High-quality single-crystal silicon nanolines (SiNLs) with a 24 nm linewidth and a height/width aspect ratio of 15 were fabricated. The mechanical properties of the SiNLs were characterized by nanoindentation tests with an atomic force microscope. The indentation load-displacement curves showed an instability with large displacement bursts at a critical load ranging from 9 to 30 μN. This phenomenon was attributed to a transition of the buckling mode of the SiNLs under indentation, which occurred preceding the final fracture of the nanolines. The mechanics of SiNLs under indentation was analyzed by finite element simulations, which revealed two different buckling modes depending on the contact friction at the nanoscale.
We demonstrate a top-down method for fabricating nickel mono-silicide (NiSi) nanolines (also referred to as nanowires) with smooth sidewalls and line widths down to 15 nm. Four-probe electrical measurements reveal that the room temperature electrical resistivity of the NiSi nanolines remains constant as the line widths are reduced to 23 nm. The resistivity at cryogenic temperatures is found to increase with decreasing line width. This finding can be attributed to electron scattering at the sidewalls and is used to deduce an electron mean free path of 6.3 nm for NiSi at room temperature. The results suggest that NiSi nanolines with smooth sidewalls are able to meet the requirements for implementation at the 22 nm technology node without degradation of device performance.
Small angle X-ray scattering (SAXS) was used to characterize the cross section of nanoline gratings fabricated with electron beam lithography (EBL) patterning followed by anisotropic wet etching into a single crystal silicon substrate. SAXS results at normal incidence clearly bear the signature of positional dependent linewidth within the gratings; such non-uniformity is subsequently confirmed with scanning electron microscopy. The proximity effect of EBL is believed to be the cause of the spatial variations of linewidth. To quantitatively fit the SAXS results the linewidth near the periphery of the patterned field needs to be 80% greater than that in the central region, whereas the cross section of nanolines can be modeled as a simple rectangular shape, as expected from the anisotropic wet etching process.
A nanoindentation system was employed to characterize mechanical properties of silicon nanolines (SiNLs), which were fabricated by an anisotropic wet etching (AWE) process. The SiNLs had the linewidth ranging from 24 nm to 90 nm, having smooth and vertical sidewalls and the aspect ratio (height/linewidth) from 7 to 18. During indentation, a buckling instability was observed at a critical load, followed by a displacement burst without a load increase, then a full recovery of displacement upon unloading. This phenomenon was explained by two bucking modes. It was also found that the difference in friction at the contact between the indenter and SiNLs directly affected buckling response of these nanolines. The friction coefficient was estimated to be in a range of 0.02 to 0.05. For experiments with large indentation displacements, irrecoverable indentation displacements were observed due to fracture of Si nanolines, with the strain to failure estimated to be from 3.8% to 9.7%. These observations indicated that the buckling behavior of SiNLs depended on the combined effects of load, line geometry, and the friction at contact. This study demonstrated a valuable approach to fabrication of well-defined Si nanoline structures and the application of the nanoindentation method for investigation of their mechanical properties at the nanoscale.
In this study, we performed nanoindentation experiments on two sets of silicon nanolines (SiNLs) of widths 24 nm and 90 nm, respectively, to investigate the mechanical behavior of silicon structures at tens of nanometer scale. The high height-to-width aspect ratio (∼15) SiNLs were fabricated by an anisotropic wet etching (AWE) method, having straight and nearly atomically flat sidewalls. In the test, buckling instability was observed at a critical load, which was fully recoverable upon unloading. It was found that friction at the contact between the indenter and SiNLs played an important role in the buckling response. Based on a finite element model (FEM), the friction coefficient was estimated to be in a range of 0.02 to 0.05. The strain to failure was estimated to range from 3.8% for 90 nm lines to 7.5% for 24 nm lines.
The extraction of nanoscale dimensions and feature geometry of grating targets using signature-based optical techniques is an area of continued interest in semiconductor manufacturing. In the current work, we have performed angle-resolved scatterometry measurements on grating targets of 180 nm pitch fabricated by electron beam lithography and anisotropic wet etching of (110)-oriented silicon. The use of oriented silicon results in grating lines with nominally vertical sidewalls, with linewidths estimated by scanning electron microscopy (SEM) to be in the sub-50 nm range. The targets were designed to be suitable for both optical scatterometry and small-angle x-ray scattering (SAXS) measurement. As a consequence of the lattice-plane selective etch used for fabrication, the target trenches do not have a flat bottom, but rather have a wide vee shape. We demonstrate extraction of linewidth, line height, and trench profile using scatterometry, with an emphasis on modeling the trench angle, which is well decoupled from other grating parameters in the scatterometry model and is driven by the crystalline orientation of the Si lattice planes. Issues such as the cross-correlation of grating height and linewidth in the scatterometry model, the limits of resolution for angle-resolved scatterometry at the wavelength used in this study (532 nm), and prospects for improving the height and linewidth resolution obtained from scatterometry of the targets, are discussed.
