CN111451520B - Preparation method of nanogold - Google Patents
Preparation method of nanogold Download PDFInfo
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- CN111451520B CN111451520B CN202010168975.0A CN202010168975A CN111451520B CN 111451520 B CN111451520 B CN 111451520B CN 202010168975 A CN202010168975 A CN 202010168975A CN 111451520 B CN111451520 B CN 111451520B
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
Abstract
The invention discloses a preparation method of nano-gold, belonging to the technical field of inorganic nano-material preparation. The preparation method of the nano gold comprises the following steps: step 1: preparing gold seeds; step 2: preparing a nano gold ball 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: and preparing the nano gold. The nano-gold prepared by the method has excellent performances of stable structure, adjustable size of a nano-gold shell layer, obvious plasmon coupling effect, strong surface enhanced Raman scattering signal and the like, and has important reference significance for the construction of the surface Raman reinforcing agent.
Description
Technical Field
The invention relates to a preparation method of nano-gold, belonging to the technical field of inorganic nano-material preparation.
Background
The metal nano-crystal with the plasmon optical characteristic has the characteristics of excellent photon absorption, strong local electromagnetic field and the like, and shows great application potential in the fields of surface Raman enhanced scattering and the like. Metal nanocrystals with different structures, such as nanospheres, nanorods, nano-triangles, nanostars and the like, are prepared and widely applied to surface-enhanced Raman scattering ultrasensitive detection. The plasmon coupling effect between metals is proved to have higher photon absorption efficiency and stronger local electromagnetic field enhancement effect, thereby realizing stronger surface Raman enhanced scattering signals.
The gold nanocrystals prepared by the prior art have single structure and unobvious plasmon coupling effect, so the development and preparation of novel gold nanocrystals have important significance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of nanogold. The method utilizes the nanogold ball as a substrate to prepare the Au @ PbS core-shell structure, simultaneously controllably grows a nanogold shell layer on the surface of PbS, and then utilizes hydrochloric acid to dissolve PbS, thereby finally obtaining the nanogold. The nano-gold prepared by the method has excellent performances of stable structure, adjustable size of a nano-gold shell layer, obvious plasmon coupling effect, strong surface enhanced Raman scattering signal and the like, and has important reference significance for the construction of the surface Raman reinforcing agent.
The technical scheme for solving the technical problems is as follows: a preparation method of nano gold comprises the following steps:
step 1: preparation of gold seeds
Taking 4ml of 0.15-0.25 mol hexadecyl trimethyl ammonium bromide solution, 500 mu l of 4-6 mmol chloroauric acid solution and 600 mu l of 8-12 mmol sodium borohydride solution, and carrying out magnetic stirring reaction to obtain gold seeds;
step 2: preparing nano gold ball 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 gold seeds obtained in the step 1, then adding 1ml of 0.8-1.2 mol of sodium hydroxide, centrifuging after reaction, taking precipitate, and dispersing into 40ml of deionized water to obtain nano gold sphere colloidal solution;
and step 3: preparation of Au @ PbS core-shell heterogeneous nano material aqueous solution
Adding 1ml of 0.8-1.2 mol ascorbic acid solution, 1ml of 0.15-0.25 mol hexadecyl trimethyl ammonium bromide solution, 70 mu l of 0.8-1.2 mol thioacetamide solution, 40 mu l of 0.8-1.2 mol lead nitrate solution and 1ml of 0.8-1.2 mol hexamethylenetetramine solution into 5ml of the nano gold ball colloid 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-70 mu l of 8mmol-12mmol chloroauric acid solution, 0.5ml of 0.8mol-1.2mol ascorbic acid solution and 10ml of 0.03mol-0.07mol 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 1ml of deionized water to obtain an Au/PbS/Au nano-structure solution;
and 5: preparation of nano gold
Adding 5ml of 0.15-0.25 mol of hexadecyl trimethyl ammonium bromide solution and 40 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 final product.
