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At least 37 records · Page 2
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Orientation matters: Measuring the correct surface of polyamide membranes with quartz crystal microbalance

The surface of polyamide reverse osmosis (RO) membranes which regulates interface-dominated phenomena, such as partitioning and fouling, is the one facing the feed during operation. However, the opposite surface of the polyamide selective layer, the one facing the permeate and in contact with the polysulfone porous support, is commonly analyzed in quartz crystal microbalance (QCM) measurements due to limitations of state-of-the-art transfer methodologies. Such measurements on the back surface cannot be generalized because the polyamide layer is chemically and morphologically asymmetric. Herein, we introduce a simple method to coat QCM sensors with polyamide active layers in the correct orientation (i.e., exposing their front surface) and show that interface-dominated phenomena differ significantly between orientations. We start by describing a transfer protocol to coat any surface with a polyamide layer on its front surface orientation. We then systematically analyze the chemical and morphological differences between the two surfaces of the polyamide layer of a commercial RO membrane. Finally, we demonstrate that interface-dominated phenomena depend on the orientation by showing that NaCl partitioning at pH 6 was 1.3 to 2.3-fold higher on the front surface and that organic fouling with humic acid occurred at a lower rate on this surface. The new method presented herein enables measurements on the front surface of polyamide RO membranes, which should be the standard in any future QCM studies.

Fouling behavior↗
DOE OSTI2021

A practical guide to quartz crystal microbalance with dissipation monitoring of thin polymer films

Quartz crystal microbalance with dissipation (QCM-D) monitoring is a powerful tool used to sensitively examine the real-time responses of polymer films to external responses. For example, the technique is commonly used to monitor film growth, material adsorption, thin film swelling, and ion exchange. With its rapidly expanding use, this review is intended to introduce new users to the basic principles of QCM-D, along with practical challenges and remedies specific to polymer thin films. For both new and experienced users, specific case studies are highlighted including layer-by-layer assembly, electrochemical QCM-D, swelling, sensing, and biological application. Finally, the review recommends future directions for research and areas of growth.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Mercury Detection Utilizing an Aquatic Animal as a Remote-Sensing Platform

Mercury species in open water, especially the accumulated methylmercury ion, pose a threat to fish and environment. Therefore, it is important to develop a small sensor package that can be integrated into a biotelemetry sensor carried by an aquatic animal, enhancing the ability to detect mercury contamination in large water areas. A quartz crystal microbalance (QCM) sensor using metal-organic framework (MOF) as sensing material was developed to detect mercury and methylmercury ions in real time based on acoustic wave perturbation. Thiol groups were introduced into the MOF UiO-66 through the organic linker to prepare the UiO-66-SH which was confirmed by infrared spectroscopy results. Batch adsorption experiments were conducted for the Hg 2+ , CH 3 Hg + , and Ca 2+ ions adsorption in the UiO-66-SH. The adsorption capacities of the mercury ions were more than an order of magnitude higher than those of the competing Ca 2+ ions at the same concentration. The frequency changes of the QCM sensor with the UiO-66-SH sensing film were an order of magnitude higher than those of the controlled baseline QCM sensor without a sensing film. Additionally, the frequency change can be tailored by adjusting the thickness of the MOF film and the adsorption properties of the sensing material. The sensor frequency change correlates well with ion adsorption capacities.

47 OTHER INSTRUMENTATION↗
DOE OSTI2021

Detection of Chymotrypsin by Optical and Acoustic Methods

Chymotrypsin is an important proteolytic enzyme in the human digestive system that cleaves milk proteins through the hydrolysis reaction, making it an interesting subject to study the activity of milk proteases. In this work, we compared detection of chymotrypsin by spectrophotometric dynamic light scattering (DLS) and quartz crystal microbalance (QCM) methods and determined the limit of chymotrypsin detection (LOD), 0.15 ± 0.01 nM for spectrophotometric, 0.67 ± 0.05 nM for DLS and 1.40 ± 0.30 nM for QCM methods, respectively. The sensors are relatively cheap and are able to detect chymotrypsin in 3035 min. While the optical detection methods are simple to implement, the QCM method is more robust for sample preparation, and allows detection of chymotrypsin in non-transparent samples. We give an overview on methods and instruments for detection of chymotrypsin and other milk proteases.

