CN113695587B - Method for preparing jellyfish-shaped gold-copper heterostructure material based on seed growth method - Google Patents
Method for preparing jellyfish-shaped gold-copper heterostructure material based on seed growth method Download PDFInfo
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- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a method for preparing jellyfish-shaped gold-copper heterostructure materials based on a seed growth method, which takes gold nanoflowers with sharp tips as seeds and copper salts as copper sources in the presence of hexadecylamine, and because of huge lattice mismatch between gold and copper, the gold nanoflowers are not in the center position, copper can selectively grow along a certain side surface of the gold nanoflowers, so that the preparation of jellyfish-shaped gold-copper heterostructure materials is realized. The gold nanoflowers adopted by the invention have tips, are beneficial to enhancing local electromagnetic fields, have optical properties of copper in a visible light range, have a critical effect on overgrowth of copper on the gold nanoflowers due to CTAB concentration and copper salt concentration used in centrifugal washing when copper grows at one end of the copper, and determine the morphology of the Au-Cu nanostructure. The method is simple and easy to implement and easy to popularize, has good application prospect in surface enhanced Raman scattering, and provides a new thought for the design of the plasmon photo-thermal nanostructure.
Description
Technical Field
The invention belongs to the technical field of nanometer synthesis, and particularly relates to a method for preparing jellyfish-shaped gold-copper heterostructure materials based on a seed growth method.
Background
Metal nanostructures exhibit a number of useful properties in the art, the size, shape and composition of which can be tailored by fine tuning certain parameters. In many cases, the shape or morphology of the metal nanostructures plays the most critical role in their properties and applicability in particular applications. Changing the geometry of the nanostructured metal can significantly change its surface plasmon resonance characteristics. For nanostructures with anisotropic shapes, particularly gold nanoflowers used in the present invention, plasmonic field enhancement can be achieved, which makes them useful for Surface Enhanced Raman Scattering (SERS), sensing, imaging and photothermal therapy. Copper is an inexpensive and abundant metal, and copper has optical properties in the visible range. The nano copper material has wide application in catalysis, energy conversion, sensing and other aspects, and the shape and surface chemical control thereof are an important research field in nano copper synthesis, and are expected to realize local surface plasmon resonance displayed in a visible light region. There have been reports about the preparation of gold-copper heterostructures, but the nanostructures obtained at present have a certain symmetry, even a high degree of symmetry, and these nanostructures have drawbacks in terms of optical forces and nanomotor applications, so obtaining highly asymmetric gold-copper nanostructures is a problem to be solved.
Disclosure of Invention
The invention aims to provide a simple and general seed growth method for preparing jellyfish-shaped gold-copper heterostructure materials with high asymmetry.
Aiming at the purposes, the technical scheme adopted by the invention comprises the following steps:
1. preparation of gold nanoflowers with sharp tips
Adding Cetyl Trimethyl Ammonium Chloride (CTAC) and Cetyl Trimethyl Ammonium Bromide (CTAB) into deionized water, adding chloroauric acid, silver nitrate, concentrated hydrochloric acid and ascorbic acid, and fully stirring to obtain a growth solution; adding gold-silver alloy nano-particle solution as seeds into growth solution, standing at normal temperature for 1-3 hours, centrifugally washing twice with hexadecyl trimethyl ammonium bromide aqueous solution, and discarding supernatant to obtain gold nano-flower solution with sharp tips.
2. Preparation of jellyfish-shaped gold-copper heterostructure material
Adding Hexadecylamine (HAD) into deionized water, heating, stirring, dissolving, adding the gold nanoflower solution with sharp tips prepared in the step 1, stirring uniformly, sequentially adding copper salt and ascorbic acid, stirring uniformly again, standing the obtained mixed solution at normal temperature for 1-3 hours, centrifuging, removing the supernatant, and obtaining the jellyfish-shaped gold-copper heterostructure material.
In the step 1, the total concentration of the cetyl trimethyl ammonium chloride and the cetyl trimethyl ammonium bromide in the growth solution is preferably 20-40 g/L, and the mass ratio of the cetyl trimethyl ammonium bromide to the cetyl trimethyl ammonium chloride is preferably 1:5-10.
