powder_X-ray_diffraction

Powder X-Ray Diffraction Data for NaMO₂F₂ (M = Nb, Ta)

Author: Ouail Zakary
ORCID: 0000-0002-7793-3306
E-mail: [email protected]
Website: Ouail Zakary - webpage

This repository contains datasets of Powder X-Ray Diffraction (PXRD) data for the compounds NaNbO₂F₂ and NaTaO₂F₂, recorded under both room temperature (RT) and variable temperature conditions.

Overview of the Data

The dataset is organized into two main families of experiments:

1. Room Temperature PXRD Data:
   Folder: ./room_temperature_experiments

   • NaNbO₂F₂ Data:
     • Raw Data
     • Rietveld Refinement Data
   • NaTaO₂F₂ Data:
     • Raw Data
     • Rietveld Refinement Data

2. Variable Temperature PXRD Data:
   Folder: ./variable-temperature_experiments

   • NaNbO₂F₂ Data:
     • Raw Data
     • Rietveld Refinement Data
   • NaTaO₂F₂ Data:
     • Raw Data
     • Rietveld Refinement Data

Methods

PXRD Data Collection

Both RT and temperature-controlled PXRD patterns were recorded using a PANalytical θ/θ Bragg–Brentano EMPYREAN diffractometer (CuKα₁₊₂ radiations) equipped with a PIXcel1D detector. The collection methods are as follows:

• Room Temperature PXRD Patterns:

  • 2θ Range: 5° to 135°
  • Step Size: 0.0131°
  • Total Acquisition Time: Approximately 7h 30m
  • Sample Preparation: Raw powders were dusted through a 63 μm sieve on a glass holder to minimize preferential grain orientation.

• Temperature-Controlled PXRD Patterns:

  • Temperature Range: RT to 300°C using a HTK 900 Anton Paar furnace attachment
  • Sample Holder: Glass ceramic Macor
  • Data Collection Intervals: 20°C (25–220°C) and 10°C (220–300°C) increments with a heating rate of 5°C/min
  • Temperature Stabilization: 20 minutes before each measurement
  • 2θ Range: 10° to 100°
  • Step Size: 0.0131°
  • Total Acquisition Time: 3 hours for each pattern.

Rietveld Refinement

The Rietveld refinement method was employed for both the RT and temperature-controlled PXRD data using the FullProf software.

Directory Structure

The following directories contain the datasets:

• Room Temperature PXRD Data:

  • NaNbO₂F₂ Raw Data
  • NaNbO₂F₂ Rietveld Refinement Data
  • NaTaO₂F₂ Raw Data
  • NaTaO₂F₂ Rietveld Refinement Data

• Variable Temperature PXRD Data:

  • NaNbO₂F₂ Raw Data
  • NaNbO₂F₂ Rietveld Refinement Data
  • NaTaO₂F₂ Raw Data
  • NaTaO₂F₂ Rietveld Refinement Data

Requirements

To successfully conduct the PXRD experiments and perform the Rietveld refinements, the following requirements must be met:

• Equipment:

  • A PANalytical θ/θ Bragg–Brentano EMPYREAN diffractometer with a PIXcel1D detector.
  • An HTK 900 Anton Paar furnace attachment for temperature-controlled experiments.

• Software:

  • FullProf for Rietveld refinements. You can download this software from the FullProf Suite.
  • VESTA (download) and Diamond (download) for 3D visualization of crystal structures and for computing structural features such as bond lengths, distances, angles, volume of the unit cell, quadratic elongation, and distortion index.

---

For further details, please refer to the respective folders or contact the author via the provided email.