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TEM Studies of Segregation in a Ge–Sb–Te Alloy During Heating

Springer Proceedings in Materials

Singh, Manish K.; Ghosh, Chanchal; Kotula, Paul G.; Bakan, Gokhan; Silva, Helena; Carter, Clive B.

Phase-change materials are important for optical and electronic computing memory. Ge–Sb–Te (GST) is one of the important phase-change materials and has been studied extensively for fast, reversible, and non-volatile electronic phase-change memory. GST exhibits structural transformations from amorphous to metastable fcc at ~150 ℃ and fcc to hcp at ~300 ℃. The investigation of the structural, microstructural, and microchemical changes with high-temporal resolution during heating is crucial to gain insights on the changes that materials undergo during phase transformations. The as-deposited GST film has amorphous island morphology which transform to the metastable fcc phase at ~130 ℃. The second-phase transformation, from fcc to hexagonal, is observed at ~170 ℃. While the as-deposited amorphous islands show a homogeneous distribution of Ge, Sb and Te, these islands boundaries become Ge-rich after heating. Morphological and structural evolutions were captured during heating inside an aberration corrected environmental TEM equipped with a high-speed camera under a low-dose conditions to minimize beam-induced changes in the samples. Microchemical studies were carried out employing ChemiSTEM technique in probe-corrected mode with a monochromated beam.

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Characterization of Amplification Properties of the Superconducting-Ferromagnetic Transistor

IEEE Transactions on Applied Superconductivity

Nevirkovets, Ivan P.; Kojima, Takafumi; Uzawa, Yoshinori; Kotula, Paul G.; Missert, Nancy A.; Mukhanov, Oleg A.

We report on the measurement results of the superconducting-ferromagnetic transistors (SFTs). The devices were made at Northwestern University and Hypres (SeeQC), Inc. (Nevirkovets et al., 2014; 2015). SFT is a multiterminal device with the SISFIFS (or SFIFSIS) structure (where S, I, and F denote a superconductor, an insulator, and a ferromagnetic material, respectively) exploiting intense quasiparticle injection in order to modify the nonlinear I-V curve of a superconducting tunnel junction. SFT is capable of providing voltage, current, and power amplification while having good input/output isolation. We characterized the devices using different measurement techniques. We measured S parameters of the single- and double-acceptor devices at frequencies up to 5 MHz. Importantly, we confirmed that the isolation between the input and output of the device is quite good. However, the techniques typically employed to characterize semiconductor devices do not allow for revealing the full potential of our low-resistive SFT devices, especially those having two acceptors. In the latter case, we also tested the devices using the battery-powered current sources with floating grounds. Analyzing double-acceptor I-V curves recorded at different levels of injection currents, for an optimal load, we deduced a small-signal voltage gain of 33 and a power gain of 2.4. We suggest that further improvement of the SFT device parameters is possible in optimized devices, so that the device potentially may serve as a preamplifier for readout of output signals of cryogenic detectors and be useful as an element of other superconductor-based circuits. In addition, we used scanning transmission electron microscopy to identify some problems in the fabrication of the devices without any planarization.

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In situ TEM study of crystallization and chemical changes in an oxidized uncapped Ge2Sb2Te5film

Journal of Applied Physics

Singh, Manish K.; Ghosh, Chanchal; Miller, Benjamin; Kotula, Paul G.; Watt, John; Bakan, Gokhan; Silva, Helena; Carter, Clive B.

Ge2Sb2Te5 (GST-225) has been the most used active material in nonvolatile phase-change memory devices. Understanding the kinetics and dynamics involved in crystallization is critical for the optimization of materials and devices. A GST-225 thin film of 20 nm thickness was prepared by sputtering directly onto a Protochip and left uncapped and exposed to atmosphere for approximately 1 year. Early stages of crystallization and growth of the film have been studied inside the TEM from room temperature to 140 °C. The morphological and structural transformations have been studied by a Cs-corrected environmental TEM, and images have been recorded using a high-speed low electron dose camera (Gatan K3 IS). The amorphous to crystalline transformation has been observed at ~35 °C. From the large field, high-resolution images obtained using the Gatan K3 IS camera early crystallization can be detected and nucleation rates and growth velocities can be obtained.

