Perovskite quantum dot quantum composite film coating process

Abstract

The invention relates to the technical field of photoelectric material processing, and discloses a perovskite quantum dot quantum composite film coating process which comprises the following steps: step 1, preparing raw materials to synthesize perovskite quantum dots, and preparing a composite film stock solution through a solvothermal method; 2, adding a composite material into the stock solution, and mixing; 3, a solvothermal method is used in the mixing process, temperature control is carried out, the temperature ranges from 150 DEG C to 250 DEG C, and a perovskite quantum solution is obtained after treatment; 4, dripping the solution on a substrate, and uniformly distributing the solution through rotation to form a film; 5, the coated film needs to be subjected to heat treatment; and 6, after heat treatment, coating work of the perovskite quantum dot quantum composite film is completed. By adding the polymer substrate material, oxidation and hydrolysis reactions are slowed down, so that the environmental stability of the material is improved, and the polymer substrate material can also provide a physical barrier for the quantum dots to prevent the influence of external factors on the perovskite quantum dots.

Description

Technical Field

[0001] The present invention relates to the technical field of optoelectronic material processing, and particularly to a coating process for a perovskite quantum dot quantum composite film. Background Art

[0002] Perovskite quantum dots are a type of nanomaterial based on the perovskite structure and have excellent optoelectronic properties. Perovskite is a class of materials with a specific crystal structure (ABX3 type structure), and perovskite quantum dots are quantum dots prepared from materials with this structure at the nanoscale, usually showing strong quantum effects and excellent optoelectronic properties. The perovskite quantum dot quantum composite film is a thin film material composed of perovskite quantum dots and other materials, and this film material has wide applications in the fields of optoelectronics, optics, electronics, etc., especially in technologies such as solar cells, optoelectronic sensors, light-emitting diodes (LEDs), and lasers.

[0003] A coating process for a perovskite quantum dot quantum composite film refers to a technology that uses perovskite quantum dots and other materials to form a composite material and coats it on the surface of a substrate. In the operation of the perovskite quantum dot quantum composite film coating process in the prior art, the perovskite quantum dots may be affected by external factors, resulting in a situation where the coating process affects the quality. Summary of the Invention

[0004] In view of the deficiencies of the prior art, the present invention provides a coating process for a perovskite quantum dot quantum composite film, which solves the problem of the coating quality being affected by external factors during the coating work.

[0005] To achieve the above object, the present invention is realized through the following technical solutions: A coating process for a perovskite quantum dot quantum composite film, comprising the following steps: Step 1: Prepare materials to synthesize perovskite quantum dots, and prepare a composite film stock solution by a solvothermal method; Step 2: Add a composite material to the stock solution and mix; Step 3: Use the solvothermal method during the mixing process and control the temperature, the temperature is 150°C to 250°C, and a perovskite quantum solution is obtained after treatment; Step 4: Drop the solution on a substrate and rotate it to make the solution evenly distributed to form a film; Step 5: The coated film needs to be heat-treated; Step 6: After heat treatment, the coating work of the perovskite quantum dot quantum composite film is completed.

[0006] Preferably, the raw materials in Step 1 are twenty parts of a precursor, forty parts of a solvent, and forty parts of a surface modifier.

[0007] Preferably, the composite material in step two is polyethylene terephthalate, and the ratio to the raw material is 10:1.

[0008] Preferably, the low-temperature synthesis temperature in the solvothermal method of step three is: 150°C to 180°C.

[0009] Preferably, the medium-temperature synthesis temperature in the solvothermal method of step three is: 180°C to 220°C.

[0010] Preferably, the high-temperature synthesis temperature in the solvothermal method of step three is: 220°C to 250°C.

[0011] Preferably, the rotations in step four are low speed, medium speed, and high speed respectively. The low speed is 500 rpm to 1500 rpm per minute.

[0012] Preferably, the medium speed is 2000 rpm to 4000 rpm per minute.

[0013] Preferably, the high speed is 10000 rpm per minute.

[0014] Preferably, the heat treatment in step five is an annealing process. The annealing process is soft baking, with a temperature of 90°C to 110°C, a time of 1 min to 3 min, and a rotation speed of 1500 rpm.

