CN113210624A - Preparation method of gold nanoflowers - Google Patents
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Abstract
The invention discloses a preparation method of gold nanoflowers, belonging to the technical field of preparation of inorganic nano materials. The preparation method of the gold nanoflowers comprises the following steps: step 1: preparing gold seeds; step 2: preparing gold nanosphere colloidal solution; and step 3: preparing an Au @ PbS core-shell heterogeneous nano material aqueous solution; and 4, step 4: preparing Au/PbS/Au nano-structure solution; and 5: gold nanoflowers are prepared. The gold nanoflowers prepared by the method have the characteristics of stable structure, adjustable petal number, rich plasmon electromagnetic hot spots, excellent surface enhanced Raman scattering performance and the like, and are expected to be applied to detection of pesticide residues and viruses.
Description
Technical Field
The invention relates to a preparation method of gold nanoflowers, belonging to the technical field of preparation of inorganic nano materials.
Background
The plasmon metal nano crystal has the characteristics of excellent photon absorption, large electromagnetic field enhancement and the like, shows huge application potential in the field of surface enhanced Raman spectroscopy, and is widely applied to ultra-sensitive detection of molecules, viruses, pesticides and the like. However, the reported metal nanocrystals have single morphology and few plasmon electromagnetic hot spots, and the practical application performance of the surface enhanced raman is greatly limited. In addition, common metal nanocrystals have limited molecular adsorption capacity and have certain difficulty in detecting ultra-low concentration raman molecules.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of gold nanoflowers. The gold nanospheres are used as substrates to prepare the Au @ PbS core-shell structure, the gold nanoshells can grow on the surface of the PbS in a controllable mode, and the PbS is dissolved by hydrochloric acid to obtain the gold nanoflowers. The gold nanoflowers prepared by the method have the characteristics of stable structure, adjustable petal number, rich plasmon electromagnetic hot spots, excellent surface enhanced Raman scattering performance and the like, and are expected to be applied to detection of pesticide residues and viruses.
The technical scheme for solving the technical problems is as follows: a preparation method of gold nanoflowers comprises the following steps:
step 1: preparation of gold seeds
Taking 8ml of 0.08-0.12 mol hexadecyl trimethyl ammonium bromide solution, 500 mu l of 0.04-0.06 mmol chloroauric acid solution and 600 mu l of 0.008-0.012 mmol sodium borohydride solution, and carrying out magnetic stirring reaction to obtain gold seeds;
step 2: preparation of gold nanosphere colloidal solution
Adding 30ml of a mixed solution of 0.15-0.25 mol of hexadecyl trimethyl ammonium bromide solution, 6ml of 4-6 mmol of chloroauric acid solution and 3.5ml of 8-12 mmol of ascorbic acid solution into 40 mu l of the gold seeds obtained in the step 1, then adding 1ml of 0.8-1.2 mol of sodium hydroxide, centrifuging after reaction, taking a precipitate, and dispersing the precipitate into 40ml of deionized water to obtain a gold nanosphere colloidal solution;
and step 3: preparation of Au @ PbS core-shell heterogeneous nano material aqueous solution
Adding 1ml of 0.05-0.15 mol ascorbic acid solution, 1ml of 0.15-0.25 mol hexadecyl trimethyl ammonium bromide solution, 40 mu l of 0.08-0.12 mol thioacetamide solution, 1ml of 0.002-0.008 mol sodium hydroxide solution and 25 mu l of 0.08-0.12 mol lead nitrate solution into 5ml of the gold nanosphere colloidal solution obtained in the step 2 to obtain a second mixed solution;
packaging the second mixed solution, drying in vacuum, cooling to room temperature, centrifuging, taking out a precipitate, cleaning the precipitate with deionized water, and dispersing into 5ml of deionized water to obtain an Au @ PbS core-shell heterogeneous nano material aqueous solution;
and 4, step 4: preparation of Au/PbS/Au nanostructured solution
Adding 30 mu l of 0.008mmol-0.012mmol chloroauric acid solution, 0.5ml 0.08mol-0.12mol ascorbic acid solution and 10ml 0.04mol-0.06mol hexadecyl trimethyl ammonium bromide solution into 1ml of the Au @ PbS core-shell heterogeneous nano material aqueous solution obtained in the step 3 under the stirring state to obtain a third mixed solution;
packaging the third mixed solution, reacting at normal temperature under a stirring state, centrifuging, taking a precipitate, cleaning the precipitate with deionized water, and dispersing into 2ml of deionized water to obtain an Au/PbS/Au nano-structure solution;
and 5: preparation of gold nanoflowers
Adding 5ml of 0.15-0.25 mol of hexadecyl trimethyl ammonium bromide solution and 100 mu l of 4-6 mol of hydrochloric acid into 1ml of the Au/PbS/Au nano-structure solution obtained in the step 4 to obtain a fourth mixed solution;
packaging the fourth mixed solution, drying in vacuum, cooling to room temperature, centrifuging, and taking a precipitate; washing with deionized water and ethanol for several times, and drying to obtain the gold nanoflower.
