CN112893859B - AuPd alloy nano-cluster and synthesis method thereof - Google Patents
AuPd alloy nano-cluster and synthesis method thereof Download PDFInfo
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Abstract
The invention provides an AuPd alloy nanocluster and a synthesis method thereof, and particularly relates to the AuPd alloy nanocluster which comprises the following steps: dissolving gold salt and phase transfer agent in water and organic solvent, stirring for a period of time, and removing water phase. And simultaneously dissolving palladium salt and a phosphine ligand in an alcohol solvent, stirring for a period of time, mixing the two solutions, adding the ligand for reaction, adding a reducing agent for reduction after the reaction for a period of time to obtain zero-valent AuPd alloy nano particles, and finally obtaining the AuPd alloy nano cluster with accurate atomic number along with the lengthening of the reaction time. The AuPd alloy nanoclusters with accurate atomic number and different sizes are obtained by adjusting the atomic ratio of gold and palladium. The method provided by the invention has feasibility and simple operation, and AuPd nanoclusters with different sizes are obtained by changing the atomic ratio of gold and palladium.
Description
Technical Field
The invention relates to the technical field of synthesis of metal alloy nanoclusters, in particular to an AuPd alloy nanocluster and a synthesis method thereof.
Background
In recent years, metal nanoclusters with precise numbers of atoms have been a leading issue of nanoscience research. The metal nanoclusters are generally composed of metal and ligands, and metal atoms serve as cores and ligands serve as shell layers to form different core-shell structures. The metal nanoclusters are smaller than 2nm in size and have specific metal atom number and ligand number, and play important roles in many aspects such as catalysis, biological imaging, sensing, drug delivery, cancer treatment and the like due to good stability and physicochemical properties. Understanding how the atoms in the nanoclusters are arranged, and how the surface is protected, is therefore of great importance to exploring the properties and applications of metal nanoclusters.
At present, the spatial structure and application of the metal alloy nanoclusters are more and more researched, and a series of bimetallic alloy nanoclusters are synthesized, for example, Au is successfully synthesized by cation ligands for wushixiang24Pd and Au24Pt alloy clusters and their crystal structures (chem. commun.,2016,52, 9873-. For some nano-cluster synthesis methods, the steps are complicated and the operation is complex.
Disclosure of Invention
The invention aims to provide a method for synthesizing AuPd nanoclusters with controllable atomic number and size. The preparation method is simple and feasible, is convenient to operate, is mainly used for preparing the AuPd alloy nanocluster with controllable atomic number and size in the same system, and has the nanocluster size of less than 2nm and accurate atomic number.
The technical scheme of the invention is that the preparation method of the AuPd alloy nanocluster comprises the following steps:
(a) dissolving gold salt and a phase transfer agent in water and an organic solvent, stirring at 20-30 ℃ for 10-60min, and removing a water phase to obtain a reaction system a;
(b) dissolving palladium salt and phosphine ligand in an alcohol solvent, and stirring at 20-30 ℃ for 10-60min to obtain a reaction system b;
(c) mixing the reaction system a and the reaction system b, stirring for 10-60min at 20-30 ℃, adding a mercaptan ligand, and stirring for 10-60min at 20-30 ℃ to obtain a reaction system c;
(d) and adding a reducing agent into the reaction system c, stirring for 24-48h at 20-30 ℃, spin-drying, centrifuging, and extracting to obtain the AuPd alloy nanocluster.
Based on the technical scheme, the gold salt is preferably one of chloroauric acid, gold chloride or triphenylphosphine chloroauric acid.
Based on the technical scheme, preferably, the phase transfer agent is one of tetrabutylammonium bromide, tetrabutylammonium chloride and tetrabutylammonium hydrogen sulfate; the molar ratio of the phase transfer agent to the gold salt is 1:1-8: 1.
Based on the technical scheme, preferably, the organic solvent is one of toluene, tetrahydrofuran and dichloromethane.