The principle of the preparation method of the nano-gold comprises the following steps:
lead ions grow PbS on the surface of the gold ball under the action of a surfactant, thioacetamide and an ascorbic acid solution, a nanogold shell layer grows on the surface of the PbS by a chloroauric acid solution under the action of the ascorbic acid solution, and finally the PbS is directly dissolved by hydrochloric acid to obtain nanogold.
The preparation method of the nano-gold has the following beneficial effects:
1. the method utilizes the nanogold ball as a substrate to prepare the Au @ PbS core-shell structure, simultaneously controllably grows a nanogold shell layer on the surface of PbS, and then utilizes hydrochloric acid to dissolve PbS, thereby finally obtaining the nanogold. The specific structure of the nano-gold is that the nano-gold ball is centered, a nano-gold shell layer is wrapped outside the nano-gold ball, and a nano gap is formed between the nano-gold ball and the nano-gold shell layer.
2. The nano-gold prepared by the method has excellent performances of stable structure, adjustable size of a nano-gold shell layer, obvious plasmon coupling effect, strong surface enhanced Raman scattering signal and the like, and has important reference significance for the construction of the surface Raman reinforcing agent.
3. The preparation method of the nano-gold is simple, 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 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.
Further, in step 5, the nano gold is in a gold ingot shape and comprises a nano gold ball and a nano gold shell layer, the nano gold shell layer is wrapped outside the nano gold ball, and a nano gap is formed between the nano gold shell layer and the nano gold ball.
The adoption of the further beneficial effects is as follows: the nano gold is in a gold ingot shape, has excellent performances of stable structure, adjustable size of a nano gold shell layer, obvious plasmon coupling effect, strong surface enhanced Raman scattering signal and the like, and has important reference significance for the construction of the surface Raman reinforcing agent.
Further, the size of the nanogap is 4nm ± 0.2 nm.
The adoption of the further beneficial effects is as follows: in the field of spectroscopy, the nanogap has the capability of limiting light, so that the intensity of a light field in the gap is different from that of a light source per se in magnitude, and thus, molecules to be detected in the gap can generate multiplied spectral response. And smaller nanogaps have stronger optical localization effects. In the invention, the size of the nanometer gap is less than 5nm, so that the method is more suitable for manufacturing molecular devices.
Drawings
FIG. 1 shows the SEM results of the nano-Au prepared in example 1 of the present invention;
FIG. 2 is a TEM photograph of nano-gold prepared in example 1 of the present invention;
FIG. 3 is a comparison of surface Raman-enhanced scattering spectra of the prepared nano-gold p-rhodamine 6G molecule in the invention example 1.
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 the nano gold comprises the following steps:
step 1: preparation of gold seeds
4ml of 0.2mol hexadecyl trimethyl ammonium bromide solution, 500 mu l of 5mmol chloroauric acid solution and 600 mu l of 10mmol sodium borohydride solution are taken for magnetic stirring reaction, the magnetic stirring reaction time is 1.5h, and the rotating speed is 1000 r/min, so that the gold seeds are obtained.
Step 2: preparing nano gold ball 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 nanogold gold sphere colloidal solution.
And 3, step 3: preparation of Au @ PbS core-shell heterogeneous nano material aqueous solution
To 5ml of the nanogold ball colloid solution obtained in step 2, 1ml of a 1mol ascorbic acid solution, 1ml of a 0.2mol cetyltrimethyl ammonium bromide solution, 70. mu.l of a 1mol thioacetamide solution, 40. mu.l of a 1mol lead nitrate solution, and 1ml of a 1mol hexamethylenetetramine solution were added 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 50 mu l of 10mmol chloroauric acid solution, 0.5ml of 1mol ascorbic acid solution and 10ml of 0.05mol hexadecyl trimethyl ammonium bromide solution into 1ml of 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 at 8000 rpm for 4min, taking out a precipitate, cleaning the precipitate with deionized water, and dispersing into 1ml of deionized water to obtain an Au/PbS/Au nano-structure solution;
and 5: preparation of nano gold
To 1ml of the Au/PbS/Au nanostructure solution obtained in step 4, 5ml of a 0.2mol cetyltrimethylammonium bromide solution and 40. mu.l of 5mol hydrochloric acid were added 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 nanogold.