The preparation method of the gold nanoflowers has the beneficial effects that:
1. the Au @ PbS core-shell structure is prepared by using the gold nanospheres as the substrate, the gold nanoflowers shell layers are controllably grown on the surface of the PbS, and the PbS is dissolved by using hydrochloric acid to finally obtain the gold nanoflowers.
2. The gold nanoflowers prepared by the method have the characteristics of stable structure, adjustable petal number, rich plasmon electromagnetic hot spots, excellent surface enhanced Raman scattering performance and the like, and are expected to be applied to detection of pesticide residues and viruses.
3. The gold nanoflowers are simple in preparation method, easy to operate, wide in market prospect and suitable for large-scale popularization and application.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, in the step 1, the magnetic stirring reaction time is 1.5h-2.5h, and the rotating speed is 1000 r/min.
The adoption of the further beneficial effects is as follows: by adopting the parameters, the reaction is more thorough.
Further, in the step 2, the reaction temperature is 33 ℃, and the reaction time is 0.8h-1.2 h; the rotation speed of the centrifugation is 8000 revolutions per minute, and the time is 4 minutes.
Further, in the step 3, the temperature of the vacuum drying is 85 ℃, and the time is 8 hours; the rotation speed of the centrifugation is 8000 revolutions per minute, and the time is 4 minutes.
Further, in the step 4, the rotating speed of the stirring is 1000 revolutions per minute; the reaction time is 2 h; the rotation speed of the centrifugation is 8000 revolutions per minute, and the time is 4 minutes.
Further, in the step 5, the temperature of the vacuum drying is 60 ℃, and the time is 12 hours; the rotation speed of the centrifugation is 8000 revolutions per minute, and the time is 4 minutes.
Further, in the step 5, the drying temperature is 65 ℃ and the drying time is 8 h.
Drawings
Fig. 1 is a scanning electron microscope photograph of gold nanoflowers prepared in example 1 of the present invention, and (a) to (d) are gold nanoflowers having 1 to 4 pieces of petals, respectively.
FIG. 2 is a comparison of surface Raman enhanced scattering spectra of gold nanoflowers prepared in example 1 of the present invention against rhodamine B molecules.
Detailed Description
The principles and features of this invention are described below in conjunction with the following detailed drawings, which are given by way of illustration only and are not intended to limit the scope of the invention.
Example 1
The preparation method of gold nanoflowers in the embodiment comprises the following steps:
step 1: preparation of gold seeds
Taking 8ml of 0.1mol hexadecyl trimethyl ammonium bromide solution, 500 mu l of 0.05mmol chloroauric acid solution and 600 mu l of 0.01mmol sodium borohydride solution, and carrying out magnetic stirring reaction, wherein the magnetic stirring reaction time is 1.5h, and the rotating speed is 1000 r/min, so as to obtain the gold seeds.
Step 2: preparation of gold nanosphere colloidal solution
To 40. mu.l of the gold seed obtained in step 1, 30ml of a mixed solution of 0.2mol of cetyltrimethyl ammonium bromide solution, 6ml of 5mmol of chloroauric acid solution and 3.5ml of 10mmol of ascorbic acid solution was added, followed by addition of 1ml of 1mol of sodium hydroxide, reaction at 33 ℃ for 1 hour, centrifugation at 8000 rpm for 4min, and the precipitate was dispersed in 40ml of deionized water to obtain a gold nanosphere colloidal solution.
And step 3: preparation of Au @ PbS core-shell heterogeneous nano material aqueous solution
Adding 1ml of 0.1mol ascorbic acid solution, 1ml of 0.2mol hexadecyl trimethyl ammonium bromide solution, 40 mu l of 0.1mol thioacetamide solution, 1ml of 0.005mol sodium hydroxide solution and 25 mu l of 0.1mol lead nitrate solution into 5ml of the gold nanosphere colloidal solution obtained in the step 2 to obtain a second mixed solution;
packaging the second mixed solution, and drying for 8 hours at 85 ℃ in vacuum; and then centrifuging for 4min at 8000 rpm, cooling to room temperature, centrifuging for 4min at 8000 rpm, taking the precipitate, cleaning the precipitate with deionized water, and dispersing into 5ml of deionized water to obtain the aqueous solution of the Au @ PbS core-shell heterogeneous nano material.
