Application of High-Contrast µCT and FIB-SEM for the Improvement in the Permeability Prediction of Tight Rock Samples

2021 ◽  
Author(s):  
Alexander Avdonin ◽  
Mohammad Ebadi ◽  
Vladislav Krutko
Keyword(s):  
Focused Ion Beam ◽  
Pore Space ◽  
Ion Beam ◽  
High Contrast ◽  
Rock Samples ◽  
Digital Rock ◽  
Permeability Prediction ◽  
Permeable Rock ◽  
Rock Analysis

Abstract Digital rock analysis has proven to be useful for the prediction of petrophysical properties of conventional reservoirs, where the pore space is captured well by a modern µCT scanner with a resolution of 1-5 µm. Nevertheless, this resolution is not enough to accurately capture the pore space of tight (low-permeable) rock samples. As a result, derived digital rock models do not reflect the real rock topology, and permeability predictions yield unreliable results. Our approach deploys high-contrast µCT scanning technique and Focused Ion Beam milling combined with Scanning Electron Microscopy to improve the quality of digital rock models and, hence, the permeability prediction. This workflow is successfully applied to a low-permeable rock sample of Achimov deposits. The computed permeability compares well to the experimental value.

scholarly journals Rendering Semisynthetic FIB-SEM Images of Rock Samples

2021 ◽  
Author(s):  
Ilia Safonov ◽  
Anton Kornilov ◽  
Iryna Reimers
Keyword(s):  
Focused Ion Beam ◽  
Oil And Gas ◽  
Rock Sample ◽  
Pore Space ◽  
Ion Beam ◽  
Ground Truth ◽  
Fine Tuning ◽  
Back Side ◽  
Sem Images ◽  
Rock Samples

Digital rock analysis is a prospective approach to estimate properties of oil and gas reservoirs. This concept implies constructing a 3D digital twin of a rock sample. Focused Ion Beam - Scanning Electron Microscope (FIB-SEM) allows to obtain a 3D image of a sample at nanoscale. One of the main specific features of FIB-SEM images in case of porous media is pore-back (or shine-through) effect. Since pores are transparent, their back side is visible in the current slice, whereas, in fact, it locates in the following ones. A precise segmentation of pores is a challenging problem. Absence of annotated ground truth complicates fine-tuning the algorithms for processing of FIB-SEM data and prevents successful application of machine- learning-based methods, which require a huge training set. Recently, several synthetic FIB- SEM images based on stochastic structures were created. However, those images strongly differ from images of real samples. We propose fast approaches to render semisynthetic FIB- SEM images, which imply that intensities of voxels of mineral matrix in a milling plane, as well as geometry of pore space, are borrowed from an image of rock sample saturated by epoxy. Intensities of voxels in pores depend on the distance from milling plane to the given voxel along a ray directed at an angle equal to the angle between FIB and SEM columns. The proposed method allows to create very realistic FIB-SEM images of rock samples with precise ground truth. Also, it opens the door for numerical estimation of plenty of algorithms for processing FIB-SEM data.

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.

The Novel Dopant Profile Inspection Methodology by FIB

2010 ◽  
Author(s):  
Po Fu Chou ◽  
Li Ming Lu
Keyword(s):  
High Resolution ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Real Sample ◽  
Physical Analysis ◽  
The Novel ◽  
High Contrast ◽  
Dopant Profile ◽  
P Type

Abstract Dopant profile inspection is one of the focused ion beam (FIB) physical analysis applications. This paper presents a technique for characterizing P-V dopant regions in silicon by using a FIB methodology. This technique builds on published work for backside FIB navigation, in which n-well contrast is observed. The paper demonstrates that the technique can distinguish both n- and p-type dopant regions. The capability for imaging real sample dopant regions on current fabricated devices is also demonstrated. SEM DC and FIB DC are complementary methodologies for the inspection of dopants. The advantage of the SEM DC method is high resolution and the advantage of FIB DC methodology is high contrast, especially evident in a deep N-well region.

