Scalable Synthesis of a New Class of Polymer Microrods by a Liquid–Liquid Dispersion Technique
✍ Scribed by R. G. Alargova; K. H. Bhatt; V. N. Paunov; O. D. Velev
- Publisher
- John Wiley and Sons
- Year
- 2004
- Tongue
- English
- Weight
- 224 KB
- Volume
- 16
- Category
- Article
- ISSN
- 0935-9648
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✦ Synopsis
Fabrication of PPy Nanoparticles: For the synthesis of the PPy nanoparticles with an average diameter of 2 nm, octyltrimethylammonium bromide (OTAB; 6.0 g) was magnetically stirred in 40 mL of distilled water at 3 C. Pyrrole (1.0 g) was then added dropwise to the surfactant solution, and iron(III) chloride (5.561 g) dissolved in a small amount of distilled water was added to the reaction mixture. Chemical polymerization proceeded for 3 h at 3 C. The reaction product was then transferred to a separating funnel and excess methanol was added to remove the surfactant and residual iron(III) chloride. A small amount of isooctane was added to promote the precipitation of the PPy nanoparticles. The upper solution containing surfactant and unreacted iron(III) chloride was discarded and the nanoparticle precipitate was dried in a vacuum oven at room temperature. PPy nanoparticles with a diameter of about 6 nm were prepared using decyltrimethylammonium bromide (DeTAB; 2.3 g), following the same procedure.
Carbonization Process: In a typical carbonization procedure, the PPy nanoparticles (about 2 g) collected from two runs of the microemulsion polymerization were precarbonized at 800 C for 3 h under Ar gas flow (0.2 L min ±1 ). Carbon felt was put at the inlet of Ar flow to reduce the oxidation of the polymer precursor. After the pretreatment at 800 C, the weight of the carbonized product was reduced to 30±35 % of the initial loading weight. The ªmissingº components, formed as a result of carbonization reactions such as denitrogenation, dehydrogenation, and dehalogenation, are removed by the Ar flow. The products of two runs of the pretreatment were collected and transferred to a quartz tube 4 cm in diameter. The quartz tube was evacuated and refilled with argon repeatedly. The argon-filled quartz tube was then placed in an electrical furnace equipped with a larger diameter alumina tube (6 cm in diameter). The valve of the quartz tube was opened and the alumina tube containing the quartz tube was evacuated and refilled with argon repeatedly. The second carbonization proceeded with streaming argon at a heating rate of 3 C min ±1 . After 6 h of carbonization, the residual soot was collected and toluene was added to the quartz tube containing the sublimed fullerene film. The quartz tube was sonicated with gentle heating. The crude soot was refluxed with toluene in a standard Soxhlet extractor at 100 C for 12 h.
Instrumental Analysis: TEM images were taken with a JEOL 2010 F microscope and EDX analysis was performed using a Philips CM 20 microscope. MALDI-TOF mass spectra were obtained with a Voyager-DE STR Biospectrometry Workstation (Applied Biosystems) operating in positive mode at an accelerating voltage of 20 kV using dithranol as the matrix. HPLC analysis was performed with a HP1100 liquid chromatograph. A 250 mm 4.6 mm i.d. monomeric octadecylsilica (ODS) column was used as the stationary phase. A mixture of toluene and methanol (55:45) was used as the mobile phase at a flow rate of 0.6 mL min ±1 . Detection was performed with a diode-array detector at a detection wavelength of 330 nm.
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