Controlled preparation method of three-dimensional honeycomb-structured ZnO nano-material

A technology of honeycomb structure and nanomaterials, which is applied in the field of controllable preparation of three-dimensional honeycomb structure zinc oxide nanomaterials, can solve the problem that the requirements of high-performance gas sensing and catalytic materials cannot be met, the honeycomb scale is not suitable for flexible control, and the scale of honeycomb ZnO is large and other problems, to achieve the effect of improving gas sensitivity and photocatalytic performance, strong surface activity and good stability

Active Publication Date: 2018-08-17
四川威斯顿建材有限公司
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Problems solved by technology

[0003] "Chemical Research" 2007, 18(1): 23-27 published a "Study on the Hydrothermal Synthesis and Shape Control of ZnO Microcrystals". In this paper, the hydrothermal method was used to change the concentration of the precursor at low temperature, Reaction time and reaction temperature have produced flower-shaped, honeycomb-shaped, and columnar ZnO microcrystals; however, the honeycomb-shaped ZnO prepared in this paper has a large scale and is micron-scale, which cannot meet the requirements of high-performance gas-sensing and catalytic materials.
"Journal of Chifeng University (Natural Science Edition)" 2010, 26(7): 106-107 published an article "Hydrothermal synthesis, characterization and field emission characteristics of zinc oxide nanostructures with different shapes". In this paper, the improved The hydrothermal method, by controlling the reaction solution concentration, reaction temperature and reaction time and other parameters, synthesized nanostructures such as ZnO nanorod arrays, honeycomb ZnO nanorods, and flower-like ZnO nanorods on the glass substrate; but the The honeycomb zinc oxide material prepared in the paper is a two-dimensional nano-rod interlaced structure, which has not yet formed a three-dimensional honeycomb channel structure, and has fewer reactive active sites on the surface
The Chinese invention patent application with publication number CN107321347A in 2017 discloses a preparation method of a honeycomb zinc oxide nanowall array. The method uses aluminum foil as the substrate, first sputters a seed layer on the substrate by radio frequency magnetron method, and then utilizes hydrothermal However, the honeycomb zinc oxide material prepared by this method has a micron-scale honeycomb diameter, which has a larger specific surface area and limited reactivity than nano-scale honeycombs, and the honeycomb scale is not suitable for flexibility. controllable

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Embodiment 1

[0031] A controllable preparation method of a three-dimensional honeycomb structure ZnO nanomaterial, comprising the following steps:

[0032] Step 1. Dissolve glucose in deionized water to prepare a glucose solution with a concentration of 0.5mol / L; transfer it to a hydrothermal reaction kettle and react at 180°C for 4 hours; after cooling, wash and dry at 60°C. Uniform and well-dispersed carbon nanospheres with a particle size of about 80nm were obtained; figure 2 The scanning electron micrograph of the carbon nanospheres prepared in Example 1;

[0033] Step 2. Soak the carbon nanospheres in step 1 in deionized water at a solid-to-liquid mass ratio of 1:30 to obtain a coating reaction bottom solution; adjust the pH value of the coating reaction bottom solution to 5.6 with acetic acid;

[0034] Step 3. Slowly drop 100 mL of zinc acetate solution with a concentration of 1 mol / L and dilute ammonia water with a mass concentration of 7% into the coating reaction bottom solution...

Embodiment 2

[0037] A controllable preparation method of a three-dimensional honeycomb structure ZnO nanomaterial, comprising the following steps:

[0038] Step 1. Dissolve glucose in deionized water to prepare a glucose solution with a concentration of 0.25mol / L; transfer it to a hydrothermal reaction kettle and react at 160°C for 4 hours; after cooling, wash and dry at 60°C. Uniform and well-dispersed carbon nanospheres with a particle size of about 60nm were obtained;

[0039] Step 2. Soak the carbon nanospheres in step 1 in deionized water at a solid-to-liquid mass ratio of 1:40 to obtain a coating reaction bottom solution; adjust the pH value of the coating reaction bottom solution to 6.0 with acetic acid;

[0040] Step 3. Slowly drop 100 mL of zinc acetate solution with a concentration of 0.5 mol / L and dilute ammonia water with a mass concentration of 5% into the coating reaction bottom solution in step 2 at the same time at a rate ratio of 5:1 to control the reaction pH value 6.0 a...

Embodiment 3

[0043] A controllable preparation method of a three-dimensional honeycomb structure ZnO nanomaterial, comprising the following steps:

[0044] Step 1. Dissolve sucrose in deionized water to prepare a sucrose solution with a concentration of 1mol / L; transfer it to a hydrothermal reaction kettle and react at 200°C for 5 hours; after cooling, wash and dry at 60°C to prepare Uniform and well-dispersed carbon nanospheres with a particle size of about 90nm were obtained;

[0045] Step 2. Soak the carbon nanospheres in step 1 in deionized water at a solid-to-liquid mass ratio of 1:50 to obtain a coating reaction bottom solution; adjust the pH value of the coating reaction bottom solution to 6.5 with acetic acid;

[0046] Step 3. Slowly drop 100 mL of zinc acetate solution with a concentration of 1 mol / L and dilute ammonia water with a mass concentration of 10% into the coating reaction bottom solution in step 2 at the same time at a rate ratio of 3:1, and control the reaction pH to ...

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Abstract

The invention discloses a controlled preparation method of a three-dimensional honeycomb-structured ZnO nano-material. The controlled preparation method comprises the following steps: (1) preparing nano carbon balls; (2) soaking the nano carbon balls in deionized water, and preparing a wrapping reaction base solution; and regulating pH value of the wrapping reaction base solution; (3) separately dropwise adding a zinc salt solution and an alkali solution in the wrapping reaction base solution simultaneously at a certain speed ratio, controlling the pH value of reaction and constant reaction temperature, stirring the wrapping reaction base solution, finishing reaction, and centrifuging, washing and drying to obtain a Zn(OH)2/carbon ball composite material; and (4) calcining the Zn(OH)2/carbon ball composite material to obtain the three-dimensional honeycomb-structured ZnO nano-material. The prepared three-dimensional honeycomb-structured ZnO nano-material is large in specific surface area and high in surface activity, and the gas sensitivity and photocatalytic performance of the material can be improved effectively; and the three-dimensional honeycomb-structured ZnO nano-material islow in cost, high in yield, good in stability and pollution-free, and is expected to be popularized and used in the fields of gas sensitivity and photocatalysis.

Description

technical field [0001] The invention relates to a controllable preparation method of a three-dimensional honeycomb structure zinc oxide nanometer material, belonging to the technical field of high-performance inorganic non-metallic functional materials. Background technique [0002] Zinc oxide is a high-performance semiconductor functional material with excellent catalytic, optical, magnetic and electrical properties, stable physical and chemical properties, and environmental friendliness. It is widely used in many fields such as ceramics, chemical industry, electronics, optics, and biology. Especially when the size of zinc oxide particles is at the nanometer level, the material has a large specific surface area and high surface activity, and is often used as a gas-sensing material, catalyst, etc., and plays an important role in gas monitoring and environmental governance. However, the high energy of the surface of nanoparticles leads to the easy aggregation of nano-zinc oxi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G9/02B82Y40/00
CPCB82Y40/00C01G9/02C01P2002/72C01P2004/03C01P2004/30C01P2004/64C01P2006/12
Inventor 刘海峰聂川昊吴小玉张行泉
Owner 四川威斯顿建材有限公司
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