Self-assembled molecular nanostructures embody an enormous potential for new technologies, therapeutics, and understanding of molecular biofunctions. Their structure and function are dependent on local environments, necessitating in-situ/operando investigations for the biggest leaps in discovery and design. However, the most advanced of such investigations involve laborious labeling methods that can disrupt behavior or are not fast enough to capture stimuli-responsive phenomena. We utilize X-rays resonant with molecular bonds to demonstrate an in-situ nanoprobe that eliminates the need for labels and enables data collection times within seconds. Our analytical spectral model quantifies the structure, molecular composition, and dynamics of a copolymer micelle drug delivery platform using resonant soft X-rays. We additionally apply this technique to a hydrocarbon sequestrating polysoap micelle and discover that the critical organic-capturing domain does not coalesce upon aggregation but retains distinct single-molecule cores. This characteristic promotes its efficiency of hydrocarbon sequestration for applications like oil spill remediation and drug delivery. Such a technique enables operando, chemically sensitive investigations of any aqueous molecular nanostructure, label-free.

Extreme ultraviolet (EUV) lithography is one of the most promising printing techniques for high-volume semiconductor manufacturing at the 14-nm half-pitch device node and beyond. However, key challenges around EUV photoresist materials, such as the exposure-dose sensitivity or the line-width roughness, continue to impede its full adoption into industrial nanofab facilities. Metrology tools are required to address these challenges by helping to assess the impact of the EUV materials' properties and processing conditions along different steps of the nanofabrication process. We apply the resonant soft x-ray scattering (RSoXS) technique to gain insights into the structure of patterned EUV resists before the development step takes place. By using energies around the carbon K-edge to take advantage of small differences in chemistry, the electronic density contrast between the exposed and unexposed regions of the resists could be enhanced in order to image the patterns with subnanometer precision. Critical-dimension grazing-incidence small-angle x-ray scattering is then performed at energies where the contrast is maximized, enabling the reconstruction of the three-dimensional shape of the latent image. We demonstrate the potential of RSoXS to provide a high-resolution height-sensitive profile of patterned EUV resists, which will help in quantifying the evolution of critical features, such as the line-edge roughness, at a key step of the nanofabrication process.

Extreme ultraviolet lithography is one of the most promising printing techniques for high volume semiconductor manufacturing at the 14 nm half-pitch device node and beyond. However, key challenges around EUV photoresist materials such as the exposure-dose sensitivity or the line-width roughness continue to impede the full adoption into industrial nanofab facilities. New metrology tools are required to address these challenges by helping to determine the impact of the EUV materials' properties and processing conditions on the roughness through the different step of the process. Here, we apply the resonant soft x-ray scattering (RSOXS) technique to gain insights into the structure of patterned EUV resists before the development step takes place. By using energies around the carbon absorption edge to take advantage of small differences in chemistry, the electronic density contrast between the exposed and unexposed regions of the resists could be enhanced in order to image the patterns with sub-nm precision. Critical-dimension grazing incidence small-angle X-ray scattering (CDGISAXS) was then performed at energies where the contrast was maximized, enabling the reconstruction of the 3D shape of the latent image. This demonstrates the potential of RSOXS to provide a high-resolution heightsensitive profile of patterned EUV resists, which will help to quantify the evolution of critical features, such as the line edge roughness, at each step of the nanofabrication process.