Strong cube-textured titanium nitride conductive films directly on flexible metal substrate
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Materials Science↗
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Tribology of Pore-Textured Hard Surfaces under Physiological Conditions: Effects of Texture Scales
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37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Texturizing Wind Turbine Towers to Reduce Bat Mortality
There is still a great need for the development of mitigation strategies that are economically viable and can be used alone or in combination with other options (e.g., operational minimization, acoustic deterrents) to ensure that bat fatalities are effectively reduced at wind facilities across the U.S. Our goal was to develop a wind turbine tower coating that 1) bats show little or no interest in approaching, 2) can be applied to currently deployed wind turbine towers and to towers as they are constructed, 3) is economically feasible to produce and apply, and 4) ultimately contributes to a reduction in bat mortality at utility-scale wind facilities. Wind turbine tower monopoles are large, smooth surfaces and numerous studies have reported bats making close investigative approaches at turbine tower surfaces that are suggestive of drinking and foraging behavior. We therefore hypothesized that such activity could be contributing to bat-wind turbine fatalities by increasing the amount of time that bats spend in or around the rotor-swept zone. We further hypothesized that a texturizing the tower might minimized bat activity at the towers and therefore reduce fatality risk. To explore this, we designed a series of experiments to characterize how bats interact with smooth and texture-treated surfaces in a controlled environment. We conducted 64 behavioral trials in a flight facility from 10 June to 25 September 2015 and an additional 76 behavioral trials from 9 June to 30 August 2016. The first set of trials showed that while bats did make contact with smooth surfaces, they did not make contact with textured surfaces. We ascertained that bat activity occurred at 0 to 1 m distances from surfaces, suggesting that the bats (used in this study) may need to be this close to a surface to accurately discern its texture. From the results were developed a texture coating. For the second set of trials, we tested the texture coating. Bats showed a >40% reduction in activity within 1 m of the textured surfaces in comparison to the smooth surfaces. Following these controlled experiments, we conducted field tests at Wolf Ridge Wind, LLC. We applied the texture coating to the midsection of turbine monopoles. The texture coating was manually applied to 2 turbine towers, although we noted during the application there was variation in texture coating between turbines. We considered that this variation could potentially impact bat behavior. We then conducted bat activity surveys at both texture-treated towers and 2 nearby control towers, over 55 nights from 24 June to 22 September, 2017. All species of bats known to be present at the site were detected in the acoustic recordings at these turbine towers. We found no significant differences in overall numbers of bats observed and levels of acoustic activity at the smooth and texture-treated towers. When we analyzed the experimental pairs separately, however, we found that a greater proportion of the close range bat activity within Pair 1 occurred at the texture-treated tower and that much of this activity could be attributed to foraging behavior. In contrast at turbine Pair 2, we observed no difference in the proportion of close range bat activity between the smooth and texture-treated tower, with no clear differences in behavior at the two tower types. When we examined acoustic bat activity at the tower pairs separately, we found species-specific differences in activity that differed between the smooth and texture-treated towers within the pairs. For example, hoary bat acoustic activity was significantly higher at the texture-treated tower in Pair 1, but significantly lower at the texture-treated tower in Pair 2. Given the observational nature of the field test, our limited sample size (2 turbine pairs), variation in the texture-coating between the 2 turbine pairs, and different patterns of bat activity observed at the 2 turbine pairs, inferences from this one field test are limited at best. In conclusion, the results from the flight facility experiments were promising (i.e., we observed a significant decrease in bat activity at smooth compared to texture-treated surfaces); however, due to coating installation and application challenges prior to our field test, we were unable to collect sufficient information to understand how these coatings affect bat activity at operational wind turbine towers. Although the results from the field test are inconclusive, the lessons learned will be informative for future research into turbine surface materials that can modify the surface of the turbine tower and therefore alter how bats perceive wind towers. Thus, the outcomes of this research project may have a significant impact on wind energy operators, wind developers, and OEMs by contributing to future impact mitigation strategies. In future research we will test new ideas to improve the development, application, and evaluation of this mitigation technique.
