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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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The fracture toughness of NiAl single crystals is evaluated with a new method based on the Jintegral concept. The new technique allows the measurement of continuous crack resistance curves at the microscale by continuously recording the stiffness of the microcantilevers with a nanoindenter. The experimental procedure allows the determination of the fracture toughness directly at the onset of stable crack growth. Experiments were performed on notched microcantilevers which were prepared by focused ion beam milling from NiAl single crystals. Stoichiometric NiAl crystals and NiAl crystals containing 0.14 wt% Fe were investigated in the so-called "hard" orientation. The fracture toughness was evaluated to be 6.4 6 0.5 MPa m 1/2 for the stoichiometric sample and 7.1 6 0.5 MPa m 1/2 for the iron containing sample, indicating that the addition of iron enhances the ductility. This effect is intensified with ongoing crack propagation where the Fe-containing sample exhibits a stronger crack resistance behavior than the stoichiometric NiAl single crystal. These findings are in good agreement with macroscopic fracture toughness measurements, and validate the new micromechanical testing approach.