CN112247157A - 2-ethylthiophenol protected silver-palladium alloy nanocluster and preparation method thereof - Google Patents
2-ethylthiophenol protected silver-palladium alloy nanocluster and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a silver-palladium alloy nanocluster protected by 2-ethylthiophenol and a preparation method thereof, belonging to the technical field of inorganic synthetic chemistry and nano material preparation. The method comprises the following steps: silver nitrate and palladium nitrate are used as metal sources, 2-ethyl thiophenol is used as a protective ligand, and a one-step method with simple operation is adopted to prepare the monodisperse silver-palladium alloy nanocluster with accurate atomic number. On one hand, the preparation method of the silver-palladium alloy nanocluster is simplified by adopting a one-step synthesis method with simple operation, and on the other hand, a protective ligand for stabilizing the silver-palladium alloy nanocluster is developed, so that the types of the silver-palladium alloy nanocluster are enriched. The prepared silver-palladium alloy nanocluster is monodisperse, easily available in raw materials, simple in synthesis operation, simple in separation and cleaning process and good in repeatability, widens and enriches the types of the silver-palladium alloy nanoclusters, and provides theoretical and material basis for related research and development.
Description
Technical Field
The invention belongs to the technical field of inorganic synthetic chemistry and nano material preparation, and particularly relates to a silver-palladium alloy nanocluster protected by 2-ethylthiophenol and a preparation method thereof.
Background
The silver nanoclusters are aggregates formed by physicochemical action of several to hundreds of metal atoms, and generally have a size of 2nm or less and a definite structure and composition. Due to the determined molecular structure, the special optical performance, the good biocompatibility and the low toxicity of the silver nanocluster, the silver nanocluster has potential application prospects in the fields of biosensing, cell marking, drug transportation and the like, and attracts more and more attention of scientific researchers. Due to the harsh preparation conditions of the silver nanoclusters, the poor stability of the silver nanoclusters at normal temperature and the like, the research and development of the silver nanoclusters are slow.
Compared with the single-metal silver nanocluster, the silver palladium alloy nanocluster often shows peculiar physicochemical properties, but the silver palladium alloy nanocluster protected by the ligand is few in variety, and only one preparation method has the problems of complexity and complexity, so that the research and development in the field are not facilitated.
Disclosure of Invention
In order to solve the above problems, the present invention aims to provide a silver-palladium alloy nanocluster protected by 2-ethylthiophenol and a preparation method thereof, wherein the operation is simple, the repeatability is good, and the types of the silver-palladium alloy nanoclusters are expanded and enriched.
The invention is realized by the following technical scheme:
the invention discloses a silver-palladium alloy nanocluster protected by 2-ethylthiophenol, wherein the framework structure of the nanocluster is a cuboid with 8 sulfur atomsThe atoms are respectively positioned at 8 vertex angles, 2 palladium atoms are respectively positioned at the centers of 2 opposite bottom surfaces, 4 silver atoms are respectively positioned at the middle points of 4 long edges, and 8 dehydrogenated 2-ethylthiophenols are respectively connected with 8 sulfur atoms; the average bond length between the palladium atom and the sulfur atom is
The average bond length between silver atoms is
The average bond length between the silver atom and the sulfur atom is
The invention discloses a preparation method of the silver-palladium alloy nanocluster protected by 2-ethylthiophenol, which comprises the following steps:
step 1: mixing silver source silver nitrate, palladium source palladium nitrate and dichloromethane-methanol, stirring until the silver nitrate and the palladium nitrate are completely dissolved, adding ligand 2-ethyl thiophenol under a continuous stirring state, and obtaining a system A after the reaction is finished;
step 2: adding a reducing agent into the system A under a continuous stirring state, and obtaining a system B after the reaction is finished;
and step 3: and (3) carrying out water-oil phase separation on the system B, and cleaning the oil phase to obtain the 2-ethylthiophenol protected silver-palladium alloy nanocluster.
Preferably, in the step 1, the molar ratio of silver ions in the silver nitrate to palladium ions in the palladium nitrate is (3-6): the molar ratio of 1, 2-ethylthiophenol to silver ions is (2-8): 1.
Preferably, in the step 1, the initial stirring speed is 800-1600 r/min, and the stirring time is 10-30 min; the stirring speed is 400-900 r/min when the ligand 2-ethyl thiophenol is added, and the stirring time is 10-30 min.