In the step 1, the concentration of silver nitrate in the growth solution is preferably 0.02-0.2 mmol/L, and the molar ratio of the silver nitrate to chloroauric acid, hydrochloric acid and ascorbic acid is preferably 1:3-8:150-250:5-10.
In the step 1, the molar ratio of silver to gold in the gold-silver alloy nanoparticle solution is preferably 30-50:1.
In the above step 1, the concentration of the aqueous solution of cetyltrimethylammonium bromide is preferably 0.01 to 1.5mmol/L.
In the step 1, the infrared absorption wavelength of the gold nanoflower solution with the sharp tip is 600-1000 nm.
In the step 2, hexadecylamine is preferably added to deionized water and dissolved by heating and stirring at 65 to 120 ℃.
In the step 2, the concentration of hexadecylamine in the obtained mixed solution is preferably 0.4-3.5 mg/mL, the concentration of the gold nanoflower solution with sharp tips is preferably 0.1-0.3 mL/mL, the concentration of copper salt is preferably 1-4 mmol/L, and the concentration of ascorbic acid is preferably 16-64 mmol/L.
In the above step 2, the copper salt is preferably any one of copper chloride, copper bromide, copper nitrate, and the like.
The beneficial effects of the invention are as follows:
1. in the invention, gold nanoflowers are used as seeds in the presence of hexadecylamine, copper salts are used as copper sources, and the principle that huge lattice mismatch exists between gold and copper, and asymmetric copper deposition can generate an asymmetric shape is utilized.
2. The invention provides a simple and general wet chemical method for synthesizing Au-Cu heterostructure materials with high asymmetry, the adopted gold nanoflowers have tips, which are beneficial to enhancing local electromagnetic fields, the optical property of copper is in the visible light range, the invention combines the advantages of the two, when copper grows at one end of the gold nanoflowers, CTAB concentration and copper salt concentration used in centrifugal washing play a critical role in overgrowth of copper on the gold nanoflowers, and the morphology of the Au-Cu nanostructure is determined.
3. The method is simple and easy to implement and easy to popularize, provides an alternative strategy for synthesizing the space separation hybridization nano-block of the high-efficiency electrochemical reaction, has good application prospect in surface enhanced Raman scattering, provides a new thought for the design of the plasmon photo-thermal nano-structure, and is expected to provide a plurality of new opportunities for the manufacture of novel functional materials and devices, especially in large-scale application where gold and silver are too expensive to use.
Drawings
Fig. 1 is an SEM image of gold nanoflowers.
Fig. 2 is an SEM image of the jellyfish-shaped gold-copper heterostructure material prepared in example 1.
Fig. 3 is an SEM image of the jellyfish-shaped gold-copper heterostructure material prepared in example 2.
Fig. 4 is an SEM image of the jellyfish-shaped gold-copper heterostructure material prepared in example 3.
Fig. 5 is an SEM image of the jellyfish-shaped gold-copper heterostructure material prepared in example 4.
Fig. 6 is an SEM image of the jellyfish-shaped gold-copper heterostructure material prepared in example 5.
Fig. 7 is an SEM image of the jellyfish-shaped gold-copper heterostructure material prepared in example 6.
Fig. 8 is an SEM image of the jellyfish-shaped gold-copper heterostructure material prepared in example 7.
Fig. 9 is an SEM image of the jellyfish-shaped gold-copper heterostructure material prepared in example 8.
Fig. 10 is an SEM image of the jellyfish-shaped gold-copper heterostructure material prepared in example 9.
Fig. 11 is an SEM image of the jellyfish-shaped gold-copper heterostructure material prepared in example 10.
Fig. 12 is an SEM image of the jellyfish-shaped gold-copper heterostructure material prepared in example 11.
Fig. 13 is an SEM image of the jellyfish-shaped gold-copper heterostructure material prepared in example 12.
Fig. 14 is an SEM image of the jellyfish-shaped gold-copper heterostructure material prepared in example 13.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, but the scope of the present invention is not limited to these examples.
The molar ratio of silver to gold in the gold-silver alloy nanoparticle solution described in the examples below was 40:1, which was prepared according to the method in literature "Han, q., zhang, c., gao, w., han, z., liu, t., li, c., et al (2016). Ag-Au alloy Nanoparticles: synthesis and In Situ Monitoring SERS of Plasmonic catalysts.sensors detectors B: chem.231,609-614.doi: 10.1016/j.snb.2016.03.068".
