Supplementary Information
Dynamically tunable nanoparticle engineering enabled by short
contact-time microfluidic synthesis with a reactive gas
Md. Taifur Rahman , Prasanna G. Krishnamurthy , Pravien Parthiban , Abhinav Jain , Chan
Pil Park , Dong-Pyo Kim and Saif A. Khan
Experimental Details
Materials: 3-aminopropyl tris(trimethylsiloxy)silane (APTTS, 99%), hydrogen
tetrachloroaurate(III) trihydrate (HAuCl4, 99.99%), tetrakis(hydroxymethyl) phosphonium
chloride (THPC, 80% in water), sodium hydroxide (NaOH, Reagent grade, 97%), acetonitrile
(CH3CN, HPLC grade 99.9%), potassium carbonate (K2CO3, 99.99%),
Octadecafluorodecahydronaphthalene (Perfluorodecalin, Fluka, mixture of cis and trans,
95%) from Sigma-Aldrich Co. Ltd., Singapore, were all used as obtained without any further
purification. De-ionized water and glassware washed in aqua regia and rinsed thoroughly in
water were used for all experiments.
Synthesis of amino-functionalized silica spheres: 230 nm silica particles were
synthesized by the Stöber method.
1
The surfaces of silica spheres were functionalized with
APTTS in refluxing acetonitrile. Amino-functionalized silica particles were washed with
acetonitrile, ethanol and DI water by sonication and several cycles of centrifugation.
2,3
Gold-seeded silica particles: 2-3 nm colloidal gold particles used for seeding the amino-
functionalized silica was made according to the procedure of Duff et al.
4
Under rapid stirring
1.5 mL of 0.2 mM aqueous NaOH and 1.0 mL of 67.7 mM aqueous THPC were sequentially
added to 45.5 mL of DI water followed by addition of 2 mL of aqueous 25 mM HAuCl
4
. The
solution immediately turned brown-red indicative of the colloidal gold formation. 150 µL of
amino-functionalized silica particles suspension with 20ml of colloidal gold solution was
shaken for 8 hours at room temperature and centrifuged to separate the gold-seeded silica
particles. These particles were washed three times with water by cycles of centrifugation to
remove the unattached colloidal gold particles.
K-Gold Solution: 3 mL of 1 wt% HAuCl4 was taken with 50 mg K
2
CO
3
in 200 mL DI
water (1.8mM) and aged for 1 day to produce a colorless gold plating solution, so-called K-
gold, containing gold hydroxide ions.
5
Microfabrication: Microfluidic device patterns were fabricated onto silicon wafers by
standard photolithography using negative photoresist SU-8 2050.
6
Devices were subsequently
moulded in poly(dimethyl siloxane) (PDMS) using the soft lithography technique. PDMS
was molded onto the SU-8 masters at 70˚C for 2 hrs, peeled, cut and cleaned. Inlet and outlet
holes (1/16-in. o.d.) were punched into the device. The microchannels were irreversibly
bonded to a glass slide pre-coated with a thin layer of PDMS after a brief 35 s air plasma
treatment. The bonded devices were then cured for 24 hours at 100˚C. The microchannels
have rectangular cross-section and the details of the channel dimensions are: width and depth
of the liquid and gas channel are 300 μm and ~124 μm and 100 μm and ~124 μm
respectively, and the parallel liquid and gas channels are separated by 200 μm. Devices with
lengths of the parallel channel section of 91.5 cm and 21.8 cm were used.
Electronic Supplementary Material (ESI) for RSC Advances
This journal is © The Royal Society of Chemistry 2013