Atomic force microscope-(AFM-) based indentation tests were performed to examine mechanical properties of parallel single-crystal silicon nanolines (SiNLs) of sub-100-nm line width, fabricated by a process combining electron-beam lithography and anisotropic wet etching. The SiNLs have straight and nearly atomically flat sidewalls, and the cross-section is almost perfectly rectangular with uniform width and height along the longitudinal direction. The measured load-displacement curves from the indentation tests show an instability with large displacement bursts at a critical load ranging from 480 µN to 700 µN. This phenomenon is attributed to a transition of the buckling mode of the SiNLs under indentation. Using a set of finite element models with postbuckling analyses, we analyze the indentation-induced buckling modes and investigate the effects of tip location, contact friction, and substrate deformation on the critical load of mode transition. The results demonstrate a unique approach for the study of nanomaterials and patterned nanostructures via a combination of experiments and modeling.
We designed and fabricated silicon probe with nanophotonic force sensor to directly stimulate neurons (PC12) and measured its effect on neurite initiation and elongation. A single-layer pitch-variable diffractive nanogratings was fabricated on silicon nitride probe using e-beam lithography, reactive ion etching and wet-etching techniques. The nanogratings consist of flexure folding beams suspended between two parallel cantilevers of known stiffness. The probe displacement, therefore the force, can be measured through grating transmission spectrum. We measured the mechanical membrane characteristics of PC12 cells using the force sensors with displacement range of 10 mum and force sensitivity 8 muN/mum. Young's moduli of 425 +/- 30 Pa are measured with membrane deflection of 1% for PC12 cells cultured on polydimethylsiloxane (PDMS) substrate coated with collagen or laminin in Ham's F-12K medium. In a series of measurements, we have also observed stimulation of directed neurite contraction up to 6 mum on extended probing for a time period of 30 min. This method is applicable to measure central neurons mechanics under subtle tensions for studies on development and morphogenesis. The close synergy between the nano-photonic measurements and neurological verification can improve our understanding of the effect of external conditions on the mechanical properties of cells during growth and differentiation.
A comparison study has been conducted on the formation of catalyst nanoparticles on a high surface tension metal and low surface tension oxide for carbon nanotube (CNT) growth via catalytic chemical vapor deposition (CCVD). Silicon dioxide (SiO2) and tantalum have been deposited as supporting layers before deposition of a thin layer of iron catalyst. Iron nanoparticles were formed after thermal annealing. It was found that densities, size distributions, and morphologies of iron nanoparticles were distinctly different on the two supporting layers. In particular, iron nanoparticles revealed a Volmer-Weber growth mode on SiO2 and a Stranski-Krastanov mode on tantalum. CCVD growth of CNTs was conducted on iron∕tantalum and iron∕SiO2. CNT growth on SiO2 exhibited a tip growth mode with a slow growth rate of less than 100nm∕min. In contrast, the growth on tantalum followed a base growth mode with a fast growth rate exceeding 1μm∕min. For comparison, plasma enhanced CVD was also employed for CNT growth on SiO2 and showed a base growth mode with a growth rate greater than 2μm∕min. The enhanced CNT growth rate on tantalum was attributed to the morphologies of iron nanoparticles in combination with the presence of an iron wetting layer. The CNT growth mode was affected by the adhesion between the catalyst and support as well as CVD process.
Carbon nanotubes (CNTs) have been grown by catalytical chemical vapor deposition (CCVD) with a thin iron layer as the catalyst. High surface tension metal, tantalum (Ta), and low surface tension, SiC 2 , have been deposited as the supporting layers before depositing the catalysts. SEM, TEM, STEM and EELS have been used to examine the morphology, structure, and chemical profile of iron nanoparticles and CNTs. The results have shown that the catalyst nanoparticle morphologies were distinctly different on two supports. In particular, Fe nanoparticles on SiC 2 were found to follow a Vollmer-Weber (VW) growth mode and a Stranski-Krastanov (SK) growth mode on Ta. It was also found that CNT growth varied significantly on two supports in terms of morphology, growth rate and growth mode. Dense CNTs were grown on Ta with fast growth rates (> 1µm/min) and vertical alignment for the iron thicknesses of 1.5-9 nm. In contrast, CNTs grown on SiC 2 exhibited a slow growth rate (< 100 nm/min) with all deposited iron thicknesses, indicating a severe catalyst poisoning. The results suggested that the catalyst morphology in combination with the presence of an iron wetting layer contributed to the enhanced CCVD growth of CNTs on Ta.
This letter demonstrates a method for fabricating single-crystal Si nanolines, with rectangular cross sections and nearly atomically flat sidewalls. The high quality of these nanolines leads to superb mechanical properties, with the strain to fracture measured by nanoindentation tests exceeding 8.5% for lines of 74 nm width. A large displacement burst before fracture was observed, which is attributed to a buckling mechanism. Numerical simulations show that the critical load for buckling depends on the friction at the contact surface.
