Method Development for Contactless Resonant Cavity Dielectric Spectroscopic Studies of Cellulosic Paper

The current analytical techniques for characterizing printing and graphic arts substrates are largely ex situ and destructive. This limits the amount of ...

National Institute of Standards and Technology

In this work, we compare the electrical characteristics of MoS2 field-effect transistors (FETs) with Ag source/drain contacts with those with Ti and demonstrate that the metal-MoS2 interface is crucial to the device performance. MoS2 FETs with Ag contacts show more than 60 times higher ON-state current than those with Ti contacts. In order to better understand the mechanism of the better performance with Ag contacts, 5 nm Au/5 nm Ag (contact layer) or 5 nm Au/5 nm Ti film was deposited onto MoS2 monolayers and few layers, and the topography of metal films was characterized using scanning electron microscopy and atomic force microscopy. The surface morphology shows that, while there exist pinholes in Au/Ti film on MoS2, Au/Ag forms a smoother and denser film. Raman spectroscopy was carried out to investigate the metal-MoS2 interface. The Raman spectra from MoS2 covered with Au/Ag or Au/Ti film reveal that Ag or Ti is in direct contact with MoS2. Our findings show that the smoother and denser Au/Ag contacts lead to higher carrier transport efficiency.

Influence of metal-MoS2 interface on MoS2 transistor performance: comparison of Ag and Ti contacts.

In this paper, we attempt to understand the physico-chemical changes that occur in devices during device "burn-in". We discuss the use of low frequency dielectric spectroscopy to detect, characterize and monitor changes in electrical defects present in the dielectrics of through silicon vias (TSV) for three dimensional (3D) interconnected integrated circuit devices, as the devices are subjected to fluctuating thermal loads. The observed changes in the electrical characteristics of the interconnects were traceable to changes in the chemistry of the isolation dielectric used in the TSV construction. The observed changes provide phenomenological insights into the practice of burn-in. The data also suggest that these "chemical defects" inherent in the 'as-manufactured' products may be responsible for some of the unexplained early reliability failures observed in TSV enabled 3D devices.

Towards Understanding Early Failures Behavior during Device Burn-In: Broadband RF Monitoring of Atomistic Changes in Materials.

In this work we studied the impact of pulse electroplating parameters on the cross-sectional and surface microstructures of blanket copper films using electron backscattering diffraction and x-ray diffraction. The films evaluated were highly (111) textured in the direction perpendicular to the film surface. The degree of preferential orientation was found to decrease with longer pulse on-times, due to strain energy driven growth of other grain orientations. Residual biaxial stresses were also measured in the films and higher pulse frequencies during deposition led to smaller biaxial stresses in the films. Film stress was also found to correlate with the amount of twinning in the copper film cross-sections. This has been attributed to the twins' thermal stability and mechanical properties.

The Influence of Pulsed Electroplating Frequency and Duty Cycle on Copper Film Microstructure and Stress State.

In this paper, we discuss the use of broadband microwaves (MW) to characterize the thermal stability of organic and hybrid silicon-organic thin films meant for insulation applications in micro- and nanoelectronic devices. We take advantage of MW propagation characteristics to extract and examine the relationships between electrical properties and the chemistry of prototypical low-k materials. The impact of thermal anneal at modest temperatures is examined to shed light on the thermal-induced performance and reliability changes within the dielectric films. These changes are then correlated with the chemical changes in the films, and could provide basis for rational selection of organic dielectrics for integrated devices.

Broadband Dielectric Spectroscopic Characterization of Thermal Stability of Low-k Dielectric Thin Films for Micro- and Nanoelectronic Applications.

Organic additives are typically used in the pulse electrodeposition of copper (Cu) to prevent void formation during the filling of high aspect ratio features. In this work, the role of bath chemistry as modified by organic additives was investigated for its effects on Cu trench microstructure. Polyethylene glycol (PEG), bis(3-sulfopropyl) disulfide (SPS), and Janus green b (JGB) concentrations were varied in the Cu electrodeposition bath. Results indicated a correlation between the JGB/SPS ratio and the surface roughness and residual stresses in the Cu. Electron backscattering diffraction (EBSD) and transmission Kikuchi diffraction (TKD) were used to study the cross-sectional microstructure in the trenches. Finer grain morphologies appeared in trenches filled with organic additives as compared to additive-free structures. Cu trench (111) texture also decreased with increasing organic additive concentrations due to more pronounced influence of sidewall seed layers on trench features. Twin density in the microstructure closely tracked calculated stresses in the Cu trenches. A comprehensive microstructural analysis was conducted in this study, on an area of focus that has garnered little attention from the literature, yet can have a major impact on microelectronic reliability.