Based on the technical scheme, preferably, the palladium salt is one of palladium chloride and ammonium tetrachloropalladate; the molar ratio of the palladium salt to the gold salt is 0.1:1-1: 1.
Based on the technical scheme, preferably, the phosphine ligand is one of triphenylphosphine and diphenylphosphine; the molar ratio of the phosphine ligand to the palladium salt is 1:1-10: 1.
Based on the technical scheme, preferably, the alcohol solvent is one of methanol and ethanol.
Based on the technical scheme, preferably, the thiol ligand is one of phenethyl thiol, tert-butyl thiol and adamantane thiol; the molar ratio of the thiol ligand to the gold salt is 1:1-10: 1.
Based on the technical scheme, preferably, the reducing agent is one of sodium borohydride and potassium borohydride, and the molar ratio of the reducing agent to the gold salt is 1:1-20: 1.
The invention also provides the AuPd alloy nano-cluster obtained by the synthesis method, wherein the size of the AuPd alloy nano-cluster is 1.3-1.9 nm.
(1) Dissolving chloroauric acid and phase transfer agent in H2Reacting in O and methylbenzene for 10-60 minutes, and removing a water phase to obtain a reaction system a;
(2) dissolving ammonium tetrachloropalladate and triphenylphosphine in methanol, and reacting for 10-60 minutes to obtain a reaction system b;
(3) adding the reaction system b into the reaction system a, and stirring for 10-60 minutes to obtain a reaction system b-1;
(4) adding a ligand into the reaction system b-1, and stirring for 10-60 minutes at 20-30 ℃ to obtain a reaction system c;
(5) adding sodium borohydride into the reaction system c, and reacting for 1-2 days at 20-30 ℃ to obtain a product;
(6) and spin-drying, centrifuging and extracting the product to obtain the AuPd alloy nano-cluster.
As a preferable technical scheme, in the step (1), chloroauric acid, TOAB and H2The molar ratio of O to toluene is 1 (1-6): (1-5) and (1-10).
As a preferable technical scheme, in the step (2), the molar ratio of ammonium tetrachloropalladate to triphenylphosphine is 1 (1-10).
As a preferred technical scheme, in the step (4), the ligand is a thiol ligand; the addition amount of the ligand is 1-10 times of that of the chloroauric acid in terms of molar ratio.
As a preferred embodiment, the thiol ligand includes phenethyl thiol, tert-butyl benzyl thiol, and the like.
As a preferable technical scheme, in the step (5), the adding amount of the sodium borohydride is 1-20 times of that of the chloroauric acid in terms of molar ratio.
Advantageous effects
(1) The method is capable of preparing the AuPd alloy nanocluster with controllable atomic number and size by stirring for 24-48h at 20-30 ℃, and is simple to operate and easy to control.
(2) The method uses the phosphine ligand in the synthesis process, and is more favorable for synthesizing the AuPd alloy nanocluster.
(3) The method can be generally applied to synthesis of the noble metal alloy nanocluster.
Drawings
FIG. 1 is a diagram showing an ultraviolet-visible absorption spectrum of a product obtained in example 1.
Detailed Description
The invention is described in more detail below with reference to examples:
example 1
Synthesis of AuPd alloy nanocluster
40mg of HAuCl4And 200mg of TOAB (Tetraoctylammonium bromide) in 5mL of H2Dissolving 15mg of ammonium tetrachloropalladate and 65mg of triphenylphosphine in 3mL of methanol in 10mL of toluene, stirring for thirty minutes, mixing reactants in the methanol solution with reactants in a toluene system, and adding the reactants in a ratio to chloroauric acidExample 5:1 Tert-butylmercaptan ligand was stirred at room temperature for thirty minutes, then 90mg of sodium borohydride was dissolved in 4mL of 4 ℃ water and added to the above solution to reduce, and the solution slowly turned reddish brown, indicating that AuPd nanoparticles were formed. And finally, purifying the alloy nanoclusters, spin-drying the product, washing the product for 3 times by using methanol, and finally extracting and spin-drying the product by using dichloromethane.
