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The purpose of the Temperature-Controlled Quartz Crystal Microbalance (TQCM) system on STS-2 was to measure condensible molecular flux in the payload bay of the Space Shuttle as a function of temperature, direction, and time. Five quartz crystal microbalance sensors were located in the IECM to measure molecular adsorption in each of the Orbiter axes, +X (fore), -X (aft), +Y (starboard), -Y (port), and -Z (up, perpendicular to payload bay). The temperature of each sensor was controlled by a thermoelectric device so contamination could be measured as a function of four preset temperatures: +30, 0, -30, and -60 C. When orbital altitude was reached, the TQCM sensors began their orbital measuring cycle routine. The sensors were commanded to 80 C for 30 min, which was used as an initial clean-up. They were then stepped through a program of 2-nr collection periods at each temperature with a 30-min, 80 C period between each collection period. The collection periods progressed in descending order from +30 to -60 C and, then the cycle was repeated. Since the STS-2 orbital phase lasted approximately 53 hrs, the TQCM system completed four cycles and was in the fifth when the mission was terminated.
Quartz crystal microbalance sensors are recommended to verify and monitor surface deposition on the early transverse boom as well as the later dual-keel Space Station configurations. Performance and placement of these sensors are discussed and compared to imposed maximum mass deposition rate requirements at the science instrument and critical power locations. Additional measurements are suggested to gain further knowledge on properties of the deposited material.
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.
The Stratospheric Aerosol and Gas Experiment (SAGE) III - International Space Station (ISS) instrument will be used to study ozone, providing global, long-term measurements of key components of the Earth's atmosphere for the continued health of Earth and its inhabitants. SAGE III is launched into orbit in an inverted configuration on SpaceX;s Falcon 9 launch vehicle. As one of its four supporting elements, a Contamination Monitoring Package (CMP) mounted to the top panel of the Interface Adapter Module (IAM) box experiences high-frequency response due to structural coupling between the two structures during the SpaceX launch. These vibrations, which were initially observed in the IAM Engineering Development Unit (EDU) test and later verified through finite element analysis (FEA) for the SpaceX launch loads, may damage the internal electronic cards and the Thermoelectric Quartz Crystal Microbalance (TQCM) sensors mounted on the CMP. Three-dimensional (3D) vibration isolators were required to be inserted between the CMP and IAM interface in order to attenuate the high frequency vibrations without resulting in any major changes to the existing system. Wire rope isolators were proposed as the isolation system between the CMP and IAM due to the low impact to design. Most 3D isolation systems are designed for compression and roll, therefore little dynamic data was available for using wire rope isolators in an inverted or tension configuration. From the isolator FEA and test results, it is shown that by using the 3D wire rope isolators, the CMP high-frequency responses have been suppressed by several orders of magnitude over a wide excitation frequency range. Consequently, the TQCM sensor responses are well below their qualification environments. It is indicated that these high-frequency responses due to the typical instrument structural coupling can be significantly suppressed by a vibration passive control using the 3D vibration isolator. Thermal and contamination issues were also examined during the isolator selection period for meeting the SAGE III-ISS instrument requirements.
Fabrication of metal–organic framework (MOF) thin films over macroscopic surface areas is a subject of great interest for gas sensor application platforms such as optics and microelectronics. However, a direct synthesis of MOF films at ambient conditions, in particular pillared-layer MOF films due to their anisotropic structures, remains a significant challenge. Herein, we demonstrate for the first time a facile construction of dense and continuous pillared-layer MOF thin films on a centimeter scale via an aluminum-doped zinc oxide template and hydroxy double salt (HDS) intermediates at room temperature. A series of Cu(II)-based pillared MOFs with different 1,4-benzenedicarboxylic acid (bdc) ligands were explored for optimizing MOF film formation for CO 2 sensor applications. Nonpolar ligands with lower water solubility preferentially formed crystalline pillared MOF structures from HDS intermediates. A Cu 2 (ndc) 2 (dabco) (ndc = 1,4-naphthalene-bdc; dabco = 1,4-diazabicyclo[2.2.2]octane) MOF demonstrated the most dense and uniform film growth with micrometer thickness over one square centimeter area. This synthetic approach for growing Cu 2 (ndc) 2 (dabco) MOF thin films was successfully translated toward two sensing platforms: a quartz crystal microbalance and an optical fiber sensor. These Cu 2 (ndc) 2 (dabco) MOF-coated sensors displayed sensitivity toward CO 2 and response/recovery time on the scale of seconds, even at moderate humidity levels. Finally, this work provides a road map for producing continuous and anisotropic crystalline MOF thin films over a centimeter scale area on various substrates, which will greatly facilitate their utilization in MOF-based sensor devices, among other applications.