59 BASIC BIOLOGICAL SCIENCES↗
NASA NTRS1995

Use of the quartz crystal microbalance to determine the monomeric friction coefficient of polyimides

When a thin film of polymer is coated on to a quartz crystal microbalance (QCM), the QCM can be used to detect the rate of increase in weight of the polymer film as the volatile penetrant diffuses into the polymer. From this rate information the diffusion coefficient of the penetrant into the polymer can be computed. Calculations requiring this diffusion coefficient lead to values which approximate the monomeric friction coefficient of the polymer. This project has been concerned with the trial of crystal oscillating circuits suitable for driving polymer coated crystals in an atmosphere of penetrant. For these studies done at room temperature, natural rubber was used as an easily applied polymer that is readily penetrated by toluene vapors, qualities anticipated with polyimides when they are tested at T(g) in the presence of toluene. Three quartz crystal oscillator circuits were tested. The simplest circuit used +/- 5 volt dc and had a transistor to transistor logic (TTL) inverter chip that provides a 180 deg phase shift via a feed back loop. This oscillator circuit was stable but would not drive the crystal when the crystal was coated with polymer and subjected to toluene vapors. Removal of a variable resistor from this circuit increased stability but did not otherwise increase performance. Another driver circuit tested contained a two stage differential input, differential output, wide band video amplifier and also contain a feed back loop. The circuit voltage could not be varied and operated at +/- 5 volts dc; this circuit was also stable but failed to oscillate the polymer coated crystal in an atmosphere saturated with toluene vapors. The third oscillator circuit was of similar construction and relied on the same video amplifier but allowed operation with variable voltage. This circuit would drive the crystal when the crystal was submerged in liquid toluene and when the crystal was coated with polymer and immersed in toluene vapors. The frequency readings obtained when using this oscillating circuit are highly variable. This circuit requires further modification to stabilize frequency readings before its use in studies to determine the diffusion coefficient of penetrant molecules into a polymer film coated on a QCM.

Bechtold, Mary M.↗
NASA NTRS1996

Cost Models for MMC Manufacturing Processes

Processes for the manufacture of advanced metal matrix composites are rapidly approaching maturity in the research laboratory and there is growing interest in their transition to industrial production. However, research conducted to date has almost exclusively focused on overcoming the technical barriers to producing high-quality material and little attention has been given to the economical feasibility of these laboratory approaches and process cost issues. A quantitative cost modeling (QCM) approach was developed to address these issues. QCM are cost analysis tools based on predictive process models relating process conditions to the attributes of the final product. An important attribute, of the QCM approach is the ability to predict the sensitivity of material production costs to product quality and to quantitatively explore trade-offs between cost and quality. Applications of the cost models allow more efficient direction of future MMC process technology development and a more accurate assessment of MMC market potential. Cost models were developed for two state-of-the art metal matrix composite (MMC) manufacturing processes: tape casting and plasma spray deposition. Quality and Cost models are presented for both processes and the resulting predicted quality-cost curves are presented and discussed.

