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

Research output: Contribution to journalResearch articleContributedpeer-review

Contributors

  • Stefan Kaskel - , Chair of Inorganic Chemistry I, Max Planck Institute for Coal Research (Author)
  • Meikh Khanna - , Max Planck Institute for Coal Research (Author)
  • Bodo Zibrowius - , Max Planck Institute for Coal Research (Author)
  • Hans Werner Schmidt - , Max Planck Institute for Coal Research (Author)
  • Dirk Ullner - , Max Planck Institute for Coal Research (Author)

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

Original languageEnglish
Pages (from-to)99-104
Number of pages6
JournalJournal of crystal growth
Volume261
Issue number1
Publication statusPublished - 15 Jan 2004
Peer-reviewedYes

Keywords

Sustainable Development Goals

Keywords

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