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2010210144

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Supporting Online Material for
Candle Soot as a Template for a Transparent Robust
Superamphiphobic Coating
Xu Deng, Lena Mammen, Hans-Jürgen Butt, Doris Vollmer*
*To whom correspondence should be adddressed. E-mail: vollmerd@mpip-mainz.mpg.de
Published 1 December 2011 on Science Express
DOI: 10.1126/science.1207115
This PDF file includes:
Materials and Methods
SOM Text
Figs. S1 to S11
Tables S1 and S2
References
Captions for Movies S1 to S3
Other Supporting Online Material for this manuscript includes the following:
(available at www.sciencemag.org/cgi/content/full/science.1207115/DC1)
Movies S1 to S3
Materials and Methods
Materials
Tetraethoxysilane (TES) (Acros Organics, 98%), ammonia (VWR, 28%), (tridecafluoro-
1,1,2,2-tetrahydrooctyl)-1-trichlorosilane (Sigma Aldrich, 97%), milli-Q water,
diiodomethane, ethylene glycol, penaut oil (commercial), olive oil (commercial), hexadecane
and tetradecane were used without further purification.
Characterization
The morphology of the soot particles and the coating were characterized by
Scanning Electron Microscopy (low voltage LEO 1530 Gemini, Germany, and SU8000,
Hitachi, Japan). The samples were prepared on a silicon wafer and investigated without
further treatment. After calcination the hollow silica networks were imaged by
Transmission Electron Microscopy (FEI, 200 kV). Static, advancing, receding, and roll
off angles were measured with a contact angle meter, Dataphysics OCA35 (Data Physics
Instruments GmbH, Germany). Transmission was measured using an ultraviolet-visible
spectrometer (Lambda 900, Perkin Elmer) in double-beam mode, using an uncovered
glass slide as a reference. High speed movies were taken with a high speed camera
(Photron, Fastcam SA1).
Methods
Chemical vapor deposition of TES: The soot coated substrates (glass or silicon)
were placed in a desiccator together with two open glass vessels containing about 2 ml of
tetraethoxysilane (TES) and aqueous ammonia solution, respectively (Fig. S1). The
desiccator was closed again and chemical vapor deposition (CVD) of TES was carried
out for 24 h, if not stated otherwise. Similar to a Stöber reaction (33), silica is formed by
hydrolysis and condensation of TES catalysed by ammonia (34).
Fig. S1. Sketch of a desiccator together with the soot coated substrate (middle) and two
glass vessels, containing tetraethoxysilane (TES) and ammonia solution (NH3),
respectively.
Silica shells prepared by the Stöber reaction are nano-porous. During calcination, carbon
(in general a polymer) cores thermally degrade and carbon diffuses through the silica
shell (35-37). After calcination of the fractal-like carbon/silica network at 600°C for 2 h
in air, the hydrophilic silica coating is hollow. To transform it into a superamphiphobic
coating chemical vapor deposition (CVD) of a semi-fluorinated silane on the films was
performed. Therefore, the coated substrate and an open glass vessel containing about 0.1
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