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Phosphine-stabilized gold nanoparticles

Phosphine-stabilized gold nanoparticles have a rich chemistry and are excellent building blocks for functional groups, however they have typically been synthesized through cumbersome and unsafe methods. This process is a safer, more convenient, and more versatile procedure to synthesize small, phosphine-stabilized gold nanoparticles under ambient conditions.

Contributors: 

Weare WW, Reed SM, Warner MG, Hutchinson JE

Lab: 

Department of Chemistry and Materials Science Institute, University of Oregon

Manufactured Material or Structure: 
Phosphine-Stabilized Gold Nanoparticles
Chemical Composition: 
Au101(PPh3)21Cl5
Physical Form: 
solid, powder
Material Properties: 
chemical: purity: 75.8% optical: surface plasmon resonance: 520 nm physical: diameter: 1.5 nm
Environmental, Health & Safety Considerations: 
Pleaes refer to the NBI Knowledgebase nanomaterial library (http://oregonstate.edu/nbi/nanomaterial.php)

Step 1:

Dissolve hydorgen tetrachloroaurate trihydrate (1.00 g, 2.554 mmol) and tetraoctylammonium bromide (1.60 g, 2.93 mmol) in nitrogen sparged water/toulene misture (50 mL/65 mL).

Step 2:

After golden color transfers to organic phase, add triphenylphosphine (2.32 g, 8.85 mmol) to the solution and stir vigorously for 10 min until phase is white and cloudy.

Step 3:
Caution

Add aqueous sodium borohydride (1.41 g, 37.3 mmol, dissolved in 10 mL of water immediately prior to use) to solution. Organic phase will immediately turn dark purple.

Step 4:

Stir for 3 hours under nitrogen.

Step 5:

Separate toluene layer and wash with water (2 x 100 mL). Remove solvent in vacuo or with nitrogen stream, yielding a black solid.

Step 6:

Wash resulting solid with solvents (hexanes, saturated aqueous sodium nitrite, and 2:3 methanol:water mixture) to remove phase transfer catalyst, byproducts, and unreacted starting materials.

Step 7:

Purify by precipitation from chloroform and pentane.

Process Notes: 

Process yields 170 mg of purified nanoparticle from 1 g of HAuCl4.

Raw Materials: 
  • hydrogen tetrachloroaurate trihydrate
  • tetraoctylammonium bromide
  • triphenylphosphine
  • sodium borohydride
References: 
Weare WW, Reed SM, Warner MG, and Hutchinson JE. 2000. Improved Synthesis of Small (dCore = 1.5 nm) Phosphine-Stabilizied Gold Nanoparticles JACS 122(51): 12890-12891.
Schmid G, Pfiel R, Boese R, Bandermann F, Meyer S, Calis GHM, van der Velden JWA. 1981. A. Chem. Ber 114: 3634.
InterNano Taxonomy: