Journal Article

PUBDB-2024-00836

http://join2-wiki.gsi.de/foswiki/pub/Main/Artwork/join2_logo100x88.png Nitride Synthesis under High-Pressure, High-Temperature Conditions: Unprecedented In Situ Insight into the Reaction

Ambach, S.Extern* ; Pritzl, R. M.Extern* ; Bhat, S.DESY* ; Farla, R.DESY* ; Schnick, W. (Corresponding author)Extern*

2024
American Chemical Society Washington, DC

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Please use a persistent id in citations: doi:10.1021/acs.inorgchem.3c04433  doi:10.3204/PUBDB-2024-00836

Abstract: 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$_3$N$_2$ and phosphorus(V) nitride P$_3$N$_5$ to the nitride semiconductor Zn$_2$PN$_3$ 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.

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Contributing Institute(s):

1. DOOR-User (DOOR ; HAS-User)
2. PETRA-D (FS-PETRA-D)

Research Program(s):

1. 632 - Materials – Quantum, Complex and Functional Materials (POF4-632) (POF4-632)
2. 6G3 - PETRA III (DESY) (POF4-6G3) (POF4-6G3)

Experiment(s):

1. PETRA Beamline P61.2 (PETRA III)

Appears in the scientific report 2024

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Database coverage:
; ; ; Clarivate Analytics Master Journal List ; Current Contents - Physical, Chemical and Earth Sciences ; Ebsco Academic Search ; Essential Science Indicators ; IF < 5 ; JCR ; Nationallizenz ; SCOPUS ; Science Citation Index Expanded ; Web of Science Core Collection

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