In the reaction process, the absorption peak of the product is represented by an ultraviolet visible absorption spectrum, and stronger absorption peaks exist at 350nm and 440nm, so that the AuPd alloy nano-cluster is generated.
As shown in fig. 1, example 1 measured the uv-visible absorption spectrum of the AuPd alloy nanocluster by a uv-visible spectrometer.
Example 2
Synthesis of AuPd alloy nanocluster
40mg of AuCl3And 200mg of TOAB (Tetraoctylammonium bromide) in 5mL of H2Dissolving 15mg of palladium chloride and 65mg of triphenylphosphine in 3mL of methanol in 10mL of toluene, stirring for thirty minutes, mixing reactants in a methanol solution with reactants in a toluene system, adding phenethyl mercaptan with a chloroauric acid ratio of 5:1, stirring for thirty minutes at room temperature, dissolving 90mg of sodium borohydride in 4mL of water at 4 ℃, adding the mixture into the solution, and reducing the solution to obtain reddish brown, which indicates that AuPd nanoparticles are generated. And finally, purifying the alloy nano-cluster, spin-drying the product, washing the product for 3 times by using methanol, and finally extracting and spin-drying the product by using dichloromethane to finally obtain the AuPd alloy nano-cluster.
Example 3
Synthesis of AuPd alloy nanocluster
40mg of AuCl3And 200mg of tetrabutylammonium chloride in 5mL of H2Dissolving 15mg of palladium chloride and 65mg of triphenylphosphine in 3mL of methanol in 10mL of toluene, stirring for thirty minutes, mixing reactants in a methanol solution with reactants in a toluene system, adding tert-butyl mercaptan with a chloroauric acid ratio of 5:1, stirring for thirty minutes at room temperature, dissolving 90mg of sodium borohydride in 4mL of water at 4 ℃, adding the solution, and reducing, wherein the solution slowly becomes reddish brown, which indicates that AuPd nanoparticles are generated. Most preferablyAnd then purifying the alloy nano-cluster, spin-drying the product, washing the product for 3 times by using methanol, and finally extracting and spin-drying the product by using dichloromethane to finally obtain the AuPd alloy nano-cluster.
Example 4
Synthesis of AuPd alloy nanocluster
40mg of AuCl3And 200mg of tetrabutylammonium chloride in 5mL of H2Dissolving 15mg of palladium chloride and 100mg of triphenylphosphine in 3mL of methanol in 10mL of toluene, stirring for thirty minutes, mixing reactants in a methanol solution with reactants in a toluene system, adding tert-butyl mercaptan with a chloroauric acid ratio of 5:1, stirring for thirty minutes at room temperature, dissolving 100mg of potassium borohydride in 4mL of 4 ℃ water, adding the solution, and reducing, wherein the solution slowly becomes reddish brown, which indicates that AuPd nanoparticles are generated. And finally, purifying the alloy nano-cluster, spin-drying the product, washing the product for 3 times by using methanol, and finally extracting and spin-drying the product by using dichloromethane to finally obtain the AuPd alloy nano-cluster.
Example 5
Synthesis of AuPd alloy nanocluster
40mg of HAuCl4And 200mg of tetrabutylammonium chloride in 5mL of H2Dissolving 15mg of palladium chloride and 100mg of triphenylphosphine in 3mL of methanol in 10mL of toluene, stirring for thirty minutes, mixing reactants in a methanol solution with reactants in a toluene system, adding tert-butyl mercaptan with a chloroauric acid ratio of 5:1, stirring for thirty minutes at room temperature, dissolving 100mg of potassium borohydride in 4mL of 4 ℃ water, adding the solution, and reducing, wherein the solution slowly becomes reddish brown, which indicates that AuPd nanoparticles are generated. And finally, purifying the alloy nano-cluster, spin-drying the product, washing the product for 3 times by using methanol, and finally extracting and spin-drying the product by using dichloromethane to finally obtain the AuPd alloy nano-cluster.
