Characterization of LPCVD and PECVD silicon oxynitride films

The chemical composition and structure of silicon oxynitrides, deposited in low pressure and plasma enhanced chemical vapour deposition processes are discussed. From an extrapolation of the characteristics of plasma grown oxynitrides a model for the deposition of LPCVD material is derived. A main conclusion of this model is that Si-Si bonds have a larger tendency to occur in this material than Si dangling bonds.     

Carbon-13 NMR study of some isomeric n-nitroindazole derivatives

The ¹³C NMR spectra of 1,5- and 2,x-dinitroindazoles “x=4-7” and 3-bromo-1,x-dinitroindazoles are recorded and discussed. The data on he 2,x-dinitroindazoles confirm our previous structurea assignment based on ¹H NMR spectroscopy. The ¹³C NMR spectra established that in the novel 3-bromo-1,x-dinitroindazoles the N-nitro group is attached at N-1.     

On the nitro group transfer from 2-nitro-4,5,6,7-tetrachloro-2H-benzotriazole and 2-nitro-2H-phenanthro[9,10-d]triazole to secondary amines

The synthesis of 2-nitro-4,5,6,7-tetrachloro-2H-benzotriazole 1 and of 2-nitro-2H-phenanthro[9,10-d]-triazole 2 and their transfer of the nitro group to give 1-nitropyrrolidine 4a and 1-nitromorpholine 4b in high yields when reacted with pyrrolidine or morpholine are reported. The reaction of 1 also gives the pyrrolidinium and morpholinium salts 5a-b of 1 .     

Pyrazoles VI: The electron-releasing capacity of the pyrazole ring

UV and PMR spectral data and C?O frequencies of some methylpyrazoles containing in the 3-, 4- or 5-position, a formyl-, acetyl- or ethoxycarbonyl group are reported. These data confirm earlier conclusions that, in particular, the 4-pyrazolyl group acts as an electron releasing group. The syntheses of a number of formyl-, acetyl- and ethoxycarbonyl pyrazoles are described. In addition, some 4-dicyanovinyl- and 4-tricyanovinylpyrazoles were investigated.     

Synthesis of 3-dialkylaminomethyl-5-methyl-4-substituted-1H-pyrazoles. Selective functionalization of one methyl group via n-nitration of 3,5-dimethyl-4-substituted-1H-pyrazoles

Treatment of 4-substituted 3,5-dimethyl-1-nitro-1H-pyrazoles 1 and 10a-c with secondary amines in acetonitrile, in the presence of 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU), affords the novel dialkyl-aminomethyl-1H-pyrazoles 5, 6, 7, 8, 11a-c, 12a-c and 13a-c in good to excellent yields. In this way one of the, in general, inert methyl groups of 3,5-dimethyl-4-substituted-1H-pyrazoles is functionalized creating a new synthetic route to azoles containing a coordinating substituent.     

Peptide block copolymers by N‐carboxyanhydride ring‐opening polymerization and atom transfer radical polymerization: The effect of amide macroinitiators

The synthesis of polypeptide‐containing block copolymers combining N‐carboxyanhydride (NCA) ring‐opening polymerization and atom transfer radical polymerization (ATRP) was investigated. An amide initiator comprising an amine function for the NCA polymerization and an activated bromide for ATRP was used. Well‐defined polypeptide macroinitiators were obtained from γ‐benzyl‐L ‐glutamate NCA, O‐benzyl‐serine NCA, and N‐benzyloxy‐L ‐lysine. Subsequent ATRP macroinitiation from the polypeptides resulted in higher than expected molecular weights. Analysis of the reaction products and model reactions confirmed that this is due to the high frequency of termination reactions by disproportionation in the initial phase of the ATRP, which is inherent in the amide initiator structure. In some cases selective precipitation could be applied to remove unreacted macroinitiator to yield well‐defined block copolymers. © 2009 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2009     

Characterization of the ion cathode fall region in relation to the growth rate in plasma sputter deposition

In plasma-assisted magnetron sputtering, the ion cathode fall region is the part of the plasma where the DC electric field and ion current evolve from zero to their maximum values at the cathode. These quantities are straightforwardly related to the deposition rate of the sputtered material. In this work we derive simple relations for the measurable axially averaged values of the ion density and the ion current at the ion cathode fall region and relate them with the deposition rate. These relations have been tested experimentally in the case of an argon plasma in a magnetron sputtering system devoted to depositing amorphous silicon. Using a movable Langmuir probe, the profiles of the plasma potential and ion density were measured along an axis perpendicularly to the cathode and in front of the so-called race-track. The deposition rate of silicon, under different conditions of pressure and input power, has been found to compare well with those determined with the relations derived.     

Aryldiazonium Salts as Nitrogen‐Based Lewis Acids: Facile Synthesis of Tuneable Azophosphonium Salts

Inspired by the commercially available azoimidazolium dyes (e.g., Basic Red 51) that can be obtained from aryldiazonium salts and N‐heterocyclic carbenes, we developed the synthesis of a unique set of arylazophosphonium salts. A range of colours were obtained by applying readily tuneable phosphine donor ligands and para‐substituted aryldiazonium salts as nitrogen‐based Lewis acids. With cyclic voltammetry, a general procedure was designed to establish whether the reaction between a Lewis acid and a Lewis base occurs by single‐electron transfer or electron‐pair transfer.