CN117324618A - Simple method for preparing gold nanoparticles with high-index crystal faces - Google Patents
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Abstract
本发明提供了一种用于制备大尺寸（441）高指数晶面的二十四面体金纳米颗粒的种子生长法。该方法避免了大尺寸纳米颗粒制备过程中的多步重复制备流程，节省了制备时间；同时外加离子的引入有助于高晶面形貌的调控和保持。通过透射电镜分析表征，可见所制备的金纳米颗粒具有较为均一的形貌；同时通过衍射确认拍摄方向（110）并测量其特征角度，确认晶面指数为（441）。而且通过目的性改变实验条件，可以实现不同尺寸金纳米颗粒的制备，最终可实现大尺寸且具有高指数晶面的二十四面体金纳米颗粒的简单高效制备。
The present invention provides a seed growth method for preparing large-sized (441) high-index crystal face icosahedral gold nanoparticles. This method avoids the repeated multi-step preparation process in the preparation of large-sized nanoparticles and saves preparation time; at the same time, the introduction of external ions helps to control and maintain the high crystal surface morphology. Through transmission electron microscopy analysis and characterization, it can be seen that the prepared gold nanoparticles have a relatively uniform morphology; at the same time, the shooting direction (110) was confirmed through diffraction and its characteristic angle was measured, and the crystal face index was confirmed to be (441). Moreover, by purposefully changing the experimental conditions, the preparation of gold nanoparticles of different sizes can be achieved, and ultimately the simple and efficient preparation of large-sized icotetrahedral gold nanoparticles with high-index crystal faces can be achieved.
Description
Technical Field
The invention belongs to the technical field of nano material preparation, and relates to a simple preparation method of a icosahedron gold nanoparticle with a (441) high-index crystal face.
Background
Size and morphology control of metal nanoparticles has been attracting researchers' eyes over the last decades. Gold nanoparticles are favored by many researchers for their potential optical, catalytic, electronic and biomedical applications. It is known that the physicochemical properties of gold nanoparticles are largely dependent on their size and morphology. For example, when the size of the spherical gold nanoparticles increases, experimental results indicate that their LSPR peaks may red shift. When the gold nanoparticles have the morphology of a polyhedron such as a twenty tetrahedron, a forty octahedron and the like, high crystal faces on the surfaces of the gold nanoparticles can have kinks, steps and other active sites, so that the catalytic performance of the gold nanoparticles is greatly improved. Therefore, it remains a work that we need to do to explore methods that can precisely control gold nanoparticles of various sizes and morphologies.
The polyhedral nano-particles with high-index crystal faces have important application in the aspects of electrocatalysis, self-assembly and the like. The most common at present are the icosahedron gold nanoparticles with (331) high-index crystal faces, which are mainly prepared by a seed growth method. In addition, for the preparation of nano particles with larger size (> 100 nm), the preparation is limited by the limitation of the morphology-controllable epitaxial growth thickness, and a multi-step seed growth method is needed to be utilized, so that the complexity of experimental operation is greatly increased, and the uncontrollability of the morphology of the final product is increased in an intangible way. Nanoparticles with higher index crystal planes (441, 551, etc.) also face more uncertainty in their preparation due to their higher surface energy. Therefore, development of a simple and efficient method for preparing gold nanoparticles with large-size and higher-index crystal faces is needed to solve the problems of long preparation period and difficult preparation.
Disclosure of Invention
Aiming at the problems of long preparation period and difficult preparation of gold nanoparticles with large-size and higher-index crystal faces, the invention provides a method for preparing the twenty-tetrahedral gold nanoparticles with large-size (441) and high-crystal faces simply and efficiently by an additional ion assisted method based on a seed growth method, which comprises the following steps:
adding a certain amount of chloroauric acid aqueous solution into a certain amount of surfactant solution to obtain a mixed solution, adding a certain amount of sodium borohydride solution into the mixed solution, continuously stirring for a period of time to obtain a mixed dispersion, and finally curing the mixed dispersion in a constant-temperature water bath for a period of time to obtain gold seed dispersion;
step two, adding a certain amount of chloroauric acid aqueous solution and copper ion solution into a certain amount of surfactant solution, and stirring for a period of time to obtain a precursor mixed solution;
sequentially adding a certain amount of reducer solution and gold seed dispersion liquid into the precursor mixed solution, stirring for a period of time, and then curing for a period of time in a constant-temperature water bath to obtain the large-size (441) high-crystal-face icosahedron gold nanoparticles.
Further, the concentration of the chloroauric acid aqueous solution in the first step is 10-30 mM, and the volume is 0.15-0.45 mL; the surfactant is any one of Cetyl Trimethyl Ammonium Chloride (CTAC) and Cetyl Trimethyl Ammonium Bromide (CTAB); the concentration of the surfactant solution is 0.1-0.2M, and the volume is 10-20 mL; the concentration of the sodium borohydride solution is 10-30 mM, and the volume is 0.3-0.6 mL; the stirring time is 2-5 min, and the curing time is 2-5 h.