17 WIND ENERGY↗
Microstructure, texture and mechanical properties of AA 1060 aluminum alloy processed by cryogenic accumulative roll bonding
Highlights: • The Al sheets were accumulative roll bonded to five cycles at cryogenic temperature. • The microstructure, texture and mechanical properties of ARB sheets were investigated. • The texture evolution at surface layer was quantified by mathematical formulae. • The strength of the β fiber at center layer was affected by the initial texture and the strain. - Abstract: AA 1060 aluminum alloy sheet was processed to five accumulative roll bonding (ARB) cycles at cryogenic temperature. The microstructure, texture and mechanical properties of the ARB processed sheets were investigated. The results show that the surface layer of the ARB processed sheets exhibits a significant r-cube shear texture. Initial cube orientation at the surface layer was gradually rotated to the r-cube orientation during the ARB process, leading to the increase in the strength of the r-cube shear texture with ARB cycles. The texture evolution at the surface layer was quantified in terms of a simple relation between the texture volume fractions and accumulated true strain. The strength of the β fiber rolling texture and the distribution of orientation intensities along the β fiber at the center layer were strongly affected by the initial texture. As the ARB cycles increased, the initial texture was changed from the cube texture to the r-cube texture, leading to a continuous increase in the strength of the β fiber rolling texture dominated by the C orientation. The yield and ultimate tensile strength of the ARB processed sheets increased markedly after the first ARB cycle and then increased slowly with increasing ARB cycles, while the elongation decreased accordingly.
36 MATERIALS SCIENCE↗
Development of microstructure and texture during single and multiple pass friction stir processing of a strain hardenable aluminium alloy
Highlights: • Development of microstructure and texture during single and multiple pass FSP of a strain hardenable aluminium alloy • Strain induced boundary migration (SIBM) is the dominant nucleation mechanism for recrystallization • Weak crystallographic texture development influenced by SIBM with the relative dominance of shear texture components • Stable microstructure and texture development after multiple pass FSP • FSP is a promising method for the secondary processing of strain hardenable aluminium alloys - Abstract: In the present study, microstructure and texture development during single and multiple pass friction stir processing (FSP) of a strain hardenable wrought AlMg alloy (AA5086) was investigated. Subtle differences were observed while comparing with heat treatable alloys in the nucleation mechanism of the recrystallized microstructure observed in the nugget zone. Strain induced boundary migration was the dominant mechanism of microstructure evolution in the alloy, which influenced the crystallographic texture development by weakening it. Micro-texture measurements reveal variations in the crystallographic texture along the thickness of the sample. Recrystallization texture components were observed in the nugget zone indicative of a pronounced static recrystallization in the alloy as compared to the heat treatable alloys. Bulk texture measurements within the nugget zone of the optimally processed sample reveal a relatively dominant C component of shear texture. Average grain size in the nugget zone remained the same and the bulk crystallographic texture components were retained during multiple-pass FSP. The lower strain energies involved and the enhanced recovery processes due to the high temperature materials processing of the alloy during FSP resulted in a stable microstructure and texture. In summary, FSP could be promoted as a competent and suitable secondary processing technique for the bulk production of ultra-fine-grained materials in strain hardenable aluminium alloys.
