In situ formation of intermetallic/ceramic composites composed of molybdenum silicides (Mo5Si3 and Mo3Si) and magnesium aluminate spinel (MgAl2O4) was conducted by combustion synthesis with reducing stages in the mode of self-propagating high-temperature synthesis (SHS). The SHS process combined intermetallic combustion between Mo and Si with metallothermic reduction of MoO3 by Al in the presence of MgO. Experimental evidence showed that combustion velocity and temperature decreased with increasing molar content of Mo5Si3 and Mo3Si, and therefore, the flammability limit determined for the reaction at Mo5Si3 or Mo3Si/MgAl2O4 = 2.0. Based upon combustion wave kinetics, the activation energies, Ea = 68.8 and 63.8 kJ/mol, were deduced for the solid-state SHS reactions producing Mo5Si3– and Mo3Si–MgAl2O4 composites, respectively. Phase conversion was almost complete after combustion, with the exception of trivial unreacted Mo existing in both composites and a minor amount of Mo3Si in the Mo5Si3–MgAl2O4 composite. Both composites display a dense morphology formed by connecting MgAl2O4 crystals, within which micro-sized molybdenum silicide grains were embedded. For equimolar Mo5Si3– and Mo3Si–MgAl2O4 composites, the hardness and fracture toughness are 14.6 GPa and 6.28 MPa m1/2, and 13.9 GPa and 5.98 MPa m1/2, respectively.
In the present article, we report a novel colorimetric probe (TNT@MB) for the detection of the phosphate ion, which is based on the strong binding affinity between the phosphate ion and titanium dioxide nanotubes (TNTs). TNTs were synthesized from TiO2 nanoparticles by hydrothermal treatment. The obtained TNTs had an average length of 200 ± 50 nm and an average width of 12 ± 5 nm. TNT@MB was prepared by adsorbing methyl blue onto TNTs in acidic condition. The optimal synthesis conditions for TNT@MB consisted in having 0.05 g of TNTs react with 1 μmole of methyl blue at pH 2 for 90 min. TNTs and TNT@MB were characterized by UV–vis diffuse reflection spectroscopy, TEM, FTIR, and XPS. The phosphate-ion sensing behavior of TNT@MB was investigated by UV–visible spectroscopy. The phosphate-ion concentration linear range and detection limit of this method based on TNT@MB were 1–40 μM and 0.59 μM, respectively. A sample of lake water was used as a real sample, and analyte recovery rates were measured in the 102.5–103.6% range, with relative standard deviations below 5.6% (n = 3). We also found that this probe could be reused after regeneration in alkaline solution. These results indicate that as a colorimetric probe, TNT@MB has the advantages of being environmentally friendly, inexpensive, and simple to use, as well as giving rise to an easily observable color change.
The formation of NbB2–MgAl2O4 composites from the MgO-added thermite-based reaction systems was investigated by self-propagating high-temperature synthesis (SHS). Two thermite mixtures, Nb2O5/B2O3/Al and Nb2O5/Al, were, respectively, adopted in Reactions (1) and (2). The XRD analysis confirmed the combination of Al2O3 with MgO to form MgAl2O4 during the SHS process and that excess boron of 30 atom.% was required to yield NbB2–MgAl2O4 composites with negligible NbB and Nb3B4. The microstructure of the composite reveals that rod-shaped MgAl2O4 crystals are closely interlocked and granular NbB2 are embedded in or scattered over MgAl2O4. With the addition of MgAl2O4, the fracture toughness (KIC) of 4.37–4.82 MPa m1/2 was obtained for the composites. The activation energies Ea = 219.5 ± 16 and 167.9 ± 13 kJ/mol for Reactions (1) and (2) were determined from combustion wave kinetics.
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