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A study of like-charged, bimodal colloidal suspensions was conducted in microgravity aboard the International Space Station as part of NASA's Advanced Colloids Experiments-Heated-2 (ACE-H-2) experiments. Samples comprised of silsesquioxane microparticles (600 nm) and zirconia nanoparticles (5–15 nm) in 1.5 pH nitric acid were mixed and allowed to agglomerate over time while being imaged with NASA's Light Microscopy Module (LMM). The samples contained 1% of microparticles with varying concentrations of nanoparticles in 0.1%, 0.055%, and 0.01% by volume. Digital images were captured periodically by the LMM over 12 days. Image analysis, including cluster size and distribution, was performed in Python using the “Colloidspy” package. The study found that cluster size had increased over time in at least seven of nine samples, but two samples exhibited nonlinear growth rates, while others showed very slow growth with cluster sizes two orders of magnitude greater than the free microparticles. We hypothesize that all samples experienced nonlinear growth, but early transient effects after mixing were missed due to timing limitations in image acquisition. Transport limitations of clusters in these systems may have dominated agglomeration behavior in microgravity, despite the samples being thermodynamically unstable, but more study is required.

While similar in nature, the properties of silica and silsesquioxane are very different, but little is known about these differences. In this paper, functionalized silsesquioxane microparticles are synthesized by adapting the modified St\"ober method and post-functionalized with rhodamine-B. The as synthesized silsesquioxane particles are characterized by a variety of physical and chemical methods. The synthesized particles are amorphous and nonporous in nature and are less dense than silica. While silsesquioxane and silica have some similar physical properties from their siloxane core, the organic functional group of silsesquioxane and the one-half oxygen difference in its structure impact many other properties of these particles like their charging behavior in liquids. These differences not only allow for the ease surface modification as compared to that necessary to modify silica, but also the use in a variety of colloidal systems that due to pH or electrolyte concentrations may not be suitable for silica particles. Keywords: silsesquioxane, Stober method, density, morphology, zeta potential

Nanofluids are a class of heat transport fluids created by suspending nano-scaled metallic or nonmetallic particles into a base fluid. Some experimental investigations have revealed that the nanofluids have remarkably higher thermal conductivities than those of conventional pure fluids and are more suited for practical application than the existing techniques of heat transfer enhancement using millimeter and/or micrometer-sized particles in fluids. Use of nanoparticles reduces pressure drop, system wear, and overall mass of the system leading to a reduction in costs over existing enhancement techniques. The focus of this study is to determine the role of nanoparticle motion in the enhancement of the overall heat transfer coefficient of a nanofluid at different nanoparticle loadings. The enhancement of the heat transfer coefficient is determined experimentally by dispersing CuO nanoparticles (40 nm) with different particle loadings (0.25 wt% and 1 wt%) into water and then flowing the resulting nanofluid through a heated copper tube. The experimental results illustrated that numerous factors including Reynolds number and particle concentration are all capable of impacting the enhancement ratio. To further explain the impact of these variables on the hydrodynamic and thermal parameters of a nanofluid, we developed a CFD model using a Eulerian-Lagrangian approach to study the nature of both the laminar and turbulent flow fields of the fluid phase as well as kinematic and dynamic motion of the dispersed nanoparticles. The main goal is to provide additional information about the fluid and particle dynamics to explain the observed behavior in the experimentally observed trends of the heat transfer coefficient enhancement relative to both nanoparticle concentrations and fluid flow behavior. Our results indicate that heat transfer enhancement significantly depends on particle motion within the system and is highly dependent upon the position of nanoparticles relative to the tube wall.

In nanoparticle haloing, charged nanoparticles have been found to enhance the stability of colloidal suspensions by forming a non-adsorbing layer surrounding neutral colloids which induces an electrostatic repulsion between them. However, there has been some debate that nanoparticles may directly deposit onto the colloidal surfaces and that the stabilization mechanism relies on nanoparticle adsorption. In this study, we have found that these two mechanisms control the stability of colloidal suspensions across a continuum over increasing nanoparticle concentrations. AFM force measurements showed that highly charged zirconia nanoparticles built up an electrostatic repulsion between negligibly charged silica surfaces, preventing them from aggregating. The follow-up adsorption measurements and force modeling indicated that minor adsorption of nanoparticles is expected at volume fractions of 10-5 to 10-3, but the amount of nanoparticle adsorption dramatically increases with increasing the nanoparticle volume fraction beyond 10-3. Based on these results, we propose that the fundamental mechanism of nanoparticle-regulated stabilization is nanoparticle haloing at low nanoparticle concentrations which transitions to adsorption at higher concentrations. Accordingly, at a nanoparticle volume fraction of around 10-3 where the transition happens, the stabilization can be influenced by both nanoparticle haloing and adsorption., 21 pages, 7 figures, 5 tables

