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5 protocols using 3 chloropropyltrimethoxysilane

1

Synthesis of Graphene-Based Composites

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Tetraethoxysilane (TEOS, 98%), 3-chloropropyltrimethoxysilane (Cl-PTES, 97%), and graphite were purchased from Alfa Aesar (China), and cetyltrimethylammonium bromide (CTAB, 99%) was purchased from Acros (Japan). Acetonitrile (ACN, 99%), dimethylformamide (DMF, 99%), and cyclohexane (99%) were obtained from Merck. (American) Ethynylferrocene (97%), lithium perchlorate (95%), lithium chloride (95%), copper sulfate (99%), sodium diethyldithiocarbamate trihydrate, and HCl (37%) were purchased from Sigma-Aldrich. Sodium nitrate (99%), ascorbic acid (97%), tetrabutylammonium bromide (99%), and poly(vinyl alcohol) (PVA, MW = 72,000 g/mol) originated from Fluka. graphite foils and scotch tape were purchased from Shanghai Carbon Co. Ltd (Shanghai, China). and 3M, respectively. Sodium sulfate anhydrous (99%), manganese sulfate (95%), concentrated sulfuric acid (98%), and aniline (99%) were from Meryer, Kaitong, Kermal, and Macklin, respectively. All compounds were used directly without further purification. The (3-azidopropyl) triethoxysilane (AzPTES) was synthesized with the protocol reported previously [34 (link)].
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2

Synthesis of Functionalized Nanoparticles

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PEG 1500, PEG 8000, LUDOX® SM colloidal silica, silica nanopowder (diameter 12 nm, surface area 175–225 m2/g), N-methylpyrrolidine, hexamethylene diisocyanate, methanesulfonyl chloride and sodium azide were purchased form MilliporeSigma (Darmstad, Germany). 2-Amino-4-hydroxy-6-methylpyrimidine was received form TCI (Eschborn, Germany). (3-chloropropyl)trimethoxysilane and triethylamine were purchased form Alfa Aesar (Kandel, Germany). (Dodecyl)dimethylsilane was obtained from Acros Organics (Geel, Belgium). Triphenylphosphine was purchased form Roth. Lithium bis(trifluoromethylsulfonyl)imide (LiTFSI) was received form IoLiTec (Eschborn, Germany).
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3

Synthesis of Azide-Functionalized Silane Precursor

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Tetraethoxysilane (TEOS, 98%), 3-chloropropyltrimethoxysilane (Cl-PTES, 97%) and graphite were purchased from Alfa Aesar and cetyltrimethylammonium bromide (CTAB, 99%) from Acros. Acetonitrile (ACN, 99%), dimethylformamide (DMF, 99%) and cyclohexane (99%) were obtained from Merck. Ethynylferrocene (97%), lithium perchlorate (95%), lithium chloride (95%), copper sulfate (99%), Sodium diethyldithiocarbamate trihydrate, and HCl (37%) were purchased from Sigma-Aldrich. Sodium nitrate (99%), ascorbic acid (97%), tetrabutylammonium bromide (99%) and poly(vinyl alcohol) (PVA, MW = 72000 g/mol) originated from Fluka. All compounds were used directly without further purification.
Preparation of 3-azidopropyltrimethoxysilane (AzPTMS). The AzPTMS precursor was synthesized by adding 2 g of Cl-PTES, 1.08 g sodium azide and 1.29 g tetrabutylammonium bromide) in 100 mL ACN, which was stirred and refluxed at 90 o C for 24 h under nitrogen atmosphere. Then, the ACN solvent was removed by rotary evaporation at 80 o C under a vacuum of 0.2 bar. The residual mixture was suspended in cyclohexane and filtered with filter paper. The residual cyclohexane was further removed by rotary evaporation at 80 o C under pressure of 0.2 bar and the oily Az-PTMS can be finally obtained. Yield: ~1.3 g, 65 %. 1 H NMR (400 MHz, CDCl3): δ (ppm) 3.82 (s, 9H), 3.65 (t, 2H, 8.25 Hz), 1.24 (m, 2H), 0.75 (t, 2H, 8.31 Hz).
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4

Fabrication of Thermoplastic Starch Composites

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The thermoplastic starch in this study was obtained from S.D. Fine Chemicals in India. The majority (97%) of the obtained 3-chloropropyl trimethoxysilane was obtained from Alfa Aesar in India. Acetic acid, dichloromethane, and methanol (99%) were purchased from Sigma Aldrich in India. All chemicals obtained were used without any further purification.
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5

Electrochemical Polymer Composite Characterization

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Poly(vinylidene fluoride-co-hexafluoropropylene) (PVDF-HFP), 1-butyl-3-methylimidazolium tetrafluoroborate ([BMIM][BF4]), and 1-bromohexane were purchased from Sigma Aldrich and were used as received. (3-Chloropropyl)trimethoxysilane, 4,4′-bipyridine, ferrocene (Fc), and ammonium hexafluorophosphate (NH4PF6) were purchased from Alfa Aesar. Dimethylformamide, acetonitrile, methanol, acetone, and diethyl ether were obtained commercially and used without further purification. Indium tin oxide (ITO) coated glass specimens with thicknesses of 68.5 nm, 140.3 nm, and 252.1 nm were purchased from Wooyang GMS (Korea). Before use, the ITO-coated glasses were cleaned successively with deionized water, acetone, and isopropyl alcohol under sonication.
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