The Impact of Organic Additives on Copper Trench Microstructure.

Traditional metrology has been unable to adequately address the needs of the emerging integrated circuits (ICs) at the nano scale; thus, new metrology and techniques are needed. For example, the reliability challenges in fabrication need to be well understood and controlled to facilitate mass production of through-substrate-via (TSV) enabled three-dimensional integrated circuits (3D-ICs). This requires new approaches to the metrology. In this paper, we use the microwave propagation characteristics to study the reliability issues that precede the physical damage caused by electromigration in the Cu-filled TSVs. The pre-failure microwave insertion losses and group delay are dependent on both the device temperature and the amount of current forced through the devices-under-test. The microwave insertion losses increase with the increase in the test temperature, while the group delay increases with the increase in the forced direct current magnitude. The microwave insertion losses are attributed to the defect mobility at the Cu-TiN interface, and the group delay changes are due to resistive heating in the interconnects, which perturbs the dielectric properties of the cladding dielectrics of the copper fill in the TSVs. https://doi.org/10.1063/1.4992135.

Microwave evaluation of electromigration susceptibility in advanced interconnects.

The advent of recent technologies in the nanoscience arena requires new and improved methods for the fabrication of multiscale features ( e.g., from micro- to nanometer scales). Specifically, biological applications generally demand the use of transparent substrates to allow for the optical monitoring of processes of interest in cells and other biological materials. Whereas wet etching methods commonly fail to produce essential nanometer scale features, plasma-based dry etching can produce features down to tens of nanometers. However, dry etching methods routinely require extreme conditions and extra steps to obtain features without residual materials such as sidewall deposits (veils). This work presents the development of a gold etching process with gases that are commonly used to etch glass. Our method can etch gold films using reactive ion etching (RIE) at room temperature and mild pressure in a trifluoromethane (CHF)/oxygen (O) environment, producing features down to 50 nm. Aspect ratios of 2 are obtainable in one single step and without sidewall veils by controlling the oxygen present during the RIE process. This method generates surfaces completely flat and ready for the deposition of other materials. The gold features that were produced by this method exhibited high conductivity when carbon nanotubes were deposited on top of patterned features (gold nanoelectrodes), hence demonstrating an electrically functional gold after the dry etching process. The production of gold nanofeatures on glass substrates would serve as biocompatible, highly conductive, and chemically stable materials in biological/biomedical applications.

Generating Multiscale Gold Nanostructures on Glass without Sidewall Deposits Using Minimal Dry Etching Steps.

Current product composition and quality test methods for the paper and pulp industry are mainly based on manual ex-situ wet-bench chemistry techniques. For example, the standard method for determining the furnish of paper, TAPPI T 401 "Fiber analysis of paper and paperboard," relies on the experience and visual acuity of a specially trained analyst to determine the individual plant species present and to quantify the amount of each constituent fiber type in a sheet of paper. Thus, there is a need for a fast, nondestructive analytical technique that leverages intrinsic attributes of the analytes. In this paper, we demonstrate an application of dielectric spectroscopy (DS) as a potential metrology to differentiate between nonwood pulp and wood pulp fibers. This in-situ, noncontact and nondestructive assessment method has inherent forensic capabilities and is also amiable to quality assurance techniques such as gauge capability studies and real-time statistical process control (SPC).

Dielectric spectroscopic studies of biological material evolution and application to paper.

Traditional metrology has been unable to adequately address the reliability needs of emerging integrated circuits at the nano scale; thus, new metrology and techniques are needed. In this paper, we use microwave propagation characteristics (insertion loss and dispersion) to study the atmospheric interconnect corrosion under accelerated stress conditions. The results presented in this work indicate that the corrosion resilience of the test device is limited by the thermal aging of the passivation layer.

Yaw S. Obeng

Nanoscale Device Characterization Division,
Physical Measurement Laboratory,
Nanoscale Device Characterization Division, Physical Measurement Laboratory

National Institute of Standards and Technology

Method Development for Contactless Resonant Cavity Dielectric Spectroscopic Studies of Cellulosic Paper

Yaw S. Obeng

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National Institute of Standards and Technology

Method Development for Contactless Resonant Cavity Dielectric Spectroscopic Studies of Cellulosic Paper

Nanoscale Device Characterization Division,
Physical Measurement Laboratory,
Nanoscale Device Characterization Division, Physical Measurement Laboratory