Classic design of experiment relies on a time-intensive workflow that requires planning, data interpretation, and hypothesis building by experienced researchers. Here, in this paper, we describe an integrated, machine-intelligent experimental system which enables simultaneous dynamic tests of electrical, optical, gravimetric, and viscoelastic properties of materials under a programmable dynamic environment. Specially designed software controls the experiment and performs on-the-fly extensive data analysis and dynamic modeling, real-time iterative feedback for dynamic control of experimental conditions, and rapid visualization of experimental results. The system operates with minimal human intervention and enables time-efficient characterization of complex dynamic multifunctional environmental responses of materials with simultaneous data processing and analytics. The system provides a viable platform for artificial intelligence (AI)-centered material characterization, which, when coupled with an AI-controlled synthesis system, could lead to accelerated discovery of multifunctional materials.
On the basis of early estimates of the Shuttle induced environment, Scialdone (1979) concluded that in the vicinity of the cargo, the cargo would have the largest influence on the environment. As a contamination control device, realtime monitors can indicate safe operational periods for sensitive attached payloads. It was, therefore, decided to develop the OSS-1/Contamination Monitor Package (CMP) experiment which was seen as a forerunner of an operational monitor. A description of the CMP is provided, taking into account four actively temperature controlled quartz crystal microbalances (TQCM). The TQCM temperatures could be varied from -60 C to +80 C. The sensor consisted of a matched pair of quartz crystals. The crystals were designated as a sensor and reference crystal. Results obtained during the STS-3 mission are discussed. These results show the feasibility and advantages of a small real-time contamination monitor.
A gas sensor (100,200) includes at least one sensor device including a surface acoustic wave (SAW) device (110) or a quartz crystal microbalance (QCM) device (210), and a layer of metal organic framework (MOF) material (120,220) disposed on each of the at least one sensor device. The at least one sensor device is structured to sense a change in mass of the MOF material.
Airborne particulate size distribution measurements were made in the stabilized ground cloud from a Titan III C rocket just after launch from the Kennedy Space Center on May 12, 1977. The measurements were made from aboard a small twin engine aircraft instrumented with particle and gas sensors. The plume was followed for about 1 hour while making multiple passes through the cloud at varying altitudes. The results obtained with a ten-stage cascade quartz crystal microbalance impactor show that the mass concentration as a function of particle diameter is bimodal with the first maximum between 0.05 micrometers and 0.1 micrometers and the second maximum between 0.8 and 1.0 micrometer. Scanning electron microscope analysis were performed on the material collected and show distinctly different kinds of particles in the two modes.
Femtometrics of Costa Mesa, CA, developed the Model 200-1 SAW Mass Microbalance under a NASA Small Business Innovation Research (SBIR) contract with Langley Research Center. The product is described as "the next generation of aerosol mass microbalance technology," because a new type of sensor, the Surface Acoustic Wave (SAW) piezoelectric crystal, offers mass resolution two orders of magnitude greater than the Quartz Crystal Microbalance cascade impactor (QCM) (used at Langley since 1979 for collection and measurement of aerosol particles in the upper atmosphere). The Model 200-1 SAW Mass Microbalance, which provides a 400-fold increase in mass sensitivity per unit area over the QCM, can be used for real-time particle monitoring in clean rooms, measuring chemical vapors in very low concentrations, measuring target chemicals in the stratosphere and in industry as a toxic vapor monitor.
Design changes in the thermoelectrically-cooled quartz microbalance, which is used to monitor surface contamination in space simulation chambers, is described in terms of its extended temperature range, increased temperature control, mass sensitivity, and cooling power. The mass sensor uses 20 MHz quartz crystals having a sensitivity of 8.8 x 10 to the minus tenth power g/sq cm - Hz. The crystals are optically polished, metal plated, and overplated with magnesium fluoride to simulate an optical surface. The microbalance temperature circuitry is designed to readout and control surface temperature between 100 C and minus 59 C to plus or minus 0.5 C, and readout only temperature between minus 60 C and minus 199 C using auxiliary liquid nitrogen cooling. Data is included on the measurement of oil contamination of surfaces as a function of temperature in space simulation chambers.
