DOI > 10.5291/ILL-DATA.LTP-5A-5

This proposal is publicly available since 07/19/2018

Title

New directions in time-resolved neutron diffraction; Probing high power microwave materials synthesis in situ.

Abstract

We propose the improvement of a device able to perform in situ neutron powder diffraction studies of solid state reactions promoted by microwave (MW) heating. This development phase is part of an on-going project, for which 3 days of beamtime (for off- and in-line tests of the device) have been already allocated on D20 (5-25-202). For this new stage of the project we are proposing, we wish to focus mainly on: 1)Optimization of all the possible adjustable parameters – aligning sample, tuning frequency, varying waveguide lengths,...- necessary to reach the best operating conditions; 2)Pushing the reaction timescale below the range of seconds, i.e. perform fast reactions in situ; 3) Establish a protocol for reproducible reactions, focusing on the synthesis of titanium carbide (TiC) first and then expanding the methodology to other p- and d-block metal carbides. This device will add to ILL's capabilities in sample environment. It is designed to work mainly on D20,but we will explore the potential of the method for other neutron scattering instruments, starting with other powder diffractometers (D1B, D2B, and D4).

Experimental Report

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Data Citation

The recommended format for citing this dataset in a research publication is in the following format:

BOSCAINO Annalisa; DRYSDALE Tim; GREGORY Duncan; Thomas C. Hansen; KENNEDY Jennifer and WHITTAKER Gavin. (2012). New directions in time-resolved neutron diffraction; Probing high power microwave materials synthesis in situ.. Institut Laue-Langevin (ILL) doi:10.5291/ILL-DATA.LTP-5A-5

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Metadata

Experiment Parameters

  • Environment temperature

    1200-1800

Sample Parameters

  • Formula

    • Ti (alpha)
    • C (graphite)
    • Ta
    • Nb
    • W
  • Consistence

    powder
  • Mass

    1000
  • Size

    800
  • Space

    P63 / mmc
  • Unit cell A

    2.45
  • Unit cell B

    2.45
  • Unit cell C

    6.86
  • Alpha

    90
  • Beta

    90
  • Gamma

    120
  • Container

    quartz tube and flat plate (BN)