scholarly journals Collection of continuous rotation MicroED Data from Ion Beam Milled Crystals of Any Size

2018 ◽  
Author(s):  
Michael W. Martynowycz ◽  
Wei Zhao ◽  
Johan Hattne ◽  
Grant J. Jensen ◽  
Tamir Gonen
Keyword(s):  
Data Collection ◽  
Sample Preparation ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Air Interface ◽  
Structure Solution ◽  
Continuous Rotation ◽  
Macromolecular Protein ◽  
Subsequent Sample

AbstractMicrocrystal electron diffraction (MicroED) allows for macromolecular structure solution from nanocrystals. To create crystals of suitable size for MicroED data collection, sample preparation typically involves sonication or pipetting a slurry of crystals from a crystallization drop. The resultant crystal fragments are fragile and the quality of the data that can be obtained from them is sensitive to subsequent sample preparation for cryoEM as interactions in the water-air interface can damage crystals during blotting. Here, we demonstrate the use of a focused ion beam to generate lamellae of macromolecular protein crystals for continuous rotation MicroED that are of ideal thickness, easy to locate, and require no blotting optimization. In this manner, crystals of nearly any size may be scooped and milled to ideal dimensions prior to data collection, thus streamlining the methodology for sample preparation for MicroED.

scholarly journals Qualitative analyses of polishing and pre-coating FIB milled crystals for MicroED

2019 ◽  
Author(s):  
Michael W. Martynowycz ◽  
Wei Zhao ◽  
Johan Hattne ◽  
Grant J. Jensen ◽  
Tamir Gonen
Keyword(s):  
Electron Diffraction ◽  
Data Collection ◽  
Sample Preparation ◽  
Strong Interaction ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Protein Structures ◽  
Crystal Surfaces ◽  
Small Crystals ◽  
Qualitative Analyses

SummaryMicrocrystal electron diffraction (MicroED) leverages the strong interaction between matter and electrons to determine protein structures from vanishingly small crystals. This strong interaction limits the thickness of crystals that can be investigated by MicroED, mainly due to absorption. Recent studies have demonstrated that focused ion beam (FIB) can thin even very large crystals into ideal sized lamellae however it is not clear how to best apply FIB-milling for MicroED. Here, The effects of polishing the lamellae, whereby the last few nanometers are milled away using a low-current gallium beam, are explored in both platinum pre-coated and uncoated samples. Our results suggest that pre-coating samples with a thin layer of platinum followed by polishing the crystal surfaces prior to data collection consistently led to superior results as indicated by higher signal/noise ratio, higher resolution and better refinement statistics. This study lays the foundation for routine and reproducible methodology for sample preparation in MicroED.

Nanocomposite Polyurethane Foams Via POSS Blends

2002 ◽  
Vol 733 ◽  
Author(s):  
Brock McCabe ◽  
Steven Nutt ◽  
Brent Viers ◽  
Tim Haddad
Keyword(s):  
High Temperature ◽  
Sample Preparation ◽  
Room Temperature ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Polyurethane Foams ◽  
Development Projects ◽  
Polymer Systems ◽  
Polyurethane Resin ◽  
Military Development

AbstractPolyhedral Oligomeric Silsequioxane molecules have been incorporated into a commercial polyurethane formulation to produce nanocomposite polyurethane foam. This tiny POSS silica molecule has been used successfully to enhance the performance of polymer systems using co-polymerization and blend strategies. In our investigation, we chose a high-temperature MDI Polyurethane resin foam currently used in military development projects. For the nanofiller, or “blend”, Cp7T7(OH)3 POSS was chosen. Structural characterization was accomplished by TEM and SEM to determine POSS dispersion and cell morphology, respectively. Thermal behavior was investigated by TGA. Two methods of TEM sample preparation were employed, Focused Ion Beam and Ultramicrotomy (room temperature).

Optimizing Gas-Assisted FIB Processes: The Importance of Oft-Ignored Secondary Parameters

2004 ◽  
Author(s):  
C. Rue ◽  
S. Herschbein ◽  
C. Scrudato ◽  
L. Fischer ◽  
A. Shore
Keyword(s):  
Focused Ion Beam ◽  
Vacuum Chamber ◽  
Ion Beam ◽  
Memory Capacity ◽  
Metal Films ◽  
Deposited Metal ◽  
Influence Process ◽  
Focused Beams ◽  
Gas Pressures

