CN115609003A - Preparation method of spherical gold palladium/iron oxide hybrid nanoparticles - Google Patents
Preparation method of spherical gold palladium/iron oxide hybrid nanoparticles Download PDFInfo
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- CN115609003A CN115609003A CN202211353768.8A CN202211353768A CN115609003A CN 115609003 A CN115609003 A CN 115609003A CN 202211353768 A CN202211353768 A CN 202211353768A CN 115609003 A CN115609003 A CN 115609003A
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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
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- B82—NANOTECHNOLOGY
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Abstract
The invention provides a preparation method of spherical gold palladium/ferric oxide hybrid nanoparticles, belonging to the technical field of materials. The method adopts an auto-oxidation-reduction assembly method to prepare Au by utilizing ferrous chloride under the alkalescent condition 3+ And Pd 2+ Reducing the gold-palladium nano particles into gold-palladium nano particles, and forming iron oxide to wrap the gold-palladium nano particles. By finely regulating the proportion, the stirring speed, the reaction time and the like of all reaction components, the spherical gold-palladium/iron oxide hybrid nano particles with the volume of more than 1L can be synthesized in batches and in one pot at room temperature. Compared with the synthesis process of other composite nano particles, the methodThe method has the characteristics of simple and rapid operation, capability of synthesizing in multiple batches and large volume, and can meet the conditions of industrial production.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a preparation method of spherical gold palladium/iron oxide hybrid nanoparticles.
Background
With the progress of science and technology, metal nanoparticles, especially noble metal nanoparticles, have been widely used in the fields of biology, medicine, environment, etc. because of their unique optical and photothermal properties and high catalytic activity. In addition, iron oxide nanoparticles are favored for their low cost and high catalytic activity. However, compared to a single-material metal nanoparticle, a multi-metal-material hybrid nanoparticle has more excellent optical properties and higher catalytic activity. However, the synthesis of hybrid nanoparticles usually requires harsh conditions such as high temperature and high pressure, which greatly hinders the production scale and application range.
The synthesis of metal nanoparticles by using an autoredox assembly method has the characteristics of simple operation and rapid preparation, but the application of the method is limited by the characteristics of poor particle dispersibility, and nonuniform morphology and particle size.
Disclosure of Invention
The invention aims to provide a preparation method of spherical gold-palladium/iron oxide hybrid nanoparticles, which can synthesize the spherical gold-palladium/iron oxide hybrid nanoparticles with the volume of more than 1L in batches in one pot at room temperature by finely regulating the proportion, the stirring speed and the reaction time of each reaction component.
The invention provides a preparation method of spherical gold palladium/ferric oxide hybrid nanoparticles, which comprises the following steps:
step 1: adding HAuCl 4 Solution, na 2 PdCl 4 Mixing the solution and deionized water, and uniformly stirring to obtain a mixed solution;
step 2: adding an ammonia solution into the mixed solution obtained in the step 1, and uniformly stirring to obtain a reaction solution;
and 3, step 3: adding FeCl into the reaction solution of step 2 2 Stirring the solution for reaction, and synthesizing gold palladium/ferric oxide hybrid nanoparticles by using an auto-oxidation-reduction assembly method;
and 4, step 4: and (4) centrifugally washing the reaction product solution obtained in the step (3), and dispersing the reaction product solution in deionized water to obtain a spherical gold palladium/ferric oxide hybrid nanoparticle solution.
Preferably, the HAuCl is described in step 1 4 And Na 2 PdCl 4 In a mass ratio of1.5:1～5:1。
Preferably, the HAuCl is described in step 1 4 And Na 2 PdCl 4 The concentration of the solution is 0.01-0.05 mol L -1 。
Preferably, the mass fraction of the ammonia water in the step 2 is 0.01-1%.
Preferably, the stirring time in step 2 is 1 to 10min.
Preferably, the HAuCl described in Steps 1 and 2 4 Solution and Na 2 PdCl 4 The mass ratio of the total mass of the solution to the mass of the ammonia water is 1:8-1.
Preferably, the FeCl in step 3 2 The concentration of the solution is 0.05-0.5 mol L -1 。
Preferably, the stirring time in step 3 is 10 to 60min.
Preferably, the HAuCl described in Steps 1 and 3 4 And Na 2 PdCl 4 Amount of total substances and FeCl 2 The mass ratio of (A) is 1:5-1.
