The reagents phthalonitrile (TCI, Philadelphia, PA, USA), trimethylsilyl trifluoromethanesulfonate (Synquest, Alachua, FL, USA), chlorotrimethylsilane (Acros, Fair Lawn, NJ, USA), silicon tetrachloride (Sigma, Sheboygan, WI, USA) and 1,3-diiminoisoindoline (TCI, Philadelphia, PA, USA) were obtained commercially and used as received. Lithium bis(trimethylsilylamide) etherate [30 (link)], HCl gas [31 (link)] and bis(3,4,5-trifluorophenoxy) silicon phthalocyanine [32 (link)] were prepared as outlined in literature. All solvents were ACS grade; dry solvents were obtained by passing through activated alumina on a J.C. Meyer solvent purification system. Quinoline (Oakwood, Estill, SC, USA) was distilled over zinc dust. All reactions were performed under an atmosphere of dry nitrogen. NMR spectra were run in either DMSO-d6 or MeCN-d3 solutions at room temperature on a Bruker Avance 300 or 400 MHz spectrometer (Billerica, MA, USA, Figures S2–S4 ). 19F-NMR spectra were referenced to trifluoroacetic acid at −76.55 ppm (Figure S5 ). IR spectra of solid samples were recorded on an Agilent Technologies Cary 630 FT-IR spectrometer (Cary, NC, USA).
Silicon tetrachloride
Manufactured by Merck Group
Sourced in United States
Silicon tetrachloride is a colorless, volatile liquid chemical compound with the formula SiCl4. It is widely used as a precursor in the production of various silicon-based materials and compounds.
Automatically generated - may contain errors
Lab products found in correlation
N n diisopropylcarbodiimide, by Merck Group (2 mentions)
Chlorotrimethylsilane, by Thermo Fisher Scientific (1 mentions)
Cary 630 ftir spectrometer, by Agilent Technologies (1 mentions)
Tetraoctylammonium bromide, by Merck Group (1 mentions)
Absolute ethanol, by Merck Group (1 mentions)
Butyl lithium, by Merck Group (1 mentions)
Chloroform, by Merck Group (1 mentions)
N hexane, by Merck Group (1 mentions)
Cucl2 2h2o, by Merck Group (1 mentions)
Sodium borohydride, by Merck Group (1 mentions)
N butyllithium, by Merck Group (1 mentions)
Carbon coated copper grid, by Electron Microscopy Sciences (1 mentions)
Acetone, by ITW Reagents (1 mentions)
Isopropanol, by ITW Reagents (1 mentions)
Tetraethylene glycol dimethyl ether, by Merck Group (1 mentions)
Ethanol, by ITW Reagents (1 mentions)
Phosphate buffer saline (pbs), by Thermo Fisher Scientific (1 mentions)
Toluene, by Merck Group (1 mentions)
6 protocols using silicon tetrachloride
1
Synthesis and Characterization of Fluorinated Phthalocyanines
2
Synthesis of Nanoparticle Precursors
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Tetraoctyl ammonium bromide
(TOAB), silicon tetrachloride (99%), lithium aluminum hydride in tetrahydrofuran
(LAH in THF), and chloroplatonic acid hexa-hydrated in Isopropanol
were purchased from Sigma-Aldrich. Toluene (99%), methanol, allylamine,
ammonium thiocyanate, potassium thiocyanate, phosphate-buffered saline
(PBS) buffer, and ammonium chloride were purchased from the Marck,
Mumbai, India. Double-distilled water obtained from the water double
distillation set. After distillation, toluene and methanol were used
after distillation.
(TOAB), silicon tetrachloride (99%), lithium aluminum hydride in tetrahydrofuran
(LAH in THF), and chloroplatonic acid hexa-hydrated in Isopropanol
were purchased from Sigma-Aldrich. Toluene (99%), methanol, allylamine,
ammonium thiocyanate, potassium thiocyanate, phosphate-buffered saline
(PBS) buffer, and ammonium chloride were purchased from the Marck,
Mumbai, India. Double-distilled water obtained from the water double
distillation set. After distillation, toluene and methanol were used
after distillation.
3
Synthesis of Trisilane via Carbodiimide
4
Synthesis of Cu-SiOx Catalysts
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For the synthesis of 2.5% silica-loaded Cu catalysts, 0.5984 g of CuCl2.2H2O (Sigma-Aldrich, ACS reagent, ≥99.0%) was dissolved into 180 mL ethanol under magnetic stirring. Then 90 μL of silicon tetrachloride (Sigma-Aldrich, 99.998% trace metals basis) was injected into the Cu(II) solutions. Afterward, 0.6 g of sodium borohydride (Sigma-Aldrich, powder, ≥98.0%) dispersed in 120 mL of ethanol was added into the above-mentioned solution under stirring. The color of the solutions changed from blue to darkish. After stirring for 5 min, precipitates formed in the solution were kept for 30 mins and then centrifuged. The as-prepared Cu-SiOx precipitates were washed with ethanol under intense ultrasonication at least three times to remove all unreacted reagents. The Cu-SiOx catalysts were then dried under vacuum at room temperature overnight. The silica-loaded Cu catalysts with different Si/Cu ratios of 0, 0.01, and 0.05 were synthesized by following a procedure similar to that described above, except for changing the amount of silicon tetrachloride.
5
Synthesis of Nanostructured Materials
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N,N′-Diisopropylcarbodiimide (99%), silicon tetrachloride (99%), n-butyllithium (2.5 M in hexane), and NaH (90%) were purchased from Sigma-Aldrich and used without further purification. Fomblin Y oil was purchased from Merck (CAS:69991-67-9). NVH-type oil was purchased from Cargille Laboratories, NJ, USA. Silicon particles were purchased from Nanomakers (40 nm). n-Bu4PF6 (electrochemical grade) was purchased from Fluka. Tetrahydrofuran (THF) was obtained from an MBraun MBSPS 5 solvent purification system. Toluene, dimethylformamide (DMF), and formamide were dried using an Innovative Technology solvent purification system, then oxygen was removed by three freeze–pump–thaw cycles. The purified solvents were stored over 3 Å molecular sieves in an argon filled glovebox. Carbon-coated copper grids were purchased from Electron Microscopy Sciences (Hatfield, PA). All the experiments were carried out under inert atmosphere, with Schlenk techniques or in an argon-filled glovebox.
6
Titanium Surface Preparation Protocol
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Commercially pure grade 2 titanium was purchased as 2m rods of 10mm in diameter, which were cut into disks of 2mm disks (VDM metals, Germany). Silicon carbide grinding paper of different particle size (P400, P600, P800, P1200 and P2500) and colloidal silica suspension (Eposil M11, particle size 0.06µm) were purchased from Neurtek (Spain). Isopropanol (>99.7%), ethanol (96%) and acetone (99%) were obtained from Panreac (Germany) and used without further purification. Toluene (99.9%), tetraethylene glycol dimethyl ether (tetraglyme, 99%), PEG (M w =1000g/mol), bis(3-aminopropyl)-poly(ethylene glycol) (PEG-amine), trimethylamine, silicon tetrachloride were purchased from Sigma Aldrich (USA) and used without further purification. Phosphate buffer saline (PBS, pH=7.4, Gibco, US) is purchased as 5g tablets which are dissolved in 500mL of distilled water and autoclaved at 121ºC for 1h before using.
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