And 4, step 4: preparation of Au/PbS/Au nanostructured solution
Adding 30 mu l of 0.01mmol chloroauric acid solution, 0.5ml 0.1mol ascorbic acid solution and 10ml 0.05mol hexadecyl trimethyl ammonium bromide solution into 1ml of the Au @ PbS core-shell heterogeneous nano material aqueous solution obtained in the step 3 under the stirring state to obtain a third mixed solution;
and packaging the third mixed solution, reacting at normal temperature under a stirring state, centrifuging at 8000 rpm for 4min, taking out a precipitate, cleaning the precipitate with deionized water, and dispersing into 2ml of deionized water to obtain the Au/PbS/Au nano-structure solution.
And 5: preparation of gold nanoflowers
Adding 5ml of 0.2mol cetyl trimethyl ammonium bromide solution and 100 mu l of 5mol hydrochloric acid into 1ml of the Au/PbS/Au nano-structure solution obtained in the step 4 to obtain a fourth mixed solution;
packaging the fourth mixed solution, vacuum-drying at 85 deg.C for 8h, cooling to room temperature, centrifuging at 8000 rpm for 4min, and collecting precipitate; washing with deionized water and ethanol for several times, and drying at 65 deg.C for 8 hr to obtain gold nanoflower.
Scanning electron microscope results of the gold nanoflowers prepared in example 1 are shown in fig. 1.
The gold nanoflowers prepared in the embodiment 1 are subjected to rhodamine B detection, and the specific method comprises the following steps: mu.l of gold nanoflowers prepared in example 1 was taken and dropped into 2ml of 10-6And stirring the rhodamine B at the temperature of 30 ℃ for 4 hours in mol/L, dropping 20 mu L of sample on a glass slide, and drying at the temperature of 60 ℃.
Observing the Raman scattering intensity of the sample by using a Raman spectrometer; the integration time is 10s twice, the laser wavelength is 532nm, the laser intensity is 1mw, three sampling points are measured, and an average value is taken.
The surface Raman enhanced scattering spectrum contrast of rhodamine B molecules is shown in figure 2. From this, it can be seen that the surface raman signal of the gold nanoflowers prepared in example 1 is stronger than that of the gold nanospheres.
And (4) conclusion: the gold nanoflowers prepared in the embodiment 1 have the characteristics of stable structure, adjustable petal number, rich plasmon electromagnetic hot spots, excellent surface-enhanced Raman scattering performance and the like, and are expected to be applied to detection of pesticide residues and viruses.
Example 2
The preparation method of gold nanoflowers in the embodiment comprises the following steps:
step 1: preparation of gold seeds
Taking 8ml of 0.08mol cetyl trimethyl ammonium bromide solution, 500 mu l of 0.04mmol chloroauric acid solution and 600 mu l of 0.008mmol sodium borohydride solution, and carrying out magnetic stirring reaction, wherein the magnetic stirring reaction time is 1.5h, and the rotating speed is 1000 r/min, so as to obtain the gold seeds.
Step 2: preparation of gold nanosphere colloidal solution
To 40. mu.l of the gold seed obtained in step 1, 30ml of a mixed solution of 0.15mol of cetyltrimethyl ammonium bromide solution, 6ml of 4mmol of chloroauric acid solution and 3.5ml of 8mmol of ascorbic acid solution was added, followed by addition of 1ml of 0.8mol of sodium hydroxide, reaction at 33 ℃ for 1 hour, followed by centrifugation at 8000 rpm for 4 minutes, and the precipitate was dispersed in 40ml of deionized water to obtain a gold nanosphere colloidal solution.
And step 3: preparation of Au @ PbS core-shell heterogeneous nano material aqueous solution
Adding 1ml of 0.08mol ascorbic acid solution, 1ml of 0.15mol hexadecyl trimethyl ammonium bromide solution, 40 mu l of 0.08mol thioacetamide solution, 1ml of 0.004mol sodium hydroxide solution and 25 mu l of 0.08mol lead nitrate solution into 5ml of the gold nanosphere colloidal solution obtained in the step 2 to obtain a second mixed solution;
packaging the second mixed solution, and drying for 8 hours at 85 ℃ in vacuum; and then centrifuging for 4min at 8000 rpm, cooling to room temperature, centrifuging for 4min at 8000 rpm, taking the precipitate, cleaning the precipitate with deionized water, and dispersing into 5ml of deionized water to obtain the aqueous solution of the Au @ PbS core-shell heterogeneous nano material.
