Application of Stereological Relations for the Characterization of Porous Materials via Microscopic Image Analysis

2015 ◽  
Vol 647 ◽  
pp. 180-187 ◽  
Author(s):  
Tereza Uhlířová ◽  
Eva Gregorová ◽  
Willi Pabst

In this work we demonstrate the application of stereology-based image analysis for the characterization of highly porous cellular ceramics (alumina foams) prepared by biological foaming with yeast and subsequent drying (80-105 °C) and firing (1570 °C). It is shown that the ceramics prepared usually have total porosities in the range 78-84 % and that the porosities made up by large pores (volume fraction of foam bubbles) are usually in the range 58-75 %. Further it is shown that the mean chord length and the Jeffries size, i.e. pore size measures related to the interface density and the mean curvature integral density, respectively, are relatively close to each other (usually 0.8-1.4 and 0.8-1.2 mm) with a ratio close to unity (0.9-1.3) and that the mean surface-to-surface distance of pores gives a realistic picture of the average pore wall thickness (usually 0.46-0.69 mm). Using a special processing variant (excess ethanol addition) it is possible to obtain microstructures with lower porosity (total porosity 68-70 %, foam bubble volume fractions 50-56 %) and smaller pore size (approx. 0.5 mm). Absolute errors are calculated using normalized deviations corresponding to 95 % reliability in the Student distribution and the standard errors for the quantities in question (both observed and estimated). Relative errors are found to be below 12 % when the number of measurements is of order 400-1000.

2017 ◽  
Vol 54 (3) ◽  
pp. 181-201
Author(s):  
Rebecca Johnson ◽  
Mark Longman ◽  
Brian Ruskin

The Three Forks Formation, which is about 230 ft thick along the southern Nesson Anticline (McKenzie County, ND), has four “benches” with distinct petrographic and petrophysical characteristics that impact reservoir quality. These relatively clean benches are separated by slightly more illitic (higher gamma-ray) intervals that range in thickness from 10 to 20 ft. Here we compare pore sizes observed in scanning electron microscope (SEM) images of the benches to the total porosity calculated from binned precession decay times from a suite of 13 nuclear magnetic resonance (NMR) logs in the study area as well as the logarithmic mean of the relaxation decay time (T2 Log Mean) from these NMR logs. The results show that the NMR log is a valid tool for quantifying pore sizes and pore size distributions in the Three Forks Formation and that the T2 Log Mean can be correlated to a range of pore sizes within each bench of the Three Forks Formation. The first (shallowest) bench of the Three Forks is about 35 ft thick and consists of tan to green silty and shaly laminated dolomite mudstones. It has good reservoir characteristics in part because it was affected by organic acids and received the highest oil charge from the overlying lower Bakken black shale source rocks. The 13 NMR logs from the study area show that it has an average of 7.5% total porosity (compared to 8% measured core porosity), and ranges from 5% to 10%. SEM study shows that both intercrystalline pores and secondary moldic pores formed by selective partial dissolution of some grains are present. The intercrystalline pores are typically triangular and occur between euhedral dolomite rhombs that range in size from 10 to 20 microns. The dolomite crystals have distinct iron-rich (ferroan) rims. Many of the intercrystalline pores are partly filled with fibrous authigenic illite, but overall pore size typically ranges from 1 to 5 microns. As expected, the first bench has the highest oil saturations in the Three Forks Formation, averaging 50% with a range from 30% to 70%. The second bench is also about 35 ft thick and consists of silty and shaly dolomite mudstones and rip-up clast breccias with euhedral dolomite crystals that range in size from 10 to 25 microns. Its color is quite variable, ranging from green to tan to red. The reservoir quality of the second bench data set appears to change based on proximity to the Nesson anticline. In the wells off the southeast flank of the Nesson anticline, the water saturation averages 75%, ranging from 64% to 91%. On the crest of the Nesson anticline, the water saturation averages 55%, ranging from 40% to 70%. NMR porosity is consistent across the entire area of interest - averaging 7.3% and ranging from 5% to 9%. Porosity observed from samples collected on the southeast flank of the Nesson Anticline is mainly as intercrystalline pores that have been extensively filled with chlorite clay platelets. In the water saturated southeastern Nesson Anticline, this bench contains few or no secondary pores and the iron-rich rims on the dolomite crystals are less developed than those in the first bench. The chlorite platelets in the intercrystalline pores reduce average pore size to 500 to 800 nanometers. The third bench is about 55 ft thick and is the most calcareous of the Three Forks benches with 20 to 40% calcite and a proportionate reduction in dolomite content near its top. It is also quite silty and shaly with a distinct reddish color. Its dolomite crystals are 20 to 50 microns in size and partly abraded and dissolved. Ferroan dolomite rims are absent. This interval averages 7.1% porosity and ranges from 5% to 9%, but the pores average just 200 nanometers in size and occur mainly as microinterparticle pores between illite flakes in intracrystalline pores in the dolomite crystals. This interval has little or no oil saturation on the southern Nesson Anticline. Unlike other porosity tools, the NMR tool is a lithology independent measurement. The alignment of hydrogen nuclei to the applied magnetic field and the subsequent return to incoherence are described by two decay time constants, longitudinal relaxation time (T1) and transverse relaxation time (T2). T2 is essentially the rate at which hydrogen nuclei lose alignment to the external magnetic field. The logarithmic mean of T2 (T2 Log Mean) has been correlated to pore-size distribution. In this study, we show that the assumption that T2 Log Mean can be used as a proxy for pore-size distribution changes is valid in the Three Forks Formation. While the NMR total porosity from T2 remains relatively consistent in the three benches of the Three Forks, there are significant changes in the T2 Log Mean from bench to bench. There is a positive correlation between changes in T2 Log Mean and average pore size measured on SEM samples. Study of a “type” well, QEP’s Ernie 7-2-11 BHD (Sec. 11, T149N, R95W, McKenzie County), shows that the 1- to 5-micron pores in the first bench have a T2 Log Mean relaxation time of 10.2 msec, whereas the 500- to 800-nanometer pores in the chlorite-filled intercrystalline pores in the second bench have a T2 Log Mean of 4.96 msec. This compares with a T2 Log Mean of 2.86 msec in 3rd bench where pores average just 200 nanometers in size. These data suggest that the NMR log is a useful tool for quantifying average pore size in the various benches of the Three Forks Formation.


