阅读说明：本技术 界面结构可控银纳米颗粒/纳米金刚石复合材料及制备方法 (Interface structure controllable silver nanoparticle/nano diamond composite material and preparation method thereof ) 是由 苏丽霞 刘子凡 周恺 郝好山 王远 于 2020-12-10 设计创作，主要内容包括：本发明提供了一种界面结构可控银纳米颗粒/纳米金刚石复合材料及制备方法,包括以下步骤：(1)纳米金刚石在空气气氛中热处理；(2)将步骤(1)热处理后的纳米金刚石进行酸处理；(3)将步骤(2)酸处理后的纳米金刚石与SOCl-2和二甲基甲酰胺混合,加热回流处理,冷却至室温、离心沉淀；(4)将步骤(3)得到的沉淀物用四氢呋喃清洗,真空干燥,得到氯化金刚石；(5)将氯化金刚石加入到AgNO-3水溶液中,紫外灯辐照得到银纳米颗粒/纳米金刚石复合材料。(The invention provides a silver nanoparticle/nano-diamond composite material with a controllable interface structure and a preparation method thereof, wherein the preparation method comprises the following steps: (1) heat treatment of the nano-diamond in air atmosphere; (2) after the heat treatment of the step (1)Performing acid treatment on the nano-diamond; (3) the nano-diamond treated by the acid in the step (2) and SOCl 2 Mixing with dimethylformamide, heating and refluxing, cooling to room temperature, and centrifuging to precipitate; (4) washing the precipitate obtained in the step (3) with tetrahydrofuran, and drying in vacuum to obtain chlorinated diamond; (5) adding chlorinated diamond to AgNO 3 In the water solution, the silver nanoparticle/nano-diamond composite material is obtained by ultraviolet lamp irradiation.)

1. The preparation method of the interface structure controllable silver nanoparticle/nano diamond composite material is characterized by comprising the following steps:

(1) heat treatment of the nano-diamond in air atmosphere;

(2) carrying out acid treatment on the nano-diamond subjected to the heat treatment in the step (1);

(3) the nano-diamond treated by the acid in the step (2) and SOCl₂Mixing with dimethylformamide, heating and refluxing, cooling to room temperature, and centrifuging to precipitate;

(4) washing the precipitate obtained in the step (3) with tetrahydrofuran, and drying in vacuum to obtain chlorinated diamond;

(5) adding chlorinated diamond to AgNO₃In the water solution, the silver nanoparticle/nano-diamond composite material is obtained by ultraviolet lamp irradiation.

2. The method for preparing the interface structure controllable silver nanoparticle/nanodiamond composite material according to claim 1, characterized in that: in the step (1), the size of the nano-diamond is 5 nm, the heat treatment temperature is 420-.

3. The method for preparing the interface structure controllable silver nanoparticle/nanodiamond composite material according to claim 1, characterized in that: in the step (2), the acid is hydrochloric acid with the mass fraction of 35-50%, the acid treatment temperature is 80-90 ℃, and the ultrasonic treatment is carried out for 12-48 h.

4. The method for preparing the interface structure controllable silver nanoparticle/nanodiamond composite material according to claim 1, characterized in that: the reflux temperature in the step (3) is 65-80 ℃, and the treatment time is 20-48 h.

5. The method for preparing the interface structure controllable silver nanoparticle/nanodiamond composite material according to claim 1, characterized in that: AgNO in the step (5)₃The concentration of the aqueous solution is 0.5-4.0 mg/ml, and the diamond chloride and the AgNO are mixed₃The mass-volume ratio of the aqueous solution is 1: 5.

6. the method for preparing the interface structure controllable silver nanoparticle/nanodiamond composite material according to claim 1, characterized in that: and (5) irradiating for 10 min under an ultraviolet lamp of 365 nm.

7. A silver nanoparticle/nanodiamond composite material produced by the production method according to any one of claims 1 to 6.

Technical Field

The invention relates to the technical field of photocatalytic materials, in particular to a silver nanoparticle/nano-diamond composite material with a controllable interface structure and a preparation method thereof.

Background

At present, nano materials are rapidly developed, particularly, the nano composite materials integrate the advantages of various materials, and have better application prospects in the fields of catalysis, sensors, biological imaging, medical diagnosis and the like. The interface structure and the appearance of the composite material, so that the controllable preparation of the nano composite material is favored by extensive researchers. However, developing simple protocols to synthesize multicomponent nanocomposites has been a challenge. At present, several novel nanocomposite structures such as core-shell nanostructures, segmented nanowires, coated nanoparticles, and anisotropic structured nanomaterials are reported in succession. These studies have been focused on developing nano-heterojunction materials with unique structures, but there are still more challenges to precisely control the nano-interface structure and thus regulate certain specific properties thereof. At present, although the nano-diamond (ND) and the silver (Ag) are successfully synthesized, the Ag is mostly randomly deposited on the ND surface, so the interface structure is uncontrollable, and the properties and the repeatability of the prepared composite material are not ideal. At present, the research of precisely controlling the interface structure of ND and Ag by a certain technical means so as to control the photoelectric property of ND and Ag is not reported yet.

Disclosure of Invention

The invention provides an interface structure controllable silver nanoparticle/nano diamond composite material and a preparation method thereof, and solves the problem that the interface structure of the existing Ag/ND composite material is uncontrollable.

