CN111057898B

CN111057898B - Method for preparing two-dimensional bone-type gold nanosheet/graphene oxide composite material

Info

Publication number: CN111057898B
Application number: CN201911390074.XA
Authority: CN
Inventors: 李忠; 唐书钦; 罗再刚; 陈祥亭
Original assignee: Anhui University of Science and Technology
Current assignee: Anhui University of Science and Technology
Priority date: 2019-12-30
Filing date: 2019-12-30
Publication date: 2021-04-16
Anticipated expiration: 2039-12-30
Also published as: CN111057898A

Abstract

The invention relates to a method for preparing a two-dimensional bone-type gold nanosheet/graphene oxide composite material. The method comprises the following specific steps: mixing graphene oxide with a reaction solution for growing the gold nanoplatelets, carrying out ultrasonic reaction, standing at a constant temperature, and aging for a certain time. The method has the advantages of green and mild reaction conditions, simple operation and high yield. The two-dimensional bone-type gold nanosheet/graphene oxide composite material prepared by the invention has the characteristics of large specific surface area, unique gold nanosheet shape and uniform distribution, and has wide application prospects in the fields of catalysis, biosensing, medicine and the like.

Description

Method for preparing two-dimensional bone-type gold nanosheet/graphene oxide composite material

Technical Field

The invention relates to a method for preparing a two-dimensional bone-type gold nanosheet/graphene oxide composite material, and belongs to the field of nanotechnology.

Background

Gold is a chemically very stable metal element, but nano-sized gold has special physicochemical properties. Besides the small-size effect, the surface effect and the macroscopic quantum tunneling effect of common nano materials, the gold nanoparticles also have special optical properties, electrical properties and good biocompatibility, so the gold nanoparticles have good application prospects in the fields of catalysis, biosensing, medicine and the like. By controlling the morphology of the gold nanoparticles, the Surface Plasmon Resonance (SPR) signals of the gold nanoparticles can be changed to influence the optical properties, and different crystal face selectivities can be displayed, so that the gold nanoparticles with specific morphologies can be controlled and synthesized, and the method has profound significance for the application of the gold nanoparticles in the fields of catalysis, biomedicine and the like. The two-dimensional gold nano material is easy to generate irreversible agglomeration due to high surface energy, is easy to generate shape change when being used as a catalyst under the condition of gas phase or liquid phase, and the activity and the selectivity of the two-dimensional gold nano material are weakened or even disappear after being circulated for several times. Therefore, it becomes important to select a proper carrier material to achieve the effects of dispersing and stabilizing the nano material and to maintain high activity and stability in a certain service period. Due to the special structure of the graphene oxide, the graphene oxide can be well dispersed in water and organic solvents, and is large in specific surface area and good in conductivity. Meanwhile, the surface of the nano-particle is rich in carbonyl and carboxyl, which is the basis for the combination of the nano-particle. Graphene oxide is an ideal support for heterogeneous reaction catalysts. Therefore, the method for preparing the two-dimensional gold nanosheet/graphene oxide composite material with large specific surface area, uniform distribution and unique appearance is green and mild and is simple and convenient to operate, and has important significance.

Disclosure of Invention

Aiming at the requirement of the shape control synthesis of the gold nano material, the invention aims to provide a method for preparing a two-dimensional bone-type gold nano sheet/graphene oxide composite material.

The invention provides a preparation method of a two-dimensional bone-type gold nanosheet/graphene oxide composite material, which comprises the following specific steps:

(1) weighing 1mg of graphene oxide, adding the graphene oxide into 10mL of hexadecyl trimethyl ammonium bromide solution (0.1M), and performing ultrasonic dispersion for 30min at 240W; sequentially adding 250 mu L of chloroauric acid solution (0.01M) and 600 mu L of sodium borohydride solution (0.01M), carrying out 200-500W ultrasonic reaction for 20-60min, and standing at the constant temperature of 25-30 ℃ for 2-6 h;

(2) sequentially adding 90 mu L of silver nitrate solution (0.01M), 500 mu L of chloroauric acid solution (0.01M) and 55-80 mu L of ascorbic acid solution (0.1M) into 9.5mL of hexadecyl trimethyl ammonium bromide solution (0.1M), and uniformly stirring; adding 12 mu L of the solution prepared in the step (1), uniformly stirring, and standing for reaction for 1 h;

(3) and (3) centrifuging the product obtained in the step (2) at a high speed (11000rpm for 12min), removing supernatant, washing with deionized water for three times, and centrifuging and precipitating to obtain the final product.

Drawings

FIG. 1 is a transmission electron microscope image of a two-dimensional bone-type gold nanosheet/graphene oxide composite material

FIG. 2 is a high-power transmission electron microscope image of a two-dimensional bone-type gold nanosheet/graphene oxide composite material

Detailed Description

The present invention is further illustrated by the following examples.

