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 Zn3N2 and phosphorus(V) nitride
P3N5 to the nitride semiconductor Zn2PN3 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.