36 MATERIALS SCIENCE↗
Global and local texture development during initial plastic deformation of cold-pilgered Zircaloy-4 tubing
In this work we present a thorough characterization of the texture development during the initial step of a cold pilgering process of a Zircaloy-4 TREX tube, on which the axial cross section is reduced by 80% over a 40cm length with an overall Q-ratio of 2.34, followed by a recrystallization thermal treatment. Texture across a tapered specimen representing this working zone was characterized by neutron diffraction and high energy synchrotron x-ray diffraction at 28 positions (4 locations along its length and 7 locations across its thickness with 0.3 mm spatial resolution), and on the deformed end after the thermal treatment. Results show that the starting material (TREX tube) presents a texture gradient through its wall thickness, with the c poles aligned to the hoop direction at the outer surface (with radial and hoop Kearns factors: f R =0.36, f H = 0.50), and gradually rotating around the axial direction to become a quasi-radial orientation (~35 o out of the radial direction) at the inner surface ( f R =0.43, f H =0.35). The overall texture becomes more radial due to the cold pilgering, but the texture gradient remains during the whole deformation process, being always more radial at the inner surface, ( f R =0.53, f H =0.37 at 80%) than at the outer surface ( f R =0.41, f H =0.50at 80%). The most remarkable changes in texture produced by the rolling process is a 30 o rotation of the grains around their c-axis, producing a marked increase of the <11 2 ¯ 0> // axial fiber texture at expenses of the original <10 1 ¯ 0> // axial fiber texture observed in the TREX tube. The observed changes in texture during deformation were correctly explained by visco-plastic self-consistent (VPSC) modelling. This was achieved after the inclusion of the basal <a> slip system, which plays a central role to explain the 30 o rotation around the c-axis during deformation. The texture evolution was correctly described after the inclusion of a drag effect to grain rotation due to the interaction with neighbouring grains. The through thickness texture differences are greatly reduced by the recrystallization thermal treatment, with similar Kearns factors at the inner surface ( f R =0.50, f H =0.28) and the outer surface ( f R =0.48, f H =0.39). The predominance of the <10 1 ¯ 0> // axial fiber texture is recovered after recrystallization.
36 MATERIALS SCIENCE↗
Annealing texture of nanostructured IF steel
In the present work, the evolution of annealing texture in nanostructured interstitial free steel fabricated via accumulative roll bonding (ARB) process was investigated. Textural evolution after post-annealing of ARB-processed samples was evaluated using X-ray diffraction. There were several texture transitions in the γ-fiber and ζ-fiber during ARB and post-annealing treatment. It was found that with increasing the number of ARB cycles, the volume fraction of the low angle grain boundary decreased and the high angle grain boundary fraction increased. Also, the shear texture was dominant after the first cycle, while for other samples, the rolling texture was dominant. The one-cycle sample clearly indicated a weak α-fiber and γ-fiber and a relatively strong ζ-fiber. In addition, during the recrystallization and before the grain growth, the intensity of α-fiber and γ-fiber decreased, the intensity of ζ-fiber increased, and the intensity of (011)〈100〉 orientation in the ε-fiber and η-fiber increased. Moreover, it was concluded that the transition from the rolling texture to the shear one was a sign of occurrence of the recrystallization (before the grain growth). Finally, with increasing the number of ARB cycles, the intensity of rolling and shear textures saturated and a stable texture formed. - Highlights: • There were texture transitions in the γ-fiber and ζ-fiber. • When the number of cycles increased, the low angle grain boundaries decreased. • The shear texture was dominant after the first cycle. • Transition from rolling texture to shear one was a sign of recrystallization. • With increasing the number of ARB cycles, a stable texture formed.
36 MATERIALS SCIENCE↗
Microstructure and texture evolution of deformed Mg-Zn alloy during recrystallization
Highlights: • The texture intensity in the Mg-Zn alloy relied on the microstructure. • Fine DRXed grains showed a fiber texture distributing between <10.0> and <11.0>. • Coarse DRXed grains mainly exhibited <11.0> fiber texture. • The preferred growth of <11.0> oriented grains resulted in texture evolution. - Abstract: The microstructure and texture evolution of Mg-Zn alloy during recrystallization was investigated by EBSD in the present study. Deformed region, fine DRXed region and coarse DRXed region were obtained in Mg-Zn alloy during deformation. It was found that the texture intensity in DRXed region was weaker compared with the deformed region. The second phase at grain boundaries resulted in the formation of fine DRXed grains with weaker texture compared with the coarse DRXed region. Additionally, a remarkable grain-size driven textural transition from <10.0>–<11.0> texture to <11.0> texture were detected with the growth of DRXed grains. The recrystallized grains with small grain size showed a fiber texture distributing homogeneously between <10.0> and <11.0>, while <11.0> fiber texture was predominant for the large recrystallized grains. It is suggested that <11.0> oriented grains grew faster than other oriented grains, which was ascribed to larger misorientation between <11.0> oriented grains and their neighboring grains.
