Preparation method of novel chiral perovskite C8H32Cl7InN4 single crystal material

Abstract

The invention relates to a preparation method of a novel chiral perovskite C8H32Cl7InN4 single crystal material. The preparation method comprises the following steps: (a) dissolving indium chloride, dimethyl ammonium chloride, oleylamine and oleic acid in dimethyl sulfoxide to form a first solution; (b) adding concentrated hydrochloric acid and absolute ethyl alcohol into the first solution to form a second solution; (c) filtering the second solution, adding the filtered second solution into a beaker, sealing the beaker with a preservative film, leaving a small amount of gaps, and finally placing the beaker at a constant temperature for reaction; and after the reaction is finished, removing the redundant solution in the beaker, cleaning with chlorobenzene for multiple times, and drying to obtain the novel titanium ore single crystal material formed at the bottom of the growth vessel. The size of the synthesized novel chiral perovskite C8H32Cl7InN4 single crystal material can reach 4 cm.

Description

Technical Field

[0001] The present invention belongs to the field of perovskite materials, and relates to a perovskite single crystal material, and specifically relates to a novel chiral perovskite C8H 32 Preparation method of Cl7InN4 single crystal material. Background Art

[0002] Perovskite single crystal materials have attracted widespread attention due to their excellent physical and chemical properties, especially showing great application potential in the field of optoelectronics. Perovskite is a class of compounds characterized by an ABX3 structure, where A and B are different cations and X is an anion. This type of material has been widely studied since the 1950s. Its unique crystal structure gives it advantages such as good light absorption ability, high carrier mobility and adjustable band gap. In photovoltaic cells, perovskite materials are gradually replacing traditional silicon-based materials due to their lower production cost and higher photoelectric conversion efficiency.

[0003] In recent years, with the continuous progress of the synthesis technology of perovskite materials, its application prospects in optoelectronic devices have become increasingly broad. In addition, this type of material also has excellent thermal stability and moisture resistance, which further enhances its competitiveness in practical applications. In the future, perovskite single crystal materials are expected to achieve greater breakthroughs in solar cells, LEDs, lasers and other fields, making important contributions to the development of renewable energy and high-efficiency optoelectronic devices. Summary of the invention

[0004] The purpose of this invention is to discover and synthesize a new chiral perovskite C8H 32 Cl7InN4 single crystal material.

[0005] In order to achieve the above object, the technical solution adopted by the present invention is: a new chiral perovskite C8H 32 The preparation method of Cl7InN4 single crystal material comprises the following steps:

[0006] (a) dissolving indium chloride, dimethyl ammonium chloride, oleylamine and oleic acid in dimethyl sulfoxide to form a first solution; the molar ratio of the indium chloride to the dimethyl ammonium chloride is 1:(0.5-4), and the concentration of the dimethyl sulfoxide is >98%;

[0007] (b) adding concentrated hydrochloric acid and anhydrous ethanol to the first solution to form a second solution;

[0008] (c) filtering the second solution and adding it into a beaker, sealing the beaker with plastic wrap and leaving a small amount of space, and finally placing the beaker at a constant temperature for reaction; after the reaction is completed, removing the solution in the beaker, washing the product with chlorobenzene for multiple times, and drying to obtain the novel chiral perovskite single crystal material.

[0009] Preferably, in step (a), the concentration of indium chloride is 0.1M to 1M.

[0010] Preferably, in step (a), the volume ratio of the oleylamine to the oleic acid is 1:(0.1-9), and the total volume of the oleylamine and the oleic acid accounts for less than 30% of the volume of the second solution.

[0011] Preferably, in step (b), the volume ratio of the concentrated hydrochloric acid to the second solution is 5% to 50%, and the initial concentration is 10% to 37%.

[0012] Preferably, in step (b), the volume ratio of the anhydrous ethanol to the second solution is 5% to 80%, and the initial concentration is >99%.

[0013] Preferably, in step (c), the constant temperature required for the reaction is 70-120°C.

[0014] Preferably, in step (c), the reaction time is 160 to 504 hours.

[0015] Preferably, in step (c), the single crystal material is placed in a vacuum drying oven and dried at 30-50°C.

