Article
Chemistry, Multidisciplinary
Osman El-Atwani, Hyosim Kim, Cayla Harvey, Mert Efe, Stuart A. Maloy
Summary: This study highlights the limitations of thermal stability analysis using in-situ transmission electron microscopy (TEM)-annealing experiments on ultrafine and nanocrystalline materials. By comparing in-situ TEM experiments with bulk material annealing experiments on nanocrystalline pure copper and HT-9 steel, they found different outcomes for pure copper but similar results for HT-9 steel. The discussion focuses on the necessity of comparing in-situ TEM annealing experimental results to bulk annealing for material thermal stability assessment.
Article
Materials Science, Multidisciplinary
N. Resnina, A. Sibirev, S. Belyaev, E. Ubyivovk
Summary: The aim of this study was to observe the movement of martensite interfaces in pre-deformed NiTi shape memory alloy during temperature variation using transmission electron microscopy (TEM). The Ni50Ti50 alloy was pre-deformed by 10% tension in the martensite state and then unloaded. Thin foils were prepared for in-situ TEM analysis of the movement of martensite interfaces during heating-cooling-heating cycles. The results showed that the martensite interfaces started moving at high temperatures during the first heating, lost their mobility during pre-deformation, and regained their mobility after the first heating.
Article
Materials Science, Multidisciplinary
Xin Li Phuah, Jie Jian, Han Wang, Xuejing Wang, Xinghang Zhang, Haiyan Wang
Summary: This study demonstrates the use of in situ transmission electron microscopy (TEM) heating to observe ceramic nanoparticles in real-time under ultra-high heating rates up to 1200 degrees C/s. It was found that ultra-high heating rate is highly effective in densifying 3 mol.% yttria-stabilized zirconia nanoparticles, while less effective for 8 mol.% yttria-stabilized zirconia or zinc oxide due to competing diffusion mechanisms.
MATERIALS RESEARCH LETTERS
(2021)
Article
Materials Science, Multidisciplinary
Yuxin Zhong, Xiaoyong Wu, Lu Wu, Sha Zhao, Hanxuan Su, Zhien Ning, Wei Zhang, Ning Liu, Jijun Yang
Summary: The structural evolution of Cr-coated Zr-4 after irradiation was investigated using in situ TEM. Krypton bubbles were observed at 700°C and increased in size with temperature. The grain size and shape of the irradiated Zr-4 substrate changed, eventually forming columnar crystals due to irradiation-induced compressive stress. Cr2Zr C14 phases were formed at both the interface and the substrate at 700°C and 1000°C. In addition, the accelerated failure process of the irradiated Cr coating at high temperatures was observed via in situ TEM analysis.
Article
Chemistry, Multidisciplinary
Hongkui Zheng, Mingjie Xu, Kai He
Summary: In this study, the phase transformation pathways and surface amorphization during sol-gel and solid-state syntheses of LLZO were compared using in situ heating transmission electron microscopy (TEM). The results revealed different phase transformation pathways and the crystal growth process of LLZO. It was also found that surface amorphization significantly affected the ionic conductivity of LLZO.
Article
Chemistry, Physical
Tobias Meyer, Birte Kressdorf, Vladimir Roddatis, Jorg Hoffmann, Christian Jooss, Michael Seibt
Summary: The study investigates the rich phase diagram of Pr1-xCaxMnO3 and the structural transition in epitaxial thin films, highlighting the importance of controlling the environment during heating.
Article
Materials Science, Multidisciplinary
Marcus Tornberg, Carina B. Maliakkal, Daniel Jacobsson, Reine Wallenberg, Kimberly A. Dick
Summary: The world of environmental microscopy offers the possibility to study transformations and reactions during realistic conditions. This study presents the design and development of a metal-organic chemical vapor deposition (MOCVD) system integrated with an environmental transmission electron microscope for real-time investigations of crystal growth. The influences of temperature and reactive gas on imaging and spectroscopy are evaluated.
MICROSCOPY AND MICROANALYSIS
(2022)
Article
Anatomy & Morphology
Sriram Vijayan, Rongxuan Wang, Zhenyu Kong, Joerg R. Jinschek
Summary: This study introduces a new method to generate thermal gradients across a TEM specimen by modifying a MEMS-based heating stage. Results showed that the temperature in the central viewing area of the unmodified device was slightly lower than the setpoint temperature, while the modified device exhibited thermal gradients up to 7.0 x 10(6) degrees C/m at the edge.