36 MATERIALS SCIENCE↗
Cold rolling texture evolution of TiB2 particle reinforced Al-based composites by Neutron Diffraction and EBSD analysis
Highlights: • Texture development of in-situ TiB{sub 2} particle reinforced Al matrix composites after cold rolling were characterized. • The sum of rolling texture volume fractions has been significantly reduced by the weak texture in particle deformation zone. • Recrystallization nuclei with the Cube and Rotated-Cube orientations were observed in the particle deformation zones. • Small TiB{sub 2} particles within Al grains kept the parallel relationship with surrounding matrix during the deformation. - Abstract: Texture development of particle-reinforced metal matrix materials (P-MMCs) has not been understood well, especially the effects of second-phase particles during the deformation. In this work, we have investigated the texture evolution of TiB{sub 2}/Al composites during cold rolling by Neutron Diffraction and EBSD analysis. Two forms of TiB{sub 2} particles influenced the texture evolution in different ways. The particle-clusters aggregated along grain boundaries led to a reduction of texture volume fraction; recrystallization nuclei with weak texture appeared around these particle-clusters. Small non-shearable TiB{sub 2} particles dispersed inside Al matrix contributed to strong Copper texture component at high strains; the individual particles rotated together with Al matrix during the deformation. These revealed effects of particles on the texture development in TiB{sub 2}/Al composites provide a reference for the texture control of P-MMCs.
36 MATERIALS SCIENCE↗
SU-E-J-262: Variability in Texture Analysis of Gynecological Tumors in the Context of An 18F-FDG PET Adaptive Protocol
Purpose: This study examines the effect on texture analysis due to variable reconstruction of PET images in the context of an adaptive FDG PET protocol for node positive gynecologic cancer patients. By measuring variability in texture features from baseline and intra-treatment PET-CT, we can isolate unreliable texture features due to large variation. Methods: A subset of seven patients with node positive gynecological cancers visible on PET was selected for this study. Prescribed dose varied between 45–50.4Gy, with a 55–70Gy boost to the PET positive nodes. A baseline and intratreatment (between 30–36Gy) PET-CT were obtained on a Siemens Biograph mCT. Each clinical PET image set was reconstructed 6 times using a TrueX+TOF algorithm with varying iterations and Gaussian filter. Baseline and intra-treatment primary GTVs were segmented using PET Edge (MIM Software Inc., Cleveland, OH), a semi-automatic gradient-based algorithm, on the clinical PET and transferred to the other reconstructed sets. Using an in-house MATLAB program, four 3D texture matrices describing relationships between voxel intensities in the GTV were generated: co-occurrence, run length, size zone, and neighborhood difference. From these, 39 textural features characterizing texture were calculated in addition to SUV histogram features. The percent variability among parameters was first calculated. Each reconstructed texture feature from baseline and intra-treatment per patient was normalized to the clinical baseline scan and compared using the Wilcoxon signed-rank test in order to isolate variations due to reconstruction parameters. Results: For the baseline scans, 13 texture features showed a mean range greater than 10%. For the intra scans, 28 texture features showed a mean range greater than 10%. Comparing baseline to intra scans, 25 texture features showed p <0.05. Conclusion: Variability due to different reconstruction parameters increased with treatment, however, the majority of texture features showed significant changes during treatment independent of reconstruction effects.
60 APPLIED LIFE SCIENCES↗
Influence of strain on the formation of cold-rolling and grain growth textures of an equiatomic HfZrTiTaNb refractory high entropy alloy
Highlights: • Effect of strain on Texture formation is reported in HfZrTiTaNb for the first time. • Cold-rolled microstructure shows high density of deformation heterogeneities. • Weak texture compared to other BCC phases in HEAs • Imposed strain does not affect texture significantly unlike other BCC materials. - Abstract: The effect of cold-rolling strain on the evolution of deformation and grain growth textures in an equiatomic HfZrTiTaNb refractory high entropy alloy (RHEA) was investigated. For this purpose, the development of microstructure and texture was compared in 50% and 90% cold-rolled materials. The development of deformation microstructure was accompanied by the formation of extensive deformation heterogeneities. The 90% cold-rolled material showed ultrafine lamellar regions as well as regions severely fragmented by the fine scale deformation heterogeneities. The 50% cold-rolled material showed dominant ND-fiber (ND//), while the 90% cold-rolled material showed presence of both RD (RD//) and ND-fiber components. Profuse deformation heterogeneities presumably weakened the deformation texture considerably. The annealing texture of the 50% and 90% cold-rolled material showed stronger {111} component. Comparison of the annealing texture of the 50% and 90% cold-rolled materials with other BCC HEA phases indicated much weaker texture. The annealing texture of the RHEA was not significantly strengthened by increasing cold-rolling strain, presumably due to the high density of deformation heterogeneities in the cold-rolled microstructure. Thus, deformation heterogeneities significantly influenced the formation of cold-rolling and annealing textures of the equiatomic HfZrTiTaNb RHEA.