And 4, step 4: preparation of Au/PbS/Au nanostructured solution
Adding 30 mu l of 0.008mmol chloroauric acid solution, 0.5ml 0.08mol ascorbic acid solution and 10ml 0.04mol hexadecyl trimethyl ammonium bromide solution into 1ml of the Au @ PbS core-shell heterogeneous nano material aqueous solution obtained in the step 3 under the stirring state to obtain a third mixed solution;
and packaging the third mixed solution, reacting at normal temperature under a stirring state, centrifuging at 8000 rpm for 4min, taking out a precipitate, cleaning the precipitate with deionized water, and dispersing into 2ml of deionized water to obtain the Au/PbS/Au nano-structure solution.
And 5: preparation of gold nanoflowers
Adding 5ml of 0.15mol of hexadecyl trimethyl ammonium bromide solution and 100 mu l of 4mol of hydrochloric acid into 1ml of the Au/PbS/Au nano-structure solution obtained in the step 4 to obtain a fourth mixed solution;
packaging the fourth mixed solution, vacuum-drying at 85 deg.C for 8h, cooling to room temperature, centrifuging at 8000 rpm for 4min, and collecting precipitate; washing with deionized water and ethanol for several times, and drying at 65 deg.C for 8 hr to obtain gold nanoflower.
Example 3
The preparation method of gold nanoflowers in the embodiment comprises the following steps:
step 1: preparation of gold seeds
Taking 8ml of 0.12mol cetyl trimethyl ammonium bromide solution, 500 mu l of 0.06mmol chloroauric acid solution and 600 mu l of 0.012mmol sodium borohydride solution, and carrying out magnetic stirring reaction for 1.5h at the rotating speed of 1000 r/min to obtain the gold seeds.
Step 2: preparation of gold nanosphere colloidal solution
To 40. mu.l of the gold seed obtained in step 1, 30ml of a mixed solution of 0.25mol of cetyltrimethyl ammonium bromide solution, 6ml of 6mmol of chloroauric acid solution and 3.5ml of 12mmol of ascorbic acid solution was added, followed by addition of 1ml of 1mol of sodium hydroxide, reaction at 33 ℃ for 1 hour, centrifugation at 8000 rpm for 4min, and the precipitate was dispersed in 40ml of deionized water to obtain a gold nanosphere colloidal solution.
And step 3: preparation of Au @ PbS core-shell heterogeneous nano material aqueous solution
Adding 1ml of 0.1mol ascorbic acid solution, 1ml of 0.2mol hexadecyl trimethyl ammonium bromide solution, 40 mu l of 0.12mol thioacetamide solution, 1ml of 0.006mol sodium hydroxide solution and 25 mu l of 0.12mol lead nitrate solution into 5ml of the gold nanosphere colloidal solution obtained in the step 2 to obtain a second mixed solution;
packaging the second mixed solution, and drying for 8 hours at 85 ℃ in vacuum; and then centrifuging for 4min at 8000 rpm, cooling to room temperature, centrifuging for 4min at 8000 rpm, taking the precipitate, cleaning the precipitate with deionized water, and dispersing into 5ml of deionized water to obtain the aqueous solution of the Au @ PbS core-shell heterogeneous nano material.
And 4, step 4: preparation of Au/PbS/Au nanostructured solution
Adding 30 mu l of 0.012mmol chloroauric acid solution, 0.5ml 0.12mol ascorbic acid solution and 10ml 0.06mol hexadecyl trimethyl ammonium bromide solution into 1ml of the Au @ PbS core-shell heterogeneous nano material aqueous solution obtained in the step 3 under the stirring state to obtain a third mixed solution;
and packaging the third mixed solution, reacting at normal temperature under a stirring state, centrifuging at 8000 rpm for 4min, taking out a precipitate, cleaning the precipitate with deionized water, and dispersing into 2ml of deionized water to obtain the Au/PbS/Au nano-structure solution.
And 5: preparation of gold nanoflowers
Adding 5ml of 0.25mol of hexadecyl trimethyl ammonium bromide solution and 100 mu l of 6mol of hydrochloric acid into 1ml of the Au/PbS/Au nano-structure solution obtained in the step 4 to obtain a fourth mixed solution;
packaging the fourth mixed solution, vacuum-drying at 85 deg.C for 8h, cooling to room temperature, centrifuging at 8000 rpm for 4min, and collecting precipitate; washing with deionized water and ethanol for several times, and drying at 65 deg.C for 8 hr to obtain gold nanoflower.
