Crystal growth in supercritical ammonia using high surface area silicon nitride feedstock

Publikation: Beitrag in FachzeitschriftForschungsartikelBeigetragenBegutachtung

Beitragende

  • Stefan Kaskel - , Professur für Anorganische Chemie (I) (AC1), Max Planck Institute for Coal Research (Autor:in)
  • Meikh Khanna - , Max Planck Institute for Coal Research (Autor:in)
  • Bodo Zibrowius - , Max Planck Institute for Coal Research (Autor:in)
  • Hans Werner Schmidt - , Max Planck Institute for Coal Research (Autor:in)
  • Dirk Ullner - , Max Planck Institute for Coal Research (Autor:in)

Abstract

The use of amorphous high surface area silicon nitride is proposed as a raw material for crystallization experiments in supercritical ammonia. Compared with earlier studies, the use of highly dispersed solids results in the crystallization of inorganic nitrides under relatively mild conditions (673K). Mineralizers such as amides (LiNH2, NaNH2, KNH 2) are found to be effective crystallization aids. The crystalline products, detected using powder X-ray diffraction, are either MSi 2N3 (M = Li, Na) or Si2N2NH. Si 2N2NH is also characterized using 29Si MAS NMR. The spectrum shows a narrow line located at -44.7ppm, whereas for amorphous silicon nitride-based materials the line is broad. The ammonothermal reaction of NaAl(NH2)4 and high surface area silicon nitride at 673 K affords a new orthorhombic phase, isostructural with NaSi 2N3, but with extended lattice constants (a = 9.634, b = 5.643, c = 5.011Å). Effective crystallization is also achieved using fluoride mineralizers (KF, CsF) at 673 K. A new small scale autoclave, suitable for laboratory syntheses at temperatures up to 873 K, is presented that can be loaded under inert gas.

Details

OriginalspracheEnglisch
Seiten (von - bis)99-104
Seitenumfang6
FachzeitschriftJournal of crystal growth
Jahrgang261
Ausgabenummer1
PublikationsstatusVeröffentlicht - 15 Jan. 2004
Peer-Review-StatusJa

Schlagworte

Ziele für nachhaltige Entwicklung

Schlagwörter

  • A1. High surface area, A1. Precursor, A3. Solvothermal growth, B1. Ammonia, B1. Nitrides