36 MATERIALS SCIENCE↗
TU-AB-BRA-12: Impact of Image Registration Algorithms On the Prediction of Pathological Response with Radiomic Textures
Purpose: Tumor regions-of-interest (ROI) can be propagated from the pre-onto the post-treatment PET/CT images using image registration of their CT counterparts, providing an automatic way to compute texture features on longitudinal scans. This exploratory study assessed the impact of image registration algorithms on textures to predict pathological response. Methods: Forty-six esophageal cancer patients (1 tumor/patient) underwent PET/CT scans before and after chemoradiotherapy. Patients were classified into responders and non-responders after the surgery. Physician-defined tumor ROIs on pre-treatment PET were propagated onto the post-treatment PET using rigid and ten deformable registration algorithms. One co-occurrence, two run-length and size zone matrix textures were computed within all ROIs. The relative difference of each texture at different treatment time-points was used to predict the pathologic responders. Their predictive value was assessed using the area under the receiver-operating-characteristic curve (AUC). Propagated ROIs and texture quantification resulting from different algorithms were compared using overlap volume (OV) and coefficient of variation (CoV), respectively. Results: Tumor volumes were better captured by ROIs propagated by deformable rather than the rigid registration. The OV between rigidly and deformably propagated ROIs were 69%. The deformably propagated ROIs were found to be similar (OV∼80%) except for fast-demons (OV∼60%). Rigidly propagated ROIs with run-length matrix textures failed to significantly differentiate between responders and non-responders (AUC=0.65, p=0.07), while the differentiation was significant with other textures (AUC=0.69–0.72, p<0.03). Among the deformable algorithms, fast-demons was the least predictive (AUC=0.68–0.71, p<0.04). ROIs propagated by all other deformable algorithms with any texture significantly predicted pathologic responders (AUC=0.71–0.78, p<0.01) despite substantial variation in texture quantification (CoV>70%). Conclusion: Propagated ROIs using deformable registration for all textures can lead to accurate prediction of pathologic response, potentially expediting the temporal texture analysis process. However, rigid and fast-demons deformable algorithms are not recommended due to their inferior performance compared to other algorithms. The project was supported in part by a Kaye Scholar Award.
60 APPLIED LIFE SCIENCES↗
WE-FG-206-12: Enhanced Laws Textures: A Potential MRI Surrogate Marker of Hepatic Fibrosis in a Murine Model
Purpose: To compare enhanced Laws texture derived from parametric proton density (PD) maps to other MRI-based surrogate markers (T2, PD, ADC) in assessing degrees of liver fibrosis in a murine model of hepatic fibrosis using 11.7T scanner. Methods: This animal study was IACUC approved. Fourteen mice were divided into control (n=1) and experimental (n=13). The latter were fed a DDC-supplemented diet to induce hepatic fibrosis. Liver specimens were imaged using an 11.7T scanner; the parametric PD, T2, and ADC maps were generated from spin-echo pulsed field gradient and multi-echo spin-echo acquisitions. Enhanced Laws texture analysis was applied to the PD maps: first, hepatic blood vessels and liver margins were segmented/removed using an automated dual-clustering algorithm; secondly, an optimal thresholding algorithm was applied to reduce the partial volume artifact; next, mean and stdev were corrected to minimize grayscale variation across images; finally, Laws texture was extracted. Degrees of fibrosis was assessed by an experienced pathologist and digital image analysis (%Area Fibrosis). Scatterplots comparing enhanced Laws texture, T2, PD, and ADC values to degrees of fibrosis were generated and correlation coefficients were calculated. Unenhanced Laws texture was also compared to assess the effectiveness of the proposed enhancements. Results: Hepatic fibrosis and the enhanced Laws texture were strongly correlated with higher %Area Fibrosis associated with higher Laws texture (r=0.89). Only a moderate correlation was detected between %Area Fibrosis and unenhanced Laws texture (r=0.70). Strong correlation also existed between ADC and %Area Fibrosis (r=0.86). Moderate correlations were seen between %Area Fibrosis and PD (r=0.65) and T2 (r=0.66). Conclusions: Higher degrees of hepatic fibrosis are associated with increased Laws texture. The proposed enhancements improve the accuracy of Laws texture. Enhanced Laws texture features are more accurate than PD and T2 in assessing fibrosis, and can potentially serve as an accurate surrogate marker for hepatic fibrosis.