Abstract The efficiency of Gas-Assisted Etching (GAE) and depositions performed using the Focused Ion Beam (FIB) technique is subject to numerous factors. Besides the wellknown primary parameters recommended by the FIB manufacturer (pixel spacing, dwell time, and gas pressures), certain secondary factors can also have a pronounced effect on the quality of these gas-assisted FIB operations. The position of the gas delivery nozzle during XeF2 mills on silicon is examined and was found to affect both the milling speed and the texture on the floor of the FIB trench. Limitations arising from the memory capacity of the FIB computer can also influence process times and trench quality. Exposing the FIB vacuum chamber to TMCTS during SiO2 depositions is found to temporarily impede the performance of subsequent tungsten depositions, especially following heavy or prolonged TMCTS exposure. A delay period may be required to achieve optimal tungsten depositions following TMCTS use. Finally, the focusing conditions of the ion beam are found to have a significant impact on the resistance of FIB-deposited metal films. This effect is attributed to partial milling of the deposition film due to the intense current density of the collimated ion beam. The resistances of metal depositions performed with intentionally defocused ion beams were found to be lower than those performed with focused beams.

TEM Sample Preparation Tricks for Advanced DRAMs

2015 ◽  
Author(s):  
Ching Shan Sung ◽  
Hsiu Ting Lee ◽  
Jian Shing Luo
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Sample Preparation ◽  
Integrated Circuit ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Tem Analysis ◽  
Cross Sectional ◽  
Transmission Electron ◽  
Characterization Of Materials

Abstract Transmission electron microscopy (TEM) plays an important role in the structural analysis and characterization of materials for process evaluation and failure analysis in the integrated circuit (IC) industry as device shrinkage continues. It is well known that a high quality TEM sample is one of the keys which enables to facilitate successful TEM analysis. This paper demonstrates a few examples to show the tricks on positioning, protection deposition, sample dicing, and focused ion beam milling of the TEM sample preparation for advanced DRAMs. The micro-structures of the devices and samples architectures were observed by using cross sectional transmission electron microscopy, scanning electron microscopy, and optical microscopy. Following these tricks can help readers to prepare TEM samples with higher quality and efficiency.

To Eliminate Curtain Effect of FIB TEM Samples by a Combination of Sample Dicing and Backside Milling

2014 ◽  
Author(s):  
Jian-Shing Luo ◽  
Hsiu Ting Lee
Keyword(s):  
Sample Preparation ◽  
Focused Ion Beam ◽  
Preparation Method ◽  
Low Cost ◽  
Ion Beam ◽  
Sample Preparation Method ◽  
Site Specific ◽  
Dual Beam ◽  
Transmission Electron

Abstract Several methods are used to invert samples 180 deg in a dual beam focused ion beam (FIB) system for backside milling by a specific in-situ lift out system or stages. However, most of those methods occupied too much time on FIB systems or requires a specific in-situ lift out system. This paper provides a novel transmission electron microscopy (TEM) sample preparation method to eliminate the curtain effect completely by a combination of backside milling and sample dicing with low cost and less FIB time. The procedures of the TEM pre-thinned sample preparation method using a combination of sample dicing and backside milling are described step by step. From the analysis results, the method has applied successfully to eliminate the curtain effect of dual beam FIB TEM samples for both random and site specific addresses.

A Methodology to Reduce Ion Beam Induced Damage in TEM Specimens Prepared by FIB

2002 ◽  
Author(s):  
Chin Kai Liu ◽  
Chi Jen. Chen ◽  
Jeh Yan.Chiou ◽  
David Su
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Sample Preparation ◽  
Integrated Circuit ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Specimen Preparation ◽  
Tem Analysis ◽  
Sensitive Issue ◽  
Transmission Electron

Abstract Focused ion beam (FIB) has become a useful tool in the Integrated Circuit (IC) industry, It is playing an important role in Failure Analysis (FA), circuit repair and Transmission Electron Microscopy (TEM) specimen preparation. In particular, preparation of TEM samples using FIB has become popular within the last ten years [1]; the progress in this field is well documented. Given the usefulness of FIB, “Artifact” however is a very sensitive issue in TEM inspections. The ability to identify those artifacts in TEM analysis is an important as to understanding the significance of pictures In this paper, we will describe how to measure the damages introduced by FIB sample preparation and introduce a better way to prevent such kind of artifacts.

Solving the Voltage Contrast on Floating Substrate with Standard FA Toolset

2016 ◽  
Author(s):  
Julien Goxe ◽  
Béatrice Vanhuffel ◽  
Marie Castignolles ◽  
Thomas Zirilli
Keyword(s):  
Electron Microscope ◽  
Scanning Electron Microscope ◽  
Sample Preparation ◽  
Failure Analysis ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Silicon On Insulator ◽  
Mixed Signal ◽  
Voltage Contrast ◽  
Scanning Electron

Abstract Passive Voltage Contrast (PVC) in a Scanning Electron Microscope (SEM) or a Focused Ion Beam (FIB) is a key Failure Analysis (FA) technique to highlight a leaky gate. The introduction of Silicon On Insulator (SOI) substrate in our recent automotive analog mixed-signal technology highlighted a new challenge: the Bottom Oxide (BOX) layer, by isolating the Silicon Active Area from the bulk made PVC technique less effective in finding leaky MOSFET gates. A solution involving sample preparation performed with standard FA toolset is proposed to enhance PVC on SOI substrate.

