Design of experiments: Optimizing the polycarboxylation/functionalization of tungsten disulfide nanotubes

Daniel Raichman, David Strawser, Jean Paul Lellouche

Research output: Contribution to journalArticlepeer-review

5 Scopus citations


Design of experiments (DOE) methodology was used to identify and optimize factors that influence the degree of functionalization (polycarboxylation) of WS2 INTs via a modified acidic Vilsmeier-Haack reagent. The six factors investigated were reaction time, temperature and the concentrations of 2-bromoacetic acid, WS2 INTs, silver acetate and DMF. The significance of each factor and the associated interactive effects were evaluated using a two-level factorial statistical design in conjunction with statistical software (MiniTab® 16) based on quadratic programming. Although statistical analysis indicated that no factors were statistically significant, time, temperature and concentration of silver acetate were found to be the most important contributors to obtaining maximum functionalization/carboxylation. By examining contour plots and interaction plots, it was determined that optimal functionalization is obtained in a temperature range of 115-120 °C with a reaction time of 54 h using a mixture of 6 mL DMF, 200 mg INTs, 800 mg 2-bromoacetic acid and 60 mg silver acetate.

Original languageEnglish
Pages (from-to)455-467
Number of pages13
Issue number3
StatePublished - 2014

Bibliographical note

Publisher Copyright:
© 2014 by the authors.


  • DOE
  • Design of experiments
  • Nanotubes
  • Optimization
  • Tungsten disulfide
  • Vilsmeier-Haack reagents
  • WS2 INTs


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