Simple, inexpensive mass spectrometric analyzer for thermogravimetry

Selck, David A.; Woodfield, Brian F.; Boerio‐Goates, Juliana; Austin, Daniel E.

doi:10.1002/rcm.5301

Cited by 5 publications

(2 citation statements)

References 20 publications

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“…Thermogravimetric and differential-thermal analyses (TG/DTA) were performed using a Netzsch STA 409PC. Mass spectrometry (MS) measurements were collected in tandem with the TG/DTA measurements using a quadrupole MS unit built in-house . To characterize the water loss and thermal behavior of the Al 2 O 3 during calcination between 300 and 1200 °C, three TG/DTA-MS measurements were recorded in which 30–40 mg of the 300 °C alumina were loaded into an alumina crucible and heated at a rate of either 5°/min from 25 to 1100 °C or 3°/min from 25 to 1300 °C under a flowing He atmosphere.…”

Section: Methodsmentioning

confidence: 99%

Phase Progression of γ-Al₂O₃ Nanoparticles Synthesized in a Solvent-Deficient Environment

Smith¹,

Amin

Woodfield³

et al. 2013

Inorg. Chem.

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Our simple and uniquely cost-effective solvent-deficient synthetic method produces 3-5 nm Al2O3 nanoparticles which show promise as improved industrial catalyst-supports. While catalytic applications are sensitive to the details of the atomic structure, a diffraction analysis of alumina nanoparticles is challenging because of extreme size/microstrain-related peak broadening and the similarity of the diffraction patterns of various transitional Al2O3 phases. Here, we employ a combination of X-ray pair-distribution function (PDF) and Rietveld methods, together with solid-state NMR and thermogravimetry/differential thermal analysis-mass spectrometry (TG/DTA-MS), to characterize the alumina phase-progression in our nanoparticles as a function of calcination temperature between 300 and 1200 °C. In the solvent-deficient synthetic environment, a boehmite precursor phase forms which transitions to γ-Al2O3 at an extraordinarily low temperature (below 300 °C), but this γ-Al2O3 is initially riddled with boehmite-like stacking-fault defects that steadily disappear during calcination in the range from 300 to 950 °C. The healing of these defects accounts for many of the most interesting and widely reported properties of the γ-phase.

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Section: Methodsmentioning

confidence: 99%

Phase Progression of γ-Al₂O₃ Nanoparticles Synthesized in a Solvent-Deficient Environment

Smith¹,

Amin

Woodfield³

et al. 2013

Inorg. Chem.

Self Cite

View full text Add to dashboard Cite

show abstract

“…The thermogravimetric and differential-temperature analyses (TG/DTA) were performed using a Netzsch STA 409PC instrument. The mass spectrometry (MS) measurements were collected in tandem with the TG/DTA measurements by attaching a miniature quadrupole MS unit built in-house 39 to the out-gas line of the Netzsch TG/DTA instrument. For these experiments, roughly 30 mg of each precursor material were heated in an alumina crucible to either 300 °C (for most un-rinsed precursors made with nitrate metal salts), 350 °C (for un-rinsed precursors made with chloride metal salts), or 650 °C (for rinsed precursors and some un-rinsed nitrate precursors) at a rate of 5 °C min −1 under He gas flow.…”

Section: Characterization Methodsmentioning

confidence: 99%

Synthesis of metal oxide nanoparticles via a robust “solvent-deficient” method

et al. 2015

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We report an efficient, general methodology for producing high-surface area metal oxide nanomaterials for a vast range of metal oxides, including at least one metal oxide nanomaterial from nearly every transition metal and semi-metal group in the periodic table (groups 3-4 and 6-15) as well as several from the lanthanide group (see ). The method requires only 2-3 simple steps; a hydrated metal salt (usually a nitrate or chloride salt) is ground with bicarbonate (usually NH4HCO3) for 10-30 minutes to form a precursor that is then either untreated or rinsed before being calcined at relatively low temperatures (220-550 °C) for 1-3 hours. The method is thus similar to surfactant-free aqueous methods such as co-precipitation but is unique in that no solvents are added. The resulting "solvent-deficient" environment has interesting and unique consequences, including increased crystallinity of the products over other aqueous methods and a mesoporous nature in the inevitable agglomerates. The products are chemically pure and phase pure with crystallites generally 3-30 nm in average size that aggregate into high surface area, mesoporous agglomerates 50-300 nm in size that would be useful for catalyst and gas sensing applications. The versatility of products and efficiency of the method lend its unique potential for improving the industrial viability of a broad family of useful metal oxide nanomaterials. In this paper, we outline the methodology of the solvent-deficient method using our understanding of its mechanism, and we describe the range and quality of nanomaterials it has produced thus far.

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Facile solvent-deficient synthesis of mesoporous γ-alumina with controlled pore structures

Huang

Bartholomew

Smith

et al. 2013

Microporous and Mesoporous Materials

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Simple, inexpensive mass spectrometric analyzer for thermogravimetry

Cited by 5 publications

References 20 publications

Phase Progression of γ-Al₂O₃ Nanoparticles Synthesized in a Solvent-Deficient Environment

Phase Progression of γ-Al₂O₃ Nanoparticles Synthesized in a Solvent-Deficient Environment

Synthesis of metal oxide nanoparticles via a robust “solvent-deficient” method

Facile solvent-deficient synthesis of mesoporous γ-alumina with controlled pore structures

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Simple, inexpensive mass spectrometric analyzer for thermogravimetry

Cited by 5 publications

References 20 publications

Phase Progression of γ-Al2O3 Nanoparticles Synthesized in a Solvent-Deficient Environment

Phase Progression of γ-Al2O3 Nanoparticles Synthesized in a Solvent-Deficient Environment

Synthesis of metal oxide nanoparticles via a robust “solvent-deficient” method

Facile solvent-deficient synthesis of mesoporous γ-alumina with controlled pore structures

Contact Info

Product

Resources

About

Phase Progression of γ-Al₂O₃ Nanoparticles Synthesized in a Solvent-Deficient Environment

Phase Progression of γ-Al₂O₃ Nanoparticles Synthesized in a Solvent-Deficient Environment