Abstract
A cadmium germanium arsenide compound, Cd3Ge2As4, was synthesized using a double-containment fused quartz ampoule method within a rocking furnace and a melt-quench technique. The crystal structure was determined from single-crystal X-ray diffraction (SC-XRD), scanning and transmission electron microscopies (i.e. SEM, STEM, and TEM), and selected area diffraction (SAD) and confirmed with electron backscatter diffraction (EBSD). The chemistry was verified with electron energy loss spectroscopy (EELS).
Highlights
We report the crystal structure of the Cd3Ge2As4 crystalline phase; using XRD and analytical electron microscopies, it was shown to belong to the trigonal system in the R3 space group (No 148)
This inner ampoule was loaded into a 19Â22 mm fused quartz tube that was sealed at the base, and the annulus between the two vessels was filled with 17.8 g of Cu powder ( 75 mm)
The ampoule was heat treated in a rocking furnace where it was ramped at 3C minÀ1 from room temperature to 400C, held for 2 h in a fixed position, ramped to 625C at 3C minÀ1, held for 2 h, ramped to 850C at 3C minÀ1, held for 25 h, rocking was paused for 10 min to allow the melt to settle to the base, and the ampoule assembly was rapidly removed from the furnace and quenched in an ice bath filled with NaCl
Summary
The Cd3Ge2As4 sample, made using a double-containment quartz ampoule setup (see Fig. 3a), is discussed elsewhere in more detail (Johnson et al, 2009; Riley et al, 2012), but will be briefly described here. For the double-containment ampoule setup, high purity Cd (4.4916 g, 99.9999%), Ge (2.9030 g, 99.9999%), and As (5.9907 g, 99.99999+%) (Alfa Aesar, Ward Hill, MA) were added into a pre-cleaned fused quartz vessel [10Â12 mm; GE214, GM Associates, Inc., Oakland, CA; cleaning details are provided elsewhere (Riley et al, 2012)] while inside a nitrogen glovebox (< 0.1 ppm of O2/H2O; M-Braun, Inc., Stratham, NH). The vessel was moved out of the glovebox while connected to a sealed gate valve and 12.5-mm compression fitting to make sure that the contents of
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