Elzey, Dana M.↗
NASA NTRS2006

Stability Enhancement of Polymeric Sensing Films Using Fillers

Experiments have shown the stability enhancement of polymeric sensing films on mixing the polymer with colloidal filler particles (submicron-sized) of carbon black, silver, titanium dioxide, and fumed silicon dioxide. The polymer films are candidates for potential use as sensing media in micro/nano chemical sensor devices. The need for stability enhancement of polymer sensing films arises because such films have been found to exhibit unpredictable changes in sensing activity over time, which could result in a possible failure of the sensor device. The changes in the physical properties of a polymer sensing film caused by the sorption of a target molecule can be measured by any of several established transduction techniques: electrochemical, optical, calorimetric, or piezoelectric, for example. The transduction technique used in the current polymer stability experiments is based on piezoelectric principles using a quartz-crystal microbalance (QCM). The surface of the QCM is coated with the polymer, and the mass uptake by the polymer film causes a change in the oscillating frequency of the quartz crystal. The polymer used for the current study is ethyl cellulose. The polymer/ polymer composite solutions were prepared in 1,3 dioxolane solvent. The filler concentration was fixed at 10 weight percent for the composites. The polymer or polymer composite solutions were cast on the quartz crystal having a fundamental frequency of about 6 MHz. The coated crystal was subjected to a multistage drying process to remove all measurable traces of the solvent. In each experiment, the frequency of oscillation was measured while the QCM was exposed to clean, dry, flowing air for about 30 minutes, then to air containing a known concentration of isopropanol for about 30 minutes, then again to clean dry air for about 30 minutes, and so forth. This cycle of measurements for varying isopropanol concentrations was repeated at intervals for several months. The figure depicts some of the sensing film stability results for ethyl cellulose polymer, ethyl cellulose-carbon black, and ethyl cellulose-silicon dioxide composite systems. An ethyl cellulose film exhibited a marked decline in response in the first few months of study and settled to a steady average response after about four months. However, response varied widely around the average response for ethyl cellulose film. In contrast, ethyl cellulose- carbon black and ethyl cellulose-silicon dioxide composites also declined in the early months, but showed more repeatable sensing film activity after the initial decline. Similar trends were observed in experiments for ethyl cellulose-titanium dioxide and ethyl cellulose-silver composites.

Lin, Brian↗
DOE OSTI2026

Protein Adhesion on Semi-Fluorinated Polystyrene Surfaces in Static and Dynamic Measurements

Reducing protein adhesion is a critical strategy in fouling-resistant material innovation, with broad applications spanning biomedical and healthcare devices, biosensors, industrial and environmental systems, and other important technological domains. Here, in this study, we elucidated protein adhesion behavior on polystyrene-based thin films by neutron reflectometry (NR) and quartz crystal microbalance with dissipation (QCM-D), using both lysozyme and bovine serum albumin (BSA) as model proteins. To this end, semifluorinated polystyrene thin films with gradient wettability and surface energy were fabricated through dry processing using plasma oxidation and gas-phase deposition. Although it is believed that a fully fluorinated alkyl chain offers extremely low surface energy, thus rejecting foulants, and has been used in many fouling-resistant surface designs, enhanced protein–surface interactions were observed consistently in NR and QCM-D results, due to the combined effects of surface morphology and chemistry. On the contrary, depositing shorter fluorinated silane onto a hydrophilic PS surface contributed to a more homogeneous nanoscale fluorine coating, resulting in less initial protein adsorption and improved surface recovery. Comparative analysis of proteins with different sizes on the nanopatterned semifluorinated surface revealed the influence of molecular characteristics on surface interactions. Lysozyme, being smaller and more compact, showed faster adsorption kinetics and higher surface coverage but largely reversible binding, whereas BSA, with its larger and more flexible structure, formed broader and more stable interfacial layers. This study fills the gap in understanding protein adhesion within the range of hydrophobicity (water contact angle ∼90°), as current strategies often associate with extreme hydrophilic and superhydrophobic surfaces due to hydration or low-surface-energy rejection mechanisms, respectively. It also provides in-depth insights into current combinatorial fouling-resistant surface design.