Example 1:

(1) weighing 1mg of graphene oxide, adding the graphene oxide into 10mL of hexadecyl trimethyl ammonium bromide solution (0.1M), and performing ultrasonic dispersion for 30min at 240W; sequentially adding 250 mu L of chloroauric acid solution (0.01M) and 600 mu L of sodium borohydride solution (0.01M), carrying out ultrasonic reaction at 200W for 60min, and standing at a constant temperature of 25 ℃ for aging for 6 h;

(2) sequentially adding 90 mu L of silver nitrate solution (0.01M), 500 mu L of chloroauric acid solution (0.01M) and 60 mu L of ascorbic acid solution (0.1M) into 9.5mL of hexadecyl trimethyl ammonium bromide solution (0.1M), and uniformly stirring; adding 12 mu L of the solution prepared in the step (1), stirring uniformly, and standing for reaction for 1 h.

Fig. 1 and fig. 2 are transmission electron micrographs of the prepared two-dimensional bone-type gold nanoplatelets/graphene oxide composite material. The gold nanoplates are uniformly loaded on the surface of the graphene; the gold nanoplatelets have a length of about 50nm, a width of about 20nm and a thickness of about 5 nm.

Example 2:

(1) weighing 1mg of graphene oxide, adding the graphene oxide into 10mL of hexadecyl trimethyl ammonium bromide solution (0.1M), and performing ultrasonic dispersion for 30min at 240W; sequentially adding 250 mu L of chloroauric acid solution (0.01M) and 600 mu L of sodium borohydride solution (0.01M), carrying out ultrasonic reaction at 300W for 40min, and standing at the constant temperature of 28 ℃ for aging for 4 h;

(2) sequentially adding 90 mu L of silver nitrate solution (0.01M), 500 mu L of chloroauric acid solution (0.01M) and 55 mu L of ascorbic acid solution (0.1M) into 9.5mL of hexadecyl trimethyl ammonium bromide solution (0.1M), and uniformly stirring; adding 12 mu L of the solution prepared in the step (1), uniformly stirring, and standing for reaction for 1 h;

The results were similar to those of example 1.

Example 3:

(1) weighing 1mg of graphene oxide, adding the graphene oxide into 10mL of hexadecyl trimethyl ammonium bromide solution (0.1M), and performing ultrasonic dispersion for 30min at 240W; sequentially adding 250 mu L of chloroauric acid solution (0.01M) and 600 mu L of sodium borohydride solution (0.01M), carrying out 400W ultrasonic reaction for 20min, and standing at constant temperature of 30 ℃ for aging for 2 h;

(2) sequentially adding 90 mu L of silver nitrate solution (0.01M), 500 mu L of chloroauric acid solution (0.01M) and 70 mu L of ascorbic acid solution (0.1M) into 9.5mL of hexadecyl trimethyl ammonium bromide solution (0.1M), and uniformly stirring; adding 12 mu L of the solution prepared in the step (1), uniformly stirring, and standing for reaction for 1 h;

The results were similar to those of example 1.

Example 4:

(1) weighing 1mg of graphene oxide, adding the graphene oxide into 10mL of hexadecyl trimethyl ammonium bromide solution (0.1M), and performing ultrasonic dispersion for 30min at 240W; sequentially adding 250 mu L of chloroauric acid solution (0.01M) and 600 mu L of sodium borohydride solution (0.01M), carrying out ultrasonic reaction at 500W for 20min, and standing at the constant temperature of 28 ℃ for aging for 2 h;

(2) sequentially adding 90 mu L of silver nitrate solution (0.01M), 500 mu L of chloroauric acid solution (0.01M) and 80 mu L of ascorbic acid solution (0.1M) into 9.5mL of hexadecyl trimethyl ammonium bromide solution (0.1M), and uniformly stirring; adding 12 mu L of the solution prepared in the step (1), uniformly stirring, and standing for reaction for 1 h;

The results were similar to those of example 1.

Claims

1. A method for preparing a two-dimensional bone-type gold nanosheet/graphene oxide composite material is characterized by comprising the following specific steps:

(1) weighing 1mg of graphene oxide, adding the graphene oxide into 10mL of hexadecyl trimethyl ammonium bromide solution with the molar concentration of 0.1M, and performing 240W ultrasonic dispersion for 30 min; sequentially adding 250 mu L of chloroauric acid solution with the molar concentration of 0.01M and 600 mu L of sodium borohydride solution with the molar concentration of 0.01M, carrying out 200-500W ultrasonic reaction for 20-60min, and standing at constant temperature;

(2) sequentially adding 90 mu L of silver nitrate solution with the molar concentration of 0.01M, 500 mu L of chloroauric acid solution with the molar concentration of 0.01M and quantitative ascorbic acid solution with the molar concentration of 0.1M into 9.5mL of hexadecyl trimethyl ammonium bromide solution with the molar concentration of 0.1M, and uniformly stirring; adding 12 mu L of the solution prepared in the step (1), uniformly stirring, and standing for reaction for 1 h;

(3) and (3) centrifuging the product obtained in the step (2) at 11000rpm for 12min at a high speed, removing supernatant, washing with deionized water for three times, and centrifuging and precipitating to obtain the final product.

2. The method for preparing a two-dimensional bone-type gold nanosheet/graphene oxide composite material according to claim 1, wherein the temperature of the constant-temperature placement in step (1) is 25-30 ℃, and the reaction time is 2-6 h.

3. The method for preparing two-dimensional bone-type gold nanoplatelets/graphene oxide composite material according to claim 1, wherein the quantitative molarity of the ascorbic acid solution of 0.1M in the step (2) is 55-80 μ L.