Details

Autor(en) / Beteiligte

• Corbey, Jordan F.
• Reilly, Dallas D.
• Sweet, Lucas E.
• Lach, Timothy G.

Titel

Extraction of plutonium‐containing microcrystals from Hanford soil using a focused ion beam for single‐crystal X‐ray diffraction analysis

Ist Teil von

• Journal of applied crystallography, 2019-12, Vol.52 (6), p.1244-1252

Ort / Verlag

5 Abbey Square, Chester, Cheshire CH1 2HU, England: International Union of Crystallography

Erscheinungsjahr

2019

Quelle

Wiley Blackwell Single Titles

Beschreibungen/Notizen

• Herein, the successful use of a focused ion beam/scanning electron microscope to prepare microsamples of radioactive single crystals for X‐ray diffraction analysis is reported. This technique was used to extract and analyze crystalline Pu‐containing particles as small as 28 µm3 from Hanford soil taken from the 216‐Z‐9 waste crib, which were then crystallographically characterized using single‐crystal X‐ray diffraction to confirm the cubic structure of PuO2. As a systematic proof of concept, the technique was first tested using UO2 crystals milled into cubic shapes with approximate volumes of 4620, 1331, 125, 8 and 1 µm3, in order to empirically determine the crystal size limits for characterization by a laboratory‐based diffractometer with a sealed tube Mo or Ag anode X‐ray source and a charge‐coupled device detector. Focused ion beam/scanning electron microscope (FIB/SEM) techniques have been used to identify and extract single microcrystals of plutonium species from radioactive soil taken from the Z‐9 waste crib at the Hanford Site. Using the FIB/SEM, plutonium‐containing microcrystals as small as 28 µm3 were prepared for single‐crystal X‐ray diffraction and characterized using a laboratory‐based diffractometer.