A novel synthetic approach is presented leading to hitherto unknown nitridosilicates, oxonitridosilicates, oxonitridoaluminosilicates, carbidonitridosilicates, as well as nitridoborates and oxonitridoborates of rare earth elements, alkali, and alkaline earth metals. Typically, the respective metals were reacted with silicon diimide, aluminum nitride, or poly(boron amide imide), respectively, under pure nitrogen atmosphere utilizing a radiofrequency furnace. Usually, the compounds are obtained within short reaction periods as coarsely crystalline products. Zink nitridophosphates of the sodalite structure type were obtained by the reaction of phosphorus nitride imide with zinc or zinc chalcogenides, respectively. Several molecular metal silylamides and imides containing nitridobridges between the metals and silicon were obtained by the reaction of differently chlorinated disilazanes with metal chlorides. During these investigations hitherto unknown bis(trimethylsilyl)ammonium salts have been discovered. Furthermore, we report about the synthesis of N‐silyl metal hydrazides.
Because of its low chemical reactivity Si,N, has hardly been used as a starting material for the preparation of multinary silicon nitridcs or nitridosilicates, but has gained increasing importance as a nonoxidic material for high-performance applications. A novel synthetic approach is presented, which starts from silicon diimide (Si(NH),) and makes available a large variety of novel nitridosilicates. The structures of these nitridosilicates represent a significant extension from those found in the family of oxosilicates. Because of their outstanding chemical and physical stability, nitridosilicates might be of particular interest for the development of novel inorganic nitridic materials.
Abstract:The reaction of hexamethyldisilazane with TiCI, in CH,CI, leads to the formation of [(Me,SiNTiCl,),] (3). According to the crystal structure analysis, 3 is an octameric titanium trimethylsilylimido chloride. The mechanism of the formation of 3 was studied in detail by means of time-dependent 14N N M R spectroscopy. [(Me,Si)
Inhaltsübersicht. TiCl 4 reagiert mit Cl 2 Si(NHSiMe 3 ) 2 in n-Pentan unter Abspaltung von Me 3 SiCl quantitativ zu [µ-ClTiCl 2 N(SiMe 3 )-SiCl 2 NH 2 ] 2 (1), das als gelber, hydrolyseempfindlicher, kristalliner Feststoff in Form kleiner verwachsener Nadeln anfällt und bis ca. 80°C stabil ist. Die Molekülstruktur von 1 wurde zunächst aus Abstract. TiCl 4 reacts quantitatively with Cl 2 Si(NHSiMe 3 ) 2 in npentane under evolution of Me 3 SiCl yielding [µ-ClTiCl 2 N(SiMe 3 )-SiCl 2 NH 2 ] 2 (1), which is obtained as a yellow, crystalline solid forming small intergrown needles, that rapidly hydrolyse. The product 1 shows a thermal stability up to 80°C. The molecular structure of 1 has been solved by X-ray powder diffraction methods and it could be confirmed by single-crystal X-ray structure determination Einleitung Für die Synthese oligonärer Nichtmetallnitride können molekulare Vorläuferverbindungen von Nutzen sein, die die entsprechenden elektropositiven Elemente bereits über Nitridobrücken miteinander verknüpft und somit molekular vororganisiert enthalten. Abzielend auf die Synthese bislang unbekannter ternärer Übergangsmetallsiliciumnitride haben wir in diesem Zusammenhang vor allem solche molekularen Vorstufen untersucht, die entsprechende Nitridobrücken zwischen den Übergangsmetallen Ti, Zr oder W einerseits sowie dem Element Silicium andererseits aufweisen. So erhielten wir durch Umsetzung von TiCl 4
A rocket borne solid state spectrometer was used recently during a solar flare to detect solar x-ray emissions in the energy range 4–40 keV. The silicon detector, cooled by liquid nitrogen and incorporating an optical feedback preamplifier, is believed to be the first such detector used in this type of experiment. This paper evaluates the spectrometer and detection system under laboratory and field conditions, offering calibration data and some experimental results. Suggestions are made for future experimentation.
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