Zinc oxide nanoflower with high uniformity and preparation method thereof
Zinc oxide nanoflowers were prepared by a hydrothermal method using the synergistic effect of monoethanolamine and hexadecyltrimethylammonium bromide. This method solved the problems of uneven morphology, poor dispersibility, and complex process, achieving high uniformity and good dispersibility, reducing costs, and improving reproducibility.
Patent Information
- Application Number
- CN202511800548.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-02
- Publication Date
- 2026-02-10
AI Technical Summary
Existing methods for synthesizing zinc oxide nanoflowers suffer from problems such as uneven morphology, poor dispersibility, complex processes, high costs, and poor reproducibility.
Zinc oxide nanoflowers were prepared via a hydrothermal reaction using monoethanolamine and hexadecyltrimethylammonium bromide. The process included preparing a precursor mixture solution, hydrothermal reaction, and post-treatment steps. The process parameters were optimized to obtain nanoflowers with uniform morphology and good dispersibility.
The preparation of zinc oxide nanoflowers with high uniformity and good dispersibility was achieved. The process is simple, low-cost and highly reproducible.
Smart Images
Figure CN121494047A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of nanomaterials technology, and particularly relates to a zinc oxide nanoflower with high uniformity and its preparation method. Background Technology
[0002] Zinc oxide nanoflowers, due to their large specific surface area and unique optical and electrical properties, have broad application prospects in sensors, photocatalysis, solar cells, piezoelectric devices, and other fields. Currently, the main methods for synthesizing zinc oxide nanoflowers include hydrothermal / solvothermal methods. However, existing methods often face the following problems: 1. Uneven morphology: The product often contains other morphologies (such as rod-shaped or granular), or there are large differences in the size and petal thickness of the nanoflowers.
[0003] Second, poor dispersibility: the product is prone to agglomeration, which affects its performance.
[0004] 3. Complex process or high cost: The preparation process requires the use of expensive template agents, complex multi-step reactions, harsh conditions or high-temperature calcination to remove the template.
[0005] IV. Poor reproducibility: The process parameters are highly sensitive, and there are large batch-to-batch differences.
[0006] Therefore, there is an urgent need for a zinc oxide nanoflower with high uniformity and its preparation method to solve the above problems. Summary of the Invention
[0007] To overcome the shortcomings of the prior art, this invention provides a zinc oxide nanoflower with high uniformity and its preparation method. This invention utilizes the synergistic effect of monoethanolamine (MEA) and hexadecyltrimethylammonium bromide (CTAB) to prepare zinc oxide nanoflowers with uniform morphology and good dispersibility.
[0008] To achieve one of the above objectives, the present invention adopts the following technical solution: A method for preparing zinc oxide nanoflowers with high uniformity, the specific steps of which are as follows: S1. Preparation of precursor mixed solution: Dissolve zinc source, monoethanolamine and cationic surfactant in water, stir and mix evenly at room temperature to form precursor mixed solution; S2. Hydrothermal reaction: Transfer the precursor mixture solution to a hydrothermal reactor, seal it, and react at 140℃-180℃ for 6-14 hours. S3. Post-processing: After the hydrothermal reaction, the hydrothermal reactor is naturally cooled to room temperature. The reaction product is then removed and successively centrifuged, washed, and dried to obtain zinc oxide nanoflowers.
[0009] Preferably, the zinc source is zinc acetate (such as zinc acetate dihydrate).
[0010] Preferably, the cationic surfactant is hexadecyltrimethylammonium bromide.
[0011] Preferably, the amount of zinc source is 0.1-0.5g, the amount of monoethanolamine is 3-7ml, the amount of cationic surfactant is 0.05-0.15g, and the amount of water is 20-200ml.
[0012] Preferably, the washing process involves alternating between deionized water and anhydrous ethanol for at least three washes to thoroughly remove residual reactant ions and organic reagents.
[0013] Preferably, the drying is vacuum drying, the drying temperature is 50℃-80℃, and the drying time is 6-24 hours.
[0014] Preferably, in step S1, the raw materials are stirred in a magnetic stirrer and continuously stirred at a speed of 500 rpm for 60 minutes at room temperature (25±2℃).