A test was conducted under simulated space conditions to determine the potential thermal degradation of the ATS-F radiant cooler from any contaminants generated by a 0.44-N(0.1-lbf) hydrazine thruster. The radiant cooler, a 0.44-N(0.1-lbf)hydrazine engine, and an aluminum plate simulating the satellite interface were assembled to simulate their flight configuration. The cooler was provided with platinum sensors for measuring temperature, and its surfaces were instrumented with six quartz crystal microbalance units (QCM) to measure contaminant mass deposits. The complete assembly was tested in the molecular sink vacuum facility (Molsink) at the Jet Propulsion Laboratory. This was the first time that a radiant cooler and a hydrazine engine were tested together in a very-high-vacuum space simulator, and this test was the first successful measurement of detectable deposits from hydrazine rocket engine plumes in a high vacuum. The engine was subjected to an accelerated duty cycle of 1 pulse/min, and after 2-hr of operation, the QCMs began to shift in frequency. The tests continued for several days and, although there was considerable activity in the QCMs, the cooler never experienced thermal degradation.
A thermoelectrically temperature controlled quartz crystal microbalance (QCM) system was developed for the measurement of ion thrustor generated mercury contamination on spacecraft. Meaningful flux rate measurements dictated an accurately held sensing crystal temperature despite spacecraft surface temperature variations from -35 C to +60 C over the flight temperature range. An electronic control unit was developed with magentic amplifier transformer secondary power supply, thermal control electronics, crystal temperature analog conditioning and a multiplexed 16 bit frequency encoder.
Here, a straightforward in situ detection method for dengue infection was demonstrated through the molecular imprinting of a dengue nonstructural protein 1 (NS1) epitope into an electropolymerized molecularly imprinted polyterthiophene (E-MIP) film sensor. The key enabling step in the sensor fabrication is based on an epitope imprinting strategy, in which short peptide sequences derived from the original target molecules were employed as the main template for detection and analysis. The formation of the E-MIP sensor films was facilitated using cyclic voltammetry (CV) and monitored in situ by electrochemical quartz crystal microbalance (EC-QCM). Surface properties were analyzed using different techniques including atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), and polarization modulation-infrared reflection-adsorption (PM-IRRAS). The standard calibration curve (R = 0.9830) was generated for the detection of the epitope, Ac-VHTWTEQYKFQ-NH 2 , with a linear range of 0.2 to 30 μg/mL and detection limit of 0.073 μg/mL. A separate calibration curve (R = 0.9786) was obtained using spiked buffered solutions of dengue NS1 protein, which resulted in a linear range of 0.2 to 10 μg/mL and a detection limit of 0.056 μg/mL. The fabricated E-MIP sensor exhibited long-term stability, high sensitivity, and good selectivity towards the targeted molecules. These results indicated that the formation of the exact and stable cavity imprints in terms of size, shape, and functionalities was successful. In our future work, we aim to use our E-MIP sensors for NS1 detection in real-life samples such as serum and blood.
The Midcourse Space Experiment (MSX) is an SDIO sponsored space based sensor experiment with a full complement of optical sensors. Because of the possible deleterious effect of both molecular and particulate contamination on these sensors, a suite of environmental monitoring instruments are also being flown with the spacecraft. These instruments are the Total Pressure Sensor based on the cold-cathode gauge, a quadrupole mass spectrometer, a Bennett-type ion mass spectrometer, a cryogenic quartz crystal microbalance (QCM), four temperature-controlled QCM's, and a Xenon and Krypton Flash Lamp Experiment. These instruments have been fully space-qualified, are compact and low cost, and are possible candidate sensors for near-term planetary and atmospheric monitoring. The philosophy adopted during design and fabrication, calibration and ground testing, and modeling will be discussed .
Proton-conducting ionomers used in electrodes of electrochemical devices form nanometer-scale films covering metallic catalyst surfaces, wherein they experience confinement and interfacial effects absent in the bulk polymer. This confinement alters the physical properties of the ionomer film, which is postulated to increase the density and is attributed to the transport limitations observed in fuel-cell electrodes. Despite studies showing reduced swelling, no systematic measurement has validated this phenomenon by demonstrating both densification and stiffening as the film gets thinner. Here, this study aims to fill this gap by reporting the humidity-driven changes in swelling, mass uptake, and density of Nafion ionomer films cast at varying thicknesses (10–320 nm) onto a gold-plated sensor. The films were simultaneously probed during humidification using spectroscopic ellipsometry (SE) and a quartz crystal microbalance with dissipation (QCM-D), which allowed for determination of the density and shear stiffness. The effects of confinement were prominently observed below ∼30 nm, with films showing increased density along with decreased swelling and mass uptake during hydration. In addition, the confined films show a negative excess volume upon initial water sorption, implying a larger proportion of absorbed water might bound to ionic groups in accord with notion of localized densification.
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.