This work-in-progress research paper explores the differences of engineering identity in second year chemical engineering and industrial engineering students. The study aims to seek similarities and differences in engineering identity after the College of Engineering’s First Year program. The research questions investigated in this paper include: 1) What factors are related to chemical engineering self-identification? and 2) What factors are related to industrial engineering self-identification? To answer these questions, researchers collected data, using a modified version of the SaGE survey. The data was collected within a required sophomore level course for chemical engineers in summer 2017 and a required sophomore level course for industrial engineers in fall 2017. The results showed that there are differences in Industrial and Chemical Engineering students’ identities by the sophomore level. Chemical engineering students seem to have established a chemical engineering identity by the beginning of their sophomore year at the university, whereas Industrial Engineering students are just beginning to form an engineering identity.

The silica sphere-plate interaction forces in zirconia nanoparticle suspensions have been successfully measured to explain how negligibly charged silica microspheres can be stabilized through the addition of highly charged zirconia nanoparticles. However, the influence of nanoparticle volume fraction on the stabilization as well as how various forces (the attractive van der Waals force, repulsive electrostatic force, and depletion force) contribute to the total interaction force still remains unclear. Therefore, an effective zeta potential fitting model is developed to explain the experimental interaction force curves based on a variable effective Debye length and a measured effective zeta potential using a continuum assumption.

Respiratory syncytial virus (RSV) primarily causes bronchiolitis and pneumonia in infants. In spite of intense research, no safe and effective vaccine has been developed yet. For understanding its pathogenesis and development of anti-RSV drugs/therapeutics, it is indispensable to study the RSV-host interaction. Although, there are limited studies using electron microscopy to elucidate the infection process of RSV, to our knowledge, no study has reported the morphological impact of RSV infection using atomic force microscopy. We report the cytoplasmic and nuclear changes in human epidermoid cell line type 2 using atomic force microscopy. Human epidermoid cell line type 2 cells, grown on cover slips, were infected with RSV and fixed after various time periods, processed and observed for morphological changes using atomic force microscopy. RSV infected cells showed loss of membrane integrity, with degeneration in the cellular content and cytoskeleton. Nuclear membrane was disintegrated and nuclear volume was decreased. The chromatin of the RSV infected cells was condensed, progressing towards degeneration via pyknosis and apoptosis. Membrane protrusions of ~150-200 nm diameter were observed on RSV infected cells after 6 h, suggestive of prospective RSV budding sites. To our knowledge, this is the first study of RSV infection process using atomic force microscopy. Such morphological studies could help explore viral infection process aiding the development of anti-RSV therapies.

Gold nanoparticles (GNPs) are widely used in biological and clinical applications due to their favorable chemical and optical properties. GNPs can be used for drug delivery to targeted cells. In addition, GNPs serve as ideal probes for biological and cell imaging applications. Recent studies indicate that the size diversity of GNPs plays an important role in targeting cellular components for biomedical applications. In this study, we conducted a series of studies using different sizes of gold nanoparticles, including 3, 10, 25, and 50 nm, to determine the effect of size variations on their intracellular localizations. Our cytotoxicity studies of GNPs into the HEp-2 cells using MTT assay indicated that 3 nm GNPs possess the highest toxicity. We exposed HEp-2 cells with various sizes of gold nanoparticles for different time intervals (1, 2, 4, 12, and 24 h) followed by imaging using scanning electron microscope (SEM) and atomic force microscope (AFM). Our SEM and AFM results showed that, after 1 hr incubation, 3 and 10 nm gold nanoparticles entered the nucleus, whereas 25 and 50 nm particles accumulated around the nucleus. As the time of exposure increased, GNPs entered the cells and accumulated in the cytosol and nucleus based solely on their sizes.

