Highly degradable imine-doped mesoporous silica particles

2/4/2019 12:00:00 AM

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Authors:Leana Travaglini, Pierre Picchetti, Ricardo Totovao, Eko Adi Prasetyanto, Luisa De Cola

Publication date: Januari 2019

Materials Chemistry Frontiers

Volume:  1, S1-S16

Link : http://www.rsc.org/suppdata/c8/qm/c8qm00438b/c8qm00438b1.pdf

 

Materials Chemistry Frontiers, vol 1. S1-S16. January 2019, http://www.rsc.org/suppdata/c8/qm/c8qm00438b/c8qm00438b1.pdf

1. Instruments Nuclear magnetic resonance (NMR):1H and 13C NMR spectra were recorded on Bruker Avance 400 spectrometer. The 1H NMR chemical shiftsδ are reported in parts per million (ppm) with residual protons of the deuterated solvent as the reference standard. Signal splittings are described as singlet (s), quartet (q), triplett (t), multiplet (m).Scanning(SEM)and Scanning Transmission(STEM) Electron Microscopy:SEM and STEM images were recorded with a FEI Quanta FEG 250 instrument (FEI corporate, Hillsboro, Oregon, USA) with an acceleration voltage of 20 kV. The SEM sampleswereprepared by drop-casting a dispersion of particles in EtOH onto a glass cover slip, subsequently sputter coated with Au (Emitech K575X Peltier cooled) for 30s at 60 mA prior to fixation on an Al support.The STEM samples were prepared by drop casting dispersions of particles in EtOH (0.1 mg/mL) onto Formvar-coated Cu grids (400 mesh) and allowed to dry overnight prior visualization. Transmission Electron Microscopy (TEM):TEM samples were analyzed on a FEI/PHILIPS CM120 system operating at 100 kV. Samples were prepared by drop casting dispersions of particles in EtOH (0.1 mg/mL) onto Formvar-coated Cu grids (400 mesh) and allowed to dry overnight prior visualization. Porosimetry:Nitrogen physisorption isotherms were obtained with a Micromeritics ASAP-2020 physisorption instrument. The MSPs sample was degassed at 350 °C for 4h, while the Im-MSPs onesat 80 °C for 6h. The N2adsorption/desorption measurementswereperformed at -196 °C. The surface areas were calculated by Brunauer-Emmett-Teller (BET) method in the relative pressure range p/p00.06-0.3.[1]The pore size distributions and pore volumes were calculated by density functional theory (DFT) method on the adsorption branch using a cylindrical model. The total pore volume was estimated at p/p0= 0.99.Small Angle X-ray Scattering (SAXS):SAXS set-up comprised the SAXSess mc2 instrument from Anton Paar GmbH, containing a slit collimation system, and the PW3830 laboratory X-ray generator (40 kV, 50 mA) with a long-fine focus sealed X-ray tube (CuKα wavelength of λ= 0.1542 nm) from PANalytical. Detection was performed with the 2D imaging-plate reader Cyclone® by Perkin Elmer. Measurements were performed on powder samplesfor 5 minand the data collected up to a scattering vector qvalue of 7 nm-1, where q= (4πsinθ)/λ and 2θ the scattering angle. The 2D data were converted to 1D data and background-corrected by using the SAXSQuant software (Anton Paar GmbH, Austria)