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Assessing atomically thin delta-doping of silicon using mid-infrared ellipsometry

Journal of Materials Research

Katzenmeyer, Aaron M.; Luk, Ting S.; Bussmann, Ezra B.; Young, Steve M.; Anderson, Evan M.; Marshall, Michael T.; Ohlhausen, J.A.; Kotula, Paul G.; Lu, Ping L.; Campbell, DeAnna M.; Lu, Tzu-Ming L.; Liu, Peter Q.; Ward, Daniel R.; Misra, Shashank M.

Hydrogen lithography has been used to template phosphine-based surface chemistry to fabricate atomic-scale devices, a process we abbreviate as atomic precision advanced manufacturing (APAM). Here, we use mid-infrared variable angle spectroscopic ellipsometry (IR-VASE) to characterize single-nanometer thickness phosphorus dopant layers (δ-layers) in silicon made using APAM compatible processes. A large Drude response is directly attributable to the δ-layer and can be used for nondestructive monitoring of the condition of the APAM layer when integrating additional processing steps. The carrier density and mobility extracted from our room temperature IR-VASE measurements are consistent with cryogenic magneto-transport measurements, showing that APAM δ-layers function at room temperature. Finally, the permittivity extracted from these measurements shows that the doping in the APAM δ-layers is so large that their low-frequency in-plane response is reminiscent of a silicide. However, there is no indication of a plasma resonance, likely due to reduced dimensionality and/or low scattering lifetime.

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Role of Oxygen on Chemical Segregation in Uncapped Ge2Sb2Te5 Thin Films on Silicon Nitride

ECS Journal of Solid State Science and Technology

Tripathi, Shalini; Kotula, Paul G.; Singh, Manish K.; Ghosh, Chanchal; Bakan, Gokhan; Silva, Helena; Carter, Clive B.

Germanium antimony telluride has been the most used and studied phase-change material for electronic memory due to its suitable crystallization temperature, amorphous to crystalline resistance contrast, and stability of the amorphous phase. In this paper, the segregation of Ge in a Ge2Sb2Te5 film of 30 nm thickness during heating inside the transmission electron microscope was observed and characterized. Furthermore, Ge2Sb2Te5 film was deposited using sputtering on a Protochips Fusion holder and left uncapped in atmosphere for about four months. Oxygen incorporated within the film played a significant role in the chemical segregation observed which resulted in amorphous Ge-O island boundaries and Sb and Te rich crystalline domains. Such composition changes can occur when the phase-change material interfaces insulating oxide layers in an integrated device and can significantly impact its electrical and thermal properties.

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Complexion dictated thermal resistance with interface density in reactive metal multilayers

Physical Review B

Saltonstall, Christopher B.; Mcclure, Zachary D.; Abere, Michael J.; Guzman, David; Reeve, Samuel T.; Strachan, Alejandro; Kotula, Paul G.; Adams, David P.; Laros, James H.

Multilayers composed of aluminum (Al) and platinum (Pt) exhibit a nonmonotonic trend in thermal resistance with bilayer thickness as measured by time domain thermoreflectance. The thermal resistance initially increases with reduced bilayer thickness only to reach a maximum and then decrease with further shrinking of the multilayer period. These observations are attributed to the evolving impact of an intermixed amorphous complexion approximately 10 nm in thickness, which forms at each boundary between Al- and Pt-rich layers. Scanning transmission electron microscopy combined with energy dispersive x-ray spectroscopy find that the elemental composition of the complexion varies based on bilayer periodicity as does the fraction of the multilayer composed of this interlayer. These variations in complexion mitigate boundary scattering within the multilayers as shown by electronic transport calculations employing density-functional theory and nonequilibrium Green's functions on amorphous structures obtained via finite temperature molecular dynamics. The lessening of boundary scattering reduces the total resistance to thermal transport leading to the observed nonmonotonic trend thereby highlighting the central role of complexion on thermal transport within reactive metal multilayers.