Enzymatic hydrolysis of cellulose often involves cellulases produced by Trichoderma reesei, of which cellobiohydrolase1 (CBH1) is the most abundant (about 60% of total cellulases) and plays an important role in the hydrolysis of crystalline cellulose. A method for separating sufficient quantities from the bulk cellulase cocktail is highly desirable for many studies, such as those that aim to characterize binding and hydrolysis kinetics of CBH1. In this work, CBH1 was separated from other Spezyme CP cellulases by ion-exchange chromatography using an efficient modification of a smaller scale process. The ion-exchange column was connected to a vacuum manifold system to provide a steady flow through parallel columns and thus achieve scale-up for enzyme separation. With five 5-mL columns running in parallel, about 55 mg of CBH1 was separated from 145 mg of Spezyme CP in a single separation. Step elution was used to replace the continuous gradient used at smaller scale. The purified CBH1 was collected in the fraction eluted with a buffer containing 0.33 M salt and showed comparable purity and activity as the enzyme purified by a fast protein liquid chromatography system. The stability of separated CBH1 was studied for up to 2 days and good thermal stability was observed. Separated CBH1 also showed both high adsorption to bacterial microcrystalline cellulose with ~4 μmol/g maximum adsorption and a K(a) of 5.55 ± 2.34 μM(-1) , and good hydrolytic activity based on atomic force microscopy observations that show a reduction in fiber height.

Respiratory syncytial virus is the leading cause of lower respiratory tract infection in infants and currently lacks an effective vaccine or treatment beyond symptom relief. The atomic force microscope is particularly well suited for imaging biological samples including cells, DNA, viruses and proteins. Analysis of fixed HEP-2 cells with the AFM after infection and incubation with RSV for periods of 0.5–24 h reveals several physical changes within the cells that may lead to a better understanding of the viral effects on living cells. Analysis of force–distance curves reveals changes in the mechanical properties of the cells throughout the infection period as well as changes in the surface chemistry, specifically in the presence of hydrophobic domains, of the cell membrane as shown by variability in the measured adhesion force. Elastic moduli of the fixed cells did not show a statistically significant trend, but hydrophobic molecular expression on the cellular surface decreased with increasing infection pe...

Since 2001, silica microspheres have been reported to be stabilized by highly charged hydrous ZrO(2) nanoparticles which form halos around the microspheres at pH 1.5. However, the exact mechanisms behind this novel stabilization method in terms of the relevant interaction forces remain unclear. In order to gain a greater insight into this mechanism, the interaction between a silica flat and a silica sphere in different ZrO(2) nanoparticle suspensions was investigated by the colloid probe technique. The interaction force between a silica flat and a 600 nm silica sphere was first investigated in a ZrO(2) nanoparticle (D approximately 8 nm) suspension with volume fractions of 10(-3), 10(-4), 10(-5), and 10(-6). When the volume fraction of ZrO(2) is 10(-6), only a purely attractive van der Waals force was observed between the silica surfaces. With an increase in the ZrO(2) nanoparticle volume fraction, a peak was detected on the transition force curve at a ZrO(2) volume fraction of 10(-5) while a purely repulsion force was observed for ZrO(2) volume fractions of 10(-4) and 10(-3). The average distance difference between the peak and the zero distance point on the transition force curve which should define the distance between the halo on the microsphere is approximately 2.3 nm. Additionally, the repulsion increases with the effective zeta potential of the binary composite sphere (BCS, the entity of the silica sphere and the surrounding zirconia particles) on an increase of the nanoparticle volume fraction while the adhesion force decreases, which indicates a denser nanoparticle halo.

In this work, it has been shown that, through a highly controlled process, the chemical etching of the anodic aluminum oxide membrane barrier layer can be performed in such a way as to achieve nanometer-scale control of the pore opening. As the barrier layer is etched away, subtle differences revealed through AFM phase imaging in the alumina composition in the barrier layer give rise to a unique pattern of hexagonal walls surrounding each of the barrier layer domes. These nanostructures observed in both topography and phase images can be understood as differences in the oxalate anion contaminated alumina versus pure alumina. This information bears significant implication for catalysis, template synthesis, and chemical sensing applications. From the pore opening etching studies, the etching rate of the barrier layer (1.3 nm/min) is higher than that of the inner cell wall (0.93 nm/min), both of which are higher than the etching rate of pure alumina layer (0.5-0.17 nm/min). The established etching rates together with the etching temperature allow one to control the pore diameter systematically from 10 to 95 nm.

