scholarly journals Towards Volatile Organoselenium Compounds with Cost-Effective Synthesis

Molecules ◽  
2020 ◽  
Vol 25 (21) ◽  
pp. 5212
Author(s):  
Jaroslav Charvot ◽  
Daniel Pokorný ◽  
Milan Klikar ◽  
Veronika Jelínková ◽  
Filip Bureš

The current portfolio of organoselenium compounds applicable as volatile precursors for atomic layer deposition can be denoted as very limited. Hence, we report herein facile and cost-effective preparation of two bis(trialkylstannyl)selenides as well as one selenole and three bis(trialkylsilyl)selenides. Their syntheses have been optimized to: (i) use readily available and inexpensive starting materials, (ii) involve operationally simple methodology (heating in a pressure vessel), (iii) use a minimum amount of additives and catalysts, and (iv) either exclude additional purification or involve only simple distillation. The chemical structure of prepared Se derivatives was confirmed by multinuclear NMR and GC/MS. Their fundamental thermal properties were investigated by differential scanning calorimetry (DSC) and TGA methods that revealed thermal stability within the range of 160–300 °C.

2021 ◽  
Author(s):  
Michael Land ◽  
Goran Bacic ◽  
Katherine Robertson ◽  
Sean Barry

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.


2020 ◽  
Author(s):  
David Zanders ◽  
Goran Bačić ◽  
Dominique Leckie ◽  
Oluwadamilola Odegbesan ◽  
Jeremy M. Rawson ◽  
...  

Attempted preparation of a chelated Co(II) β-silylamide re-sulted in the unprecedented disproportionation to Co(0) and a spirocyclic cobalt(IV) bis(β-silyldiamide): [Co[(NtBu)2SiMe2]2] (1). Compound 1 exhibits a room temperature magnetic moment of 1.8 B.M and a solid state axial EPR spectrum diagnostic of a rare S = 1/2 configuration. Semicanonical coupled-cluster calculations (DLPNO-CCSD(T)) revealed the doublet state was clearly preferred (–27 kcal/mol) over higher spin configurations for which density functional theory (DFT) showed no energetic preference. Unlike other Co(IV) complexes, 1 had remarkable thermal stability, and was demonstrated to form a stable self-limiting monolayer in initial atomic layer deposition (ALD) surface saturation tests. The ease of synthesis and high-stability make 1 an attractive starting point to begin investigating otherwise inaccessible Co(IV) intermediates and synthesizing new materials.


2020 ◽  
pp. 095400832097759
Author(s):  
Ke Li ◽  
Hua Yin ◽  
Kun Yang ◽  
Pei Dai ◽  
Ling Han ◽  
...  

Designing novel low-melting, high-rigidity phthalonitrile resin is of great significance in the current context of development. In this study, rigid spirocycle acetal structure was introduced into phthalonitrile to reduce the melting point and maintain their thermal stability. The chemical structure of resins was confirmed by nuclear magnetic resonance (NMR) spectrometry, matrix-assisted laser desorption/ionization time of flight (MALDI-TOF) mass spectrometry and Fourier-transform infrared (FTIR) spectroscopy. The curing behaviors were studied by differential scanning calorimetry (DSC). Thermal stability and mechanical properties of the cured resins were investigated by dynamic mechanical thermal analysis (DMTA) and thermogravimetric analysis (TGA). The processability was studied by rheological analysis. The results indicated the three monomers had a low melting temperature, wide processing windows and low viscosities. These polymers did not exhibit Tg from room temperature to 400°C, exhibited superb dynamic mechanical property and thermal stability.


Author(s):  
Changyu Park ◽  
Changmin Lee ◽  
Woohui Lee ◽  
Jehoon Lee ◽  
Jinyong Kim ◽  
...  

2017 ◽  
Vol 7 (1) ◽  
Author(s):  
Min Baik ◽  
Hang-Kyu Kang ◽  
Yu-Seon Kang ◽  
Kwang-Sik Jeong ◽  
Youngseo An ◽  
...  

Coatings ◽  
2021 ◽  
Vol 11 (9) ◽  
pp. 1028
Author(s):  
Laura Keskiväli ◽  
Pirjo Heikkilä ◽  
Eija Kenttä ◽  
Tommi Virtanen ◽  
Hille Rautkoski ◽  
...  

The growth mechanism of Atomic Layer Deposition (ALD) on polymeric surfaces differs from growth on inorganic solid substrates, such as silicon wafer or glass. In this paper, we report the growth experiments of Al2O3 and ZnO on nonwoven poly-L-lactic acid (PLLA), polyethersulphone (PES) and cellulose acetate (CA) fibres. Material growth in both ALD and infiltration mode was studied. The structures were examined with a scanning electron microscope (SEM), scanning transmission electron microscope (STEM), attenuated total reflectance-fourier-transform infrared spectroscopy (ATR-FTIR) and 27Al nuclear magnetic resonance (NMR). Furthermore, thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) analysis were used to explore the effect of ALD deposition on the thermal properties of the CA polymer. According to the SEM, STEM and ATR-FTIR analysis, the growth of Al2O3 was more uniform than ZnO on each of the polymers studied. In addition, according to ATR-FTIR spectroscopy, the infiltration resulted in interactions between the polymers and the ALD precursors. Thermal analysis (TGA/DSC) revealed a slower depolymerization process and better thermal resistance upon heating both in ALD-coated and infiltrated fibres, more pronounced on the latter type of structures, as seen from smaller endothermic peaks on TA.


2012 ◽  
Vol 727-728 ◽  
pp. 1552-1556
Author(s):  
Renata Barbosa ◽  
Dayanne Diniz Souza ◽  
Edcleide Maria Araújo ◽  
Tomás Jefférson Alves de Mélo

Studies of degradation have verified that the decomposition of some quaternary ammonium salts can begin to be significant at the temperature of about 180 ° C and like most thermoplastics are processed at least around this temperature, the thermal stability of the salt in clay should always be considered. Some salts are more stable than others, being necessary to study the degradation mechanisms of each case. In this work, four quaternary ammonium salts were characterized by differential scanning calorimetry (DSC) and thermogravimetry (TG). The results of DSC and TG showed that the salts based chloride (Cl-) anion begin to degrade at similar temperatures, while the salt based bromide (Br-) anion degrades at higher temperature. Subsequently, a quaternary ammonium salt was chosen to be used in organoclays, depending on its chemical structure and its thermal behavior.


2011 ◽  
Vol 23 (7) ◽  
pp. 513-517 ◽  
Author(s):  
Mohsen Ghorbani ◽  
Mohammad Soleimani Lashkenari ◽  
Hossein Eisazadeh

This study investigated the preparation and properties of polyaniline/silver (PAn/Ag2O) nanocomposite in aqueous media by chemical polymerization of aniline in the presence of ammonium peroxydisulphate as an oxidant. The products were investigated in terms of morphology, chemical structure, thermal stability and thermal degradation using scanning electron microscopy, Fourier transform infrared, thermal gravimetric analysis and differential scanning calorimetry, respectively. The results indicated that the properties of products were dependent on the nanocomposite structure.


2019 ◽  
Vol 3 (6) ◽  
pp. 1517-1525 ◽  
Author(s):  
James A. Raiford ◽  
Rebecca A. Belisle ◽  
Kevin A. Bush ◽  
Rohit Prasanna ◽  
Axel F. Palmstrom ◽  
...  

ALD vanadium oxide and a low-absorbing hole transport material (HTM) enable semi-transparent perovskite solar cells with high photocurrent and thermal stability.


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