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.
Claims (7)
1. The preparation method of gold nanoflowers is characterized by comprising the following steps:
step 1: preparation of gold seeds
Taking 8ml of 0.08-0.12 mol hexadecyl trimethyl ammonium bromide solution, 500 mu l of 0.04-0.06 mmol chloroauric acid solution and 600 mu l of 0.008-0.012 mmol sodium borohydride solution, and carrying out magnetic stirring reaction to obtain gold seeds;
step 2: preparation of gold nanosphere colloidal solution
Adding 30ml of a mixed solution of 0.15-0.25 mol of hexadecyl trimethyl ammonium bromide solution, 6ml of 4-6 mmol of chloroauric acid solution and 3.5ml of 8-12 mmol of ascorbic acid solution into 40 mu l of the gold seeds obtained in the step 1, then adding 1ml of 0.8-1.2 mol of sodium hydroxide, centrifuging after reaction, taking a precipitate, and dispersing the precipitate into 40ml of deionized water to obtain a gold nanosphere colloidal solution;
and step 3: preparation of Au @ PbS core-shell heterogeneous nano material aqueous solution
Adding 1ml of 0.05-0.15 mol ascorbic acid solution, 1ml of 0.15-0.25 mol hexadecyl trimethyl ammonium bromide solution, 40 mu l of 0.08-0.12 mol thioacetamide solution, 1ml of 0.002-0.008 mol sodium hydroxide solution and 25 mu l of 0.08-0.12 mol lead nitrate solution into 5ml of the gold nanosphere colloidal solution obtained in the step 2 to obtain a second mixed solution;
packaging the second mixed solution, drying in vacuum, cooling to room temperature, centrifuging, taking out a precipitate, cleaning the precipitate with deionized water, and dispersing into 5ml of deionized water to obtain an Au @ PbS core-shell heterogeneous nano material aqueous solution;
and 4, step 4: preparation of Au/PbS/Au nanostructured solution
Adding 30 mu l of 0.008mmol-0.012mmol chloroauric acid solution, 0.5ml 0.08mol-0.12mol ascorbic acid solution and 10ml 0.04mol-0.06mol hexadecyl trimethyl ammonium bromide solution into 1ml of the Au @ PbS core-shell heterogeneous nano material aqueous solution obtained in the step 3 under the stirring state to obtain a third mixed solution;
packaging the third mixed solution, reacting at normal temperature under a stirring state, centrifuging, taking a precipitate, cleaning the precipitate with deionized water, and dispersing into 2ml of deionized water to obtain an Au/PbS/Au nano-structure solution;
and 5: preparation of gold nanoflowers
Adding 5ml of 0.15-0.25 mol of hexadecyl trimethyl ammonium bromide solution and 100 mu l of 4-6 mol of hydrochloric acid into 1ml of the Au/PbS/Au nano-structure solution obtained in the step 4 to obtain a fourth mixed solution;
packaging the fourth mixed solution, drying in vacuum, cooling to room temperature, centrifuging, and taking a precipitate; washing with deionized water and ethanol for several times, and drying to obtain the gold nanoflower.
2. The method for preparing gold nanoflowers according to claim 1, wherein in the step 1, the magnetic stirring reaction time is 1.5h-2.5h, and the rotation speed is 1000 rpm.
3. The method for preparing gold nanoflowers according to claim 1, wherein in the step 2, the reaction temperature is 33 ℃ and the reaction time is 0.8-1.2 h; the rotation speed of the centrifugation is 8000 revolutions per minute, and the time is 4 minutes.
4. The preparation method of gold nanoflowers according to claim 1, wherein in step 3, the temperature of vacuum drying is 85 ℃ and the time is 8 h; the rotation speed of the centrifugation is 8000 revolutions per minute, and the time is 4 minutes.
5. The method for preparing gold nanoflowers according to claim 1, wherein in step 4, the rotation speed of the stirring is 1000 rpm; the reaction time is 2 h; the rotation speed of the centrifugation is 8000 revolutions per minute, and the time is 4 minutes.
6. The method for preparing gold nanoflowers according to claim 1, wherein in step 5, the temperature of vacuum drying is 60 ℃ and the time is 12 h; the rotation speed of the centrifugation is 8000 revolutions per minute, and the time is 4 minutes.
7. The method for preparing gold nanoflowers according to any one of claims 1 to 6, wherein in step 5, the drying temperature is 65 ℃ and the drying time is 8 hours.
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