Example 2
The preparation method of the nano gold comprises the following steps:
step 1: preparation of gold seeds
Taking 4ml of 0.15mol cetyl trimethyl ammonium bromide solution, 500 mu l of 4mmol chloroauric acid solution and 600 mu l of 8mmol sodium borohydride solution, and carrying out magnetic stirring reaction for 2h at the rotating speed of 1000 r/min to obtain the gold seeds.
Step 2: preparing nano gold ball 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 0.8h, centrifugation at 8000 rpm for 4min, and precipitation was taken and dispersed in 40ml of deionized water to obtain a nanogold sphere colloidal solution.
And step 3: preparation of Au @ PbS core-shell heterogeneous nano material aqueous solution
To 5ml of the nanogold ball colloid solution obtained in step 2, 1ml of a 0.8mol ascorbic acid solution, 1ml of a 0.15mol cetyltrimethyl ammonium bromide solution, 70. mu.l of a 0.8mol thioacetamide solution, 40. mu.l of a 0.8mol lead nitrate solution, and 1ml of a 0.8mol hexamethylenetetramine solution were added 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 8mmol chloroauric acid solution, 0.5ml 0.8mol ascorbic acid solution and 10ml 0.03mol 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 at 8000 rpm for 4min, taking out a precipitate, cleaning the precipitate with deionized water, and dispersing into 1ml of deionized water to obtain an Au/PbS/Au nano-structure solution;
and 5: preparation of nano gold
To 1ml of the Au/PbS/Au nanostructure solution obtained in step 4, 5ml of a 0.15mol cetyltrimethylammonium bromide solution and 40. mu.l of 4mol hydrochloric acid were added 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 nanogold.
Example 3
The preparation method of the nano gold comprises the following steps:
step 1: preparation of gold seeds
Taking 4ml of 0.25mol cetyl trimethyl ammonium bromide solution, 500 mu l of 6mmol chloroauric acid solution and 600 mu l of 12mmol sodium borohydride solution, and carrying out magnetic stirring reaction, wherein the magnetic stirring reaction time is 2.5h, and the rotating speed is 1000 r/min, so as to obtain the gold seeds.
Step 2: preparing nano gold ball colloid 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 1.2mol of sodium hydroxide, reaction at 33 ℃ for 1.2 hours, followed by centrifugation at 8000 rpm for 4 minutes, and the precipitate was taken and dispersed in 40ml of deionized water to obtain a nanogold gold sphere colloidal solution.
And step 3: preparation of Au @ PbS core-shell heterogeneous nano material aqueous solution
To 5ml of the nanogold ball colloid solution obtained in step 2, 1ml of a 1.2mol ascorbic acid solution, 1ml of a 0.25mol cetyltrimethyl ammonium bromide solution, 70. mu.l of a 1.2mol thioacetamide solution, 40. mu.l of a 1.2mol lead nitrate solution, and 1ml of a 1.2mol hexamethylenetetramine solution were added 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 70 mu l of 12mmol chloroauric acid solution, 0.5ml of 1.2mol ascorbic acid solution and 10ml of 0.07mol 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 at 8000 rpm for 4min, taking out a precipitate, cleaning the precipitate with deionized water, and dispersing into 1ml of deionized water to obtain an Au/PbS/Au nano-structure solution;
and 5: preparation of nano gold
To 1ml of the Au/PbS/Au nanostructure solution obtained in step 4, 5ml of a 0.25mol cetyltrimethylammonium bromide solution and 40. mu.l of 6mol hydrochloric acid were added 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 nanogold.
Examples of the experiments
The scanning electron microscope results of the nanogold prepared in example 1 are shown in fig. 1. The transmission electron microscope results are shown in FIG. 2.
The nano-gold prepared in the embodiment 1 is in a gold ingot shape and uniform in appearance, and comprises a nano-gold ball and a nano-gold shell layer, wherein the diameter of the nano-gold ball is 20nm, the nano-gold shell layer is wrapped outside the nano-gold ball, a nano gap is formed between the nano-gold shell layer and the nano-gold ball, and the nano gap is 4nm +/-0.2 nm.