The concentration of the chloroauric acid aqueous solution in the second step is 10-30 mM, and the volume is 0.25-0.75 mL; the concentration of copper ions is 1-2 mM, and the volume is 40-60 mu L; the surfactant is any one of Cetyl Trimethyl Ammonium Chloride (CTAC) and Cetyl Trimethyl Ammonium Bromide (CTAB); the concentration of the surfactant solution is 50 mM-0.1M, and the volume is 10-20 mL; the stirring time is 2-5 min;
the reducing agent in the third step is one of hydrazine hydrate and ascorbic acid; the concentration of the reducing agent solution is 0.1-0.3M, and the volume is 50-100 mu L; the volume of the gold seeds is 50-100 mu L of gold seed dispersion liquid diluted 10000 times; the stirring time is 5-10 min; the curing time is 6-12 h.
The invention provides a seed growth method for preparing a large-size (441) high-index crystal face icosahedron gold nanoparticle. The method avoids the multi-step repeated preparation flow in the preparation process of the large-size nano particles, and saves the preparation time; meanwhile, the introduction of the additional ions is beneficial to the regulation and the maintenance of the morphology of the high crystal face, and finally, the simple and efficient preparation of the icosahedron gold nanoparticles with the high-index crystal face is realized.
Drawings
FIG. 1 is a flow chart of a preparation process of a large-size (441) high-index crystal face icosahedron gold nanoparticle provided by an embodiment of the present invention;
FIG. 2 is a transmission electron micrograph and diffraction pattern of a 200 nm diameter icosahedron gold nanoparticle having (441) high index crystal planes prepared in example 1 of the present invention;
FIG. 3 is a transmission electron micrograph of icosahedron gold nanoparticles of different sizes prepared according to various embodiments of the present invention.
Description of the embodiments
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
In order to fully understand how the invention may be embodied by those skilled in the art, this section is an illustrative embodiment in which the claims are presented for purposes of illustration.
As shown in fig. 1, the preparation method of the icosahedron gold nanoparticle with (441) high-index crystal face provided by the embodiment of the invention comprises the following steps:
s101, adding a certain amount of chloroauric acid aqueous solution into a certain amount of surfactant solution to obtain a mixed solution, adding a certain amount of sodium borohydride solution into the mixed solution, continuously stirring for a period of time to obtain a mixed dispersion liquid, and finally curing the mixed dispersion liquid in a constant-temperature water bath for a period of time to obtain gold seed dispersion liquid;
s102, adding a certain amount of chloroauric acid aqueous solution and copper ion solution into a certain amount of surfactant solution, and stirring for a period of time to obtain a precursor mixed solution;
and S103, sequentially adding a certain amount of reducer solution and gold seed dispersion liquid into the precursor mixed solution, stirring for a period of time, and then curing for a period of time in a constant-temperature water bath to obtain the large-size (441) high-crystal-face icosahedron gold nanoparticles.
Example 1
A method for preparing a twenty-tetrahedral gold nanoparticle with a diameter of 200 nm and a (441) high-index crystal face, comprising the following steps:
1) Adding 0.15 mL aqueous solution of chloroauric acid with the concentration of 10 mM into 10 mL cetyltrimethylammonium chloride with the concentration of 0.1M to obtain a mixed solution, adding 0.3 mL sodium borohydride with the concentration of 10 mM into the mixed solution, continuously stirring for 2 min to obtain a mixed dispersion, and finally curing the mixed dispersion in a constant-temperature water bath for 2 h to obtain gold seed dispersion;
2) Adding 0.25 mL aqueous chloroauric acid solution with the concentration of 10 mM and 40 mu L copper ion solution with the concentration of 1 mM into 10 mL cetyltrimethylammonium chloride solution with the concentration of 50 mM, and stirring for 2 min to obtain a precursor mixed solution;
3) Adding 50 mu L of ascorbic acid solution with the concentration of 0.1 and M and 100 mu L of gold seed dispersion liquid diluted 10000 times into the precursor mixed solution in sequence, stirring for 5 min, and then curing in a constant-temperature water bath for 12 h to obtain the icosahedron gold nanoparticle with the diameter of 200 nm and the high crystal face (441).
Example 2
A method for preparing a twenty-tetrahedral gold nanoparticle with diameter 230 and nm and high-index crystal face (441), comprising the following steps:
1) Adding 0.3 mL aqueous solution of chloroauric acid with the concentration of 10 mM into 10 mL cetyltrimethylammonium bromide with the concentration of 0.2M to obtain a mixed solution, adding 0.6 mL sodium borohydride with the concentration of 20 mM into the mixed solution, continuously stirring for 5 min to obtain a mixed dispersion, and finally curing the mixed dispersion in a constant-temperature water bath for 3 h to obtain gold seed dispersion;
2) Adding 0.75 mL aqueous chloroauric acid solution with the concentration of 30 mM and 60 mu L copper ion solution with the concentration of 2 mM into 20 mL cetyltrimethylammonium bromide solution with the concentration of 0.1M, and stirring for 5 min to obtain a precursor mixed solution;
3) Adding 50 mu L of ascorbic acid solution with the concentration of 0.1 and M and 75 mu L of gold seed dispersion liquid diluted 10000 times into the precursor mixed solution in sequence, stirring for 10 min, and then curing in a constant-temperature water bath for 8 h to obtain the icosahedron gold nanoparticle with the diameter of 230 nm and the high crystal face (441).