Organic conductors and superconductors based on charge-transfer salts, such as (BEDT-TTF)2X [BEDT-TTF = bis(ethylenedithio)tetrathiafulvalene or ET], exhibit a wide variety of interesting phenomena that would be useful in numerous sensor and electronic applications. Unfortunately, there has been difficulty in creating thin, patterned films of these materials, which would be required for any potential application. In an effort to resolve this problem, a BEDT-TTF-like compound with a dodecanethiol chain has been synthesized and characterized. The application of this new compound in the templating of ET patterned films through the use of microcontact printing and dip-pen nanolithography is currently under investigation. In addition, an ET salt pattern has also been prepared through the use of a general hydrophilic surface derivatization method. Preliminary results will be discussed with particular attention paid to the success of pattern reproduction and identity of the templated species, as well as how thes...

Porous alumina membranes are commercially available and have been widely used in recent nanoscale research, for example, as templates in nanowire fabrication through electrodeposition. In this report, we present a new use for porous alumina membranes in the fabrication of alumina nanotubes/nanowires desired in electrochemical devices and catalytic applications. A high yield of alumina nanotubes/nanowires is obtained by etching porous alumina membranes in an aqueous sodium hydroxide solution. We studied the effects of etching time and solution concentration and characterized the alumina nanotubes/nanowires using a scanning electron microscope (SEM). A discussion of the possible mechanism for the formation of nanotubes/nanowires is given. Our results also imply that in nanowire fabrication through the template approach where alumina membranes are removed with sodium hydroxide solution to release the nanowires special attention is needed in characterizing the nanowires with the SEM because alumina nanotubes/nanowires can be easily mistaken for electrodeposited nanowires.

A statistical analysis technique, developed by Beebe and co-workers (Han, T.; Williams, J. M.; Beebe, T. P., Jr. Anal. Chim. Acta 1995, 307, 365. Williams, J. M.; Han, T.; Beebe, T. P., Jr. Langmui...

The adhesion of particles to solid surfaces is an important factor in the performance of a number of technologically significant systems. A combination of scanning probe microscopy (SPM) techniques, including adhesion mapping and force integration to equal limits imaging, is used to correlate the adhesion of particles with areas of distinct surface physicochemical properties. The utility of this approach is demonstrated using lactose particles and a gelatin capsule from a pharmaceutical dry powder inhalant drug delivery system. The particle adhesion forces were found to be higher on specific domains of the gelatin capsule identified as extraneous surface contamination. Furthermore, the dynamic nature of these contaminant domains on the capsule surface was found to result in a variance in the particle adhesion over time.

The colloidal probe technique is commonly employed to determine the adhesion force between a particle and a solid surface. Characterization of the adhesion of a particle across a surface can be as important, if not more so, as the determination of an average value for the adhesion. Unfortunately, the measurement of the variation in adhesion can be difficult at best. A new approach for studying particle-surface adhesion based on the force-volume technique is presented. Upon combining the force-volume technique with a colloidal probe, not only is it possible to determine the average adhesion force, but an image of the spatial variation of the adhesion can also be obtained. This method is envisioned to have great potential for examining and analyzing the adhesion behavior in complex natural and technological systems. Copyright 2000 Academic Press.

Measurements are presented of forces between two cellulose spheres in both air and aqueous solution. Forces in air are interpreted in terms of a dispersion interaction between two surfaces achieving poor mechanical contact, while the forces in aqueous solution are well described by a double-layer interaction. No evidence for a steric interaction between the surfaces was discovered, in contrast to earlier work on related systems. The technique is proposed as an ideal one for modelling interactions in papermaking and pumping systems.