1994 ◽  
Vol 366 ◽  
Author(s):  
Fouad M. Aliev

ABSTRACTWe performed dielectric spectroscopy measurements to study dynamics of collective modes of ferroelectric (FLC) and molecular motion of nematic (NLC) liquid crystals with polar molecules confined in silica macroporous and microporous glasses with average pore sizes of 1000 Å (volume fraction of pores 40%) and 100 Å (27%) respectively. For FLC the Goldstone and the soft modes are found in macropores. The rotational viscosity associated with the soft mode is about 10 times higher in pores than in the bulk. These modes are not detected in micropores although low frequency relaxation is present. The last one probably is not connected with the nature of liquid crystal but is associated with surface polarization effects typical for two component heterogeneous media. The difference between the dynamics of orientational motion of the polar molecules of NLC in confined geometries and in the bulk is qualitatively determined by the total energy Fs of the interaction between molecules and the surface of the pore wall, which is found Fs ≈ 102erg/cm2.


2014 ◽  
Vol 488-489 ◽  
pp. 620-624
Author(s):  
Long Zhou ◽  
Xu Liang Hou ◽  
Zhong Ping Wang

The pore structure of cement-based materials is closely related to the freeze-thaw resistance durability. And this paper focused on nanometer pores to verify the connection of freeze-thaw cycles in the nanometer pores with the structure deterioration and to explore the stress in the pore wall during the freeze-thaw process. And BET method was adopted to analyze the pore structure of the cement and results indicated the changing trends of parameters such as the pore volume, average pore size and surface area of specimens. Moreover, pore size distribution presented prominent fluctuations of pore sizes in the range of 0 ~ 20 nm, while the changes on the scale of 20 ~ 100 nm were limited.


2010 ◽  
Vol 638-642 ◽  
pp. 1995-2000 ◽  
Author(s):  
Reny Angela Renzetti ◽  
M.J.R. Sandim ◽  
Hugo Ricardo Zschommler Sandim ◽  
K.T. Hartwig ◽  
Heide H. Bernardi ◽  
...  

Polycrystalline iron was deformed by eight ECAE passes using the route Bc to a total strain of 9.2. After deformation the material was annealed at temperatures up to 800oC. Scanning electron microscopy (SEM) and high-resolution electron backscatter diffraction (EBSD) were used to characterize both deformed and annealed structures. In the as-deformed state, the mean grain size is 650 nm and the volume fraction of high angle boundaries (VHAB) is 56%. Upon annealing there is a pronounced softening above 300oC. At the beginning of recrystallization, at about 400oC, the VHAB increases to 71%. The results indicate that discontinuous recrystallization is the main softening mechanism in severely deformed iron.


RSC Advances ◽  
2018 ◽  
Vol 8 (59) ◽  
pp. 33927-33938 ◽  
Author(s):  
Heyao Zhang ◽  
Qiantao Lei ◽  
Jinliang Song ◽  
Min Liu ◽  
Can Zhang ◽  
...  

Nanopore pyrolytic graphite coatings (PyC, average pore size ∼64 nm) were prepared on graphite to inhibit liquid fluoride salt and Xe135 penetration.