Example 1
1. Preparation of gold nanoflowers with sharp tips
0.08g CTAB and 0.56g CTAC are added into 19mL deionized water, the mixture is put into a water bath kettle at 30 ℃ and stirred uniformly, and 1mL of 10mmol/L chloroauric acid aqueous solution, 200 mu L of 10mmol/L silver nitrate aqueous solution, 33.5 mu L of 12mol/L HCl aqueous solution and 160 mu L of 100mmol/L ascorbic acid aqueous solution are sequentially added, and the mixture is stirred fully to obtain a growth solution. Then 60 mu L of gold-silver alloy nanoparticle solution is added into the growth solution to be used as seeds, after standing and growing for 3 hours at normal temperature, the gold nanoflower solution with sharp tips and infrared absorption wavelength of about 1000nm is obtained by centrifugally washing twice with 0.1mmol/L CTAB aqueous solution at a rotating speed of 3000rpm for 5min each time. As can be seen from FIG. 1, the obtained gold nanoflowers have sharp tips with particle sizes of 70-180 nm.
2. Preparation of jellyfish-shaped gold-copper heterostructure material
After 6mg of HAD and 3.5mL of deionized water are added into a glass bottle, stirring and dissolving are carried out in a water bath kettle at 85 ℃, then 1mL of gold nanoflower solution with sharp tips prepared in the step 1 is added, 50 mu L of 100mmol/L copper chloride aqueous solution and 800 mu L of 200mmol/L ascorbic acid aqueous solution are sequentially added after uniform stirring, and the mixture is stirred again and then is kept stand in the water bath at 85 ℃ for 1h. And finally, centrifuging for 5min at a rotating speed of 3000rpm, and removing the supernatant to obtain the jellyfish-shaped gold-copper heterostructure material.
Example 2
In step 2 of this example, 100. Mu.L of 100mmol/L copper chloride aqueous solution was added, and the other steps were the same as in example 1, to obtain jellyfish-shaped gold-copper heterostructure material.
Example 3
In step 2 of this example, 150. Mu.L of 100mmol/L copper chloride aqueous solution was added, and the other steps were the same as in example 1, to obtain a jellyfish-shaped gold-copper heterostructure material.
Example 4
In step 2 of this example, 2mg of HAD was added, and the other steps were the same as in example 1, to obtain a jellyfish-shaped gold-copper heterostructure material.
Example 5
In step 2 of this example, 10mg of HAD was added, and the other steps were the same as in example 1, to obtain a jellyfish-shaped gold-copper heterostructure material.
Example 6
In step 2 of this example, 12mg of HAD was added, and the other steps were the same as in example 1, to obtain a jellyfish-shaped gold-copper heterostructure material.
Example 7
In step 2 of this example, 14mg of HAD was added, and the other steps were the same as in example 1, to obtain a jellyfish-shaped gold-copper heterostructure material.
Example 8
In this example, step 1, using 0.01mmol/L CTAB aqueous solution at 3000rpm centrifugal washing two times, each time 5 minutes. Other steps were the same as in example 1, to obtain an jellyfish-shaped gold-copper heterostructure material.
Example 9
In this example, step 1, using 0.4mmol/L CTAB aqueous solution at 3000rpm centrifugal washing two times, each time 5 minutes. Other steps were the same as in example 1, to obtain an jellyfish-shaped gold-copper heterostructure material.
Example 10
In this example, step 1, using 0.8mmol/L CTAB aqueous solution at 3000rpm centrifugal washing two times, each time 5 minutes. Other steps were the same as in example 1, to obtain an jellyfish-shaped gold-copper heterostructure material.
Example 11
In this example, step 1, with 1.5mmol/L CTAB aqueous solution at 3000rpm centrifugal washing two, each time 5 minutes. Other steps were the same as in example 1, to obtain an jellyfish-shaped gold-copper heterostructure material.
Example 12
In step 2 of this example, 100. Mu.L of 100mmol/L copper bromide aqueous solution was added, and the other steps were the same as in example 1, to obtain a jellyfish-shaped gold-copper heterostructure material.