Aqueous chloramine diffusion into styrene butadiene rubber (SBR) and natural rubber was analyzed using approximate analytical and numerical solutions of Fick's second law of diffusion to develop long-term mass intake prediction curves. Diffusion coefficients were calculated for 1 mg/L chloramine concentration at three temperatures (23, 45, and 70°C) and also for 23°C at three chloramine concentrations (1, 30, and 60 mg/L). The reasonableness of using increased temperature and/or chloramine concentration to accelerate the diffusion process to obtain long-term information was discussed. For 1 mg/L chloramine concentration, the activation energy for the diffusion of chloramines into SBR and natural rubber were computed to be 51.13 and 77.29 kJ/mol, respectively. Also, concentration profiles were developed to understand the extent of penetration through the elastomer thickness over time and temperature. Considering the reports of elastomeric compound failure in chloramine disinfectant water distribution systems because of swelling, this study will be helpful in understanding the performance of the elastomeric compounds in the system.

In this project, a university-wide, academic center has been established entitled Institute for Advanced Materials and Renewable Energy. In this institute, a comprehensive materials characterization facility has been established by co-locating several existing characterization equipment and acquiring several state of the art instrumentation such as field emission transmission electron microscope, scanning electron microscope, high resolution X-ray diffractometer, Particle Size Distribution/Zeta Potential measurement system, and Ultra-microtome for TEM specimen. In addition, a renewable energy conversion and storage research facility was also established by acquiring instrumentation such as UV-Vis absorption spectroscopy, Atomic Layer Deposition reactor, Solar light simulator, oxygen-free glove box, potentiostat/galvanostats and other miscellaneous items. The institute is staffed with three full-time staff members (one senior research technologist, a senior PhD level research scientist and a junior research scientist) to enable proper use of the techniques. About thirty faculty, fifty graduate students and several researchers access the facilities on a routine basis. Several industry RD (b)more » enable offering of several laboratory courses on advanced materials science and engineering; and (c) develop university-industry partnerships based on the advanced materials research. The Institute's efforts were guided by an advisory board comprising eminent researchers from outside KY. Initial research efforts were focused on the discovery of new materials and processes for solar cells and Li ion battery electrodes. Initial sets of results helped PIs to secure a successful EPSCoR cluster implementation grant by teaming with additional researchers from UK. In addition to research efforts, the project enabled several other outcomes: (a) helped recruit a junior faculty member (Dr. Moises Carreon) and establish a lab focused on meso-porous materials toward separation and catalysis; (b) enabled offering of three new, graduate level courses (Materials characterization using spectroscopy and microscopy; Electron and x-ray diffraction; and renewable energy systems); and (c) mentoring of a junior faculty members (Dr. Gerold Willing).« less

The investigation of Protein A and antibody adsorption on surfaces in a biological environment is an important and fundamental step for increasing biosensor sensitivity and specificity. The atomic force microscope (AFM) is a powerful tool that is frequently used to characterize surfaces coated with a variety of molecules. We used AFM in conjunction with scanning electron microscopy to characterize the attachment of protein A and its subsequent binding to the antibody and Salmonella bacteria using a gold quartz crystal. The rms roughness of the base gold surface was determined to be approximately 1.30 nm. The average step height change between the solid gold and protein A layer was approximately 3.0 +/- 1.0 nm, while the average step height of the protein A with attached antibody was approximately 6.0 +/- 1.0 nm. We found that the antibodies did not completely cover the protein A layer, instead the attachment follows an island model. Salt crystals and water trapped under the protein A layer were also observed. The uneven adsorption of antibodies onto the biosensor surface might have led to a decrease in the sensitivity of the biosensor. The presence of salt crystals and water under the protein A layer may deteriorate the sensor specificity. In this report, we have discussed the application and characterization of protein A bound to antibodies which can be used to detect bacterial and viral pathogens.

Nanowires and nanotubes have attracted significant interest during recent years due to their novel electrical, magnetic, and photonic properties. Quantum confinement, proximity interaction, and surface plasmon enhancement effects are among a few unique phenomena associated with these materials. A convenient procedure to prepare these materials is through anodized aluminum oxide (AAO) template synthesis. Nanoporous AAO membranes with pore diameters ranging from 10 to 200 nm can be prepared with anodization in oxalic, sulfuric and phosphoric acids under various reaction conditions. With repeated anodization-etching cycles, highly ordered straight channels can be prepared through self-organization. With electro- and electroless deposition, a variety of nanowires and nanotubes such as Ni, Co, Au, Pb, Bi, etc. have been prepared. The synthesis, characterization, and physical properties of these materials are presented.

