Micron-Nano Pore Structures and Microscopic Pore Distribution of Oil Shale in the Shahejie Formation of the Dongying Depression, Bohai Bay Basin, Using the Argon-Scanning Electron Microscope Method

2021 ◽  
Vol 21 (1) ◽  
pp. 750-764
Author(s):  
Wei Wu ◽  
Guangxu Wang ◽  
Gaofeng Liu ◽  
Xinjun Dong ◽  
Jing Yu ◽  
...  

To investigate the pore structure of shale oil reservoirs, seven organic-rich shales from the Shahejie Formation in the Dongying Depression were studied by rock pyrolysis analysis, X-ray diffraction analysis and scanning electron microscopy with argon ion beam polishing. The proportions of the different types of pores at different scales, the statistical relationships between the mineral contents and pore development, and the development of pores in the mineral laminae combination were discussed. The results demonstrated that the nanometer to micron pore structures were divided into intraparticle pores, interparticle pores, intercrystalline pores, organic pores, microfissures and diagenetic contraction fractures. Interparticle pores and intraparticle pores are both essential components of the sample pores. The original residual pores are mainly small pores and mesopores, while the secondary dissolution pores are primarily mesopores and macropores. For different pore sizes, there are small surface pore contributions of diagenetic contraction fractures, microfissures, intercrystalline pores, and organic pores. The carbonate minerals content controls the oil storage capacity of shale by dominating the development of the various pore types, while the clay mineral bands content can affect the permeability of shale by influencing the development of large-scale microfissures. In the laminae development sample, surface pore development is closely related to the sedimentary mineral microcircle, which consists of a falling semicycle and a rising semicircle. The total surface porosity, including microfissures, diagenetic contraction fractures, interparticle pores and intraparticle pores, mainly developed at the intersection of the rising semicircle and the falling semicircle, and this development corresponds to the highest level of a cycle. In summary, interparticle pores and intraparticle pores are the main components of pores developed in low thermal maturity shale and shale laminae where their heterogeneity is influenced by mineral composition and laminae microcircles.

Author(s):  
M. Spector ◽  
A. C. Brown

Ion beam etching and freeze fracture techniques were utilized in conjunction with scanning electron microscopy to study the ultrastructure of normal and diseased human hair. Topographical differences in the cuticular scale of normal and diseased hair were demonstrated in previous scanning electron microscope studies. In the present study, ion beam etching and freeze fracture techniques were utilized to reveal subsurface ultrastructural features of the cuticle and cortex.Samples of normal and diseased hair including monilethrix, pili torti, pili annulati, and hidrotic ectodermal dysplasia were cut from areas near the base of the hair. In preparation for ion beam etching, untreated hairs were mounted on conducting tape on a conducting silicon substrate. The hairs were ion beam etched by an 18 ky argon ion beam (5μA ion current) from an ETEC ion beam etching device. The ion beam was oriented perpendicular to the substrate. The specimen remained stationary in the beam for exposures of 6 to 8 minutes.


Author(s):  
E. Hendarto ◽  
S.L. Toh ◽  
J. Sudijono ◽  
P.K. Tan ◽  
H. Tan ◽  
...  

Abstract The scanning electron microscope (SEM) based nanoprobing technique has established itself as an indispensable failure analysis (FA) technique as technology nodes continue to shrink according to Moore's Law. Although it has its share of disadvantages, SEM-based nanoprobing is often preferred because of its advantages over other FA techniques such as focused ion beam in fault isolation. This paper presents the effectiveness of the nanoprobing technique in isolating nanoscale defects in three different cases in sub-100 nm devices: soft-fail defect caused by asymmetrical nickel silicide (NiSi) formation, hard-fail defect caused by abnormal NiSi formation leading to contact-poly short, and isolation of resistive contact in a large electrical test structure. Results suggest that the SEM based nanoprobing technique is particularly useful in identifying causes of soft-fails and plays a very important role in investigating the cause of hard-fails and improving device yield.


Author(s):  
H. J. Bender ◽  
R. A. Donaton

Abstract The characteristics of an organic low-k dielectric during investigation by focused ion beam (FIB) are discussed for the different FIB application modes: cross-section imaging, specimen preparation for transmission electron microscopy, and via milling for device modification. It is shown that the material is more stable under the ion beam than under the electron beam in the scanning electron microscope (SEM) or in the transmission electron microscope (TEM). The milling of the material by H2O vapor assistance is strongly enhanced. Also by applying XeF2 etching an enhanced milling rate can be obtained so that both the polymer layer and the intermediate oxides can be etched in a single step.


Author(s):  
Becky Holdford

Abstract On mechanically polished cross-sections, getting a surface adequate for high-resolution imaging is sometimes beyond the analyst’s ability, due to material smearing, chipping, polishing media chemical attack, etc.. A method has been developed to enable the focused ion beam (FIB) to re-face the section block and achieve a surface that can be imaged at high resolution in the scanning electron microscope (SEM).


Author(s):  
Julien Goxe ◽  
Béatrice Vanhuffel ◽  
Marie Castignolles ◽  
Thomas Zirilli

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.


Author(s):  
Thomas M. Moore

Abstract The availability of the focused ion beam (FIB) microscope with its excellent imaging resolution, depth of focus and ion milling capability has made it an appealing platform for materials characterization at the sub-micron, or "nano" level. This article focuses on nanomechanical characterization in the FIB, which is an extension of the FIB capabilities into the realm of nano-technology. It presents examples that demonstrate the power and flexibility of nanomechanical testing in the FIB or scanning electron microscope with a probe shaft that includes a built-in strain gauge. Loads that range from grams to micrograms are achievable. Calibration is limited only by the availability of calibrated load cells in the smallest load ranges. Deflections in the range of a few nanometers range can be accurately applied. Simultaneous electrical, mechanical, and visual data can be combined to provide a revealing study of physical behavior of complex and dynamic nanostructures.