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Localized corrosion of low-carbon steel at the nanoscale

npj Materials Degradation

Jungjohann, Katherine L.; Chisholm, Claire; Grudt, Rachael O.; Aguiar, Jeffery A.; Mook, William M.; Kotula, Paul G.; Pilyugina, Tatiana S.; Bufford, Daniel C.; Hattar, Khalid M.; Kucharski, Timothy J.; Taie, Ihsan M.; Ostraat, Michele L.

Mitigating corrosion remains a daunting challenge due to localized, nanoscale corrosion events that are poorly understood but are known to cause unpredictable variations in material longevity. Here, the most recent advances in liquid-cell transmission electron microscopy were employed to capture the advent of localized aqueous corrosion in carbon steel at the nanoscale and in real time. Localized corrosion initiated at a triple junction formed by a solitary cementite grain and two ferrite grains and then continued at the electrochemically-active boundary between these two phases. With this analysis, we identified facetted pitting at the phase boundary, uniform corrosion rates from the steel surface, and data that suggest that a re-initiating galvanic corrosion mechanism is possible in this environment. These observations represent an important step toward atomically defining nanoscale corrosion mechanisms, enabling the informed development of next-generation inhibition technologies and the improvement of corrosion predictive models.

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Spin transport in an insulating ferrimagnetic-antiferromagnetic-ferrimagnetic trilayer as a function of temperature

AIP Advances

Chen, Yizhang; Cogulu, Egecan; Roy, Debangsu; Ding, Jinjun; Mohammadi, Jamileh B.; Kotula, Paul G.; Missert, Nancy A.; Wu, Mingzhong; Kent, Andrew D.

We present a study of the transport properties of thermally generated spin currents in an insulating ferrimagnetic-antiferromagnetic-ferrimagnetic trilayer over a wide range of temperature. Spin currents generated by the spin Seebeck effect (SSE) in a yttrium iron garnet (YIG) YIG/NiO/YIG trilayer on a gadolinium gallium garnet (GGG) substrate were detected using the inverse spin Hall effect (ISHE) in Pt. By studying samples with different NiO thicknesses, the spin diffusion length of NiO was determined to be ∼3.8 nm at room temperature. Surprisingly, a large increase of the SSE signal was observed below 30 K, and the field dependence of the signal closely follows a Brillouin function for an S=7/2 spin. The increase of the SSE signal at low temperatures could thus be associated with the paramagnetic SSE from the GGG substrate. Besides, a broad peak in the SSE response was observed around 100 K. These observations are important in understanding the generation and transport properties of spin currents through magnetic insulators and the role of a paramagnetic substrate in spin current generation.

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Visualization of Kirkendall Voids at Cu-Au Interfaces by In Situ TEM Heating Studies

JOM

Kotula, Paul G.; Prasad, Somuri V.

Gold-plated copper alloys are used extensively in electrical contacts where diffusional processes are known to cause contact degradation. An in situ transmission electron microscopy (TEM) heating study was carried out to provide fundamental understanding of the aging phenomena in reasonable timescales. Samples to visualize the interface in TEM were prepared by focused ion beam (FIB) microscopy and heated in situ up to 350°C while holding at intermediate temperatures to enable imaging. The grain boundaries in Au coatings, specifically the columnar boundaries, provided rapid pathways for diffusion of Cu all the way to the Au surface. This unequal diffusion created vacancies in Cu which coalesced into Kirkendall voids. This in situ technique has been applied to visualize the diffusion pathways in electroplated and sputtered Au films deposited directly on Cu, as well the role of Ni and NiP as barrier layers for mitigating Cu diffusion.

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Advanced high-spatial-resolution diffraction diagnostics

Kotula, Paul G.

Diffraction series data have been acquired and analyzed via multivariate statistical analysis. For two different data series analyzed, the data analysis was able to reduce the raw diffraction data series into a much smaller easier-to-interpret solution consisting mainly of crystallographic phase and orientation information.

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Results 51–75 of 363
Results 51–75 of 363