阅读说明：本技术 C3n4量子点室温磷光材料的合成方法及产品和应用 (C3N4Synthesis method, product and application of quantum dot room temperature phosphorescent material ) 是由 刘畅 陈久存 黄孝华 于 2020-08-27 设计创作，主要内容包括：本发明公开了C<Sub>3</Sub>N<Sub>4</Sub>量子点室温磷光材料的合成方法及产品和应用,合成方法是以尿素或其它类尿素小分子为原料,在高压反应釜中进行高温固相反应,制得的产品为灰白色粉末,具有固相荧光,同时在室温条件能持续发射3～6s的肉眼可见蓝绿色磷光；其制备方法简单,不含有害金属,是一种新型的室温磷光材料；在3D打印、防伪、装饰、成像等领域具有潜在的应用价值。(The invention discloses a 3 N 4 The synthesis method comprises the steps of taking urea or other urea micromolecules as raw materials, carrying out high-temperature solid-phase reaction in a high-pressure reaction kettle, and obtaining a product which is off-white powder and has solid-phase fluorescence and can continuously emit blue-green phosphorescence for 3-6 s under the room temperature condition; the preparation method is simple, does not contain harmful metal, and is a novel room temperature phosphorescent material; the method has potential application value in the fields of 3D printing, anti-counterfeiting, decoration, imaging and the like.)

1.C₃N₄The synthesis method of the quantum dot room temperature phosphorescent material is characterized by comprising the following steps: using urea or urea-like organic matter as precursor, synthesizing by high-temp. solid-phase synthesis method, cooling, collecting powder C₃N₄Quantum dot room temperature phosphorescent material.

2. C according to claim 1₃N₄The synthesis method of the quantum dot room temperature phosphorescent material is characterized by comprising the following steps: the high-temperature solid-phase synthesis method is characterized in that the reaction is carried out for 2-3 h at the temperature of 250-300 ℃, the pressure of 4-8 MPa and the rotating speed of 500-800 rpm.

3. C according to claim 1₃N₄The synthesis method of the quantum dot room temperature phosphorescent material is characterized by comprising the following steps: the urea-like organic matter is biuret, hydroxyurea or thiourea.

4. C according to claim 1₃N₄The synthesis method of the quantum dot room temperature phosphorescent material is characterized by comprising the following steps: cooling and purification, wherein the purification comprises water washing to remove unreacted raw materials, acid washing to remove alkaline byproducts, and alcohol washing to remove other organic byproducts.

5. C according to claim 1₃N₄The synthesis method of the quantum dot room temperature phosphorescent material is characterized by comprising the following steps: and adding 0.2-0.4 g of precursor into each 1ml of reaction container.

6. C obtained by the synthesis method of any one of claims 1 to 5₃N₄The quantum dot room temperature phosphorescent material is characterized in that: the optimal excitation wavelength of the phosphorescent material is 380nm, the phosphorescence wavelength is 420nm,the phosphorescence lifetime was 69.9 ms.

7. C according to claim 6₃N₄The quantum dot room temperature phosphorescent material is characterized in that: after the phosphorescent material is irradiated by a 365nm ultraviolet lamp, the visible blue-green phosphorescence of 3-6 s can be continuously emitted by naked eyes after a light source is removed.

8. C according to claim 6 or 7₃N₄Application of quantum dot room temperature phosphorescent material in preparing luminescent material.

Technical Field

The invention relates to the field of materials, in particular to C₃N₄A synthetic method of the quantum dot room temperature phosphorescent material also relates to a product prepared by the method and application.

Background

The room temperature phosphorescent material is widely applied to the fields of organic electronics, photoelectric devices, chemical and biological detection and the like. Most of the traditional phosphorescent materials are inorganic materials containing rare earth elements, noble metal complexes and pure organic compounds. However, these materials have disadvantages of high cost, cytotoxicity, complicated preparation process, etc. In addition, many conventional phosphorescent materials have phosphorescent lifetimes of microseconds to milliseconds, and such short decay times have limited application in many areas of persistent emission.

C₃N₄Is a typical polymer semiconductor and has graphite phase carbon nitride g-C with a unique structure₃N₄Due to its good photocatalytic performance, it has become a hot spot of current research. Compared with other photocatalysts, the photocatalyst has the advantages that: can absorb visible light, has good thermal stability and chemical stability, no toxicity, rich sources and simple preparation and forming process. Derivative product thereof-C₃N₄Quantum dots as a novel fluorescent nano material have attracted extensive attention due to excellent properties, simple preparation and modification means and good biocompatibility.