Yuan, Yue [Oak Ridge National Laboratory (ORNL), O↗
DOE OSTI2022

ECEI characterization of pedestal fluctuations in quiescent H-mode plasmas in DIII-D

Here, electron cyclotron emission imaging (ECEI) is employed to characterize the magneto hydraulics dynamics (MHD) fluctuations at the quiescent H-mode pedestals in DIII-D. Pedestal MHD fluctuations cause ECE radiation temperature fluctuations $\delta {T_{e{\text{,rad}}}}$ in both the pedestal and scrape-off-layer (SOL). A synthetic ECE platform is utilized for detailed interpretation of the ECEI signals in the SOL and pedestal regions. It is observed that the ECE radiation $\delta {T_{e{\text{,rad}}}}$, which is located in the SOL region according to the cold and optically thick plasma resonance assumption, is extremely sensitive to MHD radial displacements near the separatrix, exhibiting radiation inversion to $\delta {T_{e{\text{,rad}}}}$ at the pedestal. Here, the radiation inversion refers to the opposite phase between the radiation fluctuation at the pedestal and the radiation fluctuation at the SOL. Consequently, the quasi-coherent MHD (QCM), which displays a radiation inversion, is found to be consistent with an MHD radial structure that has a strong displacement near the separatrix. In contrast, the edge harmonic oscillation (EHO), which displays weak or no inversion, is found to be consistent with an MHD radial displacement structure peaking at the pedestal top. The ECEI data, interpreted with synthetic ECE, are in qualitative agreement with beam emission spectroscopy measurements on DIII-D for the relative radial extent and localization of the EHO and QCM. The high sensitivity of ECE radiation to separatrix displacements can be used to detect turbulence or MHD fluctuations near the separatrix, which may affect the transport across the separatrix and the wetted area in the divertor. The $\delta {T_{e{\text{,rad}}}}$ inversion measured with an ECE or ECEI system potentially provides important information on the magnetic field $\left| {{B_{{\text{sep}}}}} \right|$ at the separatrix, which helps constrain the pedestal equilibrium reconstruction and achieve an unambiguous mapping of the ECE/ECEI system with respect to the separatrix.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2025

Nonpyrophoric alternative to trimethylaluminum for the atomic layer deposition of Al 2 O 3

We have examined the atomic layer deposition (ALD) of Al 2 O 3 using a nonpyrophoric precursor, which possesses only Al–N bonds and no Al–C bonds: Al(N(CH 3 ) 2 ) 2 (–N(C 2 H 5 )–C 2 H 4 –N(C 2 H 5 ) 2 ), which we refer to as bis-dimethylamino-diamino-aluminum (BDMADA-Al). We employed a quartz crystal microbalance (QCM) to monitor ALD in situ and in real time, and the deposited thin films have been characterized using x-ray photoelectron spectroscopy, spectroscopic ellipsometry, x-ray reflectivity, and atomic force microscopy. Films deposited with BDMADA-Al result in near-stoichiometric Al2O3 at temperatures ranging from T = 120 to 285 °C using H 2 O as the coreactant and at T = 285 °C using t-BuOH as the coreactant. The properties of the films (density, C incorporation, stoichiometry, growth rates) are comparable using either BDMADA-Al or trimethylaluminum (TMA) as the precursor under similar reaction conditions. The N content in the films deposited with BDMADA-Al as the precursor is <1% at both T = 120 and 285 °C. Additionally, both BDMADA-Al|t-BuOH and TMA|t-BuOH processes deposit near-stoichiometric Al 2 O 3 at T = 285 °C, while neither process chemistry produces a constant growth rate per cycle at T = 120 °C. Close examination of single cycle QCM data from BDMADA-Al ALD indicates unique ligand exchange reaction mechanisms during each of the half-reactions. Experimentally, we have evidence supporting the mechanism in which upon the chemisorption of BDMADA-Al, the species on the surface retains the –N(CH 3 ) 2 ligands, while the diamine ligand is mostly lost on dissociative adsorption, except possibly at the higher temperature (285 °C). As a result, our work demonstrates that BDMADA-Al can be used as an effective alternative precursor to TMA for the ALD of Al 2 O 3 .