MICROSCOPY RESEARCH AND TECHNIQUE
(2022)
Article
Nanoscience & Nanotechnology
Yujiao Zhou, Gilles Ledoux, David Philippon, Sylvie Descartes, Matteo Martini, Shaozhou He, Cedric Desroches, Didier Fournier, Catherine Journet, Laurence Bois
Summary: Photoluminescent temperature sensors based on gadolinium orthovanadate (GdVO4) doped with ytterbium and erbium were developed and dispersed in different media for temperature measurement. The luminescence intensity ratio of thermally coupled erbium emission peaks varies linearly with temperature and can be corrected for laser-induced thermal effects.
ACS APPLIED NANO MATERIALS
(2022)
Article
Materials Science, Multidisciplinary
Alexey Minenkov, Natalija Santic, Tia Truglas, Johannes Aberl, Lada Vukusic, Moritz Brehm, Heiko Groiss
Summary: In this paper, a novel method for preparing TEM samples for in situ observation is presented. The method combines the wedge polishing technique and an enhanced FIB workflow, allowing the thinning of the sample to electron transparency while maintaining its pristine properties. The step-by-step guide provided makes it easy to follow and adapt the method for different equipment, opening up new possibilities for in situ TEM heating experiments on fragile materials.
Article
Chemistry, Physical
Meihong He, Guantao Wang, Yuxiang Zhu, Yanan Wang, Fu Liu, Sida Luo
Summary: By introducing joule heating as a critical in-situ treatment, the specific surface area and pore volume of the laser-induced graphene paper can be improved for enhanced capacitive performance. Optimizing the heating temperature and time can significantly increase the specific areal capacitance of the MSCs.
Article
Materials Science, Coatings & Films
Ning Zhu, Luke N. Brewer
Summary: This research studied the relationship between processing and microstructure in cold sprayed AA7050 after laser heat treatment with different levels of heat input. The ability to modify the microstructure and properties of cold sprayed AA7050 using laser heating is important for repair applications. A diode laser was used to heat treat the cold sprayed AA7050 in situ, without sectioning samples. The results showed that laser heat treatment coarsened the ultra-fine grains in the deposit's particle boundary regions, while the larger grains in the particle center regions remained the same. Precipitates were observed in the deposits after laser heat treatment, and the highest heat input deposit had the highest density of precipitates.
SURFACE & COATINGS TECHNOLOGY
(2023)
Article
Metallurgy & Metallurgical Engineering
Jianan Hu, Mengmeng Yang, Wenlong Xiao, Hao Wang, Dehai Ping, Chengze Liu, Shewei Xin, Songquan Wu, Kai Zhang, Yi Yang, Lai-Chang Zhang, Aijun Huang
Summary: In this study, the thermally induced HCP to FCC phase transition in Ti35 alloy was investigated using in situ heating TEM and ab initio calculations. The observations revealed that the phase transition occurred within the matrix/twin and at the twin boundaries, leading to the formation of FCC-Ti in different morphologies. The crystallographic orientation relationship between HCP-Ti and FCC-Ti was determined, and the phase transition mechanism involved the formation of an intermediate state through the slip of partial dislocations. Moreover, the formation of FCC-Ti was found to be influenced by thermal stress, temperature, and contamination of interstitial atoms.
ACTA METALLURGICA SINICA-ENGLISH LETTERS
(2023)
Article
Microscopy
Robert Krisper, Judith Lammer, Yevheniy Pivak, Evelin Fisslthaler, Werner Grogger
Summary: This article systematically investigates the influence of infrared radiation generated by MEMS-based in situ heating systems on the results and interpretation of energy-dispersive X-ray spectra. The study finds that IR photons significantly affect the count rates, dead time, electronic noise levels, energy resolution, and detection efficiency of semiconductor detectors, particularly limiting the traceability of low-Z elements at higher sample temperatures.
Article
Chemistry, Physical
Ya Shen, Xuechun Zhao, Ruiling Gong, Eric Ngo, Jean-Luc Maurice, Pere Roca Cabarrocas, Wanghua Chen
Summary: In this study, we used in situ transmission electron microscopy to observe the dynamic changes of Si nanowires under electron beam irradiation. Evidence of structural evolutions due to a combination of electron beam and thermal effects was found. Different evolution of Si nanowires was observed on carbon and silicon nitride membranes. The Si nanowires on the carbon membrane exhibited serious degradation and formation of Si carbide at temperatures above 800 degrees C, while reversible sectioning and welding of the Si nanowire was observed on the silicon nitride membrane.