A method to improve the quality of 2.5 dimensional micro-and nano-structures produced by focused ion beam machining

Micron ◽  
2017 ◽  
Vol 101 ◽  
pp. 8-15 ◽  
Author(s):  
Daniele De Felicis ◽  
Muhammad Zeeshan Mughal ◽  
Edoardo Bemporad
Keyword(s):  
Focused Ion Beam ◽  
Ion Beam ◽  
Nano Structures

scholarly journals Automated cryo-lamella preparation for high-throughput in-situ structural biology

2019 ◽  
Author(s):  
Genevieve Buckley ◽  
Gediminas Gervinskas ◽  
Cyntia Taveneau ◽  
Hari Venugopal ◽  
James C. Whisstock ◽  
...  
Keyword(s):  
Saccharomyces Cerevisiae ◽  
Structural Biology ◽  
Focused Ion Beam ◽  
Electron Tomography ◽  
Ion Beam ◽  
Automated Method ◽  
Cellular Environment ◽  
Transmission Electron

AbstractCryo-transmission electron tomography (cryo-ET) in association with cryo-focused ion beam (cryo-FIB) milling enables structural biology studies to be performed directly within the cellular environment. Cryo-preserved cells are milled and a lamella with a thickness of 200-300 nm provides an electron transparent window suitable for cryo-ET imaging. Cryo-FIB milling is an effective method, but it is a tedious and time-consuming process, which typically results in ~10 lamellae per day. Here, we introduce an automated method to reproducibly prepare cryo-lamellae on a grid and reduce the amount of human supervision. We tested the routine on cryo-preserved Saccharomyces cerevisiae and demonstrate that this method allows an increased throughput, achieving a rate of 5 lamellae/hour without the need to supervise the FIB milling. We demonstrate that the quality of the lamellae is consistent throughout the preparation and their compatibility with cryo-ET analyses.

scholarly journals Artifacts from manganese reduction in rock samples prepared by focused ion beam (FIB) slicing for X-ray microspectroscopy

2019 ◽  
Vol 8 (1) ◽  
pp. 97-111
Author(s):  
Dorothea S. Macholdt ◽  
Jan-David Förster ◽  
Maren Müller ◽  
Bettina Weber ◽  
Michael Kappl ◽  
...  
Keyword(s):  
Spatial Distribution ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Oxidation States ◽  
X Ray ◽  
Scientific Debate ◽  
Rock Samples ◽  
Valence States ◽  
Scanning Transmission ◽  
Visualization Techniques

Abstract. The spatial distribution of transition metal valence states is of broad interest in the microanalysis of geological and environmental samples. An example is rock varnish, a natural manganese (Mn)-rich rock coating, whose genesis mechanism remains a subject of scientific debate. We conducted scanning transmission X-ray microscopy with near-edge X-ray absorption fine-structure spectroscopy (STXM-NEXAFS) measurements of the abundance and spatial distribution of different Mn oxidation states within the nano- to micrometer thick varnish crusts. Such microanalytical measurements of thin and hard rock crusts require sample preparation with minimal contamination risk. Focused ion beam (FIB) slicing was used to obtain ∼100–1000 nm thin wedge-shaped slices of the samples for STXM, using standard parameters. However, while this preparation is suitable for investigating element distributions and structures in rock samples, we observed artifactual modifications of the Mn oxidation states at the surfaces of the FIB slices. Our results suggest that the preparation causes a reduction of Mn4+ to Mn2+. We draw attention to this issue, since FIB slicing, scanning electron microscopy (SEM) imaging, and other preparation and visualization techniques operating in the kilo-electron-volt range are well-established in geosciences, but researchers are often unaware of the potential for the reduction of Mn and possibly other elements in the samples.

Thermoelectric Transport Properties of Individual Bismuth Nanowires

2001 ◽  
Vol 691 ◽  
Author(s):  
Stephen B. Cronin ◽  
Yu-Ming Lin ◽  
Oded Rabin ◽  
Marcie R. Black ◽  
Gene Dresselhaus ◽  
...  
Keyword(s):  
Temperature Dependence ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Point Contacts ◽  
Large Spread ◽  
Thermoelectric Transport Properties ◽  
Bismuth Nanowires ◽  
Increasing Temperature ◽  
Magneto Resistance

ABSTRACTWe developed a method for making 4-point contacts to Bi nanowires with a thick oxide coat using a combination of lithographic and focused ion beam (FIB) techniques. The resistivity of Bi nanowires with diameters in the range 70-200nm is found to increase with decreasing wire diameter. In contrast to bulk Bi, the temperature dependence of the resistivity is found to decrease monotonically with increasing temperature. The results are explained on the basis of increased scattering in the nanowire and the known temperature dependence of the electronic properties of bulk Bi. A large magneto-resistance was also measured, indicating a high crystalline quality of the nanowires. A large spread in the measured values of the resistivity indicates significant systematic error in the measurement technique. Possible sources for error are discussed.

