Nano-structural changes in Li-ion battery cathodes during cycling revealed by FIB-SEM serial sectioning tomography

2015 ◽  
Vol 3 (35) ◽  
pp. 18171-18179 ◽  
Author(s):  
Bohang Song ◽  
Tan Sui ◽  
Siqi Ying ◽  
Liu Li ◽  
Li Lu ◽  
...  

This study reports the feasibility of utilizing focused ion beam-scanning electron microscopy sectioning to reconstruct the 3D structure of electrodes before and after extended electrochemical cycling. The observed fragmentation of Li-rich layered spherical particles is speculated to be a possible cause of capacity fading.

CORROSION ◽  
10.5006/3881 ◽  
2021 ◽  
Author(s):  
Zachary Karmiol ◽  
Dev Chidambaram

This work investigates the oxidation of a nickel based superalloy, namely Alloy X, in water at elevated temperatures: subcritical water at 261°C and 27 MPa, the transition between subcritical and supercritical water at 374°C and 27 MPa, and supercritical water at 380°C and 27 MPa for 100 hours. The morphology of the sample surfaces were studied using scanning electron microscopy coupled with focused ion beam milling, and the surface chemistry was investigated using X-ray diffraction, Raman spectroscopy, energy dispersive X-ray spectroscopy, and X-ray photoelectron spectroscopy before and after exposure studies. Surfaces of all samples were identified to comprise of a ferrite spinel containing aluminum.


2010 ◽  
Vol 16 (S2) ◽  
pp. 214-215
Author(s):  
T Tanigaki ◽  
K Ito ◽  
K Nakamura ◽  
Y Nagakubo ◽  
J Azuma ◽  
...  

Extended abstract of a paper presented at Microscopy and Microanalysis 2010 in Portland, Oregon, USA, August 1 – August 5, 2010.


2018 ◽  
Vol 1 (2) ◽  
pp. 115-123 ◽  
Author(s):  
Zhongdu He ◽  
Zongwei Xu ◽  
Mathias Rommel ◽  
Boteng Yao ◽  
Tao Liu ◽  
...  

In order to investigate the damage in single-crystal 6H-silicon carbide (SiC) in dependence on ion implantation dose, ion implantation experiments were performed using the focused ion beam technique. Raman spectroscopy and electron backscatter diffraction were used to characterize the 6H-SiC sample before and after ion implantation. Monte Carlo simulations were applied to verify the characterization results. Surface morphology of the implantation area was characterized by the scanning electron microscope (SEM) and atomic force microscope (AFM). The ‘swelling effect’ induced by the low-dose ion implantation of 1014−1015 ions cm−2 was investigated by AFM. The typical Raman bands of single-crystal 6H-SiC were analysed before and after implantation. The study revealed that the thickness of the amorphous damage layer was increased and then became saturated with increasing ion implantation dose. The critical dose threshold (2.81 × 1014−3.26 × 1014 ions cm−2) and saturated dose threshold (˜5.31 × 1016 ions cm−2) for amorphization were determined. Damage formation mechanisms were discussed, and a schematic model was proposed to explain the damage formation.


2006 ◽  
Vol 983 ◽  
Author(s):  
Kim M. Archuleta ◽  
David P. Adams ◽  
Michael J. Vasile ◽  
Julia E. Fulghum

AbstractMedium energy (30 keV) focused gallium ion beam exposure of silicon results in a compressive in-plane stress with a magnitude as large as 0.4 GPa. Experiments involve uniform irradiation of thin polysilicon microcantilevers (200 micron length) over a range of dose from 1 x 1016 to 2 x 1018 ions/cm2. The radii of curvature of microcantilevers are measured using white light interferometry before and after each exposure. The residual stress is determined from these radii and other measured properties using Stoney's equation. The large residual stress is attributed to ion beam damage, microstructural changes and implantation.