Large area nickel antidot arrays with density up to 10^10 /cm^2 have been fabricated by depositing nickel onto anodic aluminum oxide membranes that contain lattices of nanopores. Electron microscopy images show a high degree of order of the antidot arrays. Various sizes and shapes of the antidots were observed with increasing thickness of the deposited nickel. New features appear in the antidot arrays in both magnetization and transport measurements when the external magnetic field is parallel to the current direction, including an enhancement and a nonmonotonous field dependence of the magnetoresistance, larger values of the coercive field and remanence moment, and smaller saturation field.

Densely covered (ET)X 2 thin films can be selectively electrodeposited on gold electrodes. The insulating (ET)X 2 films are converted to (ET) 2 X conductive films through a novel conproportionation reaction. Both ET and ET salt patterns can be prepared with the PDMS stamping technique with use of an ET derivative with a dodecanethiol chain for surface derivatization. These solution procedures open up the possibility to prepare conductive and superconductive charge-transfer salt thin films as well as patterns.

The transport properties of self-supporting Au nanoparticle–ionic liquid-derived polymer composites were characterized. Topographic AFM images confirm the perforated lamellar composite architecture determined by small-angle X-ray scattering (SAXS) and further show that the in situ synthesized Au nanoparticles are localized within the hydrophilic (water) domains of the structure. At low Au nanoparticle content, the images reveal incomplete packing of spherical particles (i.e., voids) within these columns. The confinement and organization of the Au nanoparticles within the hydrophilic columns give rise to a large manifold of optical resonances in the near-IR region. The bulk composite conductivity, Rb, was determined by ac electrochemical impedance spectroscopy (EIS) for samples prepared with increasing Au3+ content over a frequency range of 10 Hz to 1 MHz. A 100-fold increase was observed in the bulk conductivity at room temperature for composites prepared with the highest amount of Au3+ (1.58 ± 0.065 µmol) versus the no Au composite, with the former reaching a value of 1.3 × 10−4 S cm−1 at 25 °C. The temperature dependence of the conductivity recorded over this range was well-modeled by the Arrhenius equation. EIS studies on samples containing the highest Au nanoparticle content over a broader range of frequencies (2 × 10−2 Hz to 5 × 105 Hz) identified a low frequency component ascribed to electronic conduction. Electronic conduction due to aggregated Au nanoparticles was further confirmed by dc conductivity measurements. This work identifies a nanostructured composite that exhibits both ionic transport through the polymeric ionic liquid and electronic conduction from the organized encapsulated columns of Au nanoparticles.

The development of colloidal probe microscopy has made it possible to directly measure the interaction forces between two different surfaces in solution. Cantilever calibration is presently a subject of intense experimental and theoretical interest due to the need for accurate force measurement. We developed a novel and direct calibration method for colloidal probe cantilevers to which a silica microsphere has been previously attached based on fitting experimental force curves for the interaction between the silica sphere and a silica flat in dilute KBr solutions to the theoretical Derjaguin, Landau, Verwey, and Overbeek force curves using the measured zeta potential of the silica surfaces.

Respiratory syncytial virus (RSV) has been recognized as one of the most common causes of severe respiratory tract infection in infants worldwide. As yet, a safe and effective vaccine has not been developed to protect humans from RSV. The F and G surface proteins have been widely investigated due to their potential to induce protective immunity. In addition, the M2 protein has been shown to be important in inducing a T-cell response. Our project involved the cl oning of the immunodominant regions of the RSV F, M2 and G proteins into a bacterial vector, pET-32a(+). The recombinant RFM2G protein was expressed in Escherichia coli and purified using His Bind columns. The purified rRFM2G protein was analyzed by poly-acrylamide gel electrophoresis and Western blotting. The predicted structure of the recombinant protein built by the Swiss PDB Viewer program suggested a rod shape with a distinct swollen head and neck which was confirmed by transmission electron microscopy and atomic force microscopy. BALB/c female mice were immunized with either RSV, rRFM2G alone, or rRFM2G in combination with flagellin as a mucosal adjuvant. Serum was collected on days 0, 14, 28 and 49 to assess the immune response by Enzyme-linked immunosorbent assay. Intranasal immunization of mice with the rRFM2G protein yielded significantly high serum IgG titers. Co-administration of the rRFM2G protein with flagellin did not augment the serum antibody response.