[0016] Using the above technical solution, the novel chiral perovskite C8H synthesized by the present invention 32 The size of Cl7InN4 single crystal material can reach 4cm. At the same time, the shape of the single crystal is a regular parallelogram, which can meet the needs of further device processing. Moreover, the growth of this new type of single crystal has low requirements for growth conditions. In theory, as long as the synthesis conditions proposed by the present invention are followed, this new chiral perovskite C8H 32 Cl7InN4 single crystal material. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 The novel chiral perovskite C8H 32 Sample photo of Cl7InN4 single crystal material;

[0018] Figure 2 The novel chiral perovskite C8H 32 Schematic diagram of the single crystal diffraction structure of Cl7InN4 single crystal material;

[0019] Figure 3 The new chiral perovskite C8H prepared in Example 1 32 X-ray diffraction (XRD) pattern of Cl7InN4 single crystal material;

[0020] Figure 4 The new chiral perovskite C8H prepared in Example 1 32Absorption spectrum of Cl7InN4 single crystal material;

[0021] Figure 5 The new chiral perovskite C8H prepared in Example 1 32 Thermogravimetric image of Cl7InN4 single crystal material;

[0022] Figure 6 The new chiral perovskite C8H prepared in Example 1 32 Photoluminescence spectrum (PL) of Cl7InN4 single crystal material;

[0023] Figure 7 These are digital camera photos of the products in Comparative Examples 1 to 4; DETAILED DESCRIPTION

[0024] The present invention discloses a novel chiral perovskite C8H 32 The preparation method of Cl7InN4 single crystal material comprises the following steps:

[0025] (a) dissolving indium chloride, dimethylammonium chloride, oleylamine and oleic acid in dimethyl sulfoxide to form a first solution; the molar ratio of the indium chloride to the dimethylammonium chloride is 1:(0.5-4), and the concentration of the dimethyl sulfoxide is >98%; (b) adding concentrated hydrochloric acid and anhydrous ethanol to the first solution to form a second solution; (c) filtering the second solution and adding it to a beaker, sealing the beaker with plastic wrap and leaving a small amount of space, and finally placing the beaker at a constant temperature for reaction; after the reaction is completed, removing the solution in the beaker, and washing the product with chlorobenzene for multiple times, and drying to obtain the novel chiral perovskite single crystal material.

[0026] In step (a), the concentration of indium chloride is 0.1M to 1M; the volume ratio of oleylamine to oleic acid is 1:(0.1 to 9), and the total volume of oleylamine and oleic acid accounts for less than 30% of the volume ratio of the second solution. In step (b), the volume ratio of concentrated hydrochloric acid to the second solution is 5% to 50%, and the initial concentration is 10% to 37%; the volume ratio of anhydrous ethanol to the second solution is 5% to 80%, and the initial concentration is >99%. In step (c), the constant temperature required for the reaction is 70 to 120°C; the reaction time is 160 to 504 hours; the single crystal material is placed in a vacuum drying oven and dried at 30 to 50°C.

[0027] In order to better explain the present invention and facilitate understanding of the technical solution of the present invention, the present invention is further described below in conjunction with the accompanying drawings and specific embodiments.

[0028] Example 1

[0029] This embodiment provides a new chiral perovskite C8H 32The preparation method of Cl7InN4 single crystal material comprises the following steps:

[0030] (a) dissolving 0.5 M indium chloride, 2 M methylamine chloride, 1 ml of 5% oleylamine and 1 ml of 5% oleic acid in 20 ml of dimethyl sulfoxide to form a first solution;

[0031] (b) adding 6 ml of 37% concentrated hydrochloric acid and 4 ml of 99.9% anhydrous ethanol to the first solution to form a second solution;

[0032] (c) The second solution was filtered and added to a glass beaker, which was sealed with plastic wrap with a small amount of space left, and the beaker was placed at a constant temperature of 80°C for reaction; after 168 hours, the reaction was completed and a single crystal was formed at the bottom of the beaker, the excess solution in the beaker was removed, and the single crystal was washed twice with chlorobenzene, and finally the single crystal was placed in a vacuum drying oven at 40°C for 2 hours. The optical image of the obtained product is shown in FIG. Figure 1 Its XRD, absorption spectrum, thermogravimetric and PL diagrams are shown in Figure 3 , Figure 4 , Figure 5 , Figure 6 shown.

[0033] Example 2

[0034] The conditions used in this embodiment are as follows: the molar concentrations of indium chloride and methylamine chloride in step (a) are 1 M and 4 M, and other conditions not mentioned are the same as those in Example 1. The size of the obtained product is about 3 cm.

[0035] Example 3

[0036] The conditions used in this embodiment are as follows: the molar concentrations of indium chloride and methylamine chloride in step (a) are 0.1 M and 0.05 M, and other conditions not mentioned are the same as those in Example 1. The size of the obtained product is about 0.5 cm.

[0037] Example 4

[0038] The conditions used in this example are as follows: 3 ml of 5% oleic acid and 3 ml of 5% oleylamine were added in step (a), and other details not mentioned were the same as those in Example 1. The size of the obtained product was about 1 cm.