36 MATERIALS SCIENCE↗
DOE OSTI2023

Accessibility and Mechanical Stability of Nanoporous Zinc Oxide and Aluminum Oxide Coatings Synthesized via Infiltration of Polymer Templates

The conformal nanoporous inorganic coatings with accessible pores that are stable under applied thermal and mechanical stresses represent an important class of materials used in the design of sensors, optical coatings, and biomedical systems. Here, we synthesize porous AlO x and ZnO coatings by the sequential infiltration synthesis (SIS) of two types of polymers that enable the design of porous conformal coatings—polymers of intrinsic microporosity (PIM) and block co-polymer (BCP) templates. Using quartz crystal microbalance (QCM), we show that alumina precursors infiltrate both polymer templates four times more efficiently than zinc oxide precursors. Using the quartz crystal microbalance (QCM) technique, we provide a comprehensive study on the room temperature accessibility to water and ethanol of pores in block copolymers (BCPs) and porous polymer templates using polystyrene-block-poly-4-vinyl pyridine (PS75-b-P4VP25) and polymers of intrinsic microporosity (PIM-1), polymer templates modified by swelling, and porous inorganic coatings such as AlO x and ZnO synthesized by SIS using such templates. Importantly, we demonstrate that no structural damage occurs in inorganic nanoporous AlO x and ZnO coatings synthesized via infiltration of the polymer templates during the water freezing/melting cycling tests, suggesting excellent mechanical stability of the coatings, even though the hardness of the inorganic nanoporous coating is affected by the polymer and precursor selections. We show that the hardness of the coatings is further improved by their annealing at 900 °C for 1 h, though for all the cases except ZnO obtained using the BCP template, this annealing has a negligible effect on the porosity of the material, as is confirmed by the consistency in the optical characteristics. These findings unravel new potential for the materials being used across various environment and temperature conditions.

36 MATERIALS SCIENCE↗
NASA NTRS1973

Plume mass flow and optical damage distributions for an MMH/N2O4 RCS thruster

The data obtained from two recent experiments conducted in a continuing series of experiments at the Lewis Research Center into the contamination characteristics of a 5-pound thrust MMH/N2O4 engine are presented. The primary objectives of these experiments were to establish the angular distribution of condensible exhaust products within the plume and the corresponding optical damage angular distribution of transmitting optical elements attributable to this contaminant. The plume mass flow distribution was measured by five quartz crystal microbalances (QCM's) located at the engine axis evaluation. The fifth QCM was located above the engine and 15 deg behind the nozzle exit plane. The optical damage was determined by ex-situ transmittance measurements for the wavelength range from 0.2 to 0.6 microns on 2.54 cm diameter fused silica discs also located at engine centerline elevation. Both the mass deposition and optical damage angular distributions followed the expected trend of decreasing deposition and damage as the angle between sensor or sample and the nozzle axis increased. A simple plume gas flow equation predicted the deposition distribution reasonably well for angles of up to 55 degrees. The optical damage measurements also indicated significant effects at large angles.

Spisz, E. W.↗
NASA NTRS1974

Skylab electronic technological advancements

The present work describes three electronic devices designed for use in the Skylab airlock module: the teleprinter system, the quartz crystal microbalance contamination monitor (QCM), and the speaker. Design considerations, operation, characteristics, and system development are described for these systems, with accompanying diagrams, graphs, and photographs. The teleprinter is a thermal dot printer used to produce hard copy messages by electrically heating print elements in contact with heat-sensitive paper. The QCM was designed to estimate contamination buildup on optical surfaces of the earth resources experiment package. A vibrating quartz crystal is used as a microbalance relating deposited mass to shifts in the crystal's resonant frequency. Audio devices provide communication between crew members and between crew and STDN, and also provide audible alarms, via the caution and warning system, of out-of-limit-conditions.

Hornback, G. L.↗
NASA NTRS1975

Correlation of an optical system degradation with contamination on a critical surface

The loss of sensitivity of a radiantly cooled radiometer during space operation was investigated. A quartz crystal microbalance (QCM), mounted in the proximity of the instrument filter lens and held at its temperature, measured the contaminant at the location during a vacuum test. The temperature cycling of the lens and the QCM verified the contamination of the lens as the cause of the deterioration. Data on the instrument performance in space and in the chamber allowed estimation of the rate of contaminant accretion on the lens in space service. That rate was used to estimate the contaminant partial pressure. The nature of material was inferred by comparison of the partial pressures and the saturated vapor pressures of materials at the temperature of the contaminated surface. These data, in conjunction with data on fields of view of the lens, are used to identify the sources of contamination.

