as in example 1;
(3) And (3) dropwise adding 60 mu L of the supersaturated HI solution of methylamine lead iodide prepared in the step (2) into 200mg of methylamine lead iodide powder prepared in the step (1), quickly grinding, and illuminating for 3h to obtain methylamine lead iodide with a passivation film on the surface.
Example 3:
(1) 1g of methyl amine iodide was weighed and mixed with 0.5g of lead iodide, and 10mL of N, N-dimethylformamide was added, and then 100mL of chlorobenzene was added to the solution to obtain a white precipitate. Drying the obtained white precipitate on a heating table at the drying temperature of 70 ℃ until the white precipitate is completely blackened to obtain methylamine lead iodide;
(2) The methylamine lead iodide saturated HI solution was prepared as in example 1;
(3) And (3) dropwise adding 70 mu L of the supersaturated HI solution of methylamine lead iodide prepared in the step (2) into 300mg of the powder of methylamine lead iodide prepared in the step (1), quickly grinding, and illuminating for 3h to obtain the methylamine lead iodide with a passivation film on the surface.
Example 4:
(1) 1g of methyl amine iodide was weighed and mixed with 0.5g of lead iodide, and 10mL of N, N-dimethylformamide was added, and then 100mL of chlorobenzene was added to the solution to obtain a white precipitate. Placing the obtained white precipitate on a heating table for drying at the drying temperature of 70 ℃ until the white precipitate is completely blackened to obtain methylamine lead iodide;
(2) The methylamine lead iodide saturated HI solution was prepared as in example 1;
(3) And (3) dropwise adding 80 mu L of the supersaturated HI solution of methylamine lead iodide prepared in the step (2) into 400mg of the powder of methylamine lead iodide prepared in the step (1), quickly grinding, and illuminating for 3h to obtain the methylamine lead iodide with a passivation film on the surface.
Example 5:
(1) 1g of methyliodiamide was weighed and mixed with 0.5g of lead iodide, and 10mL of N, N-dimethylformamide was added, and then 100mL of chlorobenzene was added to the solution to obtain a white precipitate. Drying the obtained white precipitate on a heating table at the drying temperature of 70 ℃ until the white precipitate is completely blackened to obtain methylamine lead iodide;
(2) The methylamine lead iodide saturated HI solution was prepared as in example 1;
(3) And (3) dropwise adding 90 mu L of the supersaturated HI solution of methylamine lead iodide prepared in the step (2) into 500mg of methylamine lead iodide powder prepared in the step (1), quickly grinding, and illuminating for 3h to obtain methylamine lead iodide with a passivation film on the surface.
Claims (8)
1. A preparation method of an organic-inorganic hybrid perovskite methylamine lead iodide surface in-situ growth organic passivation film is characterized by comprising the following steps:
a: dissolving methyl amine iodide and lead iodide in anhydrous N, N-dimethylformamide to form a bright yellow solution, adding chlorobenzene to form a white floccule precipitate, placing the white floccule precipitate on a heating table for drying until the white precipitate is completely blackened to obtain methyl amine lead iodide powder;
b: dissolving the methylamine lead iodide powder in an HI solution until a black precipitate is separated out again from the HI solution to obtain a supersaturated solution for in-situ preparation of a methylamine lead iodide passive film;
c: and (D) dropwise adding the supersaturated solution of the in-situ prepared methylamine lead iodide passive film obtained in the step (B) into the methylamine lead iodide powder prepared in the step (A), grinding, and then illuminating to obtain methylamine lead iodide with an organic passive film on the surface, wherein the illumination time is 3-6 hours.
2. The preparation method of the organic-inorganic hybrid perovskite lead iodide surface in-situ growth organic passivation film as claimed in claim 1, wherein the molar ratio of the amine methyl iodide to the lead iodide is 1-10.
3. The preparation method of the organic-inorganic hybrid perovskite methylamine lead iodide surface in-situ growth organic passivation film according to claim 1, wherein the heating stage drying temperature is 60-80 ℃.
