TY  - JOUR
AU  - Ambach, Sebastian
AU  - Pritzl, Reinhard M.
AU  - Bhat, Shrikant
AU  - Farla, Robert
AU  - Schnick, Wolfgang
TI  - Nitride Synthesis under High-Pressure, High-Temperature Conditions: Unprecedented In Situ Insight into the Reaction
JO  - Inorganic chemistry
VL  - 63
IS  - 7
SN  - 0020-1669
CY  - Washington, DC
PB  - American Chemical Society
M1  - PUBDB-2024-00836
SP  - 3535-3543
PY  - 2024
AB  - High-pressure, high-temperature (HP/HT) syntheses are essential for modern high-performance materials. Phosphorus nitride, nitridophosphate, and more generally nitride syntheses benefit greatly from HP/HT conditions. In this contribution, we present the first systematic in situ investigation of a nitridophosphate HP/HT synthesis using the reaction of zinc nitride Zn<sub>3</sub>N<sub>2</sub> and phosphorus(V) nitride P<sub>3</sub>N<sub>5</sub> to the nitride semiconductor Zn<sub>2</sub>PN<sub>3</sub> as a case study. At a pressure of 8 GPa and temperatures up to 1300 °C, the reaction was monitored by energy-dispersive powder X-ray diffraction (ED-PXRD) in a large-volume press at beamline P61B at DESY. The experiments investigate the general behavior of the starting materials under extreme conditions and give insight into the reaction. During cold compression and subsequent heating, the starting materials remain crystalline above their ambient-pressure decomposition points, until a sufficient minimum temperature is reached and the reaction starts. The reaction proceeds via ion diffusion at grain boundaries with an exponential decay in the reaction rate. Raising the temperature above the minimum required value quickly completes the reaction and initiates single-crystal growth. After cooling and decompression, which did not influence the resulting product, the recovered sample was analyzed by energy-dispersive X-ray (EDX) spectroscopy.
LB  - PUB:(DE-HGF)16
C6  - 38324917
UR  - <Go to ISI:>//WOS:001167008100001
DO  - DOI:10.1021/acs.inorgchem.3c04433
UR  - https://bib-pubdb1.desy.de/record/603202
ER  -