Preferably, in step 1, the reaction temperature after adding the ligand 2-ethylthiophenol is-10 ℃ to 20 ℃.
Preferably, in the step 2, the reducing agent is sodium borohydride, and the weight ratio of the reducing agent to the reducing agent is (10-80) mg:1ml of the feed-liquid ratio, and dissolving sodium borohydride in deionized water, ethanol or a mixed solution of the deionized water and the ethanol.
More preferably, the molar ratio of the sodium borohydride to the silver ions is (1-10): 1.
Preferably, in the step 2, the stirring speed is 600-1200 r/min.
Preferably, in the step 2, the reaction time is 5-20 h.
Preferably, in the step 3, methanol is adopted for centrifugal cleaning for 3-5 times, and the centrifugal rotation speed is 10000 rpm/min.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention discloses a 2-ethyl thiophenol protected silver-palladium alloy nanocluster, wherein the framework structure of the nanocluster is a cuboid formed by 4 silver atoms and 2 palladium atoms, 8 vertex angles are respectively combined with a dehydrogenated ligand, the nanocluster is free of electric charge and can analyze the precise crystal structure of the nanocluster, so that the precise association between the structure and the performance can be realized, and the variety of the silver-palladium alloy nanocluster is expanded and enriched.
The invention discloses a preparation method of the silver-palladium alloy nanocluster protected by 2-ethylthiophenol, which comprises the steps of mixing silver nitrate, palladium nitrate and dichloromethane-methanol by a simple one-step method, stirring until metal salt is completely dissolved, adding ligand 2-ethylthiophenol under the condition of continuous stirring to obtain a precursor of metal ions and the ligand, reducing the precursor solution by using a reducing agent, and finally preparing the silver-palladium alloy nanocluster protected by 2-ethylthiophenol. The prepared silver-palladium alloy nanocluster is monodisperse, easily available in raw materials, simple in synthesis operation, simple in separation and cleaning process and good in repeatability, widens and enriches the types of the silver-palladium alloy nanoclusters, and provides theoretical and material basis for related research and development.
Further, the molar ratio of silver ions in silver nitrate to palladium ions in palladium nitrate is (3-6): 1, and nanoparticles can be generated when the ratio is too large or too small; the molar ratio of the 2-ethylthiophenol to the silver ions is (2-8): 1, when the ratio is too large, the solution gradually becomes transparent and precipitates are generated at the bottom, and when the ratio is too small, nanoparticles are generated.
Further, based on a 'kinetic control' strategy, the initial stirring speed in the step 1 is 800-1600 r/min, the stirring time is 10-30 min, the stirring speed when the ligand 2-ethylthiophenol is added is adjusted to be 400-900 r/min, and the stirring time is 10-30 min, so that precursors of metal ions and the ligand can be fully generated at the moment.
Further, based on a 'thermodynamic selection' strategy, the temperature of the reaction after the ligand 2-ethylthiophenol is added is-10 ℃ to 20 ℃, nanoparticles can be generated when the temperature is too high, and the reaction time can be prolonged when the temperature is too low.
Furthermore, sodium borohydride is adopted as a reducing agent, so that the reducing property is strong.
Furthermore, the molar ratio of the sodium borohydride to the silver ions is (1-10): 1, when the ratio is too large, nanoparticles can be generated, and when the ratio is too small, precursors of the metal ions and the ligands cannot be fully reduced, so that the yield is reduced, and even the target clusters cannot be prepared.
Furthermore, the stirring speed of the step 2 is 600-1200 r/min, nanoparticles can be easily generated when the stirring speed is too high, and particle precipitates can be generated when the stirring speed is too slow.
Further, the reaction time of the step 2 is 5-20 h, nanoparticles can be generated if the reaction time is too long, and metastable clusters can be generated if the reaction time is too short, and the metastable clusters are not target clusters.
Drawings
Fig. 1 is a crystal structure diagram of the 2-ethylthiophenol protected silver palladium alloy nanoclusters of the present invention.