Article
Physics, Applied
Krishna Prasad Koirala, Aniruddha Deb, Sara Bey, Tatiana Allen, Ritesh Sachan, Venkatanarayana Prasad Sandireddy, Chenze Liu, Gerd Duscher, James Penner-Hahn, Ramki Kalyanaraman
Summary: Recent studies have found that amorphous oxide thin films made from Fe and lanthanides exhibit rich properties including magnetic, optical, and electronic features, as well as room-temperature magneto-electric coupling with multiferroics. These films show high disorder and slight oxidation after annealing, with high electrical conductivity, Hall mobility, and complex magnetic and optical properties at room temperature.
JOURNAL OF APPLIED PHYSICS
(2021)
Article
Optics
Grace Pakeltis, Enzo Rotunno, Siamak Khorassani, David A. Garfinkel, Robyn Collette, Claire A. West, Scott T. Retterer, Juan Carlos Idrobo, David J. Masiello, Philip D. Rack
Summary: This study leverages the high spatial and energy resolution of monochromated aberration-corrected scanning transmission electron microscopy to investigate the hybridization of cyclic assemblies of plasmonic gold nanorods. The experiments and simulations reveal the coupling of long-axis dipole modes into collective magnetic and electric dipole plasmon resonances, with findings on the energy splitting of the magnetic mode and antibonding modes for oligomers with different polygon edges. Optically, it was found that the extinction efficiencies of electric and magnetic modes are maximized in the n=4 arrangement among the oligomers studied.
Article
Chemistry, Multidisciplinary
Kai Wang, Lizhi Zhang, Giang D. Nguyen, Xiahan Sang, Chenze Liu, Yiling Yu, Wonhee Ko, Raymond R. Unocic, Alexander A. Puretzky, Christopher M. Rouleau, David B. Geohegan, Lei Fu, Gerd Duscher, An-Ping Li, Mina Yoon, Kai Xiao
Summary: Defects are common in 2D materials and can greatly influence their properties. The authors have developed a method using Au-assisted chemical vapor deposition to selectively form antisite defects in WS2 monolayers. Experimental and theoretical analyses confirm the effectiveness of this bottom-up synthesis approach, with potential applications in the synthesis of other 2D materials.
ADVANCED MATERIALS
(2022)
Article
Nanoscience & Nanotechnology
David A. Garfinkel, Vasudevan Iyer, Robyn Seils, Grace Pakeltis, Marc R. Bourgeois, Andrew W. Rossi, Clay Klein, Benjamin J. Lawrie, David J. Masiello, Philip D. Rack
Summary: Trimer meta-atoms composed of three gold rods were fabricated and their near-field plasmonic responses were characterized. The magnetic and electric modes of the trimer structure could be tuned by changing the length of the rods. The study also found that the intensity of the electric mode increased more than expected, while the magnetic mode showed the expected tilt dependence. This research opens up new possibilities for studying the nanoscale excited-state of other magnetic meta-atom structures.
ACS APPLIED NANO MATERIALS
(2022)
Article
Nanoscience & Nanotechnology
David A. Garfinkel, Nan Tang, Grace Pakeltis, Reece Emery, Ilia N. Ivanov, Dustin A. Gilbert, Philip D. Rack
Summary: The magnetic and optical properties of AuxCo1-x thin films and nanoparticles can be tuned by controlling their chemical composition and morphology. Annealing leads to phase separation and enhances the magnetic properties. The optical properties are greatly influenced by the chemical morphology, where phase separation enhances the quality factor and optical absorption.
ACS APPLIED MATERIALS & INTERFACES
(2022)
Article
Instruments & Instrumentation
Leo Saturday, Chris Luck, Leslie Wilson, Jason D. Fowlkes, Philip D. Rack, Nicholas J. Evans
Summary: This study presents a method to simulate the Spallation Neutron Source and characterize the thermal failure of NCD foils. A test stand with in situ diagnostics is used to track foil sublimation and thinning, and a COMSOL simulation is developed to assess potential changes to the NCD film and predict foil temperatures under different beam conditions.
NUCLEAR INSTRUMENTS & METHODS IN PHYSICS RESEARCH SECTION A-ACCELERATORS SPECTROMETERS DETECTORS AND ASSOCIATED EQUIPMENT
(2022)
Article
Chemistry, Multidisciplinary
Sumeer R. Khanna, Michael G. Stanford, Ivan V. Vlassiouk, Philip D. Rack
Summary: In this study, CuxN1-x alloy thin films were used as catalysts for graphene growth at atmospheric pressure. By adjusting the alloy composition, the growth of graphene was controlled. The results showed that graphene primarily grew as a single layer when the Cu concentration (x) was above 69 at.%.