We fabricated single-layer pitch-variable diffractive nanogratings on silicon nitride probe using e-beam lithography and subsequent pattern transfer techniques. The nanogratings consist of flexure folding beams suspended between two parallel cantilevers of known stiffness. The probe displacement, therefore the force, can be measured through grating transmission spectrum. We measured the mechanical membrane characteristics of PC 12 cells using the force sensors with displacement range of 10 mum and force sensitivity 8 muN/mum. Young's moduli of 425plusmn30 Pa are measured with membrane deflection of 1% for PC 12 cells cultured on polydimethylsiloxane(PDMS) substrate coated with collagen or laminin in Ham's F-12 K medium. We have also observed stimulation of directed neurite contraction up to 6 mum on extended probing for a time period of 30 minutes.
A new test structure has been designed and fabricated for the investigation of the effect of linewidth scaling on electron transport in nickel mono-silicide features. In the fabrication process, nickel silicide (NiSi) features were formed by annealing a nickel coating that was deposited on singlecrystal silicon features that were as narrow as 150 nm and had vertical and nearly atomically flat sidewalls. The features were patterned on (110) silicon-on-insulator wafers with i-line lithography that replicated test structures from which voltage/current (V/I) measurements could be extracted. Subsequently, the patterning of single-crystal features with direct-write electron-beam lithography has been developed in order to facilitate the future reduction of the linewidths of NiSi features having a highly controlled surface microstructure to below 40 nm.
The dual damascene process used to generate copper interconnects requires many difficult processing steps. Back End Of Line (BEOL) processing using Step and Flash Imprint Lithography (SFIL) on a directly patternable dielectric material can dramatically reduce the number of processing steps. By using multi-level SFIL rather than photolithography, two levels of interconnect structure (trench and corresponding via) can be patterned simultaneously. In addition, the imprinted material can be a imprintable dielectric precursor rather than a resist, further reducing the total number of steps in the dual damascene process. This paper presents progress towards integrating multi-level SFIL into a copper CMP process flow at ATDF, Inc. in Austin, Texas. Until now, work has focused on multi-level imprint process development. This report focuses on the development of new imprintable dielectric precursors for use with the dual damascene imprint process. SFIL compatible dielectric precursors were synthesized and characterized for integration into the ATDF copper CMP process flow. SFIL requires properties not found in currently available semiconductor dielectrics such as low viscosity and rapid photo-induced polymerization. Inorganic/organic hybrid materials derived from sol-gel chemistry and polyhedral oligomeric silsesquioxane (POSS) structures show promise for this application. The properties of three different dielectric layers are compared. The viability of each material as an interlayer dielectric is discussed and the results of multi-level patterning, metal fill, and polish are shown.
Selective growth of vertically aligned and highly dense carbon nanotubes was achieved by using thermal chemical vapor deposition via careful selection of a thin catalyst layer and an appropriate supporting layer. It was found that carbon nanotube growth was significantly enhanced when tantalum was used as the supporting layer on which a thin iron catalyst was deposited. Cross-sectional transmission electron microscopy revealed a Stranski-Krastanov mode of iron island growth on tantalum with relatively small contact angles controlled by the relative surface energies of the supporting layer, the catalyst, and their interface. The as-formed iron island morphology promoted vertical growth of carbon nanotubes.
In this paper, we investigated void formation in passivated Cu films focusing on the kinetics of void formation under isothermal annealing as a function of temperature. Interestingly, we found that the kinetics of void formation in Cu films is consistent with that observed in Cu lines, which is driven by the combined effect of thermal stress and mass transport resulting in a peak growth rate at about 250°C. To analyze the observed results, we have calculated the stress state at the <111>/<200> Cu grain boundary to demonstrate the existence of a localized triaxial stress state as a result of elastic anisotropy. To account for void density, x-ray analysis was performed to measure the grain texture using inverse pole figure plot and the result can account for the void density observed. A kinetic model was used to analyze void growth under isothermal annealing. A threshold stress of about 40MPa was deduced for void growth in passivated Cu films with an activation energy of 0.75 eV.
A thermal nano-imprint method has; been developed to pattern sub-40 nm polymer lines of Hydrogensilsesquioxane (HSQ) and electron beam resist ZEP 520A. The imprint template was the cross section surface of a selectively etched GaAs/AlGaAs heterostructure wafer. Silicon nanowires were formed using reactive ion etching (RIE) of a silicon-on-insulator wafer with the polymer nanolines as an etching mask. The obtained Si nanowires were well defined and continuous for a length up to hundreds of microns. Reaction of the silicon lines with a metal can lead to the formation of silicide interconnect lines, which is used to investigate the size effects on the transport and electromigration properties of interconnects for future microelectronics.