Thermogravimetric analysis

About: Thermogravimetric analysis is a research topic. Over the lifetime, 37248 publications have been published within this topic receiving 862144 citations. The topic is also known as: thermal gravimetric analysis & TGA.

High thermal and chemical stability in pyrazolate-bridged metal–organic frameworks with exposed metal sites

Abstract: Reactions between the tritopic pyrazole-based ligand 1,3,5-tris(1H-pyrazol-4-yl)benzene (H3BTP) and transition metal acetate salts in DMF afford microporous pyrazolate-bridged metal–organic frameworks of the type M3(BTP)2·xsolvent (M = Ni (1), Cu, (2), Zn (3), Co (4)). Ab-initioX-ray powder diffraction methods were employed in determining the crystal structures of these compounds, revealing 1 and 2 to exhibit an expanded sodalite-like framework with accessible metal cation sites, while 3 and 4 possess tetragonal frameworks with hydrophobic surfaces and narrower channel diameters. Compounds 1–4 can be desolvated without loss of crystallinity by heating under dynamic vacuum, giving rise to microporous solids with BET surface areas of 1650, 1860, 930 and 1027 m2 g−1, respectively. Thermogravimetric analyses and powder X-ray diffraction measurements demonstrate the exceptional thermal and chemical stability of these frameworks. In particular, 3 is stable to heating in air up to at least 510 °C, while 1 is stable to heating in air to 430 °C, as well as to treatment with boiling aqueous solutions of pH 2 to 14 for two weeks. Unexpectedly, 2 and 3 are converted into new crystalline metal–organic frameworks upon heating in boiling water. With the combination of stability under extreme conditions, high surface area, and exposed metal sites, it is anticipated that 1 may open the way to testing metal–organic frameworks for catalytic processes that currently employ zeolites.

Thermogravimetric Analysis of the Oxidation of Multiwalled Carbon Nanotubes: Evidence for the Role of Defect Sites in Carbon Nanotube Chemistry

Abstract: Thermogravimetric analysis (TGA) has demonstrated that multiwalled nanotubes (MWNTs) annealed at 2200 to 2800 °C are more air stable than as-produced MWNTs, diamond, graphite, and annealed diamond. The annealed MWNTs are similar in stability to annealed graphite. Defect sites along the walls and at the ends of the raw MWNTs facilitate the thermal oxidative destruction of the nanotubes. Thermal annealing removes these defects, thereby providing MWNTs with enhanced air stability.

Enhancement of photocatalytic activity of mesoporous TiO2 by using carbon nanotubes

Abstract: Titanium dioxide/carbon nanotubes (TiO 2 /CNTs) composites were prepared with the aid of ultrasonic irradiation. Products of different TiO 2 :CNTs molar ratio were characterized by X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), Brunauer–Emmett–Teller (BET) adsorption analysis, thermogravimetric and differential thermal analysis (TGA–DSC), photoluminescence (PL) and UV–vis spectroscopy measurements (UV–vis). The photocatalytic activity was evaluated by the degradation of acetone and by the detection of the hydroxyl radical (·OH) signals using electron paramagnetic resonance (EPR). It is found that the crystalline TiO 2 is composed of both anatase and brookite phases. The agglomerated morphology and the particle size of TiO 2 in the composites change in the presence of CNTs. The CNTs in the composites are virtually all covered by TiO 2 . Other than an increase of the surface area, the addition of CNTs does not affect the mesoporous nature of the TiO 2 . Meanwhile, more hydroxyl groups are available on the surface of the composite than in the case of the pure TiO 2 . The higher the content of CNTs, there is more effective in the suppression of the recombination of photo-generated e − /h + pairs. However, excessive CNTs also shield the TiO 2 from absorbing UV light. The optimal amount of TiO 2 and CNTs is in the range of 1:0.1 and 1:0.2 (feedstock molar ratio). These samples have much more highly photocatalytic activity than P25 and TiO 2 /activated carbon (AC) composite. The mechanism for the enhanced photocatalytic activity of TiO 2 by CNTs is proposed.

OH Surface Density of SiO2 and TiO2 by Thermogravimetric Analysis

Abstract: Thermogravimetric analysis (TGA) is investigated for determination of the OH surface density (OH/nm2) and carbon content of silica and titania powders made by flame aerosol and sol−gel processes. It is shown that it is possible to distinguish between physically adsorbed and chemically bound water and to rapidly determine the OH surface density even of small powder samples (<0.2 g) by TGA calibrated with LiAlH4 titration data. The high accuracy of the OH surface density determination by TGA is confirmed further with additional LiAlH4 titration data of silica powders and by comparison with the specifications of commercially available silica Aerosil and titania P25 powders. Furthermore, by connecting a CO2 sensor or a mass spectrometer to the TGA balance, it is possible to verify the carbon content and determine other components (organic residues) of the powders. Thereby, it is shown that flame-made powders have high purity while the preparation conditions of sol−gel powders greatly affect their purity. At a...