Biology ◽  
2021 ◽  
Vol 10 (1) ◽  
pp. 51
Author(s):  
Michela Relucenti ◽  
Giuseppe Familiari ◽  
Orlando Donfrancesco ◽  
Maurizio Taurino ◽  
Xiaobo Li ◽  
...  

Several imaging methodologies have been used in biofilm studies, contributing to deepening the knowledge on their structure. This review illustrates the most widely used microscopy techniques in biofilm investigations, focusing on traditional and innovative scanning electron microscopy techniques such as scanning electron microscopy (SEM), variable pressure SEM (VP-SEM), environmental SEM (ESEM), and the more recent ambiental SEM (ASEM), ending with the cutting edge Cryo-SEM and focused ion beam SEM (FIB SEM), highlighting the pros and cons of several methods with particular emphasis on conventional SEM and VP-SEM. As each technique has its own advantages and disadvantages, the choice of the most appropriate method must be done carefully, based on the specific aim of the study. The evaluation of the drug effects on biofilm requires imaging methods that show the most detailed ultrastructural features of the biofilm. In this kind of research, the use of scanning electron microscopy with customized protocols such as osmium tetroxide (OsO4), ruthenium red (RR), tannic acid (TA) staining, and ionic liquid (IL) treatment is unrivalled for its image quality, magnification, resolution, minimal sample loss, and actual sample structure preservation. The combined use of innovative SEM protocols and 3-D image analysis software will allow for quantitative data from SEM images to be extracted; in this way, data from images of samples that have undergone different antibiofilm treatments can be compared.


2014 ◽  
Vol 1065-1069 ◽  
pp. 3291-3294
Author(s):  
Xin Wei Zhao ◽  
Hui Zhi Hao

Halimeda is an important reef-building green alga. Scanning electron microscopy (SEM) and energy spectrum tests on green and white Halimeda collected from Shidao Island in the Xisha Islands show that carbonate is predominantly deposited in the cortexes and medullas, especially in the aragonite raphides of them, as the case of calcium carbonate. These modern carbonate sediments are then compared with their ancient counterparts that are collected from Xichen-1 well in the Yongle Atoll, where a large number of Halimeda segments have been recognized in about 100-m-long late Miocene-middle Miocene whole-coring succession. In addition, there are developed great numbers of algal-frame holes, including secondary dissolved pores and intercrystalline pores in the medullas and in aragonites between cysts, which have formed particular network systems and pore throats.


Energies ◽  
2021 ◽  
Vol 14 (11) ◽  
pp. 3053
Author(s):  
Ming Cheng ◽  
Yuhong Lei ◽  
Xiaorong Luo ◽  
Likuan Zhang ◽  
Xiangzeng Wang ◽  
...  

Organic-rich lacustrine shales in the Upper Triassic Yanchang Formation with thermal maturity mainly in the oil window are the main shale oil and shale gas system in the lacustrine strata of the Ordos Basin, China. Pore systems are important for the storage and transfer of shale oil and gas. The main objectives of this study are to identify the pore types and pore structures and investigate the controlling factors for pore types, pore structures, and total porosities of the lacustrine Yanchang Shale. In this study, organic-rich mudstones, mudstones with siltstone interlayers, siltstone, and sandstones were selected from 15 wells in the southern Ordos Basin. X-ray diffraction, pyrolysis, scanning electron microscopy (SEM), low-pressure nitrogen adsorption analysis, and helium porosimetry were conducted to investigate the mineral compositions, pore types, pore structures, porosities, and controlling factors. Siltstone and sandstone interlayers heterogeneously developed in the Yanchang Shale. The petrology, mineral composition, geochemistry, pore type, pore structure, and porosity of siltstone interlayers are different from those of mudstones. The siltstone and sandstone interlayers usually have more quartz and feldspars, greater detrital grain sizes, and relatively better grain sorting but are lower in clay minerals, total organic carbon (TOC), amount of free liquid hydrocarbons values (S1), and total residual hydrocarbons values (S2), compared to mudstones. Interparticle (interP), intraparticle (intraP) pores, and organic pores (OPs) were developed in both siltstones and mudstones. OPs were observed in samples with lower thermal maturity (e.g., 0.5–0.85%). The inorganic pore size is greater than that of OPs. Additionally, the inorganic pore diameters in siltstone interlayers are also greater than those in mudstones. Organic-rich mudstones generally have higher pore volumes (PVs) of pores with sizes less than 10 nm, pore volumes of pores with sizes between 10 and 50 nm (PV, 10–50 nm), and specific surface area (SSA), but they have lower PVs of pores with sizes greater than 50 nm, total PV, and porosity when compared to siltstone and sandstone interlayers. The dominant pore type in mudstones is OPs and TOC (first order), sources and OM types (second order), and thermal maturity (third order), while the abundances of rigid grains with greater sizes and grain sorting are the main controlling factors of pore structures, SSA and PV. Both inorganic pores and organic pores are abundant in the siltstone interlayers. The pore size distribution (PSD), PV, and porosity of siltstone interlayers are related to the abundance of rigid grains (first order), grain sorting (second order), grain size (third order), and carbonate cement content. The total PV and porosity of Yanchang Shale reservoirs may have increased with the increased abundance of siltstone and sandstone interlayers.


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