Example 3
A method for preparing a twenty-tetrahedral gold nanoparticle with diameter of 260 nm and high-index crystal face (441), comprising the following steps:
1) Adding 0.15 mL aqueous solution of chloroauric acid with the concentration of 10 mM into 10 mL cetyltrimethylammonium chloride with the concentration of 0.1M to obtain a mixed solution, adding 0.3 mL sodium borohydride with the concentration of 10 mM into the mixed solution, continuously stirring for 2 min to obtain a mixed dispersion, and finally curing the mixed dispersion in a constant-temperature water bath for 2 h to obtain gold seed dispersion;
2) Adding 0.5 mL aqueous chloroauric acid solution with concentration of 20 mM and 50 mu L copper ion solution with concentration of 2 mM into 10 mL cetyltrimethylammonium chloride solution with concentration of 50 mM, and stirring for 5 min to obtain precursor mixed solution;
3) Adding 50 mu L of ascorbic acid solution with the concentration of 0.3 and M and 50 mu L of gold seed dispersion liquid diluted 10000 times into the precursor mixed solution in sequence, stirring for 5 min, and then curing in a constant-temperature water bath for 12 h to obtain the icosahedron gold nanoparticle with the diameter of 260 nm and the high crystal face (441).
FIG. 2 is a transmission electron microscope analysis characterization of the twenty-tetrahedral gold nanoparticles with the diameter of 200 nm and the (441) high-index crystal face prepared in example 1 of the present invention, and it can be seen that the prepared gold nanoparticles have a relatively uniform morphology; at the same time, the imaging direction (110) is confirmed by diffraction, and the characteristic angle is measured, and the crystal face index (441) is confirmed. FIG. 3 is a transmission electron microscope picture of the icosahedron gold nanoparticles with different sizes of (441) high-index crystal planes prepared in examples 1-3 of the present invention, further confirming the feasibility of the scheme of the present invention.
The foregoing is merely illustrative of specific embodiments of the present invention, and the scope of the invention is not limited thereto, but any modifications, equivalents, improvements and alternatives falling within the spirit and principles of the present invention will be apparent to those skilled in the art within the scope of the present invention.
Claims (5)
1. An additional ion assisted method for simple and efficient preparation of large-size (441) high-crystal-plane icosahedron gold nanoparticles, comprising:
adding a certain amount of chloroauric acid aqueous solution into a certain amount of surfactant solution to obtain a mixed solution, adding a certain amount of sodium borohydride solution into the mixed solution, continuously stirring for a period of time to obtain a mixed dispersion, and finally curing the mixed dispersion in a constant-temperature water bath for a period of time to obtain gold seed dispersion;
step two, adding a certain amount of chloroauric acid aqueous solution and copper ion solution into a certain amount of surfactant solution, and stirring for a period of time to obtain a precursor mixed solution;
sequentially adding a certain amount of reducer solution and gold seed dispersion liquid into the precursor mixed solution, stirring for a period of time, and then curing for a period of time in a constant-temperature water bath to obtain the large-size (441) high-crystal-face icosahedron gold nanoparticles.
2. The method for preparing large-size (441) high-crystal-plane icosahedron gold nanoparticles according to claim 1, wherein the concentration of aqueous chloroauric acid in the first step is 10 to 30 mM and the volume is 0.15 to 0.45 mL; the surfactant is any one of Cetyl Trimethyl Ammonium Chloride (CTAC) and Cetyl Trimethyl Ammonium Bromide (CTAB); the concentration of the surfactant solution is 0.1-0.2M, and the volume is 10-20 mL; the concentration of the sodium borohydride solution is 10-30 mM, and the volume is 0.3-0.6 mL; the stirring time is 2-5 min, and the curing time is 2-5 h.
3. The method for preparing large-size (441) high-crystal-plane icosahedron gold nanoparticles according to claim 1, wherein the concentration of aqueous chloroauric acid in the second step is 10 to 30 mM and the volume is 0.25 to 0.75 mL; the concentration of copper ions is 1-2 mM, and the volume is 40-60 mu L; the surfactant is any one of Cetyl Trimethyl Ammonium Chloride (CTAC) and Cetyl Trimethyl Ammonium Bromide (CTAB); the concentration of the surfactant solution is 50 mM-0.1M, and the volume is 10-20 mL; the stirring time is 2-5 min.
4. The method for preparing the large-size (441) high-crystal-plane icosahedron gold nanoparticles according to claim 1, wherein the reducing agent in the third step is one of hydrazine hydrate and ascorbic acid; the concentration of the reducing agent solution is 0.1-0.3M, and the volume is 50-100 mu L; the volume of the gold seeds is 50-100 mu L of gold seed dispersion liquid diluted 10000 times; the stirring time is 5-10 min; the curing time is 6-12 h.
5. A large-size high-crystal-plane icosahedron gold nanoparticle prepared by the method of any one of claims 1 to 4, characterized in that the crystal plane index is (441) and the average diameter is greater than 200 nm.
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