Article
Chemistry, Multidisciplinary
Yiyi Gu, Lizhi Zhang, Hui Cai, Liangbo Liang, Chenze Liu, Anna Hoffman, Yiling Yu, Austin Houston, Alexander A. Puretzky, Gerd Duscher, Philip D. Rack, Christopher M. Rouleau, Xiangmin Meng, Mina Yoon, David B. Geohegan, Kai Xiao
Summary: This study reports an ambient-pressure chemical vapor deposition approach to synthesize metastable monoclinic PdSe2. Monoclinic PdSe2 is selectively synthesized under S-deficient conditions, and its structure and properties are characterized by first-principles calculations and experimental techniques. Monoclinic PdSe2 exhibits strong optical anisotropy and high electron mobility, which is of significant importance for the synthesis of other 2D transition metal dichalcogenides.
Article
Nanoscience & Nanotechnology
John Lasseter, Philip D. Rack, Steven J. Randolph
Summary: In this study, a method for selectively depositing 3D nanostructures using photothermal transport is reported. The ability to initiate the process on sub-diffraction-limit nanoscale features is demonstrated. Thermal simulations show that the geometric shape and optical and thermal properties of the nanostructures are crucial for controlling the CVD reaction.
ACS APPLIED NANO MATERIALS
(2022)
Article
Instruments & Instrumentation
Leo Saturday, Leslie Wilson, Philip D. Rack, Nicholas J. Evans
Summary: This study compares the performance of nanocrystalline diamond stripper foils with microcrystalline alternatives under thermal load conditions. An electron beam mimic is used to evaluate their power dissipation and thermal durability, and postmortem testing is conducted to determine their physical properties.
NUCLEAR INSTRUMENTS & METHODS IN PHYSICS RESEARCH SECTION A-ACCELERATORS SPECTROMETERS DETECTORS AND ASSOCIATED EQUIPMENT
(2022)
Article
Chemistry, Multidisciplinary
Jason D. Fowlkes, Robert Winkler, Philip D. Rack, Harald Plank
Summary: This article presents an electron dose compensation strategy, called DBEA, to address the structural artifact issue caused by temperature gradient in 3D nanoprinting using focused electron beam-induced deposition. By modulating the electron dose, the deviations caused by temperature variations can be corrected, thus improving the printing accuracy.
Article
Chemistry, Multidisciplinary
John Lasseter, Philip D. D. Rack, Steven J. J. Randolph
Summary: This study demonstrates the selective growth of high-purity gold films onto nanoscale 3D architectures using the Me2Au (acac) precursor and pulsed laser pyrolytic chemical vapor deposition. The high thermal resistance of the nanoscale geometries enables selective deposition. The effects of laser irradiance, pulse width, and precursor pressure on the growth rate were explored, and feature-targeting resolutions of approximately 100 and 5 μm were achieved using diode lasers coupled to multimode (915 nm) and single mode (785 nm) fiber optics, respectively. Finite element thermal modeling was used to rationalize the experimental results.
Article
Education, Special
Jason D. Fowlkes, Robert Winkler, Philip D. Rack, Harald Plank
Summary: 3D nanoprinting using focused electron beam-induced deposition is susceptible to structural distortions caused by temperature gradients. In this study, an electron dose compensation strategy called the Decelerating Beam Exposure Algorithm (DBEA) is proposed to correct for nanowire bending during computer-aided design. The DBEA utilizes an analytical solution derived from 3D nanoprinting simulations to offset undesired heating effects. This compensation strategy has the potential to improve the fidelity of 3D nanoscale printing.
RESEARCH IN AUTISM SPECTRUM DISORDERS
(2023)
Article
Chemistry, Multidisciplinary
Jason D. Fowlkes, Robert Winkler, Philip D. Rack, Harald Plank
Summary: 3D nanoprinting using focused electron beam-induced deposition often results in structural artifacts caused by temperature gradients during the deposition process. Researchers have developed an electron dose compensation strategy to correct for these artifacts and improve the precision of 3D nanoprinting.
Article
Materials Science, Multidisciplinary
Timothy G. Lach, Chinthaka M. Silva, Yufan Zhou, Walker L. Boldman, Philip D. Rack, William J. Weber, Yanwen Zhang
Summary: This study investigates the behavior of two sets of near-equiatomic CoCrCuFeNi thin films under irradiation in different environments. The results demonstrate the influence of composition and environmental exposure on the stability of high entropy alloys under radiation, providing insights into controlling these behaviors.
NPJ MATERIALS DEGRADATION
(2022)