[0039] Example 5

[0040] The conditions used in this example are as follows: 6 ml of 37% concentrated hydrochloric acid and 6 ml of 99.9% anhydrous ethanol were added in step (b), and other details not mentioned were the same as those in Example 1. The size of the obtained product was about 3.6 cm.

[0041] Example 6

[0042] The conditions used in this example are as follows: 6.7 ml of 37% concentrated hydrochloric acid and 10.7 ml of 99.9% anhydrous ethanol were added in step (b), and other details not mentioned were the same as those in Example 1. The size of the obtained product was about 3.5 cm.

[0043] Example 7

[0044] The conditions used in this example are: the constant growth temperature in step (c) is 70° C., and other conditions not mentioned are the same as those in Example 1. The size of the obtained product is about 3.8 cm.

[0045] Example 8

[0046] The conditions used in this example are: the constant growth temperature in step (c) is 100° C., and other conditions not mentioned are the same as those in Example 1. The size of the obtained product is about 1.5 cm.

[0047] Comparative Example 1

[0048] The conditions used in this comparative example are: oleic acid and oleylamine are not added in step (a), and other matters not mentioned are consistent with those in Example 1, and the obtained product is random small particles, rather than bulk perovskite single crystals. Figure 7 As shown in a.

[0049] Comparative Example 2

[0050] The conditions used in this comparative example are: no concentrated hydrochloric acid is added in step (b), and the other parts not mentioned are the same as those in Example 1. The obtained product is random small particles, rather than bulk perovskite single crystals. Figure 7 As shown in b.

[0051] Comparative Example 3

[0052] The conditions used in this comparative example are: no anhydrous ethanol is added in step (b), and the other parts not mentioned are the same as those in Example 1. The obtained product is random small particles, rather than bulk perovskite single crystals. Figure 7 As shown in c.

[0053] Comparative Example 4

[0054] The conditions used in this comparative example are: no heating reaction is performed in step (c), and the reaction is performed only at room temperature. Other matters not mentioned are consistent with those in Example 1. The obtained product is random small particles, rather than bulk perovskite single crystals. Figure 7 As shown in d.

[0055] The present invention illustrates the detailed process equipment and process flow of the present invention through embodiments, but the present invention is not limited by the embodiments, that is, it does not mean that the present invention must rely on the above detailed process equipment and process flow to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of various raw materials of the product of the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

Claims

1. A new chiral perovskite C8H 32 The preparation method of Cl7InN4 single crystal material is characterized in that: The following steps are involved: (a) dissolving indium chloride, dimethyl ammonium chloride, oleylamine and oleic acid in dimethyl sulfoxide to form a first solution; the molar ratio of the indium chloride to the dimethyl ammonium chloride is 1:(0.5-4), and the concentration of the dimethyl sulfoxide is >98%; (b) adding concentrated hydrochloric acid and anhydrous ethanol to the first solution to form a second solution; (c) filtering the second solution and adding it into a beaker, sealing the beaker with plastic wrap and leaving a small amount of space, and finally placing the beaker at a constant temperature for reaction; after the reaction is completed, removing the solution in the beaker, washing the product with chlorobenzene for multiple times, and drying to obtain the novel chiral perovskite single crystal material.

2. The novel chiral perovskite C8H according to claim 1 32 The preparation method of Cl7InN4 single crystal material is characterized by: In step (a), the concentration of indium chloride is 0.1M to 1M.

3. The novel chiral perovskite C8H according to claim 1 32 The preparation method of Cl7InN4 single crystal material is characterized by: In step (a), the volume ratio of the oleylamine to the oleic acid is 1:(0.1-9), and the total volume of the oleylamine and the oleic acid accounts for less than 30% of the volume of the second solution.

4. The novel chiral perovskite C8H according to claim 3 32 The preparation method of Cl7InN4 single crystal material is characterized by: In step (b), the volume ratio of the concentrated hydrochloric acid to the second solution is 5% to 50%, and the initial concentration is 10% to 37%.

5. The novel chiral perovskite C8H according to claim 1 32 The preparation method of Cl7InN4 single crystal material is characterized by: In step (b), the volume ratio of the anhydrous ethanol to the second solution is 5% to 80%, and the initial concentration is >99%.

6. The novel chiral perovskite C8H according to claim 1 32 The preparation method of Cl7InN4 single crystal material is characterized by: In step (c), the constant temperature required for the reaction is 70-120°C.

7. The novel chiral perovskite C8H according to claim 1 32 The preparation method of Cl7InN4 single crystal material is characterized by: In step (c), the reaction time is 160 to 504 hours.

8. The novel chiral perovskite C8H according to claim 1 32 The preparation method of Cl7InN4 single crystal material is characterized by: In step (c), the single crystal material is placed in a vacuum drying oven at 30-50° C. for drying.

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