Detailed Description
The invention will now be described in further detail with reference to the following drawings and specific examples, which are intended to be illustrative and not limiting:
example 1
(1) Weighing silver nitrate and palladium nitrate with the molar ratio of silver ions to palladium ions being 3:1, transferring the silver nitrate and the palladium nitrate into a 250ml single-neck round-bottom flask, then adding methanol and dichloromethane solution with the volume ratio of 2:1, and stirring for 30min under the condition that the stirring speed is 800r/min to obtain a mixed solution in which two metal salts are completely dissolved;
(2) under the condition of adjusting the stirring speed to 400r/min, adding ligand 2-ethylthiophenol, wherein the molar ratio of the ligand to the metal silver ions is 2:1, then continuously stirring for 30min, and keeping the temperature of the reaction system at-10 ℃;
(3) under the condition that the stirring rate is adjusted to 600r/min, mixing sodium borohydride and deionized water according to the proportion that the mass of the sodium borohydride and the volume of the deionized water are 10mg:1ml, adding the mixture into the solution prepared in the step (2), wherein the molar ratio of the sodium borohydride to silver ions in the solution is 1:1, continuously stirring and reacting for 20 hours, and then stopping the reaction;
(4) and (3) after the reaction is finished, separating the crude product by water-oil phase, discarding the water phase, dividing the oil phase into 5 equal parts for cleaning clusters, and centrifugally cleaning each part for 5 times by using methanol at the rotating speed of 10000rpm/min to obtain the silver-palladium alloy nanocluster protected by 2-ethylthiophenol.
Example 2
(1) Weighing silver nitrate and palladium nitrate with the molar ratio of silver ions to palladium ions being 6:1, transferring the silver nitrate and the palladium nitrate into a 250ml single-neck round-bottom flask, then adding methanol and dichloromethane solution with the volume ratio of 1:1, and stirring for 25min under the condition that the stirring speed is 1000r/min to obtain a mixed solution in which two metal salts are completely dissolved;
(2) under the condition of adjusting the stirring speed to 450r/min, adding ligand 2-ethylthiophenol, wherein the molar ratio of the ligand to the metal silver ions is 4:1, then continuously stirring for 25min, and keeping the temperature of the reaction system at-5 ℃;
(3) under the condition that the stirring rate is adjusted to 800r/min, mixing sodium borohydride and deionized water according to the proportion that the mass of the sodium borohydride and the volume of the deionized water are 50mg:1ml, adding the mixture into the solution prepared in the step (2), wherein the molar ratio of the sodium borohydride to silver ions in the solution is 6:1, continuously stirring and reacting for 15 hours, and then stopping the reaction;
(4) and (3) after the reaction is finished, separating the crude product by water-oil phase, discarding the water phase, dividing the oil phase into 5 equal parts for cleaning clusters, and centrifugally cleaning each part for 3 times by using methanol at the rotating speed of 10000rpm/min to prepare the silver-palladium alloy nanocluster protected by 2-ethylthiophenol.
Example 3
(1) Weighing silver nitrate and palladium nitrate with the molar ratio of silver ions to palladium ions being 4:1, transferring the silver nitrate and the palladium nitrate into a 250ml single-neck round-bottom flask, then adding into a methanol and dichloromethane solution with the volume ratio of 1:2, and stirring for 20min under the condition that the stirring speed is 1200r/min to obtain a mixed solution in which two metal salts are completely dissolved;
(2) under the condition of adjusting the stirring speed to 900r/min, adding ligand 2-ethylthiophenol, wherein the molar ratio of the ligand to the metal silver ions is 8:1, then continuously stirring for 10min, and keeping the temperature of the reaction system at 0 ℃;
(3) under the condition that the stirring rate is adjusted to 1000r/min, mixing sodium borohydride and deionized water according to the proportion that the mass of the sodium borohydride and the volume of the deionized water are 10mg:1ml, adding the mixture into the solution prepared in the step (2), wherein the molar ratio of the sodium borohydride to silver ions in the solution is 1:1, continuously stirring and reacting for 10 hours, and then stopping the reaction;
(4) and (3) after the reaction is finished, separating the crude product by water-oil phase, discarding the water phase, dividing the oil phase into 5 equal parts for cleaning clusters, and centrifugally cleaning each part for 4 times by using methanol at the rotating speed of 10000rpm/min to prepare the silver-palladium alloy nanocluster protected by 2-ethylthiophenol.