60 APPLIED LIFE SCIENCES↗
Carbon Dioxide Sealing Capacity: Textural or Compositional Controls? (Final Scientific/Technical Report)
This research project is aiming to assess the carbon dioxide sealing capacity of most common seal-rocks, such as shales and non-fractured limestones, by analyzing the role of textural and compositional parameters of those rocks. We hypothesize that sealing capacity is controlled by textural and/or compositional parameters of caprocks. In this research, we seek to evaluate the importance of textural and compositional parameters affecting the sealing capacity of caprocks. The conceptual framework involves two testable end-member hypotheses concerning the sealing capacity of carbon dioxide reservoir caprocks. Better understanding of the elements controlling sealing quality will advance our knowledge regarding the sealing capacity of shales and carbonates. Due to relatively low permeability, shale and non-fractured carbonate units are considered relatively impermeable formations which can retard reservoir fluid flow by forming high capillary pressure. Similarly, these unites can constitute reliable seals for carbon dioxide capture and sequestration purposes. This project is a part of the comprehensive project with the final aim of studying the caprock sealing properties and the relationship between microscopic and macroscopic characteristics of seal rocks in depleted gas fields of Oklahoma Panhandle. Through this study we examined various seal rock characteristics to infer about their respective effects on sealing capacity in special case of replacing reservoir fluid with super critical carbon dioxide (scCO 2 ). To assess the effect of textural and compositional properties on scCO 2 maximum retention column height we collected 30 representative core samples in caprock formations in three counties (Cimarron, Texas, Beaver) in Oklahoma Panhandle. Core samples were collected from various seal formations (e.g., Cherokee, Keys, Morrowan) at different depths. We studied the compositional and textural properties of the core samples using several techniques. Mercury Injection Porosimetry (MIP), Scanning Electron Microscopy SEM, and Sedigraph measurements are used to assess the pore-throat-size distribution, sorting, texture, and grain size of the samples. Also, displacement pressure at 10% mercury saturation (Pd) and graphically derived threshold pressure (P c ) were determined by MIP technique. SEM images were used for qualitative study of the minerals and pores texture of the core samples. Moreover, EDS (Energy Dispersive X-Ray Spectrometer), BET specific surface area, and Total Organic Carbon (TOC) measurements were performed to study various parameters and their possible effects on sealing capacity of the samples. We found that shales have the relatively higher average sealing threshold pressure (P c ) than carbonate and sandstone samples. Based on these observations, shale formations could be considered as a promising caprock in terms of retarding scCO 2 flow and leakage into above formations. We hypothesized that certain characteristics of shales (e.g., 3 fine pore size, pore size distribution, high specific surface area, and strong physical chemical interaction between wetting phase and mineral surface) make them an efficient caprock for sealing super critical CO 2 . We found that the displacement pressure at 10% mercury saturation could not be the ultimate representative of the sealing capacity of the rock sample. On the other hand, we believe that graphical method, introduced by Cranganu (2004) is a better indicator of the true sealing capacity. Based on statistical analysis of our samples from Oklahoma Panhandle we assessed the effects of each group of properties (textural and compositional) on maximum supercritical CO 2 height that can be hold by the caprock. We conclude that there is a relatively strong positive relationship (+.40 to +.69) between supercritical CO 2 column height based on P c and hard/ soft mineral content index (ratio of minerals with Mohs hardness more than 5 over minerals with Mohs hardness less than 5) in both shales and limestone samples. Average median pore radius and porosity display a strong negative correlation with supercritical CO 2 retention column height. Also, increasing bulk density is positively correlated with the supercritical CO 2 retention column height. One of the most important factors affecting sealing capacity and consequently the height of supercritical CO 2 column is sorting of the pore throats. We observed a strong positive correlation between pore throat sorting and height of CO 2 retention column, especially