Studying local mechanical properties of metallic alloys and composites and their defect structures such as grain boundaries, cracks, and dislocations allows a better understanding and design of these structural materials. With a nanoindenting atomic force microscope (NI-AFM), which uses diamond tips, such measurements are possible on a nanometer scale. Measurements on the microstructure of superalloys are presented, where different precipitates with sizes in the range of 100 nm are characterized by their different hardness values. In addition, this new technique was used to characterize the nanohardness of the plastic zone and stress fields of cracks and grain boundaries. Therefore, crack tips of in-situ loaded bending specimens of intermetallic alloys (NiAl) were investigated. The measurements show a change in nanohardness and elasticity from the distance of interfaces. In material science the high-resolution capabilities of the atomic force microscopy (AFM) are used for studying metallographic sections, where different phases produce topographic contrasts in the image. A extremly small height difference in the microstructure is sufficient for a height contrast in the image, which allows a quantitative determination of particle size distributions and volume contents of precipitates [1, 2]. The plastic deformation behavior of metals is strongly influenced by the distribution and movement of defects as dislocations, grain boundaries and cracks. In-situ loading experiments in an AFM on specimens loaded in 4-point bending demonstrate the good imaging properties of an AFM for such defects [3]. Mechanical properties such as Young’s modulus of elasticity and hardness values were obtainable in the past by various indentation techniques, where a load displacement curve is recorded during the indentation process. These techniques were mainly applied for studying the mechanical properties of thin films. A combination of a nanoindenting instrument with an AFM now allows the local mechanical properties of different phases and particles in metallic alloys to be measured, since the indents can be positioned very exactly with the AFM. Such a combined nanoindenting AFM (NI-AFM) requires a special force measurement technique. Piezo hysteresis and creep of the used piezo scanner have to be eliminated. In addition, indenting should be performed by a tip which is centrally fixed and not at the end of a bending beam (cantilever) [4], because otherwise the location of the indent changes during loading. These properties are fulfilled by a capacitive transducer, which is used for load generation and measurement instead of the standard laser deflection unit. A diamond tip is used for the indentation experiments and topographic imaging in a conventional AFM mode. The resulting force indentation curves contain two pieces of information: the universal hardness H and the reduced modulus of elasticity Er. The possibilities of the NI-AFM for studying local mechanical properties are demonstrated on two different examples: first the hardness of the superalloy CMSX-6 was characterized; second, local changes of mechanical properties near a crack tip in a NiAl single crystal were examined. 1 Experimental setup and sample preparation The nanoindentation measurements shown in this paper were performed with an add-on-force transducer from Hysitron Inc. This transducer, mounted on a conventional AFM, controls the z movement of the tip (indentation, applied load, and feedback signal) while the piezos of the AFM control the lateral x-y movement. Further technical details on the transducer are described in [5]. Specimens of the superalloy CMSX-6 were examined with a Nanoscope II AFM from Digital Instruments. Since the x-y movement is achieved by scanning the whole specimen, only small specimens with a maximum diameter of 20 mm can be analyzed. Crack tips in NiAl single crystals were investigated with a bending apparatus specially constructed for the Explorer AFM from TopoMetrix. (This bending apparatus is described in [6].) Because the whole transducer assembly is mounted on the x-y scanner, the combined system is more sensitive to mechanical noise. However, large specimens can be examined with