4. The preparation method of the organic-inorganic hybrid perovskite lead iodide surface in-situ growth organic passivation film as claimed in claim 1, characterized in that 1g of amine methyl iodide is mixed with 0.5g of lead iodide, 10mL of N, N-dimethylformamide is added, then 100mL of chlorobenzene is added into the solution to obtain white precipitate, and the white precipitate is placed on a heating table to be dried until the white precipitate is completely blackened to obtain the lead iodide methylamine;
dissolving the methylamine lead iodide powder in 15mL of HI solution to obtain a supersaturated solution for in-situ preparation of a methylamine lead iodide passive film;
and dripping 50 mu L of supersaturated solution for preparing the methylamine lead iodide passive film in situ into 100mg of methylamine lead iodide powder, grinding, and illuminating to obtain methylamine lead iodide with a passive film on the surface.
5. The method for preparing the organic/inorganic hybrid perovskite-type lead methylamine iodide surface in-situ grown organic passivation film according to claim 4, wherein 60 μ L of supersaturated solution of the in-situ prepared lead methylamine iodide passivation film is dripped into 200mg of the lead methylamine iodide powder, and the ground lead methylamine iodide powder with the passivation film on the surface is obtained by illumination for 3 h.
6. The preparation method of the organic-inorganic hybrid perovskite lead methyl amine iodide surface in-situ growth organic passivation film as claimed in claim 4, characterized in that 70 μ L of supersaturated solution of the in-situ preparation lead methyl amine iodide passivation film is dripped into 300mg of the lead methyl amine iodide powder, and the ground lead methyl amine iodide powder is irradiated by light for 3h to obtain the lead methyl amine iodide with the passivation film on the surface.
7. The preparation method of the organic-inorganic hybrid perovskite lead methyl amine iodide surface in-situ growth organic passivation film as claimed in claim 4, characterized in that 80 μ L of supersaturated solution of the in-situ preparation lead methyl amine iodide passivation film is dripped into 400mg of the lead methyl amine iodide powder, and the ground lead methyl amine iodide powder is irradiated by light for 3h to obtain the lead methyl amine iodide with the passivation film on the surface.
8. The method for preparing the organic passive film on the surface of the organic-inorganic hybrid perovskite lead methyl amine iodide as claimed in claim 4, wherein 90 μ L of supersaturated solution of the in-situ prepared lead methyl amine iodide passive film is dripped into 500mg of the lead methyl amine iodide powder, and the ground lead methyl amine iodide powder is irradiated for 3h to obtain the lead methyl amine iodide with the passive film on the surface.
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| CN103440988A (en) * | 2013-07-22 | 2013-12-11 | 华侨大学 | Preparation method of hybridization solar battery for perovskite-like sensitized photoanode |
| CN110776906A (en) * | 2019-10-25 | 2020-02-11 | 华南理工大学 | Perovskite thin film with stable photoluminescence efficiency and preparation method thereof |
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| CN105489778B (en) * | 2015-11-10 | 2018-05-01 | 南昌大学 | A kind of method that methylamine lead iodine perovskite thin film is prepared based on yellow acid lead source |
| US11203817B2 (en) * | 2017-06-30 | 2021-12-21 | Uchicago Argonne, Llc | One-step in situ solution growth for lead halide perovskite |
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| CN103440988A (en) * | 2013-07-22 | 2013-12-11 | 华侨大学 | Preparation method of hybridization solar battery for perovskite-like sensitized photoanode |
| CN110776906A (en) * | 2019-10-25 | 2020-02-11 | 华南理工大学 | Perovskite thin film with stable photoluminescence efficiency and preparation method thereof |
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| Remarkably Enhanced Hydrogen Generation of Organolead Halide Perovskites via Piezocatalysis and Photocatalysis;Mengye Wang，etal;《Adv. Energy Mater.》;20190820;正文Abstract-Experimental Section、supporting information * |
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