in shales. This correlation could not be observed in limestone samples. It suggests that the pore throat sorting is more controlling the sealing capacity in shales and shales with well sorted pore throats are the most reliable lithology as seal. We observed that Brunauer–Emmett–Teller (BET) surface area shows a very strong correlation with CO 2 retention column height in limestone samples while BET surface area did not display significant correlation in shales. Pore structure based on SEM micrographs exhibits strong correlation with CO 2 retention column height in limestones. Both intercrystalline and vuggy structures have negative correlations while intergranular texture has positive correlation in limestone with respect to CO 2 retention column height. Textural effects observed on SEM micrographs did not show statistically significant correlation with supercritical CO 2 retention column height in shale samples. Finally, we showed that increasing hard/soft mineral index is strongly correlated with the displacement pressure in limestone samples. Vuggy texture displays a relatively strong and negative correlation with displacement pressure values at 10% mercury saturation in shale samples.
54 ENVIRONMENTAL SCIENCES↗
Improved Oxygen-Beam Texturing of Glucose-Monitoring Optics
An improved method has been devised for using directed, hyperthermal beams of oxygen atoms and ions to impart desired textures to the tips of polymethylmethacrylate [PMMA] optical fibers to be used in monitoring the glucose content of blood. The improved method incorporates, but goes beyond, the method described in Texturing Blood-Glucose- Monitoring Optics Using Oxygen Beams (LEW-17642-1), NASA Tech Briefs, Vol. 29, No. 4 (April 2005), page 11a. The basic principle of operation of such a glucose-monitoring sensor is as follows: The textured surface of the optical fiber is coated with chemicals that interact with glucose in such a manner as to change the reflectance of the surface. Light is sent down the optical fiber and is reflected from, the textured surface. The resulting change in reflectance of the light is measured as an indication of the concentration of glucose. The required texture on the ends of the optical fibers is a landscape of microscopic cones or pillars having high aspect ratios (microscopic structures being taller than they are wide). The average distance between hills must be no more than about 5 mso that blood cells (which are wider) cannot enter the valleys between the hills, where they would interfere with optical sensing of glucose in the blood plasma. On the other hand, the plasma is required to enter the valleys, and high aspect ratio structures are needed to maximize the surface area in contact with the plasma, thereby making it possible to obtain a given level of optical glucose-measurement sensitivity with a relatively small volume of blood. There is an additional requirement that the hills be wide enough that a sufficient amount of light can propagate into them and, after reflection, can propagate out of them. The method described in the cited prior article produces a texture comprising cones and pillars that conform to the average-distance and aspect-ratio requirements. However, a significant fraction of the cones and pillars are so narrow that not enough light can propagate along them. The improved method makes it possible to form wider cones and pillars while still satisfying the average-distance and aspect-ratio requirements. In the improved method, as in the previously reported method, multiple optical fibers are first bundled together for simultaneous texturing of their distal tips. However, prior to texturing by exposure to an oxygen beam, the tips are first coated by vapor deposition of a thin, sparse layer of aluminum: The exposure to the aluminum vapor must be short enough (typically of the order of seconds) so that the aluminum nucleates into islands separated by uncoated areas. The coated tips are textured by exposure to a directed beam of hyperthermal (kinetic energy >1 eV) oxygen atoms and/or ions in a vacuum chamber, as in the previously reported method. The aluminum islands partially shield the underlying PMMA from oxidation and erosion by the beam, so that the cones or pillars remaining after texturing are wider than they would otherwise be. To some extent, the dimensions of the hills and the distances between them can be tailored through choice of the thickness of the aluminum coat and/or the oxygen-beam fluence. The figure illustrates an example of texturing of the tip of a PMMA optical fiber without and with prior aluminum coating.
Banks, Bruce A.↗