[0015] Preferably, in step S2, the precursor mixture solution is transferred to a high-pressure reactor with a 100ml volume and a polytetrafluoroethylene liner, and then the high-pressure reactor is placed in an oven and heated to 160℃ at a heating rate of 2-5℃ / min, and reacted at 160℃ for 10 hours.
[0016] To achieve the second objective mentioned above, the present invention provides a zinc oxide nanoflower with high uniformity, wherein the zinc oxide nanoflower has a uniform three-dimensional flower-like structure.
[0017] Preferably, the diameter of the zinc oxide nanoflower is 2.3-2.7 nm.
[0018] The advantages of this invention are: This invention utilizes the synergistic effect of monoethanolamine (MEA) and hexadecyltrimethylammonium bromide (CTAB) to prepare zinc oxide nanoflowers with high selectivity and high uniformity, resulting in a product with uniform morphology and good dispersibility. The process is simple, mild, low-cost, and highly reproducible. Attached Figure Description
[0019] Figure 1 This is an FESEM image of zinc oxide prepared in Example 1 of the present invention.
[0020] Figure 2 for Figure 1 A magnified view of a portion of the image.
[0021] Figure 3 This is a particle size distribution chart of zinc oxide according to the present invention.
[0022] Figure 4 FESEM image of zinc oxide prepared for Comparative Example 1. Detailed Implementation
[0023] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to the accompanying drawings and embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of this invention without creative effort are within the scope of protection of this invention.
[0024] Example 1
[0025] S1. Preparation of precursor mixed solution: Accurately weigh 0.3g of zinc acetate dihydrate (Zn(CH3COO)2·2H2O, purity ≥99%), measure 5ml of monoethanolamine (HOCH2CH2NH2, purity ≥99%) and 0.1g of hexadecyltrimethylammonium bromide (CH3(CH2)). 15 N + (CH3)3Br - Add the (purity ≥ 99%) to 60ml of deionized water.
[0026] S2. Stirring and mixing: Place the above mixture on a magnetic stirrer and stir continuously at 500 rpm for 60 minutes at room temperature (25±2℃) until a homogeneous, clear or slightly turbid precursor mixture solution is formed.
[0027] S3. Hydrothermal reaction: Transfer the precursor mixture solution to a 100ml polytetrafluoroethylene-lined high-pressure reactor and seal it. Then place the high-pressure reactor in an oven and heat it to 160℃ at a rate of 2-5℃ / min, and maintain the temperature at 160℃ for 10 hours.
[0028] S4. Post-processing: Cooling: After the reaction is complete, close the oven and allow the high-pressure reactor to cool naturally to room temperature inside the oven (approximately 3-5 hours).
[0029] Collect the precipitate: Open the high-pressure reactor, transfer the reaction product to a centrifuge tube, centrifuge at 8000 rpm for 5 minutes, and discard the supernatant.
[0030] Washing: Wash the precipitate three times alternately with deionized water and anhydrous ethanol (centrifuge at 8000 rpm for 5 minutes) to thoroughly remove residual reactant ions (such as CH3COO). - , Br - ) and organic reagents (MEA, CTAB).
[0031] Drying: Transfer the washed precipitate to a vacuum drying oven and dry at 60°C for 12 hours to obtain a white powdery product, which is the target product - zinc oxide nanoflowers.
[0032] S5. Characterize the target product: such as Figure 1-2 As shown, field emission scanning electron microscopy (FESEM) revealed that the obtained product exhibited a highly uniform flower-like structure; Figure 3 As shown, the average diameter of the nanoflowers is approximately 2.5 μm ± 200 nm, and more than 95% of the products exhibit a complete three-dimensional flower-like morphology.
[0033] Comparative Example 1
[0034] S1. Preparation of precursor mixed solution: Accurately weigh 0.3g of zinc acetate dihydrate (Zn(CH3COO)2·2H2O, purity ≥99%), 0.3g of urea (CO(NH2)2, purity ≥99%), and 0.1g of hexadecyltrimethylammonium bromide (CH3(CH2)). 15 N + (CH3)3Br - Add the (purity ≥ 99%) to 60ml of deionized water.
[0035] S2. Stirring and mixing: Place the above mixture on a magnetic stirrer and stir continuously at 500 rpm for 60 minutes at room temperature (25±2℃) until a homogeneous and transparent solution is formed.