Author(s):  
Steven B. Herschbein ◽  
Kyle M. Winter ◽  
Carmelo F. Scrudato ◽  
Brian L. Yates ◽  
Edward S. Hermann ◽  
...  

Abstract Focused Ion Beam (FIB) chip circuit editing is a well-established highly specialized laboratory technique for making direct changes to the functionality of integrated circuits. A precisely tuned and placed ion beam in conjunction with process gases selectively uncovers internal circuitry, create functional changes in devices or the copper wiring pattern, and reseals the chip surface. When executed within reasonable limits, the revised circuit logic functions essentially the same as if the changes were instead made to the photomasks used to fabricate the chip. The results of the intended revision, however, can be obtained weeks or months earlier than by a full fabrication run. Evaluating proposed changes through FIB modification rather than proceeding immediately to mask changes has become an integral part of the process for bringing advanced designs to market at many companies. The end product of the FIB process is the very essence of handcrafted prototyping. The efficacy of the FIB technique faces new challenges with every generation of fabrication process node advancement. Ever shrinking geometries and new material sets have always been a given as transistor size decreases and overall packing density increases. The biggest fundamental change in recent years was the introduction of the FinFET as a replacement for the venerable planar transistor. Point to point wiring change methodology has generally followed process scaling, but transistor deletions or modifications with the change to Fins require a somewhat different approach and much more careful control due to the drastic change in height and shape. We also had to take into consideration the importance of the 4th terminal, the body-tie, that is often lost in backside editing. Some designs and FET technology can function acceptably well when individual devices are no longer connected to the bulk substrate or well, while others can suffer from profound shifts in performance. All this presents a challenge given that the primary beam technology improvements of the fully configured chip edit FIB has only evolved incrementally during the same time period. The gallium column system appears to be reaching its maximum potential. Further, as gallium is a p-type metal dopant, there are limitations to its use in close proximity to certain active semiconductor devices. Amorphous material formation and other damage mechanisms that extend beyond what can be seen visually when endpointing must also be taken into account [1]. Device switching performance and even transmission line characteristics of nearby wiring levels can be impacted by material structural changes from implantation cascades. Last year our lab participated in a design validation exercise in which we were asked to modify the drive of a multi-finger FinFET device structure to reduce its switching speed impact on a circuit. The original sized device pulled the next node in the chain too fast, resulting in a timing upset. Deleting whole structures and bridging over/around them is commonly done, but modifications to the physical size of an FET device is a rare request and generally not attempted. It requires a level of precision in beam control and post-edit treatment that can be difficult to execute cleanly. Once again during a complex edit task we considered the use of an alternate ion beam species such as neon, or reducing the beam energy (low kV) on the gallium tool. Unfortunately, we don’t yet have easy access to a versatile viable replacement column technology grafted to a fully configured edit station. And while there should be significantly reduced implant damage and transistor functional change when a gallium column FIB is operated at lower accelerating potential [2], the further loss of visual acuity due to the reduced secondary emission, especially when combined with ultra-low beam currents, made fast and accurate navigation near impossible. We instead chose the somewhat unconventional approach of using an ultra-low voltage electron beam to do much of the navigation and surface marking prior to making the final edits with the gallium ion beam in a dual-beam FIB tool. Once we had resolved how to accurately navigate to the transistors in question and expose half of the structure without disturbing the body-tie, we were able to execute the required cut to trim away 50% of the structure and reduce the effective drive. Several of the FIB modified units functioned per the design parameters of a smaller sized device, giving confidence to proceed with the revised mask set. To our surprise, the gallium beam performed commendably well in this most difficult task. While we still believe that an inert beam of similar characteristics would be preferable, this work indicates that gallium columns are still viable at the 14 nm FinFET node for even the most rigorous of editing requirements. It also showed that careful application of e-beam imaging on the exposed underside of FinFET devices could be performed without degrading or destroying them.


