Combined nanoscale chemical and mechanical property characterization has largely been limited by the inability to extend chemical structure identification techniques such as infrared (IR) absorption spectroscopy into the nanometer regime due to diffraction limitations. The recent development of atomic force microscope (AFM) based IR spectroscopy (AFM-IR) has now enabled infrared chemical spectroscopy with resolution well below the diffraction limit. However, the combination of AFM-IR with other AFM based techniques to achieve nanoscale chemical structure-mechanical property characterization has yet to be demonstrated. In this regard, we have combined AFM-IR chemical and contact resonance AFM (CR-AFM) mechanical measurements in the investigation of low dielectric constant (low-k) / Cu damascene structures fabricated using a 90 nm interconnect process technology. We show that the combined AFM-IR and CR-AFM results can be utilized to perform nanoscale chemical-mechanical characterization of both the nano-patterned metal and the low-k dielectric whose mechanical properties are sensitive to chemical modification by the interconnect fabrication process. The continued drive to seek and exploit new materials and phenomena at nanometer dimensions has increased the demand for metrologies capable of characterizing both chemical structure and physical properties at the nanoscale. The nanoelectronics industry in particular has identified metrologies capable of performing nanoscale structureproperty measurements on new materials and devices as an area of critical need in their industry technology roadmap.1,2 Such requirements for nanoscale physical property characterization have readily been met by the development of a range of scanned probe techniques capable of assessing the thermal, 3,4 mechanical, 5,6 and electrical 7,8 properties of materials at the nanoscale. 9 However, the development of nanoscale chemical structure metrologies has been hindered by the difficulty of scaling popular micron-scale techniques such as infrared (IR) absorption spectroscopy [10][11][12] into the nanometer regime due to diffraction limits defined by the Rayleigh equation.13,14 To overcome these limitations, a number of approaches combining optical spectroscopy with scanned probe microscopy (SPM) have been proposed and demonstrated. [13][14][15][16][17][18][19][20] Of these, the atomic force microscope (AFM) IR technique, which is based on photothermally induced resonance (PTIR), 21,22 has recently garnered significant interest due to a demonstrated spatial resolution of 25-100 nm, and a close correlation to micron-scale Fourier transform infrared (FTIR) spectroscopy. 13,14 This combination has resulted in the utilization of AFM-IR in a number of biological, 23-25 polymeric, 26-28 and semiconductor [29][30][31] applications. However, AFM-IR and related techniques have yet to be routinely combined with other AFM based techniques to achieve the ultimate goal of nanoscale structure-property characterization. In this regard, we provide a compelling...