High-Throughput, Site-Specific Sample Prep of Ultra-Thin TEM Lamella for Process Metrology and Failure Analysis

2012 ◽  
Author(s):  
Roger Alvis ◽  
Jeff Blackwood ◽  
Sang-Hoon Lee ◽  
Matthew Bray
Keyword(s):  
Sample Preparation ◽  
Failure Analysis ◽  
Process Monitoring ◽  
High Throughput ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Memory Devices ◽  
Site Specific ◽  
Critical Dimensions ◽  
Tem Lamella

Abstract Semiconductor devices with critical dimensions less than 20nm are now being manufactured in volume. A challenge facing the failure analysis and process-monitoring community is two-fold. The first challenge of TEM sample prep of such small devices is that the basic need to end-point on a feature-of-interest pushes the imaging limit of the instrument being used to prepare the lamella. The second challenge posed by advanced devices is to prepare an artifact-free lamella from non-planar devices such as finFETs as well as from structures incorporating ‘non-traditional’ materials. These challenges are presently overcome in many advanced logic and memory devices in the focused ion beam-based TEM sample preparation processes by inverting the specimen prior to thinning to electron transparency. This paper reports a highthroughput method for the routine preparation of artifact-free TEM lamella of 20nm thickness, or less.

Metallic Nanoneedles Arrays for TEM Sample Preparation “Lift-Out”

2012 ◽  
Author(s):  
Romaneh Jalilian ◽  
David Mudd ◽  
Neil Torrez ◽  
Jose Rivera ◽  
Mehdi M. Yazdanpanah ◽  
...  
Keyword(s):  
Mechanical Properties ◽  
Electron Microscope ◽  
Sample Preparation ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Beam System ◽  
Transmission Electron ◽  
Nanoneedle Array ◽  
Superior Mechanical Properties ◽  
And Performance

Abstract The sample preparation for transmission electron microscope can be done using a method known as "lift-out". This paper demonstrates a method of using a silver-gallium nanoneedle array for a quicker sharpening process of tungsten probes with better sample viewing, covering the fabrication steps and performance of needle-tipped probes for lift-out process. First, an array of high aspect ratio silver-gallium nanoneedles was fabricated and coated to improve their conductivity and strength. Then, the nanoneedles were welded to a regular tungsten probe in the focused ion beam system at the desired angle, and used as a sharp probe for lift-out. The paper demonstrates the superior mechanical properties of crystalline silver-gallium metallic nanoneedles. Finally, a weldless lift-out process is described whereby a nano-fork gripper was fabricated by attaching two nanoneedles to a tungsten probe.

Carbon Coating for Electron Beam Testing and Focus Ion Beam Reconfiguration

1996 ◽  
Author(s):  
P. Perdu ◽  
G. Perez ◽  
M. Dupire ◽  
B. Benteo
Keyword(s):  
Electron Beam ◽  
Sample Preparation ◽  
Carbon Coating ◽  
Focused Ion Beam ◽  
Sacrificial Layer ◽  
Ion Beam ◽  
Electrical Characterization ◽  
Fault Analysis ◽  
Voltage Contrast ◽  
The Right

Abstract To debug ASIC we likely use accurate tools such as an electron beam tester (Ebeam tester) and a Focused Ion Beam (FIB). Interactions between ions or electrons and the target device build charge up on its upper glassivation layer. This charge up could trigger several problems. With Ebeam testing, it sharply decreases voltage contrast during Image Fault Analysis and hide static voltage contrast. During ASIC reconfiguration with FIB, it could induce damages in the glassivation layer. Sample preparation is getting a key issue and we show how we can deal with it by optimizing carbon coating of the devices. Coating is done by an evaporator. For focused ion beam reconfiguration, we need a very thick coating. Otherwise the coating could be sputtered away due to imaging. This coating is use either to avoid charge-up on glassivated devices or as a sacrificial layer to avoid short circuits on unglassivated devices. For electron beam Testing, we need a very thin coating, we are now using an electrical characterization method with an insitu control system to obtain the right thin thickness. Carbon coating is a very cheap and useful method for sample preparation. It needs to be tuned according to the tool used.

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