Example 4
(1) Weighing silver nitrate and palladium nitrate with the molar ratio of silver ions to palladium ions being 3:1, transferring the silver nitrate and the palladium nitrate into a 250ml single-neck round-bottom flask, then adding into a methanol and dichloromethane solution with the volume ratio of 1:2, and stirring for 10min under the condition that the stirring speed is 1600r/min to obtain a mixed solution in which two metal salts are completely dissolved;
(2) under the condition of adjusting the stirring speed to 800r/min, adding a ligand 2-ethylthiophenol, wherein the molar ratio of the ligand to the metal silver ions is 3:1, then continuously stirring for 10min, and keeping the temperature of a reaction system at-5 ℃;
(3) under the condition that the stirring rate is adjusted to 1200r/min, mixing sodium borohydride and deionized water according to the proportion that the mass of the sodium borohydride and the volume of the deionized water are 50mg:1ml, adding the mixture into the solution prepared in the step (2), wherein the molar ratio of the sodium borohydride to silver ions in the solution is 6:1, continuously stirring and reacting for 15 hours, and then stopping the reaction;
(4) and (3) after the reaction is finished, separating the crude product by water-oil phase, discarding the water phase, dividing the oil phase into 5 equal parts for cleaning clusters, and centrifugally cleaning each part for 5 times by using methanol at the rotating speed of 10000rpm/min to obtain the silver-palladium alloy nanocluster protected by 2-ethylthiophenol.
Example 5
(1) Weighing silver nitrate and palladium nitrate with the molar ratio of silver ions to palladium ions being 4:1, transferring the silver nitrate and the palladium nitrate into a 250ml single-neck round-bottom flask, then adding into a methanol and dichloromethane solution with the volume ratio of 1:1, and stirring for 30min under the condition that the stirring speed is 800r/min to obtain a mixed solution in which two metal salts are completely dissolved;
(2) under the condition of adjusting the stirring speed to 800r/min, adding ligand 2-ethylthiophenol, wherein the molar ratio of the ligand to the metal silver ions is 2:1, then continuously stirring for 10min, and keeping the temperature of the reaction system at 20 ℃;
(3) under the condition that the stirring rate is adjusted to 800r/min, mixing sodium borohydride and deionized water according to the proportion that the mass of the sodium borohydride and the volume of the deionized water are 80mg:1ml, adding the mixture into the solution prepared in the step (2), wherein the molar ratio of the sodium borohydride to silver ions in the solution is 10:1, continuously stirring and reacting for 10 hours, and then stopping the reaction;
(4) and (3) after the reaction is finished, separating the crude product by water-oil phase, discarding the water phase, dividing the oil phase into 5 equal parts for cleaning clusters, and centrifugally cleaning each part for 5 times by using methanol at the rotating speed of 10000rpm/min to obtain the silver-palladium alloy nanocluster protected by 2-ethylthiophenol.
Examples 1, 2, 3 and 3 were prepared using a dichloromethane/n-hexane solutionAnd 4, performing crystal growth culture on the silver-palladium alloy nanocluster raw solution prepared in the embodiment 5, wherein the volume ratio of dichloromethane to n-hexane is 3:1, obtaining of novel Ag4Pd2The crystal structures of the alloy nanoclusters are shown in fig. 1.
As can be seen from figure 1, the framework structure of the cluster is a cuboid, eight sulfur atoms occupy eight vertex angles of the cuboid, two palladium atoms are respectively positioned at the central positions of two bottom surfaces, four silver atoms are just positioned at the middle points of four long edges of the cuboid, and eight dehydrogenated 2-ethylthiophenols are connected with the sulfur atoms at the vertex angles. The average bond length between palladium and sulfur atoms is
The average bond length between silver and silver atoms is
The average bond length between silver and sulfur atoms is
While the preferred embodiments of the present invention have been described in detail, the present invention is not limited to the above embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the scope of the invention.