[0015] The present invention provides a coating process for a perovskite quantum dot quantum composite film. It has the following beneficial effects: 1. By adding a polymer substrate material, the present invention can effectively encapsulate perovskite quantum dots in a stable environment, slow down oxidation and hydrolysis reactions, thereby improving the environmental stability of the material. The polymer substrate material can also provide a physical barrier for the quantum dots to prevent the influence of external factors (such as ultraviolet rays, moisture, oxygen) on the perovskite quantum dots, enabling the composite film to achieve better use effects.

[0016] 2. By adding titanium dioxide or zinc oxide to the stock solution and compounding with perovskite quantum dots, these inorganic materials can improve the photoconductivity, stability, and charge separation efficiency of the film. When adding silicon nanoparticles or silicon thin films, the optical properties of the film can be improved, and silicon can play a role in enhancing light absorption and energy conversion efficiency.

[0017] 3. By using low-temperature synthesis in the solvothermal method to reach a temperature of 150°C to 180°C, smaller and more uniform quantum dots can be obtained. By using high-temperature synthesis in the solvothermal method to reach a temperature of 220°C to 250°C, faster-forming and larger perovskite quantum dots can be obtained.

[0018] 4. The present invention forms a thin film by rotation. Different rotation speeds can be used according to different situations to achieve different thicknesses of use. Compared with conventional knife coating, it can be more uniform and faster. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 It is a step diagram of the present invention. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0020] The technical solutions of the present invention will be clearly and completely described below with reference to the drawings of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0021] Please refer to the attached Figure 1 , the embodiment of the present invention provides a perovskite quantum dot quantum composite film coating process, including the following steps: Step 1: Prepare raw materials to synthesize perovskite quantum dots, and prepare a composite film stock solution by a solvothermal method; Step 2: Add a composite material to the stock solution and mix; Step 3: Use the solvothermal method during the mixing process and control the temperature, the temperature is 150°C to 250°C, and a perovskite quantum solution is obtained after treatment; Step 4: Drop the solution on a substrate, and make the solution evenly distributed to form a thin film by rotation; Step 5: The coated film needs to be heat-treated; Step 6: Complete the coating work of the perovskite quantum dot quantum composite film after heat treatment.

[0022] Specifically, first, the synthesis materials of perovskite quantum dots need to be prepared. Perovskite quantum dots are usually made by mixing a precursor with a metal perovskite structure with a solvent and a surface modifier. When using the solvothermal method for synthesis, the precursor generally includes metal salts and organic amines, the solvent is a polar solvent, such as dimethyl sulfoxide amide (DMSO), methyl ether, etc., and the surface modifier helps the surface treatment of quantum dots to improve their stability and dispersibility. The advantage of the solvothermal method is that it can synthesize uniform and narrow-sized perovskite quantum dots at a relatively high temperature. At this time, it is necessary to ensure that the temperature and reaction time are suitable for the reaction conditions of different precursors.

[0023] The raw materials in Step 1 are twenty parts of precursor, forty parts of solvent, and forty parts of surface modifier. The precursor is a lead precursor and a halide, and the ratio of the lead precursor to the halide is 1:1. The solvent is dimethyl sulfoxide or dimethylformamide, and the surface modifier is stearic acid or dodecyltrimethylammonium chloride.

[0024] Specifically, the combination of lead precursors and halides can produce perovskite materials with high light absorption efficiency and low electron-hole recombination rate, thereby improving the photoelectric conversion efficiency of solar cells. Dimethyl sulfoxide and dimethylformamide have good solubility, chemical reaction medium and biological application effects. Stearic acid mainly improves the dispersibility, stability and thermal stability of materials through its hydrophobic and lipophilic properties, and is suitable for occasions where the hydrophobicity of materials needs to be increased or the compatibility needs to be enhanced. As a surface modifier, dodecyltrimethylammonium chloride can improve the dispersibility, stability and hydrophilicity of materials, and at the same time can provide additional charge stability and antibacterial properties, and is particularly suitable for water-based systems and applications that require enhanced surface charge stability.

