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Method for synthesizing oil-soluble gold nanoparticles

A gold nanoparticle and synthesis method technology, which is applied in the field of synthesis of oil-soluble gold nanoparticles, can solve the problems of surface-enhanced Raman spectrum restriction, weak Raman spectrum enhancement effect, Au is not easy to grow, etc., to promote commercialization , high yield and mild reaction conditions

Active Publication Date: 2014-05-07
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] However, the size of the oily Au nanoparticles synthesized in the prior art basically does not exceed 30nm. This is mainly due to the strong surface protection during the growth of the Au nanoparticles in the oil phase system, and the reaction of the Au precursor salt is too fast. It makes it difficult for Au to grow up; and the small-sized Au nanoparticles have a weak enhancement effect on Raman spectroscopy, which is difficult to be used for practical detection
Due to the limitation of synthesis method, the application of surface-enhanced Raman spectroscopy in organic systems is greatly restricted

Method used

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  • Method for synthesizing oil-soluble gold nanoparticles
  • Method for synthesizing oil-soluble gold nanoparticles
  • Method for synthesizing oil-soluble gold nanoparticles

Examples

Experimental program
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Effect test

Embodiment 1

[0018] 1) Preparation of 6nm Au nanoparticles

[0019] (1) Add 10mL oleylamine and 10mL n-octane into a 50mL two-neck round bottom flask, place in a constant temperature water bath at 20°C, and stir for 5-10min.

[0020] (2) Add 0.1g of chloroauric acid solid powder to the round bottom flask in step (1), N 2 Protected and stirred for 5-10 minutes.

[0021] (3) Dissolve 0.25g of tert-butylamine borane powder in 1mL of n-octane and 1mL of oleylamine, pour it into the above round bottom flask, and stop stirring for 1h.

[0022] (4) The stock solution was settled with 60 mL of absolute ethanol, concentrated by centrifugation (6000 r / min, centrifuged for 5 min), and the precipitate was dispersed in 10 mL of n-hexane, and the product was named A.

[0023] 2) Preparation of 30nm Au nanoparticles

[0024] (1) Add 100mL tetralin, 90mL oleylamine, 90mL n-butylamine and 0.05mL product A to a 500mL container in sequence, place in a 60°C water bath and stir for 5-10min.

[0025] (2) Co...

Embodiment 2

[0028] Product A was prepared according to step 1) of Example 1.

[0029] Add 100mL tetralin, 90mL oleylamine, 90mL n-butylamine and 0.05mL product A to a 500mL container in sequence, place in a 60°C water bath and stir for 5-10min. A chloroform solution (100 mg / mL) of triphenylphosphine gold chloride was continuously added with a syringe pump at a rate of 0.15 mL / h. After 1 h, the addition of the sample was stopped, and the reaction was continued for 1 h to obtain 30 nm Au nanoparticles.

Embodiment 3

[0031] Product A was prepared according to step 1) of Example 1.

[0032] Add 180mL of n-octane, 80mL of oleylamine, 20mL of n-butylamine and 0.2mL of product A into a 500mL container in sequence, and stir in a 60°C water bath for 5-10min. A solution of chloroauric acid in ethanol (100 mg / mL) was continuously added with a syringe pump at a rate of 0.4 mL / h. After 24h, the addition of the sample was stopped, and the reaction was continued for 1h to obtain 47nm Au nanoparticles.

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Abstract

The invention relates to gold nanoparticles, and provides a method for synthesizing high-concentration and high-stability oil-soluble gold nanoparticles with the particle sizes of 30-100 nm in an oil phase system under mild conditions. The method comprises the following steps: adding seed crystals into a growth solution and adding a precursor of Au to obtain the oil-soluble gold nanoparticles with the particle sizes of 30-100 nm. Short-chain organic amine is introduced into the growth solution in a seed crystal growth method, on one hand, the surfaces of small-sized Au seed crystals are exchanged to reduce the protection degree of the surfaces thereof, so that a salt precursor of the Au continues to grow more easily, on the other hand, the reduction speed of the salt precursor of the Au is reduced so as to reduce the growth speed to obtain large-sized Au nanoparticles; the method has the advantages of mild reaction conditions, good reproducibility and high yield.

Description

technical field [0001] The invention relates to gold nanoparticles, in particular to a method for synthesizing oil-soluble gold nanoparticles with a particle diameter of 30-100 nm. Background technique [0002] Due to its size effect and unique electronic structure, Au nanoparticles have great application prospects in catalysis, bioimaging, photonics, and surface-enhanced Raman spectroscopy, and have attracted extensive attention for many years. The size of Au nanoparticles plays an important role in their properties, which is particularly important in applications such as catalysis and surface-enhanced Raman spectroscopy. [0003] Surface-enhanced Raman spectroscopy is a spectroscopic technique for rapidly detecting molecular structures on the surface of substances, and Au nanoparticles are widely used as an effective substrate material for surface-enhanced Raman spectroscopy. Studies have shown that the size of Au nanoparticles has a great influence on its Raman enhanceme...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/24B82Y40/00
Inventor 郑南峰刘圣杰方晓亮吴炳辉田中群
Owner XIAMEN UNIV
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