ICDD PDF-4+ 2012 Instructions

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patterns, which reduced the number of cards returned to 431. Opening SIeve+, I imported and digitised my experimental diffraction data and automatically applied my filter. The top card, with a GOM score of 3259, was card 04-‐014-‐0245 – no mineral name was listed for this entry, but the crystal system was ‘Tetragonal’, and the space group P42/mnm. Comparing with other cards that also gave a good match proved that this card, and my specimen, were indeed rutile-‐structured:
Example 2: Nb,Cu-‐doped Titanium dioxide In the same research project, I used this TiO2 as a reagent, along with CuO and Nb2O5, to investigate the possible formation of a rutile-‐structured solid solution series, Ti1-‐3xCuxNb2xO2. Appropriate amounts of each reagent were mixed in an agate mortar and pestle, then fired in Pt foil boats at 935 ºC for 60h with intermittent regrinding. I then used the imaging plate detector on our Cu-‐STOE system for phase analysis. Compositions (data shown below, in WinX POW ) with x = 0.01–0.23 yielded phase-‐pure samples, which were indexed using the rutile space group, P42/mnm, showing that co-‐ doping of TiO2 with Cu and Nb was possible: Comparison against the previous example will show that the first five reflections for the rutile are present and correct here for samples with x = 0.05, 0.13 and 0.20. No other additional reflections are observed; these samples are phase pure. Note how the rutile peaks are shifting to lower angles, i.e. higher d-‐spacings, as x increases. As I replace Ti <strong>4+</strong> with the larger Cu 2+ and Nb 5+ cations in my structure, the unit cell size is increasing. For a solid solution, generally, unit cell parameters should change linearly with composition – a phenomenon known as Vegard’s Law. In this case, the a and c cell parameters deviate away from linearity, but the cell volume does increase linearly with composition (see N. Reeves-‐ McLaren et al, “Synthesis, structure and electrical properties of Cu3.21Ti1.16Nb2.63O12 and the
Page 1 and 2: ICDD PDF-‐4+ and SIeve+ Softwar
Page 3 and 4: Setting up your data The first thin
Page 5 and 6: Searching the Database The database
Page 7 and 8: Starting SIeve+ and loading your da
Page 9 and 10: your sample. The software will then
Page 11 and 12: Common problems ‘I have found a c
Page 13: It can immediately be seen that the
Page 17 and 18: slightly different composition (whi
Page 19 and 20: By also accepting the Si card, SIev
Page 21 and 22: Next, I select the elements of inte
Page 23 and 24: Further Reading The ICDD software h
Page 25 and 26: Appendix 2: Quality Marks The edito

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