Cerâmica ◽  
2016 ◽  
Vol 62 (362) ◽  
pp. 186-190 ◽  
Author(s):  
B. Boudaira ◽  
A. Harabi ◽  
F. Bouzerara ◽  
S. Condom ◽  
F. Zenikheri ◽  
...  

Abstract The objective of the present paper was to prepare a ceramic support with membrane. Tubular ceramic supports prepared from kaolin (DD3) and calcium carbonate with 6 and 10 mm inner and outer diameters, respectively, were extruded and sintered at 1200 °C. It has been found that sintered supports had interesting characteristics: average pore size of about 5µm, porosity of about 50%, and monomodal pore size distribution. This support was used to be substrate for a membrane layer of microfiltration. This membrane layer was elaborated from zinc oxide, using slip casting technique. The specimens were subsequently sintered at 1000 °C. The microstructure and porosity as well as the permeability have also been studied. It has been found that the average pore size was about 1.2µm, the layer thickness was ~33µm, and the water permeability measured was about 880 L.h-1.m-2.bar-1.


1997 ◽  
Vol 500 ◽  
Author(s):  
G. P. Sinha ◽  
B. Batalla ◽  
F. M. Aliev

ABSTRACTWe applied ultra broad-band dielectric spectroscopy in the frequency range from 10–3 Hz to 109 Hz to investigate the effect of size, shape and volume fraction of the pores in the porous matrices on the dielectric properties of liquid crystals (LC) dispersed in these matrices. Measurements in such a broad frequency range make it possible to obtain detailed information on the important aspects of the electrical behavior of heterogeneous materials such as: conductivity, surface polarization, and influence of confinement on dynamics of molecular motion of polar molecules forming LC. We investigated alkylcyanobiphenyls in the isotropie, nematic and smectic phases dispersed in porous glasses (average pore sizes - 100 Å and 1000 Å) which have randomly oriented, interconnected pores, and anopore membranes (pore diameters - 200 Å and 2000 Å) with parallel cylindrical pores. Dispersion of LC resulted in qualitative changes of their dielectric properties. Analysis of broad-band dielectric spectra shows that in organic (LC) - inorganic (porous matrix) heterogeneous composites conductivity plays an important role at F <1 Hz. We observe the appearance of new dielectric modes: a very slow process with characteristic frequency ≃ (1 – 10) Hz and a second process in frequency range about (103 - 106) Hz. The slow process arises due to the relaxation of interfacial polarization at pore wall - LC interface. The origin of this could be due to absorption of ions at the interface. Another possibility is the preferential orientation of the permanent dipoles at pore surface. The second new mode is due to the hindered rotation of the molecules near the interface. Additionally we observed two bulk like modes due to the rotation of the molecules around their short and long axii which are modified.


2006 ◽  
Vol 519-521 ◽  
pp. 777-782
Author(s):  
Shigeo Saimoto ◽  
S. Subbaiyan ◽  
C. Gabryel

In dynamic dislocation-defect analysis, the thermodynamic deformation-mode signatures are examined as the ageing proceeds. In this method, the activation volume (ν) and the mean slip distance (λ) is simultaneously determined with the flow stress (τ) such that the inverse workhardening slope (1/θ) can be plotted versus b2λ/ν where b is the Burgers vector. The slope of this almost linear locus is directly proportional to the activation distance (d). Calibration with a model alumina-dispersed high conductivity copper reveals that punched-out loops are produced up to failure and is represented by a linear locus from 0.1 to 11 % strain. Artificial ageing of AA6111 at 180°C follows this pattern but the naturally-aged specimen manifest a distinctly different signature which shows a transition as the GP zone-type precipitates are sheared. Furthermore by selecting a suitable tensile-test temperature below 250K, the particle size and volume fraction can be determined if particle shearing does not take place. The optimum size and volume fraction necessary for sufficient strength and ductility can be assessed using this method.


Author(s):  
Andrew G Plews ◽  
Alan Atkinson ◽  
Scott McGrane

X-ray micro-tomography (XMT) was used to characterise the pore structure of two open-cell biopolymer foams (starch extrudates). A three-dimensional watershed algorithm was applied to XMT images to segment pore structure. Distributions of pore sizes and interconnecting pore aperture sizes were determined and pore geometry was visualised. The technique was used to analyse samples having an inhomogeneous porosity distribution. Results were not sensitive to threshold values set during image analysis. Pore size and pore aperture distributions were extracted. Pore size was based on volume fraction, aperture size was based on area fraction and both on number frequency. Volume fraction of porosity was calculated from image analysis and compared with that deduced from density measurements. The value from image analysis was sensitive to the set threshold contrast. Average cell wall thickness was calculated from two-dimensional image analysis. This shows that XMT, with appropriate data processing, is a powerful method for structural characterisation of starch extrudates.


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