[0025] When the composite material in Step 2 is a polymer substrate material, polyethylene terephthalate or polyacrylonitrile is used, and the ratio to the raw material is 10:1. When the composite material in Step 2 is a semiconductor material, zinc oxide or titanium dioxide is used, and the ratio to the raw material is 10:1. When the composite material in Step 2 is a silicon-based material, silicon nanoparticles or silicon thin films are used, and the ratio to the raw material is 10:1.

[0026] Specifically, when using polyethylene terephthalate and polyacrylonitrile for the composite material, the advantages of these two materials can be utilized. Polyethylene terephthalate itself has good mechanical strength and wear resistance, while polyacrylonitrile is a polymer with excellent properties, having high rigidity and strength. Combining the two can improve the overall mechanical properties of the composite material, making it more outstanding in terms of bearing capacity, impact resistance and tensile resistance. Zinc oxide as a filler can improve the strength, hardness and wear resistance of the material. Titanium dioxide can enhance the mechanical properties of the composite material, and in addition to having ultraviolet absorption and antibacterial properties, it also has photocatalytic and environmental purification capabilities. Adding silicon nanoparticles can enhance the hardness, strength and toughness of the material, and the silicon thin film has good heat resistance and can withstand high temperatures. Adding the silicon thin film to the composite material can significantly improve the high-temperature resistance of the composite material.

[0027] The low-temperature synthesis temperature in the solvothermal method of Step 3 is: 150°C to 180°C, the medium-temperature synthesis temperature in the solvothermal method of Step 3 is: 180°C to 220°C, and the high-temperature synthesis temperature in the solvothermal method of Step 3 is: 220°C to 250°C.

[0028] Specifically, in this step, the mixed solution needs to be subjected to solvothermal treatment. The specific temperature is divided into three stages to promote the interaction between the composite material and perovskite quantum dots and control the film-forming performance of the film. The low-temperature synthesis temperature is 150°C to 180°C. This temperature helps the preliminary reaction of the precursor and promotes the initial growth of perovskite quantum dots. The medium-temperature synthesis temperature is 180°C to 220°C. At this time, the reaction accelerates, which helps to generate quantum dots with appropriate sizes. The high-temperature synthesis temperature is 220°C to 250°C. In this stage, the perovskite quantum dots will complete the final crystal growth, and at the same time improve the uniformity and stability of the film. This process requires strict temperature control to ensure that the reactions in each stage can proceed stably and ensure that the synthesized quantum dots have the required sizes and distributions.

[0029] In step four, the rotations are low speed, medium speed, and high speed respectively. The low speed is 500 rpm to 1500 rpm per minute, the medium speed is 2000 rpm to 4000 rpm per minute, and the high speed is 10,000 rpm per minute.

[0030] Specifically, by different rotation speeds, the coating thickness required for different products can be adjusted. When the low speed is used, thicker coating work can be carried out on the product; through the medium speed, more uniform and conventional coating work can be carried out; through the high speed, thinner coating work can be carried out on the product, which is suitable for more precise products. The treated perovskite quantum dot composite solution is evenly dropped onto the surface of the substrate to form a film on the substrate. In this process, the thickness and uniformity of the film are controlled by spin coating technology. Using a low speed (500 rpm to 1500 rpm) can help the liquid spread evenly; using a medium speed (2000 rpm to 4000 rpm) helps to further coat evenly; while a high speed (10,000 rpm) can ensure that the film is formed in a short time and reaches the required film thickness and uniformity.

[0031] The heat treatment in step five is an annealing process. The annealing process is soft baking, with a temperature of 90°C to 110°C, a time of 1 minute to 3 minutes, and a rotation speed of 1500 rpm.

[0032] Specifically, the coated film needs to be heat-treated, usually using an annealing process. The annealing process can help optimize the perovskite quantum dot crystals and stabilize the film structure. Soft baking is a milder annealing process, with the temperature controlled between 90°C and 110°C and the time set from 1 minute to 3 minutes. During the annealing process, the substrate rotation speed can be maintained at 1500 rpm to dissipate heat evenly and ensure the integrity of the film layer. This process can effectively improve the surface quality, stability of the film, and optimize its optical properties, avoiding damage to the film structure due to overheating. After the annealing treatment, the preparation of the perovskite quantum dot quantum composite film is completed. At this time, the mechanical properties, optical properties, and stability of the film have been significantly improved. The composite film not only exhibits excellent optical properties but also has good performance in electronic properties and thermal stability, and can be widely used in optoelectronic devices, solar cells, and other electronic devices.

[0033] Example 1: Using a polymer substrate material as a composite material to prepare a perovskite quantum dot quantum composite film Select raw materials: Perovskite quantum dot synthesis materials: twenty parts of precursors, forty parts of solvent (DMSO), and forty parts of surface modifier (stearic acid); Prepare the composite film stock solution: Mix the perovskite quantum dot solution with polyethylene terephthalate to obtain the composite film stock solution; Composite material: The ratio of polyethylene terephthalate to perovskite quantum dots is 10:1.

[0034] Temperature-controlled solvothermal treatment: Use solvothermal method at 150°C to 250°C (low temperature 150°C - 180°C, medium temperature 180°C - 220°C, high temperature 220°C - 250°C) to heat-treat the mixed solution to promote the growth and stability of perovskite quantum dots; Coat the film: Through spin coating technology, first evenly coat the solution on the substrate surface at a low rotation speed (500 rpm - 1500 rpm); Annealing treatment: Perform soft baking annealing on the coated film, with the temperature at 90°C - 110°C, the time at 1 minute to 3 minutes, and the rotation speed at 1500 rpm; Complete the preparation: The heat-treated perovskite quantum dot quantum composite film has a stable structure, smooth surface, and excellent optical and electronic properties.

[0035] Example 2: Using a semiconductor material as a composite material to prepare a perovskite quantum dot quantum composite film Select raw materials: Perovskite quantum dot synthesis materials: twenty parts of precursors, forty parts of solvent (DMSO), and forty parts of surface modifier (dodecyltrimethylammonium chloride).

[0036] Composite material: The ratio of zinc oxide to perovskite quantum dots is 10:1.

[0037] Synthesis of perovskite quantum dots: According to the selected precursors (lead precursors and halides), perovskite quantum dots are synthesized by solvothermal method using DMSO and dodecyltrimethylammonium chloride.

[0038] Preparation of composite membrane stock solution: The synthesized perovskite quantum dot solution is mixed with zinc oxide to obtain the composite membrane stock solution.

[0039] Temperature-controlled solvothermal treatment: In the solvothermal treatment from low temperature (150°C - 180°C) to high temperature (220°C - 250°C), the interaction between the composite material and perovskite quantum dots is promoted.

[0040] Coating the film: Coating operation is carried out at medium speed (2000 rpm - 4000 rpm) to ensure the uniformity of the film.

[0041] Annealing treatment: The annealing temperature is 100°C, the time is set to 2 minutes, and the rotation speed is maintained at 1500 rpm.

[0042] Completion of preparation: After annealing, the obtained perovskite quantum dot quantum composite membrane has high mechanical strength, hardness, and exhibits good photocatalytic performance.

[0043] Example 3: Using silicon-based materials as composite materials to prepare perovskite quantum dot quantum composite membranes Select raw materials: Perovskite quantum dot synthesis materials: Twenty parts of precursors, forty parts of solvent (DMSO), and forty parts of surface modifier (stearic acid).

[0044] Composite material: The ratio of silicon nanoparticles to perovskite quantum dots is 10:1.

[0045] Synthesis of perovskite quantum dots: By solvothermal method, lead precursors, halides, dimethyl sulfoxide, and stearic acid are mixed to synthesize perovskite quantum dots.

[0046] Preparation of composite membrane stock solution: The synthesized perovskite quantum dot solution is mixed with silicon nanoparticles to obtain the composite membrane stock solution.

[0047] Temperature-controlled solvothermal treatment: Through the solvothermal method at 150°C - 250°C, the temperature is regulated to promote the combination between the composite material and perovskite quantum dots.

[0048] Coating the film: The film is coated at high speed (10000 rpm) to ensure the uniformity and thinness of the film, which is suitable for precision electronic devices.

[0049] Annealing treatment: The soft baking annealing process is adopted, with a temperature of 90 °C, a time set to 1 minute, and the rotation speed maintained at 1500 rpm.