The technical scheme for realizing the invention is as follows:

the preparation method of the silver nanoparticle/nano-diamond composite material with the controllable interface structure comprises the following steps:

(1) heat treatment of the nano-diamond in air atmosphere;

(2) carrying out acid treatment on the nano-diamond subjected to the heat treatment in the step (1);

(3) the nano-diamond treated by the acid in the step (2) and SOCl₂Mixing with dimethylformamide, heating and refluxing, cooling to room temperature, and centrifuging to precipitate;

(4) washing the precipitate obtained in the step (3) with tetrahydrofuran, and drying in vacuum to obtain chlorinated diamond;

(5) adding chlorinated diamond to AgNO₃In the water solution, the silver nanoparticle/nano-diamond composite material is obtained by ultraviolet lamp irradiation.

In the step (1), the size of the nano-diamond is 5 nm, the heat treatment temperature is 420-.

In the step (2), the acid is hydrochloric acid with the mass fraction of 35-50%, the acid treatment temperature is 80-90 ℃, and the ultrasonic treatment is carried out for 12-48 h.

The reflux temperature in the step (3) is 65-80 ℃, and the treatment time is 20-48 h.

AgNO in the step (5)₃The concentration of the aqueous solution is 0.5-4.0 mg/ml, and the diamond chloride and the AgNO are mixed₃The mass-volume ratio of the aqueous solution is 1: 5.

and (5) irradiating for 10 min under an ultraviolet lamp of 365 nm.

The invention has the beneficial effects that: the invention achieves the performance of the precisely controlled composite material by effectively controlling the interface structure, and provides a surface modification method to control the interface structure of Ag and ND so as to accurately control the photoelectric performance of the Ag and ND.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.

FIG. 1 is an X-ray diffraction pattern (XRD) of a sample of the present invention;

FIG. 2 is a transmission electron microscopy ("TEM") spectrum of an Ag/ND composite;

fig. 3 is an ultraviolet-visible absorption spectrum of the sample.

Detailed Description

The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.

Example 1

The preparation method of the silver nanoparticle/nano-diamond composite material with the controllable interface structure comprises the following steps:

(1) commercially available nanodiamonds (size 5 Nm) (ND) were first heat treated in an air atmosphere: keeping the temperature at 420 ℃ for 30 min, wherein the heating rate is 5 ℃/min;

(2) taking 50 mg of ND subjected to heat treatment for acid treatment, and heating 100ml of hydrochloric acid (HCl) with the mass fraction of 40% to 80-90 ℃ with ultrasonic treatment for 24 hours;

(3) 30mg of acid-treated ND was added to a solution containing 100ml of SOCl₂And 2 ml of Dimethylformamide (DMF), heating to 75 ℃ and treating for 24 h; then cooling to room temperature, centrifuging at 8000rpm, and taking the precipitate;

(4) and (3) ND chlorination: washing the precipitate with tetrahydrofuran for 3 times, and vacuum drying for 24 hr;

(5) adding 50 ml AgNO into 10mg of chlorinated ND₃In the water solution, the concentration is 2.0 mg/ml, and the solution is irradiated for 10 min under an ultraviolet lamp of 365 nm.

Fig. 1 is an X-ray diffraction pattern (XRD) of a sample, from which it is understood that characteristic diffraction peaks of both Ag and ND appear in the Ag/ND composite material. Indicating that the two are better compounded together.

FIG. 2 is a transmission electron microscopy pattern of an Ag/ND composite with the Ag and ND particles intimately bonded together.

FIG. 3 is the UV-VIS absorption spectrum of the sample, in which the absorption packet in the Ag/ND composite material at 400-500 nm is caused by the surface plasmon resonance absorption of Ag nanoparticles.

Example 2

The preparation method of the silver nanoparticle/nano-diamond composite material with the controllable interface structure comprises the following steps:

(1) commercially available nanodiamonds (size 5 Nm) (ND) were first heat treated in an air atmosphere: keeping the temperature at 430 ℃ for 50 min, wherein the heating rate is 5 ℃/min;

(2) taking 50 mg of ND subjected to heat treatment for acid treatment, and heating 100ml of hydrochloric acid (HCl) with the mass fraction of 35% to 85 ℃ with ultrasonic treatment for 12 hours;

(3) 30mg of acid-treated ND was added to a solution containing 100ml of SOCl₂And 2 ml of Dimethylformamide (DMF), heating to 65 ℃ and treating for 20 h; then cooling to room temperature, centrifuging at 8000rpm, and taking the precipitate;

(4) and (3) ND chlorination: washing the precipitate with tetrahydrofuran for 2 times, and vacuum drying for 12 hr;

(5) adding 50 ml AgNO into 10mg of chlorinated ND₃In water solution, the concentration is 0.5.0 mg/ml, and the solution is irradiated for 10 min under 365 nm ultraviolet lamp.

Example 3

The preparation method of the silver nanoparticle/nano-diamond composite material with the controllable interface structure comprises the following steps:

(1) commercially available nanodiamonds (size 5 Nm) (ND) were first heat treated in an air atmosphere: keeping the temperature at 435 ℃ for 60 min, wherein the heating rate is 5 ℃/min;

(2) taking 50 mg of ND subjected to heat treatment for acid treatment, heating 100ml of hydrochloric acid (HCl) with the mass fraction of 50% to 90 ℃, and carrying out ultrasonic treatment for 48 hours;

(3) taking 30mg of ND which is treated by acid,adding a solution containing 100ml of SOCl₂And 2 ml of Dimethylformamide (DMF), heated to 80 ℃ for 48 treatment); then cooling to room temperature, centrifuging at 8000rpm, and taking the precipitate;

(4) and (3) ND chlorination: washing the precipitate with tetrahydrofuran for 5 times, and vacuum drying for 48 hr;

(5) adding 50 ml AgNO into 10mg of chlorinated ND₃In the water solution, the concentration is 4.0 mg/ml, and the solution is irradiated for 10 min under an ultraviolet lamp of 365 nm.

The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.