Abstract
A comparative study of vacuum versus ambient pressure inert gas thermogravimetry was performed on silver carboxylates compounds. Some of the complexes from this group have been previously successfully applied as precursors for both chemical vapour deposition and electron beam-induced deposition. Considerable differences were found between the thermogravimetry methods, which we associate with changes in evaporation dynamics. Vacuum thermogravimetry sublimation onsets consistently occurred at lower temperatures than ambient pressure N2-flow thermogravimetry, where the differences reached up to 120 °C. Furthermore, compound sublimation during N2-TGA was suppressed to such an extent that significant thermal decomposition of the compounds into metal and volatile organic fragments was observed while at vacuum the same complexes sublimed as intact molecules. Moreover, thermal stability of silver complexes was investigated using isothermal thermogravimetry. These findings are interesting for the field of thin film synthesis and nanomanufacturing via chemical vapour deposition, atomic layer deposition and focused electron beam induced deposition. In all three methods, delivery of functional precursor over the substrate is crucial. The presented results prove that vacuum thermogravimetry can be used as fast method of pre-screening for novel, especially low-volatility precursors.Graphic abstract
Highlights
Thermogravimetry (TGA) is an analytical method, which allows to investigate heat-induced mass changes [1]
vacuum thermogravimetry (VTGA) measurements were taken on different silver organometallic complexes: [Ag2(μ-O2CC(Me2) Et)2], [Ag2(μ-O2CC2F5)2], already successfully applied as focused electron beam induced deposition (FEBID) silver precursors, providing high purity deposits [24, 25], and three other fluorinated and nonf luorinated silver carboxylates: [Ag2(μ-O2CCF3)2], [Ag2(μ-O2CC3F7)2], [Ag2(μ-O2tBu)2]
If sublimation occurred in a small temperature window before or simultaneously with thermal decomposition would be the subject of follow-up isothermal TGA measurements
Summary
Thermogravimetry (TGA) is an analytical method, which allows to investigate heat-induced mass changes [1]. It can be used to study different heat-related phenomena, such as evaporation, drying, sorption of gases [2], thermal decomposition [3, 4] (with formation of volatile species), oxidation [5] and/ or oxidative decomposition, as well as certain thermally induced chemical reactions [6, 7]. In-vacuum TGA measurements have been applied to study early stages of metal oxidation in low-pressure corrosive atmospheres [10]. It is possible to program nonlinear temperature changes, e.g. when the heating rate is controlled by the sample’s temperature [1]
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