Scialdone, J. J.↗
NASA NTRS1977

The Response of a Quartz Crystal Microbalance to a Liquid Deposit

A theory was developed for predicting the loss of response of a QCM (Quartz Crystal Microbalance) to a liquid deposit due to viscous effects in the deposit. The loss of response is expressed by a response factor, equal to the response of the QCM to a liquid film divided by its response to a solid film of the same mass per unit area. The theory assumes a droplet-type deposit morphology, and considers the influence of droplet distribution parameters. Experiments were conducted to examine the validity of the theory, using DC 704 silicone oil as the subject deposit material. Experiments were made in two series: one with constant deposit mass and variable temperature, the other with variable deposit mass and constant temperature. Interpretation of the data using the theory has enabled information on droplet area coverage and number density to be deduced.

Glassford, A. P. M.↗
NASA NTRS1980

Measurement of particulates

The size distributions of particles in the exhaust plumes from the Titan rockets launched in August and September 1977 were determined from in situ measurements made from a small sampling aircraft that flew through the plumes. Two different sampling instruments were employed, a quartz crystal microbalance (QCM) cascade impactor and a forward scattering spectrometer probe (FSSP). The QCM measured the nonvolatile component of the aerosols in the plume covering an aerodynamic size ranging from 0.05 to 25 micrometers diameter. The FSSP, flown outside the aircraft under the nose section, measured both the liquid droplets and the solid particles over a size range from 0.5 to 7.5 micrometers in diameter. The particles were counted and classified into 15 size intervals. The presence of a large number of liquid droplets in the exhaust clouds is discussed and data are plotted for each launch and compared.

Woods, D.↗
NASA NTRS1984

Contamination Measurements During Ius Thermal Vacuum Tests in A Large Space Chamber

The levels of contamination that originate from inside the IUS equipment support section (ESS) due to outgassing from electronics components and wiring operating at elevated temperatures (80-160 F) were investigated. Pressure was measured inside and outside the ESS. Mass deposition measurements were made with quartz crystal microbalances (QCM) facing into and away from ESS vents. The OCM's were operated at -50 C and -180 C using thermoelectrically and cryogenically cooled QCM's. Gaseous nitrogen flow inside the ESS was used to obtain the effective molecular flow vent area of the ESS, which was evaluated to be 359 sq cm (56 sq in) compared to the 978 sq cm (150 sq in) estimated by an earlier atmosphere pressure billowing test. The total outgassing rate of the ESS materials at a temperature of 60 C (140 F) decays with a time constant of 11.5 hours based on pressure measurements during the hot cycle. A time constant of 22 hours was estimated for the fraction of the outgassing which will condense on a -50 C surface. In contrast, the time constant is only 10.1 hours for the outgassing material which condenses on a surface at -180 C. A surface at -180 C collects approximately one half of the material vented from the ESS which impinges on it. Pressure measurements show very good correlation with the mass deposition measurements.

C R Mullen↗
NASA NTRS1989

Investigation of a liquid-fed water resistojet plume

Measurements of mass flux and flow angle were taken throughout the forward flow region of the exhaust of a liquid-fed water resistojet using a quartz crystal microbalance (QCM). The resistojet operated at a mass flow rate of 0.1 g/s with a power input of 330 Watts. Measured values were compared to theoretical predictions obtained by employing a source flow approximation. Excellent agreement between predicted and measured mass flux values was attained; however, this agreement was highly dependent on knowledge of nozzle flow conditions. Measurements of the temperature at which the exhaust condensed on the QCM were obtained as a function of incident mass flux.

Manzella, D. H.↗