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Features sizes in integrated circuits (ICs) are often at the scale of 10 nm and are ever shrinking. ICs appearing in today’s computers and hand held devices are perhaps the most prominent examples. These smaller feature sizes demand equivalent advances in fast and accurate dimensional metrology for both development and manufacturing. Techniques in use and continuing to be developed include X-ray based techniques, optical scattering and of course the electron and scanning probe microscopy techniques. Each of these techniques have their advantages and limitations. Here the use of small angle electron beam scattering measurements in a reflection mode (RSAES) to characterize the dimensions and the shape of nanostructures on flat and opaque substrates is demonstrated using both experimental and theoretical evidence. In RSAES, focused electrons are scattered at angles smaller than 1° with the assistance of electron optics typically used in transmission electron microscopy. A proof-of-concept experiment is combined with rigorous electron reflection simulations to demonstrate the efficiency and accuracy of RSAES as a method of non-destructive measurement of shapes of features less than 10 nm in size on flat and opaque substrates.
200-nm-thick organosilicate films deposited by mixture of tetraethyl orthosilicate (TEOS) and methyltrimethoxysilane (MTMS) dissolving in different cetrimonium bromide (CTAB)/ethanol ratios were characterized in terms of pore size determination and its distribution. Under the toluene ambient, the pores would adsorb the gas hence elevating the whole film density. The X-ray reflectivity (XRR) equipped with mass flow control was utilized to detect the film density increasing. By fitting with Gaussian function and conversing with Kelvin's equation, the pore size was increased from 6.2 to 10.8 Å as the CTAB/ethanol ratio increasing to 0.075. It was attributed to the ethanol and CTAB enhanced the TEOS hollow droplets stability and dissolvability. As the CTAB/ethanol ratio is further increased, the pore size is reversely decreased, owing to the formation of solid microspheres. The non-destructive XRR measurement can evaluate the sub-nano pore sizes and its size distribution, which would fascinate the development and characterization of back-end of line process.
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