Disclosure of Invention

In view of the above, an object of the present invention is to provide a compound C₃N₄The synthesis method of quantum dot room temperature phosphorescent material uses urea and other small molecule precursors as raw materials to carry out high temperature and high pressure reaction, and directly prepares C with room temperature phosphorescent property₃N₄And (4) quantum dots. The second object of the present invention is to provide C prepared by the above method₃N₄A quantum dot phosphorescent material at room temperature, C₃N₄The quantum dot-based phosphorescent material has good biocompatibility and phosphorescent performance; it is a further object of the present invention to provide C₃N₄The application of the quantum dot room temperature phosphorescent material in preparing luminescent materials is used in the fields of 3D printing, anti-counterfeiting, imaging, decoration and the like.

In order to achieve the purpose, the invention provides the following technical scheme:

C₃N₄the synthesis method of the quantum dot room temperature phosphorescent material comprises the following steps: using urea or urea-like organic matter as precursor, synthesizing by high-temp. solid-phase synthesis method, cooling, collecting powder C₃N₄Quantum dotsA room temperature phosphorescent material.

In the invention, the high-temperature solid-phase synthesis method is to react for 2-3 h at the temperature of 250-300 ℃, the pressure of 4-8 MPa and the rotating speed of 500-800 rpm.

In the invention, the urea-like organic substance is biuret, hydroxyurea or thiourea.

In the present invention, cooling is followed by purification which includes water washing to remove unreacted starting materials, acid washing to remove alkaline by-products, and alcohol washing to remove other organic by-products.

In the invention, 0.2-0.4 g of precursor is added into each 1ml of reaction container.

2. C obtained by the synthetic method₃N₄The optimal excitation wavelength of the quantum dot room temperature phosphorescent material is 380nm, the phosphorescence wavelength is 420nm, and the phosphorescence lifetime is 69.9 ms.

In the invention, after the phosphorescent material is irradiated by a 365nm ultraviolet lamp, the visible blue-green phosphorescence of 3-6 s can be continuously emitted by naked eyes after a light source is removed.

3. Said C is₃N₄Application of quantum dot room temperature phosphorescent material in preparing luminescent material.

The invention has the beneficial effects that: the invention discloses a C₃N₄The method for synthesizing the quantum dot room temperature phosphorescent material comprises the steps of taking single urea or urea-like precursor as a raw material, carrying out high-temperature and high-pressure solid-phase reaction in a high-pressure reaction kettle, and then utilizing water washing, acid washing and alcohol washing to prepare grey-white phosphorescent powder, wherein the grey-white phosphorescent powder can continuously emit blue-green phosphorescent afterglow which can be seen by naked eyes for 3-6 s at room temperature. Enriching the synthesis method of the nonmetal room-temperature phosphorescent material and expanding C₃N₄The application range of the quantum dots.

Drawings

In order to make the object, technical scheme and beneficial effect of the invention more clear, the invention provides the following drawings for explanation:

FIG. 1 shows a process for preparing a urea-based composition according to the invention₃N₄And (3) a picture of the quantum dot room temperature phosphorescent material.

FIG. 2 is C₃N₄The phenomenon of phosphorescence afterglow at room temperature of quantum dots.

FIG. 3 shows TEM test results, C₃N₄And (3) the morphological characteristics of the quantum dots.

FIG. 4 shows a schematic view of a process according to the present invention C₃N₄Fluorescence emission spectra of quantum dots.

FIG. 5 shows a schematic view of a process according to the present invention C₃N₄Fluorescence excitation spectrum of quantum dots.

FIG. 6 shows a schematic view of a process of the present invention C₃N₄Room temperature phosphorescence spectrum of quantum dots.

FIG. 7 shows a schematic view of a process according to the present invention C₃N₄Room temperature phosphorescence decay spectrum and fitted phosphorescence lifetime of quantum dots.

FIG. 8 is a UV-vis absorption spectrum (Uv-vis) in an aqueous solvent.

FIG. 9 is a Fourier transform infrared (FT-IR) spectrum.

Detailed Description

The present invention is further described with reference to the following drawings and specific examples so that those skilled in the art can better understand the present invention and can practice the present invention, but the examples are not intended to limit the present invention.