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High-pressure synthesis in diamond anvil cells can yield unique compounds with advanced properties, but often they are either unrecoverable at ambient conditions or produced in quantity insufficient for properties characterization. Here we report the synthesis of metallic, ultraincompressible ( K 0 = 428(10) GPa), and very hard (nanoindentation hardness 36.7(8) GPa) rhenium nitride pernitride Re 2 (N 2 )(N) 2 . Unlike known transition metals pernitrides Re 2 (N 2 )(N) 2 contains both pernitride N 2 4− and discrete N 3− anions, which explains its exceptional properties. Re 2 (N 2 )(N) 2 can be obtained via a reaction between rhenium and nitrogen in a diamond anvil cell at pressures from 40 to 90 GPa and is recoverable at ambient conditions. We develop a route to scale up its synthesis through a reaction between rhenium and ammonium azide, NH 4 N 3 , in a large-volume press at 33 GPa. Although metallic bonding is typically seen incompatible with intrinsic hardness, Re 2 (N 2 )(N) 2 turned to be at a threshold for superhard materials.

The strain-rate sensitivity of ultrafine-grained aluminum (Al) and nanocrystalline nickel (Ni) is studied with an improved nanoindentation creep method. Using the dynamic contact stiffness thermal drift influences can be minimized and reliable creep data can be obtained from nanoindentation creep experiments even at enhanced temperatures and up to 10 h. For face-centered cubic (fcc) metals it was found that the creep behavior is strongly influenced by the microstructure, as nanocrystalline (nc) as well as ultrafine-grained (ufg) samples show lower stress exponents when compared with their coarse-grained (cg) counterparts. The indentation creep behavior resembles a power-law behavior with stress exponents n being ; 20 at room temperature. For higher temperatures the stress exponents of ufg-Al and nc-Ni decrease down to n ; 5. These locally determined stress exponents are similar to the macroscopic exponents, indicating that similar deformation mechanisms are acting during indentation and macroscopic deformation. Grain boundary sliding found around the residual indentations is related to the motion of unconstrained surface grains.

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