Example 13
In step 2 of this example, 100. Mu.L of 100mmol/L copper nitrate aqueous solution was added, and the other steps were the same as in example 1, to obtain a jellyfish-shaped gold-copper heterostructure material.
Scanning electron microscope characterization is carried out on jellyfish-shaped gold-copper heterostructure materials prepared in the above examples 1 to 13, and the results are shown in fig. 2 to 14. As can be seen from fig. 2 to 4, the obtained gold-copper heterostructure materials are all jellyfish-shaped, and the volume of copper in the gold-copper heterostructure materials gradually becomes larger along with the increase of the concentration of copper chloride in the growth solution, the particle length is between 140 and 260nm, and the width is between 80 and 200 nm. As can be seen from fig. 5 to 8, the gold-copper heterostructure materials obtained are all jellyfish-shaped, and as the concentration of HDA increases, the coating on the outer surface of the gold-copper heterostructure materials increases significantly because it is difficult to wash off. As can be seen from fig. 9 to 12, the obtained gold-copper heterostructure materials are all jellyfish-shaped, and the concentration of the CTAB aqueous solution used for centrifugal washing can seriously affect the morphology of the gold-copper heterostructure materials, and the higher the CTAB concentration, the worse the adhesion of copper on the gold nanoflowers. As can be seen from fig. 12-14, different copper salts can also yield similar jellyfish-shaped gold-copper heterostructure materials, but the morphology of copper can be different.
Claims (6)
1. The jellyfish-shaped gold-copper heterostructure material is characterized by being prepared by the following steps:
(1) Preparation of gold nanoflowers with sharp tips
Adding cetyltrimethylammonium chloride and cetyltrimethylammonium bromide into deionized water, adding chloroauric acid, silver nitrate, concentrated hydrochloric acid and ascorbic acid, and fully stirring to obtain a growth solution; adding gold-silver alloy nanoparticle solution as seeds into growth solution, standing at normal temperature for 1-3 hours, centrifugally washing twice with hexadecyl trimethyl ammonium bromide aqueous solution, and discarding supernatant to obtain gold nanoflower solution with sharp tips; the total concentration of the cetyl trimethyl ammonium chloride and the cetyl trimethyl ammonium bromide in the growth liquid is 20-40 g/L, and the mass ratio of the cetyl trimethyl ammonium bromide to the cetyl trimethyl ammonium chloride is 1:5-10; the concentration of the silver nitrate in the growth solution is 0.02-0.2 mmol/L, and the mol ratio of the silver nitrate to chloroauric acid, hydrochloric acid and ascorbic acid is 1:3-8:150-250:5-10;
(2) Preparation of jellyfish-shaped gold-copper heterostructure material
Adding hexadecylamine into deionized water, heating, stirring and dissolving, adding the gold nanoflower solution with sharp tips prepared in the step (1), stirring uniformly, sequentially adding copper salt and ascorbic acid, stirring uniformly again, standing the obtained mixed solution at normal temperature for 1-3 hours, centrifuging, removing the supernatant, and obtaining the jellyfish-shaped gold-copper heterostructure material; the concentration of hexadecylamine in the obtained mixed solution is 0.4-3.5 mg/mL, the concentration of gold nanoflower solution with sharp tips is 0.1-0.3 mL/mL, the concentration of copper salt is 1-4 mmol/L, and the concentration of ascorbic acid is 16-64 mmol/L.
2. The jellyfish-shaped gold-copper heterostructure material of claim 1, wherein: in the step (1), in the gold-silver alloy nanoparticle solution, the molar ratio of silver to gold is 30-50:1.
3. The jellyfish-shaped gold-copper heterostructure material of claim 1, wherein: in the step (1), the concentration of the hexadecyl trimethyl ammonium bromide aqueous solution is 0.01-1.5 mmol/L.
4. The jellyfish-shaped gold-copper heterostructure material of claim 1, wherein: in the step (1), the infrared absorption wavelength of the gold nanoflower solution with the sharp tip is 600-1000 nm.
5. The jellyfish-shaped gold-copper heterostructure material of claim 1, wherein: in the step (2), hexadecylamine is added into deionized water, and is heated, stirred and dissolved at 65-120 ℃.
6. The jellyfish-shaped gold-copper heterostructure material of claim 1, wherein: in the step (2), the copper salt is any one of copper chloride, copper bromide and copper nitrate.
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