Author(s):  
Waseem Asghar ◽  
Priyanka P. Ramachandran ◽  
Adegbenro Adewumi ◽  
Mohammud R. Noor ◽  
Samir M. Iqbal

Break junctions provide a direct way to interrogate electrical transport properties of molecules, in pursuit of molecular electronics devices. A number of approaches are used for the fabrication of break junctions, including optical/e-beam lithography, electromigration, mechanical control of suspended conductive electrodes/strips, and electrochemical deposition of conductive material and nanowires. All approaches either require serial and slow e-beam writing of nanoscale gaps or suffer from low-yield of nanogap electrode devices. Here, we report the use of focused ion beam (FIB) to “scratch” and remove a thin layer of gold from 3 μm wide lines. The scratch results in thinning of the metal line and subsequent current-driven electromigration results into nanogaps at precise locations with high yield of devices. Combining FIB scratching with electromigration provides an elegant approach of creating nanoscale break junctions at an exact location and with a very narrow distribution of the nanogap sizes. Current-voltage measurements are done using a probe station before and after FIB scratch, and after the breaks were formed. Most of the gaps fall within 200–300 nm range and show negligible conductivity. The approach provides a novel, rapid, and high-throughput manufacturing approach of break junction fabrication that can be used for molecular sensing.


1996 ◽  
Vol 439 ◽  
Author(s):  
Miyoko Tanaka ◽  
Kazuo Furuya ◽  
Tetsuya Saito

AbstractFocused ion beam (FIB) irradiation of a thin Ni2Si layer deposited on a Si substrate was carried out and studied using an in-situ transmission electron microscope (in-situ TEM). Square areas on sides of 4 by 4 and 9 by 9 μm were patterned at room temperature with a 25keV Ga+-FIB attached to the TEM. The structural changes of the films indicate a uniform milling; sputtering of the Ni2Si layer and the damage introducing to the Si substrate. Annealing at 673 K results in the change of the Ni2Si layer into an epitaxial NiSi2 layer outside the FIB irradiated area, but several precipitates appear around the treated area. Precipitates was analyzed by energy dispersive X-ray spectroscopy (EDS). Larger amount of Ni than the surrounding matrix was found in precipitates. Selected area diffraction (SAD) patterns of the precipitates and the corresponding dark field images imply the formation of a Ni rich silicide. The relation between the FIB tail and the precipitation is indicated.


2004 ◽  
Vol 818 ◽  
Author(s):  
Tie Liu ◽  
Yihong Wu

AbstractNi nanowires were fabricated by electrochemical deposition in the pores of alumina filtration membranes, with the diameter around 200nm. To study the magnetic and electrical properties of Ni nanowires, individual nanowire was selected and connected with metal electrodes. Single and multiple constrictions were formed on the nanowires by focused ion beam (FIB). The wires were further thinned using oxygen plasma oxidation. Magnetoresistance curves were studied and compared before and after FIB trimming and oxidization.


2011 ◽  
Vol 83 ◽  
pp. 185-190 ◽  
Author(s):  
Qing Hua Wang ◽  
Hui Min Xie ◽  
Zhen Xing Hu ◽  
Jing Zhang ◽  
Jun Sun ◽  
...  

The thermo-creep deformation of interconnects related to the residual stress, directly affects their performance and lifetime. In this paper, we proposed an optical method to measure the residual thermo-creep deformation of copper interconnects. This method takes advantages of grating fabrication and the phase-shifting scanning electron microscope (SEM) moiré method. The residual thermo-creep deformation can be acquired through deformation transformation. A one-way grating with frequency of 5000 lines/mm is fabricated on the surface of the copper line in a focused ion-beam (FIB) system. The principal direction of the grating is along the axis of the copper line. The sample is heated in a high temperature furnace under 90 °C for 70 min. The SEM moiré patterns before and after heating are recorded by a field emission SEM in low vacuum. Through the random phase-shifting algorithm, the residual thermo-creep deformation of the copper interconnect line is found to be 500 με. The cause of the tensile strain is analyzed. This work offers an effective technique for measuring the creep deformation of the film lines.


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