Glasses and single crystals have traditionally been used as optical windows. Recently, there has been a high demand for harder and tougher optical windows that are able to endure severe conditions. Transparent polycrystalline ceramics can fulfill this demand because of their superior mechanical properties. It is known that polycrystalline ceramics with a spinel structure in compositions of MgAl2O4 and aluminum oxynitride (γ-AlON) show high optical transparency. Here we report the synthesis of the hardest transparent spinel ceramic, i.e. polycrystalline cubic silicon nitride (c-Si3N4). This material shows an intrinsic optical transparency over a wide range of wavelengths below its band-gap energy (258 nm) and is categorized as one of the third hardest materials next to diamond and cubic boron nitride (cBN). Since the high temperature metastability of c-Si3N4 in air is superior to those of diamond and cBN, the transparent c-Si3N4 ceramic can potentially be used as a window under extremely severe conditions.
The 660-km seismic discontinuity, which is a significant structure in the Earth’s mantle, is generally interpreted as the post-spinel transition, as indicated by the decomposition of ringwoodite to bridgmanite + ferropericlase. All precise high-pressure and high-temperature experiments nevertheless report 0.5–2 GPa lower transition pressures than those expected at the discontinuity depth (i.e. 23.4 GPa). These results are inconsistent with the post-spinel transition hypothesis and, therefore, do not support widely accepted models of mantle composition such as the pyrolite and CI chondrite models. Here, we present new experimental data showing post-spinel transition pressures in complete agreement with the 660-km discontinuity depth obtained by high-resolution in situ X-ray diffraction in a large-volume high-pressure apparatus with a tightly controlled sample pressure. These data affirm the applicability of the prevailing mantle models. We infer that the apparently lower pressures reported by previous studies are experimental artefacts due to the pressure drop upon heating. The present results indicate the necessity of reinvestigating the position of mantle mineral phase boundaries previously obtained by in situ X-ray diffraction in high-pressure–temperature apparatuses.
Silicon dioxide has eight stable crystalline phases at conditions of the Earth's rocky parts. Many metastable phases including amorphous phases have been known, which indicates the presence of large kinetic barriers. As a consequence, some crystalline silica phases transform to amorphous phases by bypassing the liquid via two different pathways. Here we show a new pathway, a fracture-induced amorphization of stishovite that is a high-pressure polymorph. The amorphization accompanies a huge volume expansion of ~100% and occurs in a thin layer whose thickness from the fracture surface is several tens of nanometers. Amorphous silica materials that look like strings or worms were observed on the fracture surfaces. The amount of amorphous silica near the fracture surfaces is positively correlated with indentation fracture toughness. This result indicates that the fracture-induced amorphization causes toughening of stishovite polycrystals. The fracture-induced solid-state amorphization may provide a potential platform for toughening in ceramics.
The Earth's mantle is characterised by a sharp seismic discontinuity at a depth of 660-km that can provide insights into deep mantle processes. The discontinuity occurs over only 2km -or a pressure difference of 0.1 GPa -and is thought to result from the post-spinel transition, that is, the decomposition of the mineral ringwoodite to bridgmanite plus ferropericlase. Existing high-pressure-temperature experiments have lacked the pressure control required to test whether such sharpness is the result of isochemical phase relations or chemically distinct upper and lower mantle domains. Here, we obtain the isothermal pressure interval of the Mg-Fe binary post-spinel transition by applying advanced multianvil techniques with in situ X-ray diffraction with help of Mg-Fe partition experiments. It is demonstrated that the interval at mantle compositions and temperatures is only 0.01 GPa, corresponding to 250 m. This interval is indistinguishable from zero at seismic frequencies. These results can explain the discontinuity sharpness and provide new support for whole mantle convection in a chemically homogeneous mantle. The present work suggests that distribution of adiabatic vertical flows between the upper and lower mantles can be mapped based on discontinuity sharpness. Main:The 660-km seismic discontinuity (D660) is the boundary between the upper and lower mantles. Seismological studies based on short-period P-wave reflections (Pʹ660Pʹ-PʹPʹ) have demonstrated that D660 is extremely sharp and less than 2 km thick 1 , which is in striking contrast to the 7-km-thick 410-km discontinuity 1 . Understanding the nature of D660 from a perspective of mineral physics provides important clues to open questions about the structure and dynamic processes in the Earth's mantle, such as slab subduction and upwelling of hot plume.Geochemical studies suggest that the Earth's upper mantle consists of ca. 60% atom-
Transparent polycrystalline nanoceramics consisting of triclinic Al2SiO5 kyanite (91.4 vol%) and Al2O3 corundum (8.6 vol%) were fabricated at 10 GPa and 1200‐1400°C. These materials were obtained by direct conversion from Al2O3‐SiO2 glasses fabricated using the aerodynamic levitation technique. The material obtained at 10 GPa and 1200°C shows the highest optical transparency with a real in‐line transmission value of 78% at a wavelength of 645 nm and a sample‐thickness of 0.8 mm. This sample shows equigranular texture with an average grain size of 34 ± 13 nm. The optical transparency increases with decreasing mean grain size of the constituent phases. The relationship between real in‐line transmission and grain size is well explained by a grain‐boundary scattering model based on a classical theory.
We measure valence-to-core x-ray emission spectra of compressed crystalline GeO 2 up to 56 GPa and of amorphous GeO 2 up to 100 GPa. In a novel approach, we extract the Ge coordination number and mean Ge-O distances from the emission energy and the intensity of the Kβ 00 emission line. The spectra of high-pressure polymorphs are calculated using the Bethe-Salpeter equation. Trends observed in the experimental and calculated spectra are found to match only when utilizing an octahedral model. The results reveal persistent octahedral Ge coordination with increasing distortion, similar to the compaction mechanism in the sequence of octahedrally coordinated crystalline GeO 2 high-pressure polymorphs.
We report the synthesis of alumina/stishovite nano‐nano composite ceramics through a pressure‐induced dissociation in Al2SiO5 at a pressure of 15.6 GPa and temperatures of 1300°C‐1900°C. Stishovite is a high‐pressure polymorph of silica and the hardest known oxide at ambient conditions. The grain size of the composites increases with synthesis temperature from ~15 to ~750 nm. The composite is harder than alumina and the hardness increases with reducing grain size down to ~80 nm following a Hall–Petch relation. The maximum hardness with grain size of 81 nm is 23 ± 1 GPa. A softening with reducing grain size was observed below this grain size down to ~15 nm, which is known as inverse Hall–Petch behavior. The grain size dependence of the hardness might be explained by a composite model with a softer grain‐boundary phase.
Phase relations in silicon and germanium nitrides (Si3N4 and Ge3N4) were investigated using a Kawai‐type multianvil apparatus and a laser‐heated diamond anvil cell combined with a synchrotron radiation. The pressure‐induced phase transition from the β to γ (cubic spinel‐type structure) phase was observed in both compositions. We observed the coexistence of the β and γ phases in Si3N4 at 12.4 GPa and 1800°C, while the appearance of single phase γ‐Ge3N4 was observed at pressures above 10 GPa. Our observations under higher pressures revealed that γ‐Si3N4 and γ‐Ge3N4 have wide stability fields and no postspinel transition was observed up to 98 GPa and 2400°C in both compositions. Using the room‐temperature compression curves of these materials, the bulk moduli (K0) and their pressure derivatives (K′0) were determined: K0 = 317 (16) GPa and K′0 = 6.0 (8) for γ‐Si3N4; K0 = 254 (13) GPa and K′0 = 6.0 (7) for γ‐Ge3N4.
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