The effect of alkyl chain length on the level of capping of silicon nanoparticles produced by a one-pot synthesis route based on the chemical reduction of micelle

  • Shane P. Ashby
  • Jason A. Thomas
  • Paul R. Coxon
  • Matthew Bilton
  • Rik Brydson
  • Timothy J. Pennycook
  • Yimin Chao
Research Paper


Silicon nanoparticles (SiNPs) can be synthesized by a variety of methods. In many cases these routines are non-scalable with low product yields or employ toxic reagents. One way to overcome these drawbacks is to use one-pot synthesis based on the chemical reduction of micelles. In the following study trichloroalkylsilanes of differing chain lengths were used as a surfactant, and the level of capping, surface bonding and size of the nanoparticles formed has been investigated. FTIR results show that the degree of alkyl capping for SiNPs with different capping layers was constant, although SiNPs bound with shorter chains display a much higher level of Si–O owing to the reaction of the ethanol used in the method with uncapped sites on the particle. SiNPs with longer chain length capping show a sharp Si–H peak on the FTIR, these were heated at reflux with the corresponding 1-alkene to fully cap these particles, resulting in a reduction/disappearance of this peak with a minimal change in the intensity of the Si–O peak. Other techniques used to analyze the surface bonding and composition, XPS, 1H-NMR, and TEM/EDX, show that alkyl-capped SiNPs have been produced using this method. The optical properties showed no significant changes between the different capped SiNPs.


Silicon Nanoparticles FTIR XPS Quantum yield HRTEM 



This study is supported by the UK Engineering and Physical Science Research Council (ESPRC), under the grant code (EP/G01664X/1) and European Thermodynamics Ltd. STEM measurements were performed at the EPSRC UK National Facility for Aberration-Corrected STEM managed by the SuperSTEM consortium. The research leading to the XPS results received funding from the European Community’s Seventh Framework Programme (FP7/2007-2013) under grant agreement No 226716 and the help of Dr Alexei Preobrajenski is gratefully received. LENNF is thanked for access to HRTEM facilities. Prof Steve Meech is thanked for critical checking and discussion of the manuscript.

Supplementary material

11051_2013_1425_MOESM1_ESM.pdf (132 kb)
Supplementary material 1 (PDF 132 kb)


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Copyright information

© Springer Science+Business Media Dordrecht 2013

Authors and Affiliations

  • Shane P. Ashby
    • 1
  • Jason A. Thomas
    • 1
  • Paul R. Coxon
    • 1
  • Matthew Bilton
    • 2
  • Rik Brydson
    • 2
  • Timothy J. Pennycook
    • 3
    • 4
  • Yimin Chao
    • 1
  1. 1.Energy Materials Laboratory, School of ChemistryUniversity of East AngliaNorwichUK
  2. 2.School of Process, Environmental and Materials Engineering, Institute for Materials ResearchUniversity of LeedsLeedsUK
  3. 3.SuperSTEM LaboratoryWarringtonUK
  4. 4.Department of MaterialsUniversity of OxfordOxfordUK

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