[0036] S3. Hydrothermal reaction: Transfer the mixed solution to a 100ml polytetrafluoroethylene-lined high-pressure reactor and seal it. Place the high-pressure reactor in an oven and heat it to 160℃ at a rate of 2-5℃ / min, then maintain the temperature at 160℃ for 10 hours.
[0037] S4. Post-processing: Cooling: After the reaction is complete, close the oven and allow the high-pressure reactor to cool naturally to room temperature inside the oven (approximately 3-5 hours). Collect the precipitate: Open the high-pressure reactor, transfer the reaction product to a centrifuge tube, and centrifuge at 8000 rpm for 5 minutes; Washing: Wash the precipitate three times alternately with deionized water and anhydrous ethanol (centrifuge at 8000 rpm for 5 minutes); Drying: Transfer the washed precipitate to a vacuum drying oven and dry at 60°C for 12 hours to obtain a white powder product.
[0038] S5. Characterize the white powder product: such as Figure 4 As shown, field emission scanning electron microscopy (FESEM) observation revealed that the obtained product had an irregular granular structure, exhibited extensive agglomeration, and lacked a uniform three-dimensional flower-like morphology. Compared with Example 1, the product lacked high homogeneity and had poor dispersibility.
[0039] The above are merely preferred embodiments of the present invention and are not intended to limit the scope of the invention. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention should be included within the protection scope of the present invention.
Claims
1. A method for preparing zinc oxide nanoflowers with high uniformity, characterized in that, The specific steps are as follows: S1. Preparation of precursor mixed solution: Dissolve zinc source, monoethanolamine and cationic surfactant in water, stir and mix evenly at room temperature to form precursor mixed solution; S2, Hydrothermal reaction: The precursor mixture solution is transferred to a hydrothermal reactor and reacted at 140℃-180℃ for 6-14 hours; S3. Post-processing: After the hydrothermal reaction, the hydrothermal reactor is naturally cooled to room temperature. The reaction product is then removed and successively centrifuged, washed, and dried to obtain zinc oxide nanoflowers.
2. The method for preparing zinc oxide nanoflowers with high uniformity according to claim 1, characterized in that: The zinc source is zinc acetate.
3. The method for preparing zinc oxide nanoflowers with high uniformity according to claim 1, characterized in that: The cationic surfactant is hexadecyltrimethylammonium bromide.
4. The method for preparing zinc oxide nanoflowers with high uniformity according to claim 1, characterized in that: The amount of zinc source used is 0.1-0.5g, the amount of monoethanolamine used is 3-7ml, the amount of cationic surfactant used is 0.05-0.15g, and the amount of water used is 20-200ml.
5. The method for preparing zinc oxide nanoflowers with high uniformity according to claim 1, characterized in that: The washing process involves alternating between deionized water and anhydrous ethanol for at least three washes.
6. The method for preparing zinc oxide nanoflowers with high uniformity according to claim 1, characterized in that: The drying process is vacuum drying, with a drying temperature of 50℃-80℃ and a drying time of 6-24 hours.
7. The method for preparing zinc oxide nanoflowers with high uniformity according to claim 1, characterized in that: In step S1, the raw materials are stirred in a magnetic stirrer and continuously stirred at 500 rpm for 60 minutes at room temperature (25±2℃).
8. The method for preparing zinc oxide nanoflowers with high uniformity according to claim 1, characterized in that: In step S2, the precursor mixture solution is transferred to a 100ml polytetrafluoroethylene-lined high-pressure reactor, and then the high-pressure reactor is placed in an oven and heated to 160℃ at a heating rate of 2-5℃ / min, and reacted at 160℃ for 10 hours.
9. Zinc oxide nanoflowers prepared by the method for preparing zinc oxide nanoflowers with high uniformity as described in any one of claims 1-8, characterized in that: The zinc oxide nanoflowers exhibit a uniform three-dimensional flower-like structure.
10. The zinc oxide nanoflowers prepared by the method for preparing zinc oxide nanoflowers with high uniformity according to claim 9, characterized in that: The diameter of the zinc oxide nanoflower is 2.3-2.7 nm.