Example 6
Synthesis of AuPd alloy nanocluster
40mg of HAuCl4And 200mg of tetrabutylammonium chloride in 5mL of H2O and 10mL of toluene, 15mg of ammonium tetrachloropalladate and 100mg of diphenylphosphine were dissolved in 3mL of methanol, and after stirring for thirty minutes, the solution in methanol wasThe reactant is mixed with the reactant in the toluene system, tert-butyl mercaptan with the chloroauric acid ratio of 5:1 is added, the mixture is stirred for thirty minutes at room temperature, then 100mg of potassium borohydride is dissolved in 4mL of water at 4 ℃, the mixture is added into the solution for reduction, and the solution slowly becomes reddish brown, which indicates that AuPd nanoparticles are generated. And finally, purifying the alloy nano-cluster, spin-drying the product, washing the product for 3 times by using methanol, and finally extracting and spin-drying the product by using dichloromethane to finally obtain the AuPd alloy nano-cluster.
Example 7
Synthesis of AuPd alloy nanocluster
40mg of HAuCl4And 200mg of tetrabutylammonium chloride in 5mL of H2Dissolving 15mg of ammonium tetrachloropalladate and 100mg of diphenylphosphine in 3mL of ethanol in 10mL of tetrahydrofuran, stirring for thirty minutes, mixing reactants in the ethanol solution with reactants in a tetrahydrofuran system, adding tert-butyl mercaptan with the chloroauric acid ratio of 5:1, stirring for thirty minutes at room temperature, dissolving 100mg of potassium borohydride in 4mL of water at 4 ℃, adding the solution, and reducing, wherein the solution slowly becomes reddish brown, which indicates that AuPd nanoparticles are generated. And finally, purifying the alloy nano-cluster, spin-drying the product, washing the product for 3 times by using methanol, and finally extracting and spin-drying the product by using dichloromethane to finally obtain the AuPd alloy nano-cluster.
Example 8
Synthesis of AuPd alloy nanocluster
40mg of HAuCl4And 200mg of tetrabutylammonium chloride in 5mL of H2Dissolving 15mg of ammonium tetrachloropalladate and 100mg of diphenylphosphine in 3mL of ethanol in 10mL of tetrahydrofuran, stirring for thirty minutes, mixing reactants in the ethanol solution with reactants in a tetrahydrofuran system, adding adamantane thiol with the chloroauric acid ratio of 5:1, stirring for thirty minutes at room temperature, dissolving 100mg of potassium borohydride in 4mL of water at 4 ℃, adding the solution, and reducing, wherein the solution slowly becomes reddish brown, which indicates that AuPd nanoparticles are generated. And finally, purifying the alloy nano-cluster, spin-drying the product, washing the product for 3 times by using methanol, and finally extracting and spin-drying the product by using dichloromethane to finally obtain the AuPd alloy nano-cluster.
Example 9
Synthesis of AuPd alloy nanocluster
40mg of HAuCl4And 200mg of tetrabutylammonium chloride in 5mL of H2Dissolving 15mg of ammonium tetrachloropalladate and 100mg of diphenylphosphine in 3mL of ethanol in 10mL of tetrahydrofuran, stirring for thirty minutes, mixing reactants in the ethanol solution with reactants in a tetrahydrofuran system, adding phenethyl mercaptan with the ratio of chloroauric acid of 5:1, stirring for thirty minutes at room temperature, dissolving 80mg of potassium borohydride in 4mL of water at 4 ℃, adding the solution, and reducing, wherein the solution slowly becomes reddish brown, which indicates that AuPd nanoparticles are generated. And finally, purifying the alloy nano-cluster, spin-drying the product, washing the product for 3 times by using methanol, and finally extracting and spin-drying the product by using dichloromethane to finally obtain the AuPd alloy nano-cluster.
