Novel Composite Nitride Nanoceramics from Reaction-Mixed Nanocrystalline Powders in the System Aluminum Nitride AlN/Gallium Nitride GaN/Titanium Nitride TiN (Al:Ga:Ti = 1:1:1)

Abstract

A study is presented on the synthesis of reaction-mixed nitride nanopowders in the reference system of aluminium nitride AlN, gallium nitride GaN, and titanium nitride TiN (Al:Ga:Ti = 1:1:1) followed by their high-pressure and high-temperature sintering towards novel multi-nitride composite nanoceramics. The synthesis starts with a 4 h reflux in hexane of the mixture of the respective metal dimethylamides, which is followed by hexane evacuation, and reactions of the residue in liquid ammonia at −33 °C to afford a mixed metal amide/imide precursor. Plausible equilibration towards a bimetallic Al/Ga-dimethylamide compound upon mixing of the solutions of the individual metal-dimethylamide precursors containing dimeric {Al[N(CH3)2]3}2 and dimeric {Ga[N(CH3)2]3}2 is confirmed by 1H- and 13C{H}-NMR spectroscopy in C6D6 solution. The precursor is pyrolyzed under ammonia at 800 and 950 °C yielding, respectively, two different reaction-mixed composite nitride nanopowders. The latter are subjected to no-additive high-pressure and high-temperature sintering under conditions either conservative for the initial powder nanocrystallinity (650 °C, 7.7 GPa) or promoting crystal growth/recrystallization and, possibly, solid solution formation via reactions of AlN and GaN towards Al0.5Ga0.5N (1000 and 1100 °C, 7.7 GPa). The sintered composite pellets show moderately high mechanical hardness as determined by the Vicker’s method. The starting nanopowders and resulting nanoceramics are characterized by powder XRD, Raman spectroscopy, and SEM/EDX. It is demonstrated that, in addition to the multi-nitride composite nanoceramics of hexagonal AlN/hexagonal GaN/cubic TiN, under specific conditions the novel composite nanoceramics made of hexagonal Al0.5Ga0.5N and cubic TiN can be prepared.

Oxygen Aspects in the High-Pressure and High-Temperature Sintering of Semiconductor Kesterite Cu2ZnSnS4 Nanopowders Prepared by a Mechanochemically-Assisted Synthesis Method

“…In this regard, the application of temperatures exceeding 550–600 °C is avoided due to the thermal instability of the kesterite nanopowders. The HP-HT sintering methodology applied to kesterite was mastered by us during recent studies on the sintering of nanopowders of the metal nitrides, including AlN, GaN, TiN, and their composites [ 26 , 27 , 28 ].…”

Exploitation of a New Nucleating Agent by Molecular Structure Modification of Aryl Phosphate and Its Effect on Application Properties of the Polypropylene

“…Figure 3 b represents the 400 MHz 1 H-NMR spectrum measured at room temperature for APAl-3C dissolved in 5 wt% CD 4 O to reconfirm the structure of APAl-3C, showing the attribution of chemical shifts of hydrogen atoms at different functional group positions in the APAl-3C structure as exhibited. The chemical shifts at 1.46 and 1.33 ppm are assigned to the H band of the tert-butyl group on the benzene ring (‘3’ and ‘4’ -CH 3 ) as reported in literature [ 38 ], respectively. The proton displacements on the benzene ring in the structure of APAl-3C appear at 7.31 ppm and 7.21 ppm (‘1’ and ‘2’ C-H) [ 39 ].…”