[0050] Completion of preparation: The perovskite quantum dot quantum composite film obtained after annealing has high thermal stability, strength and toughness, and is suitable for applications in high-temperature environments; Sample PLQY (%) Td (°C) Young's modulus (GPa) Hardness (GPa) Carrier mobility (cm² / V·s) Example 1 (polymer substrate: PET) 92 280 3.5 0.15 5.2 Example 2 (semiconductor substrate: ZnO) 85 320 8.2 0.35 12.8 Example 3 (silicon-based substrate: Si NPs) 88 400 10.5 0.50 8.5 Comparative example (traditional pure perovskite film) 78 220 1.2 0.05 2.1 Summary description: Example 1: Polyethylene terephthalate is used as the composite material. The film structure is stable, the surface is smooth, and it has excellent optical and electronic properties.

[0051] Example 2: Zinc oxide is used as the composite material, which has high mechanical strength, hardness and good photocatalytic performance.

[0052] Example 3: Silicon nanoparticles are used as the composite material, which has high thermal stability, strength and toughness, and is suitable for high-temperature environments.

[0053] Compared with the comparative example (traditional pure perovskite thin film), the three examples are superior in terms of performance indicators such as photoluminescence quantum yield (PLQY), decomposition temperature (Td), Young's modulus, hardness, carrier mobility, etc., which reflects the effectiveness of the coating process and the introduction of the composite material.

[0054] Although the embodiments of the present invention have been shown and described, for those of ordinary skill in the art, it can be understood that various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principles and spirit of the present invention. The scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A coating process for a perovskite quantum dot quantum composite film, characterized in that: It includes the following steps: Step 1: Prepare raw materials to synthesize perovskite quantum dots, and prepare a composite film stock solution by solvothermal method; Step 2: Add a composite material to the stock solution and mix; Step 3: Use the solvothermal method during the mixing process and control the temperature, the temperature is 150°C - 250°C, and a perovskite quantum solution is obtained after treatment; Step 4: Drop the solution on the substrate and rotate it to make the solution evenly distributed to form a film; Step 5: The coated film needs to be heat-treated; Step 6: After heat treatment, the coating work of the perovskite quantum dot quantum composite film is completed.

2. The perovskite quantum dot quantum composite film coating process according to claim 1, characterized in that: The raw materials in Step 1 are twenty parts of precursor, forty parts of solvent and forty parts of surface modifier.

3. The perovskite quantum dot quantum composite film coating process according to claim 2, characterized in that: The precursor is a lead precursor and a halide, the ratio of the lead precursor to the halide is 1:1, the solvent is dimethyl sulfoxide or dimethylformamide, and the surface modifier is stearic acid or dodecyltrimethylammonium chloride.

4. A perovskite quantum dot quantum composite film coating process according to claim 1, characterized in that: When the composite material in Step 2 is a polymer substrate material, polyethylene terephthalate or polyacrylonitrile is used, and the ratio to the raw materials is 10:

1.

5. A perovskite quantum dot quantum composite film coating process according to claim 1, characterized in that: When the composite material in Step 2 is a semiconductor material, zinc oxide or titanium dioxide is used, and the ratio to the raw materials is 10:

1.

6. A perovskite quantum dot quantum composite film coating process according to claim 1, characterized in that: When the composite material in Step 2 is a silicon-based material, silicon nanoparticles or a silicon thin film is used, and the ratio to the raw materials is 10:

1.

7. A perovskite quantum dot quantum composite film coating process according to claim 1, characterized in that: The low-temperature synthesis temperature in the solvothermal method of Step 3 is: 150°C - 180°C, the medium-temperature synthesis temperature in the solvothermal method of Step 3 is: 180°C - 220°C, and the high-temperature synthesis temperature in the solvothermal method of Step 3 is: 220°C - 250°C.

8. A perovskite quantum dot quantum composite film coating process according to claim 7, characterized in that: The rotations in Step 4 are low speed, medium speed and high speed respectively. The low speed is 500 rpm - 1500 rpm per minute, the medium speed is 2000 rpm - 4000 rpm per minute, and the high speed is 10000 rpm per minute.

9. A perovskite quantum dot quantum composite film coating process according to claim 7, characterized in that: The heat treatment in Step 5 is an annealing process. The annealing process is soft baking, the temperature is 90°C - 110°C, the time is 1 min - 3 min, and the rotation speed is 1500 rpm.

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