The yield of nanogold prepared in example 1 was about 90%.
Experimental example 2
The nanogold prepared in example 1 and the nanogold ball serving as a reference substance were subjected to rhodamine B detection. The specific method comprises the following steps: dripping 30ul of the nanogold or nanogold ball prepared in example 1 onto a glass slide, and drying at 60 ℃ for 8 hours; 10uL of 10 was added dropwise -6 And (3) drying the rhodamine B in mol/L for 10 minutes at the temperature of 60 ℃, and repeating the step for 3 times to obtain a nano-gold sample and a nano-gold ball sample.
And observing the Raman scattering intensity of the nanogold sample and the nanogold ball sample by using a Raman spectrometer. The integration time is twice in 5 seconds, the laser wavelength is 633nm, the laser intensity is 1mw, three sampling points are measured, and an average value is taken.
The results are shown in FIG. 3. From this, it can be seen that the surface raman signal of the nanogold prepared in example 1 is stronger than that of the nanogold ball.
And (4) conclusion: from experimental examples 1-2, it can be seen that the nanogold prepared in the embodiment 1 of the invention has excellent properties such as stable structure, obvious plasmon coupling effect, strong surface-enhanced raman scattering signal, and the like, and has important reference significance for the construction of the surface raman enhancer.
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 (8)
1. The preparation method of the nano gold is characterized by comprising the following steps:
step 1: preparation of gold seeds
Taking 4ml of 0.15-0.25 mol hexadecyl trimethyl ammonium bromide solution, 500 mu l of 4-6 mmol chloroauric acid solution and 600 mu l of 8-12 mmol sodium borohydride solution, and carrying out magnetic stirring reaction to obtain gold seeds;
step 2: preparing nano gold ball 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 μ l of 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 nano gold ball colloidal solution;
and step 3: preparation of Au @ PbS core-shell heterogeneous nano material aqueous solution
Adding 1ml of 0.8-1.2 mol ascorbic acid solution, 1ml of 0.15-0.25 mol hexadecyl trimethyl ammonium bromide solution, 70 mu l of 0.8-1.2 mol thioacetamide solution, 40 mu l of 0.8-1.2 mol lead nitrate solution and 1ml of 0.8-1.2 mol hexamethylenetetramine solution into 5ml of the nano gold ball 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 30-70 mul of 8mmol-12mmol chloroauric acid solution, 0.5ml of 0.8-1.2 mol ascorbic acid solution and 10ml of 0.03-0.07 mol hexadecyl trimethyl ammonium bromide solution into 1ml of the Au @ PbS core-shell heterogeneous nano material aqueous solution obtained in the step 3 under a 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 1ml of deionized water to obtain an Au/PbS/Au nano-structure solution;
and 5: preparation of nano gold
Adding 5ml of 0.15-0.25 mol cetyl trimethyl ammonium bromide solution and 40 mu l of 4-6 mol 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 nanogold; the nano gold is in a gold ingot shape and comprises a nano gold ball and a nano gold shell layer, wherein the nano gold shell layer is wrapped outside the nano gold ball, and a nano gap is formed between the nano gold shell layer and the nano gold ball.
2. The method for preparing nano gold 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 nano gold 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 method for preparing nano gold according to claim 1, wherein in the step 3, the temperature of the 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 nano gold according to claim 1, wherein in the 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 nano gold according to claim 1, wherein in the step 5, the temperature of the 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.
7. The method for preparing nano gold according to claim 1, wherein the drying temperature is 65 ℃ and the drying time is 8 hours in step 5.
8. The method of claim 1, wherein the nanogap has a size of 4nm ± 0.2 nm.
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| CN110739358A (en) * | 2019-09-25 | 2020-01-31 | 江苏大学 | gold-lead sulfide core-shell nanorod photodetectors and preparation method thereof |
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| CN110289353A (en) * | 2019-04-23 | 2019-09-27 | 武汉工程大学 | The perovskite photovoltaic cell being passivated with Au@CdS nano particle |
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