阅读说明：本技术 一种氮化碳纳米立方体的制备方法 (Preparation method of carbon nitride nanocubes ) 是由 滕飞 郝唯一 刘喆 马奔 于 2021-03-16 设计创作，主要内容包括：本发明公开了一种氮化碳纳米立方体的制备方法。该方法包括如下步骤：(1)将三聚氰胺和三聚氰酸加入水中,室温搅拌,离心分离沉淀,烘干,烘干产物为三聚氰胺-三聚氰酸超分子；(2)将三聚氰胺-三聚氰酸超分子和氯化钾研磨均匀,煅烧,洗涤去除多余的氯化钾,烘干,即可。本发明氮化碳纳米立方体的制作方法简易,模板易去除,成本低廉,且具有均匀的纳米立方体结构。(The invention discloses a preparation method of a carbon nitride nanocube. The method comprises the following steps: (1) adding melamine and cyanuric acid into water, stirring at room temperature, centrifugally separating and precipitating, and drying to obtain melamine-cyanuric acid supramolecules; (2) uniformly grinding the melamine-cyanuric acid supermolecule and the potassium chloride, calcining, washing to remove redundant potassium chloride, and drying. The carbon nitride nanocube has the advantages of simple manufacturing method, easy removal of the template, low cost and uniform nanocube structure.)

1. A preparation method of carbon nitride nanocubes is characterized by comprising the following steps: the method comprises the following steps:

(1) adding melamine and cyanuric acid into water, stirring at room temperature, centrifugally separating and precipitating, and drying to obtain melamine-cyanuric acid supramolecules;

(2) uniformly grinding the melamine-cyanuric acid supermolecule and the potassium chloride, calcining, washing to remove redundant potassium chloride, and drying.

2. The method of preparing carbon nitride nanocubes according to claim 1, wherein: the calcination is carried out in a tubular furnace at 500-550 ℃ for 2-4 h.

3. The method of preparing carbon nitride nanocubes according to claim 1, wherein: the temperature rise speed during the calcination is 2-5 ℃/min.

4. The method of preparing carbon nitride nanocubes according to claim 1, wherein: and (3) drying in the step (2) to obtain the carbon nitride nanocube with a uniform structure.

5. The method of preparing carbon nitride nanocubes according to claim 1, wherein: the edge length of the product obtained in the step (2) is 400 nm.

Technical Field

The invention relates to a preparation method of a nano material, in particular to a preparation method of a carbon nitride nanocube.

Background

In recent years, metal-free carbon nitride (g-C)₃N₄) The semiconductor material attracts wide attention, has simple preparation process and low preparation cost, and may be prepared through direct calcination of urea, cyanamide, dicyandiamide, melamine and other nitrogen containing organic matter. g-C₃N₄High thermal and chemical stability and no poison. However, g-C₃N₄Is controlled by morphology, bulk g-C prepared by conventional pyrogenic processes₃N₄Low specific surface area, low porosity, resulting in limited performance. Reported different morphologiesg-C₃N₄In the related patent, there is a thin layer g-C invented by Jiangling et al₃N₄The preparation method and technology (CN108654668A) of the invention, the azolla and the Liu Shi Guo₃N₄Tube-in-tube preparation methods (CN108383091A) and the like, and the preparation steps of the methods are complicated, and the problems that templates are not easy to remove exist, and the appearance is similar to that of g-C in the text₃N₄Are clearly different. Thus seeking g-C₃N₄The synthesis of novel morphologies has become the focus of research. The invention reports simple synthesis of uniform cubic carbon nitride for the first time, and the literature does not report the simple synthesis.

Disclosure of Invention

The purpose of the invention is as follows: the invention aims to provide a carbon nitride nanocube with a uniform morphological structure.

The technical scheme is as follows: the invention provides a preparation method of a carbon nitride nanocube, which comprises the following steps:

(1) adding melamine and cyanuric acid into water, stirring at room temperature, centrifugally separating and precipitating, and drying to obtain melamine-cyanuric acid supramolecules;

(2) uniformly grinding the melamine-cyanuric acid supermolecule and the potassium chloride, calcining, washing to remove redundant potassium chloride, and drying.

Further, the calcination was carried out in a tube furnace at 550 ℃ for 4 hours.

Further, the temperature increase rate at the time of the calcination was 5 ℃/min.

Further, the carbon nitride nanocube obtained after drying in the step (2) has a uniform structure.

Further, the product of the step (2) has a ridge length of 400 nm.

Has the advantages that: the carbon nitride nanocube has the advantages of simple manufacturing method, easy removal of the template, low cost, uniform nanocube structure and good appearance.

Drawings

FIG. 1 shows g-C prepared in example one₃N₄Scanning Electron microscopy of nanocubes, as seen in FIG. 1, prepared in example oneg-C₃N₄Nanocubes, said cubes g-C₃N₄The specification size of (A) is as follows: a cube with a ridge length of about 400 nm;

FIG. 2 is g-C prepared in example one₃N₄X-ray diffraction pattern of nanocubes, as can be seen from FIG. 2, the sample prepared in example one has characteristic peak pairs at 13.0 ℃ and 27.4 ℃ corresponding to g-C₃N₄The (100) and (002) planes of (1).

Detailed Description

Example 1

Adding 0.01mol of melamine and 0.01mol of cyanuric acid into 50mL of water, stirring for 24 hours at room temperature, centrifugally separating precipitates, and drying at 60 ℃, wherein the dried product is melamine-cyanuric acid supermolecule. 1g of melamine-cyanuric acid supramolecules and 0.5g of potassium chloride were ground homogeneously. Calcining at 550 deg.C for 4 hr in a tubular furnace with a crucible cover at a temperature of 5 deg.C/min, washing to remove excessive potassium chloride, and oven drying to obtain g-C₃N₄A nanocube.

Example 2

Adding 0.01mol of melamine and 0.01mol of cyanuric acid into 50mL of water, stirring for 24 hours at room temperature, and directly drying at 60 ℃, wherein the dried product is melamine-cyanuric acid supermolecule. 1g of melamine-cyanuric acid supramolecules and 0.5g of potassium chloride were ground homogeneously. Calcining in a crucible with a cover at 500 deg.C for 4 hr at a heating rate of 5 deg.C/min in a tubular furnace, washing to remove excessive potassium chloride, and drying to obtain g-C₃N₄A nanocube.

Example 3

Adding 0.01mol of melamine and 0.01mol of cyanuric acid into 50mL of water, stirring for 24 hours at room temperature, centrifugally separating precipitates, and drying at 60 ℃, wherein the dried product is melamine-cyanuric acid supermolecule. 1g of melamine-cyanuric acid supramolecules and 0.5g of potassium chloride were ground homogeneously. Calcining at 550 deg.C for 2 hr in a tubular furnace with a crucible cover at a heating rate of 2 deg.C/min, washing to remove excessive potassium chloride, and oven drying to obtain g-C₃N₄A nanocube.