Claims (10)
1. The 2-ethylthiophenol protected silver-palladium alloy nanocluster is characterized in that a framework structure of the nanocluster is a cuboid, 8 sulfur atoms are respectively located at 8 vertex angles, 2 palladium atoms are respectively located at the centers of 2 opposite bottom surfaces, 4 silver atoms are respectively located at the middle points of 4 long edges, and 8 dehydrogenated 2-ethylthiophenols are respectively connected with 8 sulfur atoms; the average bond length between the palladium atom and the sulfur atom is
The average bond length between silver atoms is
The average bond length between the silver atom and the sulfur atom is
2. The method of making 2-ethylthiophenol-protected silver-palladium alloy nanoclusters of claim 1 including the steps of:
step 1: mixing silver source silver nitrate, palladium source palladium nitrate and dichloromethane-methanol, stirring until the silver nitrate and the palladium nitrate are completely dissolved, adding ligand 2-ethyl thiophenol under a continuous stirring state, and obtaining a system A after the reaction is finished;
step 2: adding a reducing agent into the system A under a continuous stirring state, and obtaining a system B after the reaction is finished;
and step 3: and (3) carrying out water-oil phase separation on the system B, and cleaning the oil phase to obtain the 2-ethylthiophenol protected silver-palladium alloy nanocluster.
3. The 2-ethylthiophenol-protected silver-palladium alloy nanocluster of claim 2, wherein in step 1, the molar ratio of silver ions in silver nitrate and palladium ions in palladium nitrate is (3-6): 1, and the molar ratio of 2-ethylthiophenol to silver ions is (2-8): 1.
4. The 2-ethylthiophenol-protected silver-palladium alloy nanocluster according to claim 2, wherein in step 1, the initial stirring rate is 800 to 1600r/min and the stirring time is 10 to 30 min; the stirring speed is 400-900 r/min when the ligand 2-ethyl thiophenol is added, and the stirring time is 10-30 min.
5. The 2-ethylthiophenol-protected silver-palladium alloy nanocluster according to claim 2, wherein the reaction temperature after adding ligand 2-ethylthiophenol in step 1 is-10 ℃ to 20 ℃.
6. The 2-ethylthiophenol-protected silver-palladium alloy nanoclusters according to claim 2, wherein in step 2, the reducing agent is sodium borohydride, and the reducing agent is added in an amount of (10-80) mg:1ml of the feed-liquid ratio, and dissolving sodium borohydride in deionized water, ethanol or a mixed solution of the deionized water and the ethanol.
7. The 2-ethylthiophenol-protected silver-palladium alloy nanocluster of claim 6, wherein the molar ratio of sodium borohydride to silver ions is (1-10): 1.
8. The 2-ethylthiophenol-protected silver-palladium alloy nanocluster according to claim 2, wherein the stirring speed in step 2 is 600 to 1200 r/min.
9. The 2-ethylthiophenol-protected silver-palladium alloy nanocluster according to claim 2, wherein in step 2, the reaction time is 5 to 20 hours.
10. The 2-ethylthiophenol-protected silver-palladium alloy nanocluster according to claim 2, wherein in step 3, methanol is used for centrifugal cleaning for 3-5 times, and the centrifugal rotation speed is 10000 rpm/min.
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| CN115582552A (en) * | 2022-10-10 | 2023-01-10 | 武汉理工大学 | Preparation method for improving gold clusters based on solvent-assisted two-phase synthesis strategy |
| CN115537932B (en) * | 2022-09-28 | 2024-04-19 | 西北工业大学宁波研究院 | High-cadmium-doped core-shell Au16Cd16(SR)20Cluster and preparation method thereof |
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| LIZHONG HE: "Kernel Tuning and Nonuniform Influence on Optical and Electrochemical Gaps of Bimetal Nanoclusters", 《JOURNAL OF THE AMERICAN CHEMICAL SOCIETY》 * |
| 孙国栋等: "银镍合金团簇Ag_4Ni_2(SPhMe_2)_8(SPhMe_2=2,4-二甲基苯硫酚)的合成及其结构表征（英文）", 《物理化学学报》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115537932A (en) * | 2022-09-28 | 2022-12-30 | 西北工业大学宁波研究院 | High-cadmium-doped core-shell Au 16 Cd 16 (SR) 20 Cluster and preparation method thereof |
| CN115537932B (en) * | 2022-09-28 | 2024-04-19 | 西北工业大学宁波研究院 | High-cadmium-doped core-shell Au16Cd16(SR)20Cluster and preparation method thereof |
| CN115582552A (en) * | 2022-10-10 | 2023-01-10 | 武汉理工大学 | Preparation method for improving gold clusters based on solvent-assisted two-phase synthesis strategy |
| CN115582552B (en) * | 2022-10-10 | 2023-10-27 | 武汉理工大学 | Preparation method for improving gold cluster based on solvent-assisted two-phase synthesis strategy |
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