scholarly journals 50 nm Scale Alignment Method for Hybrid Manufacturing Processes for Full 3D Structuring

2020 ◽  
Vol 21 (12) ◽  
pp. 2407-2417
Author(s):  
Ki-Hwan Jang ◽  
Hae-Sung Yoon ◽  
Hyun-Taek Lee ◽  
Eunseob Kim ◽  
Sung-Hoon Ahn
Keyword(s):  
Focused Ion Beam ◽  
Ion Beam ◽  
Three Dimensional ◽  
Research Area ◽  
Manufacturing Processes ◽  
Alignment Error ◽  
Alignment Method ◽  
Major Research ◽  
Hybrid Processes

AbstractIn micro-/nano-scale, multi-material three-dimensional (3D), structuring has been a major research area for making various applications. To overcome dimensional and material limitations, several hybrid processes have been proposed. The hybrid processes were performed in the same or different numerically controlled stages. If the stages differed, the substrate was moved and locked to the stage before fabrication. During the locking, alignment error occurred. This error became problematic because this significantly compromised the quality of final structures. Here, an alignment method for a hybrid process consisted of a focused ion beam milling, aerodynamically focused nanoparticle printing, and micro-machining was developed. Two sets of collinear marks were placed at the edges of the substrate. Rotational and translational errors were calculated and compensated using the marks. Processes having different scales were bridged through this alignment method. Various materials were utilized, and accuracy was less than 50 nm when the length of the substrate was less than 13 mm. The alignment method was employed to fabricate a V-shaped structure and step-shaped structure using polymer, ceramic, and metal.

scholarly journals Focused Ion Beam Milling of Single-Crystal Sapphire with A-, C-, and M-Orientations

Materials ◽  
2020 ◽  
Vol 13 (12) ◽  
pp. 2871
Author(s):  
Qiuling Wen ◽  
Xinyu Wei ◽  
Feng Jiang ◽  
Jing Lu ◽  
Xipeng Xu
Keyword(s):  
Single Crystal ◽  
Surface Quality ◽  
Material Removal ◽  
Focused Ion Beam ◽  
Removal Rate ◽  
Ion Beam ◽  
Crystal Orientations ◽  
Aluminum Ions ◽  
Single Crystal Sapphire

Sapphire substrates with different crystal orientations are widely used in optoelectronic applications. In this work, focused ion beam (FIB) milling of single-crystal sapphire with A-, C-, and M-orientations was performed. The material removal rate (MRR) and surface roughness (Sa) of sapphire with the three crystal orientations after FIB etching were derived. The experimental results show that: The MRR of A-plane sapphire is slightly higher than that of C-plane and M-plane sapphires; the Sa of A-plane sapphire after FIB treatment is the smallest among the three different crystal orientations. These results imply that A-plane sapphire allows easier material removal during FIB milling compared with C-plane and M-plane sapphires. Moreover, the surface quality of A-plane sapphire after FIB milling is better than that of C-plane and M-plane sapphires. The theoretical calculation results show that the removal energy of aluminum ions and oxygen ions per square nanometer on the outermost surface of A-plane sapphire is the smallest. This also implies that material is more easily removed from the surface of A-plane sapphire than the surface of C-plane and M-plane sapphires by FIB milling. In addition, it is also found that higher MRR leads to lower Sa and better surface quality of sapphire for FIB etching.

High Contrast Imaging of Interphases in Ternary Polymer Blends Using Focused Ion Beam Preparation and Atomic Force Microscopy

2005 ◽  
Vol 38 (6) ◽  
pp. 2368-2375 ◽  
Author(s):  
Nick Virgilio ◽  
Basil D. Favis ◽  
Marie-France Pépin ◽  
Patrick Desjardins ◽  
Gilles L'Espérance
Keyword(s):  
Atomic Force Microscopy ◽  
Polymer Blends ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
High Contrast ◽  
Contrast Imaging ◽  
Force Microscopy ◽  
Atomic Force ◽  
High Contrast Imaging ◽  
Ternary Polymer
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