Example 10
Synthesis of AuPd alloy nanocluster
40mg of HAuCl4And 180mg of tetraoctylammonium bromide in 5mL of H2Dissolving 15mg of ammonium tetrachloropalladate and 100mg of diphenylphosphine in 3mL of ethanol in 10mL of tetrahydrofuran, stirring for thirty minutes, mixing reactants in the ethanol solution with reactants in a tetrahydrofuran system, adding phenethyl mercaptan with the ratio of chloroauric acid of 5:1, stirring for thirty minutes at room temperature, dissolving 80mg of potassium borohydride in 4mL of water at 4 ℃, adding the solution, and reducing, wherein the solution slowly becomes reddish brown, which indicates that AuPd nanoparticles are generated. And finally, purifying the alloy nano-cluster, spin-drying the product, washing the product for 3 times by using methanol, and finally extracting and spin-drying the product by using dichloromethane to finally obtain the AuPd alloy nano-cluster.
Claims (10)
1. A synthesis method of an AuPd alloy nanocluster is characterized by comprising the following steps:
(a) dissolving gold salt and a phase transfer agent in water and an organic solvent, stirring at 20-30 ℃ for 10-60min, and removing a water phase to obtain a reaction system a;
(b) dissolving palladium salt and phosphine ligand in an alcohol solvent, and stirring at 20-30 ℃ for 10-60min to obtain a reaction system b;
(c) mixing the reaction system a and the reaction system b, stirring for 10-60min at 20-30 ℃, adding a mercaptan ligand, and stirring for 10-60min at 20-30 ℃ to obtain a reaction system c;
(d) adding a reducing agent into the reaction system c, stirring for 24-48h at 20-30 ℃, spin-drying, centrifuging, and extracting to obtain the AuPd alloy nanocluster;
the phase transfer agent is one of tetrabutylammonium bromide, tetrabutylammonium chloride and tetrabutylammonium hydrogen sulfate;
the phosphine ligand is one of triphenylphosphine and diphenylphosphine.
2. The method for synthesizing AuPd alloy nanoclusters as claimed in claim 1, wherein the gold salt is one of chloroauric acid, gold chloride or triphenylphosphine chloroauric acid.
3. The method for synthesizing an AuPd alloy nanocluster according to claim 1, wherein the molar ratio of the phase transfer agent to the gold salt is 1:1 to 8: 1.
4. The method for synthesizing AuPd alloy nanoclusters according to claim 1, wherein said organic solvent is one of toluene, tetrahydrofuran, and dichloromethane.
5. The method for synthesizing an AuPd alloy nanocluster as recited in claim 1, wherein said palladium salt is one of palladium chloride and ammonium tetrachloropalladate; the molar ratio of the palladium salt to the gold salt is 0.1:1-1: 1.
6. The method for synthesizing an AuPd alloy nanocluster according to claim 1, wherein the molar ratio of the phosphine ligand to the palladium salt is 1:1 to 10: 1.
7. The method for synthesizing AuPd alloy nanoclusters according to claim 1, wherein said alcohol solvent is one of methanol and ethanol.
8. The method for synthesizing an AuPd alloy nanocluster according to claim 1, wherein the thiol ligand is one of phenethyl thiol, tert-butyl thiol, and adamantane thiol; the molar ratio of the thiol ligand to the gold salt is 1:1-10: 1.
9. The method for synthesizing AuPd alloy nanocluster as claimed in claim 1, wherein the reducing agent is one of sodium borohydride and potassium borohydride, and the molar ratio of the reducing agent to the gold salt is 1:1-20: 1.
10. The AuPd alloy nanocluster obtained by the synthesis method of any one of claims 1 to 9, wherein the AuPd alloy nanocluster has a size of 1.3-1.9 nm.
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