Preferably, the stirring speed in steps 1 to 4 is 200 to 600rpm.
The invention has the advantages of
The invention provides a preparation method of spherical gold palladium/ferric oxide hybrid nano particles, which adopts an auto-oxidation-reduction assembly method to utilize ferrous chloride to carry out Au synthesis under the alkalescent condition 3+ And Pd 2+ Reducing the gold palladium nano particles into gold palladium nano particles, and forming iron oxide to wrap the gold palladium nano particles. By finely regulating the proportion, stirring speed, reaction time and the like of each reaction component, the spherical gold-palladium/iron oxide hybrid nano particles with the volume of more than 1L can be synthesized in batches and in one pot at room temperature. Compared with other synthesis processes of composite nanoparticles, the method has the characteristics of simple and rapid operation, capability of synthesizing in multiple batches and large volume, and can better meet the conditions of industrial production.
Drawings
FIG. 1 is a schematic diagram of the present invention process for preparing spherical gold palladium/iron oxide hybrid nanoparticles;
FIG. 2 is an optical picture and TEM image of multi-batch one-pot synthesis of spherical gold palladium/iron oxide hybrid nanoparticles of example 1 of the present invention;
FIG. 3 is a high resolution TEM image of spherical gold palladium/iron oxide hybrid nanoparticles synthesized in example 1 of the present invention;
FIG. 4 is an element distribution diagram of the synthesis of spherical gold palladium/iron oxide hybrid nanoparticles according to example 1 of the present invention;
FIG. 5 is an XRD pattern of spherical gold palladium/iron oxide hybrid nanoparticles synthesized in example 1 of the present invention;
FIG. 6 is a hydrated particle size diagram of spherical gold palladium/iron oxide hybrid nanoparticles synthesized in examples 1-3 of the present invention.
Detailed Description
The invention provides a preparation method of spherical gold palladium/ferric oxide hybrid nanoparticles, which comprises the following steps:
step 1: adding HAuCl 4 Solution, na 2 PdCl 4 Mixing the solution and deionized water, and uniformly stirring to obtain a mixed solution;
and 2, step: adding an ammonia solution into the mixed solution obtained in the step 1, and uniformly stirring to obtain a reaction solution;
and step 3: adding FeCl into the reaction solution in the step 2 2 Stirring the solution for reaction, and synthesizing the gold-palladium/ferric oxide hybrid nano particles by using a self-assembly redox method;
and 4, step 4: and (4) centrifugally washing the reaction product solution obtained in the step (3), and dispersing the reaction product solution in deionized water to obtain a spherical gold palladium/ferric oxide hybrid nanoparticle solution.
According to the invention, na is firstly added 2 PdCl 4 Solution, HAuCl 4 The solution was mixed with deionized water to obtain a mixed solution. Wherein, the HAuCl 4 The concentration of the solution is preferably 0.01 to 0.05mol L -1 More preferably 0.01, 0.02, 0.03, 0.04, 0.05, or 0.01 to 0.05mol L -1 Any value in between. The Na is 2 PdCl 4 The concentration of the solution is preferably 0.01 to 0.05mol L -1 More preferably 0.01, 0.02, 0.03, 0.04, 0.05, or 0.01 to 0.05mol L -1 Any value in between; the Na is 2 PdCl 4 Solution and HAuCl 4 The molar ratio of the solution is preferably1.5, and 1 to 5:1.
According to the invention, under the stirring condition of 200-600 rpm, quickly adding an ammonia water solution into the mixed solution, and mixing and stirring to obtain a reaction solution; the mass fraction of the ammonia solution is preferably 0.01% to 1%, more preferably 0.01%, 0.1%, 0.2%, 0.4%, 0.6%, 0.8%, 1%, or any value between 0.01% and 1%. The HAuCl 4 Solution and Na 2 PdCl 4 The preferable ratio of the total mass of the solution to the mass of the ammonia water is 1:8-1; the time for mixing and stirring by adding the ammonia water solution is preferably 1-10 min, more preferably 1, 3, 5, 7, 9, 10, or any value between 1-10 min.
