A fit of the vapours

Price, Duncan M.

doi:10.1016/j.tca.2015.04.030

Cited by 29 publications

(35 citation statements)

References 76 publications

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“…The volatility of the compounds was assessed using thermogravimetric analysis (TGA), from which the vapor pressure was also estimated based on the first derivative of the mass loss curve. [55,56] Herein TV refers to the temperature at which 1 Torr of vapor pressure was achieved; this is a commonly desired pressure for ALD and CVD precursors. We also probed the thermal stability of the compounds by analysis of the residual mass from the TGA experiment.…”

Section: Volatility and Thermal Stability: Effect Of The Chelate Ligandmentioning

confidence: 99%

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Thermal Stability and Decomposition Pathways in Volatile Molybdenum(VI) Bis-Imides

Land

Bačić

Robertson³

et al. 2021

Preprint

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The vapor deposition of many molybdenum-containing films relies on the delivery of volatile compounds with the general bis(tert-butylimido)molybdenum(VI) framework, both in atomic layer deposition and chemical vapor deposition. We have prepared a series of (tBuN)2MoCl2 adducts using neutral N,N’-chelates and investigated their volatility, thermal stability, and decomposition pathways. Volatility has been determined by thermogravimetric analysis, with the 1,4-di-tert-butyl-1,3-diazabutadiene adduct (5) found to be the most volatile (1 Torr of vapor pressure at 135 ºC). Thermal stability was measured primarily using differential scanning calorimetry, and the 1,10-phenanthroline adduct (4) was found to be the most stable, with an onset of decomposition of 303 ºC. We have also investigated molybdenum compounds with other alkyl-substituted imido groups: these compounds all follow a similar decomposition pathway, γ-H activation, with varying reaction barriers. The tert-pentyl, 1-adamantyl, and a cyclic imido (from 2,5-dimethylhexane-2,5-diamine) were systematically studied to probe the kinetics of this pathway. All of these compounds have been fully characterized, including via single-crystal X-ray diffraction, and a total of 19 unique structures are reported.

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Section: Volatility and Thermal Stability: Effect Of The Chelate Ligandmentioning

confidence: 99%

“…Langmuir vapor pressure equations were derived from TGA data using a previously reported method, employing benzoic acid as the calibrant. [55,56] Differential Scanning Calorimetry. DSC experiments were performed with a TA Instruments Q10 instrument.…”

Section: Ncme2(ch2)2cme2n)mocl2mentioning

confidence: 99%

Thermal Stability and Decomposition Pathways in Volatile Molybdenum(VI) Bis-Imides

Land

Bačić

Robertson³

et al. 2021

Preprint

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“…P 0 = 0) to analyse the evaporation into a gas [4][5][6][7][8][9]. This erroneous condition delivers unrealistic values of the evaporation coefficient ε of the order of 10 -4 -10 -5 [5,[10][11][12].…”

Section: Introductionmentioning

confidence: 99%

Thermogravimetric measurement of the equilibrium vapour pressure: Application to water and triethanolamine

et al. 2018

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A model that describes the pure evaporation kinetics is introduced. This model takes into account gas diffusion and convective gas transport; it describes the evaporation kinetics under the general conditions of thermogravimetric measurements. The model is used to determine the equilibrium vapour pressure in a relatively wide temperature range. The validity of the model is checked against experimental data of triethanolamine (TEA) and water evaporation. The applicability of isoconversional methods to the evaporation kinetics is also studied. Besides, it is shown that the degree of TEA decomposition depends on the surrounding atmosphere and on the conditions for gas evaporation; the easiest the gas evaporation, the smallest the degree of decomposition.In view of the volatiles formed, a reaction pathway is proposed for the thermal decomposition of TEA.

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“…Measurements of the evaporation rate (dm/dt, rate of mass loss) of compounds were performed using TGA equipment. In order to obtain the temperature dependence of the vapor pressure of the sublimated compound (p), an approximation of a Langmuir equation was used [38,39]. Since the Langmuir approach can only be applied when the compound sublimates to a vacuum, for our termogravimetric measurements a vaporization coefficient "α" had to be introduced.…”

Section: Sublimation Measurementsmentioning

confidence: 99%

NPG–TRIS Thermal Storage System. Quantification of the Limiting Processes: Sublimation and Water’s Adsorption

et al. 2021

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The NPG–TRIS binary system (NPG = (CH3)2C(CH2OH)2 = 2,2-dimetyl-1,3-propanodiol; TRIS = NH2C(CH2OH)3 = 2-Amino-2-(hydroxymethyl)-1,3-propanediol) was intensively investigated as a thermal energy storage system, due to the reversibility of its phase transitions and their associated energy. An adapted methodology was applied to precisely quantify its sublimation tendency. Relevant thermochemical data were revisited and evaluated using some specific experimental procedures. We also determined that the widely accepted requirement of working in an inert atmosphere to avoid deviations due to hygroscopicity is not necessary. Nevertheless, to take advantage of the energetic properties of the NPG–TRIS system, closed containers will be required to avoid NPG losses, due to its quantitatively determined high sublimation tendency.

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A fit of the vapours

Cited by 29 publications

References 76 publications

Thermal Stability and Decomposition Pathways in Volatile Molybdenum(VI) Bis-Imides

Thermal Stability and Decomposition Pathways in Volatile Molybdenum(VI) Bis-Imides

Thermogravimetric measurement of the equilibrium vapour pressure: Application to water and triethanolamine

NPG–TRIS Thermal Storage System. Quantification of the Limiting Processes: Sublimation and Water’s Adsorption

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