With the aim to enhance interfacial adhesion of a hydrophobic polymer matrix and cellulosic fibers and fillers, chemical surface modifications with silane coupling agents are performed. Thermogravimetric analysis (TGA) could be used to determine the degree of surface functionalization. However, similar thermal properties of treated and untreated cellulose hamper a precise determination of silane loading. This contribution deals with quantitative determination of silane loading combining both TGA and elemental analysis. Firstly, silane modified celluloses were studied by FT-IR, Raman, solid state NMR spectroscopy, and polarized light microscopy in order to determine functional groups and to study the impact of chemical treatment on cellulose morphology. Secondly, thermal stability and pyrolysis processes were studied by TG-MS analysis. In order to determine the exact silane loading, the mass percentages of the appropriate elements were quantified by elemental analysis and correlated with the charred residues determined by TGA yielding a linear dependency. With that correlation, it was possible to determine silane loadings for additional samples utilizing simple TGA measurements. The main advantage of that approach is that only one calibration is necessary for routine analyses of further samples and TGA-MS coupling gives additional information on thermal stability and pyrolysis routes, simultaneously.
Porous networks of Pt nanoparticles interlinked by bifunctional organic ligands have shown high potential as catalysts in micro‐machined hydrogen gas sensors. By varying the ligand among p‐phenylenediamine, benzidine, 4,4‘‘‐diamino‐p‐terphenyl, 1,5‐diaminonaphthalene, and trans‐1,4‐diaminocyclohexane, new variants of such networks were synthesized. Inter‐particle distances within the networks, determined via transmission electron microscopy tomography, varied from 0.8 to 1.4 nm in accordance with the nominal length of the respective ligand. While stable structures with intact and coordinatively bonded diamines were formed with all ligands, aromatic diamines showed superior thermal stability. The networks exhibited mesoporous structures depending on ligand and synthesis strategy and performed well as catalysts in hydrogen gas microsensors. They demonstrate the possibility of deliberately tuning micro‐ and mesoporosity and thereby transport properties and steric demands by choice of the right ligand also for other applications in heterogeneous catalysis.
This paper presents a highly sensitive thermoelectric sensor for catalytic combustible gas detection. The sensor contains two low-stress (+176 MPa) membranes of a combination of stoichiometric and silicon-rich silicon nitride that makes them chemically and thermally stable. The complete fabrication process with details, especially the challenges and their solutions, is discussed elaborately. In addition, a comprehensive evaluation of design criteria and a comparative analysis of different sensor designs are performed with respect to the homogeneity of the temperature field on the membrane, power consumption, and thermal sensitivity. Evaluating the respective tradeoffs, the best design is selected. The selected sensor has a linear thermal characteristic with a sensitivity of 6.54 mV/K. Additionally, the temperature profile on the membrane is quite homogeneous (20% root mean standard deviation), which is important for the stability of the catalytic layer. Most importantly, the sensor with a ligand (p-Phenylenediamine (PDA))-linked platinum nanoparticles catalyst shows exceptionally high response to hydrogen gas, i.e., 752 mV at 2% concentration.
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