Then, feCl was rapidly added to the reaction solution 2 Stirring the solution for reaction, synthesizing spherical gold palladium/iron oxide nanoparticles by an auto-oxidation-reduction assembly method, centrifuging, washing with water for 3 times, and dispersing in water. Wherein the FeCl 2 The concentration of the solution is preferably 0.05 to 0.5mol L -1 More preferably 0.05, 0.1, 0.2, 0.3, 0.4, 0.5, or 0.05 to 0.5mol L -1 Any value in between; preferably the HAuCl 4 And Na 2 PdCl 4 Amount of total substances and FeCl 2 The mass ratio of (b) is preferably 1:5-1; said addition of FeCl 2 The time for mixing and stirring the solution is preferably 10 to 60min, more preferably 10, 20, 30, 40, 50, 60, or any value between 10 to 60min.
The present invention is described in further detail below with reference to specific examples, in which the starting materials are all commercially available.
Example 1
The preparation method of the spherical gold palladium/iron oxide hybrid nanoparticle of the embodiment comprises the following steps, and the specific preparation process is shown in figure 1:
step 1: adding 3mL of 0.024mol L -1 HAuCl 4 Solution, 2mL, 0.024mol L -1 Na 2 PdCl 4 Uniformly mixing the solution with 500mL of deionized water;
step 2: quickly adding 20mL of 0.075% ammonia water solution into the mixed solution in the step 1, and stirring at 500rpm for 2min to obtain a reaction solution;
and step 3: 1 mL of 0.1mol L -1 FeCl 2 Adding the solution into the reaction solution in the step 2, and continuously stirring at 500rpm for 20min;
and 4, step 4: and (4) after the reaction is completed, centrifuging and washing the reaction solution obtained in the step (3) for 3 times at the speed of 7500rpm for 8min, and dispersing in 100mL of deionized water to obtain the spherical gold-palladium/iron oxide hybrid nanoparticle solution.
Example 2
The preparation method of the spherical gold palladium/iron oxide hybrid nanoparticles comprises the following steps, and the specific preparation process is shown in figure 1:
step 1: adding 3mL of 0.024mol L -1 HAuCl 4 Solution, 2mL, 0.024mol L -1 Na 2 PdCl 4 Uniformly mixing the solution with 500mL of deionized water;
step 2: rapidly adding 22.5mL of 0.075% ammonia water solution into the mixed solution in the step 1, and stirring at 500rpm for 2min to obtain a reaction solution;
and 3, step 3: 1 mL of 0.1mol L -1 FeCl 2 Adding the solution into the reaction solution in the step 2, and continuously stirring at 500rpm for 20min;
and 4, step 4: and (3) after the reaction is completed, centrifugally washing the reaction solution obtained in the step (3) for 3 times at the centrifugal speed of 7500rpm for 8min, and dispersing in 100mL of deionized water to obtain the spherical gold palladium/iron oxide hybrid nanoparticle solution.
Example 3
The preparation method of the spherical gold palladium/iron oxide hybrid nanoparticles comprises the following steps, and the specific preparation process is shown in figure 1:
step 1: adding 3mL of 0.024mol L -1 HAuCl 4 Solution, 2mL, 0.024mol L -1 Na 2 PdCl 4 Uniformly mixing the solution with 500mL of deionized water;
and 2, step: adding 18mL of 0.075% ammonia water solution into the mixed solution in the step (1), and stirring at 500rpm for 2min to obtain a reaction solution;
and step 3: 10mL of 0.1mol L -1 FeCl 2 Adding the solution into the reaction solution in the step 2, and continuously stirring at 500rpmStirring for 20min;
and 4, step 4: and (3) after the reaction is completed, centrifugally washing the reaction solution obtained in the step (3) for 3 times at the centrifugal speed of 7500rpm for 8min, and dispersing in 100mL of deionized water to obtain the spherical gold palladium/iron oxide hybrid nanoparticle solution.
The method of example 1 is used to synthesize spherical gold palladium/iron oxide hybrid nanoparticles in multiple batches at the same time, as shown in fig. 2a, fig. 2a is an optical picture of the nanoparticles being synthesized. The Transmission Electron Microscope (TEM) images of the spherical gold-palladium/iron oxide hybrid nanoparticles synthesized according to the experimental procedures of example 1 are shown in FIGS. 2b-d, and the results show that the nanoparticles synthesized according to the method of example 1 for three consecutive times are all spherical, the average particle diameters are 39.5 + -3.2 nm, 38.6 + -2.5 nm and 39.2 + -2.9 nm, and the Relative Standard Deviation (RSD) of the particle diameters of the three batches of nanoparticles is 1.2%.
A high-resolution TEM image of the spherical gold-palladium/iron oxide hybrid nanoparticles synthesized according to the method of example 1 is shown in FIG. 3, and the lattice fringes obtained have lattice distances of 0.235nm and 0.192nm, respectively corresponding to Au 0 (111) plane and Pd 0 The (220) plane of (c);
fig. 4 is an element distribution diagram of the spherical gold-palladium/iron oxide hybrid nanoparticle synthesized in example 1 of the present invention, and it can be seen that the gold and palladium elements are mainly distributed in the center of the nanoparticle, and the iron elements are interspersed around the gold and palladium elements;
FIG. 5 is an XRD pattern of the spherical gold palladium/iron oxide hybrid nanoparticles synthesized in example 1 of the present invention, with only the associated diffraction peaks for gold and palladium, and no associated diffraction peaks for Fe, indicating that the iron oxide formed is amorphous.
FIG. 6 is a graph showing the hydrated particle size of spherical gold palladium/iron oxide hybrid nanoparticles synthesized in examples 1 to 3 of the present invention, and it can be seen from the results that the particle size of the nanoparticles gradually decreases with the increase of ammonia water.
The above-mentioned embodiments only express the embodiments of the present invention, but not should be understood as the limitation of the scope of the invention patent, it should be noted that, for those skilled in the art, many variations and modifications can be made without departing from the concept of the present invention, and these all fall into the protection scope of the present invention.
Claims (10)
1. A preparation method of spherical gold palladium/ferric oxide hybrid nanoparticles is characterized by comprising the following steps:
step 1: adding HAuCl 4 Solution, na 2 PdCl 4 Mixing the solution and deionized water, and uniformly stirring to obtain a mixed solution;
and 2, step: adding an ammonia solution into the mixed solution obtained in the step 1, and uniformly stirring to obtain a reaction solution;
and 3, step 3: adding FeCl into the reaction solution of step 2 2 Stirring the solution for reaction, and synthesizing the gold-palladium/ferric oxide hybrid nano particles by using an auto-oxidation-reduction assembly method;
and 4, step 4: and (4) centrifugally washing the reaction product solution obtained in the step (3), and dispersing the reaction product solution in deionized water to obtain a spherical gold palladium/ferric oxide hybrid nanoparticle solution.
2. The method for preparing spherical gold palladium/iron oxide hybrid nanoparticles according to claim 1, wherein the HAuCl is added in step 1 4 And Na 2 PdCl 4 The mass ratio of (1.5) is 1-5:1.
3. The method for preparing spherical gold palladium/iron oxide hybrid nanoparticles according to claim 1, wherein the HAuCl is added in step 1 4 And Na 2 PdCl 4 The concentration of the solution is 0.01-0.05 mol L -1 。
4. The preparation method of the spherical gold-palladium/iron oxide hybrid nanoparticles as claimed in claim 1, wherein the mass fraction of the ammonia water in step 2 is 0.01-1%.
5. The method for preparing spherical gold palladium/iron oxide hybrid nanoparticles as claimed in claim 1, wherein the stirring time in step 2 is 1-10 min.
6. The method for preparing spherical gold palladium/iron oxide hybrid nanoparticles according to claim 1, wherein the HAuCl is used in the steps 1 and 2 4 Solution and Na 2 PdCl 4 The mass ratio of the total mass of the solution to the mass of the ammonia water is 1:8-1.
7. The method for preparing spherical gold-palladium/iron oxide hybrid nanoparticles according to claim 1, wherein the FeCl in the step 3 2 The concentration of the solution is 0.05-0.5 mol L -1 。
8. The method for preparing spherical gold palladium/iron oxide hybrid nanoparticles as claimed in claim 1, wherein the stirring time in step 3 is 10-60 min.
9. The method for preparing spherical gold palladium/iron oxide hybrid nanoparticles according to claim 1, wherein the HAuCl is used in the steps 1 and 3 4 And Na 2 PdCl 4 Amount of total substance and FeCl 2 The mass ratio of (A) is 1:5-1.
10. The preparation method of spherical gold palladium/iron oxide hybrid nanoparticles as claimed in claim 1, wherein the stirring speed of steps 1-4 is 200-600 rpm.
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