Evaluating polymer/polymer-carbon black composite coated quartz crystal microbalance sensor response: an experimental and molecular modeling investigation
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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.
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.
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.
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.
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 .
A radiatively cooled Cryogenic Quartz Crystal Microbalance designed to monitor highly volatile contaminants on the shuttle is described. Measurements are made with two 15-MHz microbalances having removable, optically polished sensors mounted in a radiant cooler. One sensor operates below the freezing point of water and monitors contamination including that of water vapor. The second sensor is heated and monitors the contamination background. It provides a reference from which the density of the water vapor cloud enveloping the shuttle is determined. The design incorporates a low-power dissipation oscillator, heaters for ice removal, and a method for attaching second-surface mirrors to the radiator employing an indium type solder instead of a room temperature vulcanizer.
Spacecraft hardware thermal vacuum exposures and bakeouts have been used for years to reduce molecular outgassing to limit contamination to critical optics and sensors on-ground and in orbit. This presentation will discuss lessons learned and vacuum procedural techniques to make the most of your vacuum time. Quartz Crystal Microbalances (QCMs) and Residue Gas Analyzers (RGA) are 2 devices that help track molecular outgassing and examples will be shown on how to use them for your analytical benefit.
We are investigating the use of nitron as a potential chemical sensor for nitric acid and other electron deficient nitrogen oxides. Solutions of nitron in 1-propanol, toluene, and chloroform have been tested for use on a piezoelectric quartz crystal microbalance. We are testing various solvents and metal cations which can maximize the lifetime and reaction specificity of nitron so that they may be used as chemical coatings for stratospheric measurement of trace gases. Results of the work to date will be shown, and future direction discussed.
The Quartz Crystal Microbalance Surface Acoustic Wave (QCM/SAW) cascade impactor collects size-fractionated distributions of aerosols on a series of 10 MHz quartz crystals and employs SAW devices coated with chemical sensors for gas detection. Presently, we are calibrating the ER-2 certified QCM/SAW cascade impactor in the laboratory for the detection of ozone. Experiments have been performed to characterize the QCM and SAW mass loading, saturation limits, mass frequency relationships, and sensitivity. We are also characterizing sampling efficiency by measuring the loss of ozone on different materials. There are parallel experiments underway to measure the variations in the sensitivity and response of the QCM/SAW crystals as a function of temperature and pressure. Results of the work to date will be shown.
The Quartz Crystal Microbalance Surface Acoustic Wave (QCM/SAW) cascade impactor is an instrument designed to collect size-fractionated distributions of aerosols on a series of quartz crystals and employ SAW devices coated with chemical sensors for gas detection. We are calibrating the cascade impactor in our laboratory for future deployment for in-situ experiments to measure ozone. Experiments have been performed to characterize the QCM and SAW mass loading, saturation limits, mass frequency relationships, and sensitivity. The characteristics of mass loading, saturation limits, mass-frequency relationships, sensitivity, and the loss of ozone on different materials have been quantified.
The Temperature-Controlled Quartz Crystal Microbalance (TQCM) system was flown on the Spacelab I Mission as part of the Induced Environment Contamination Monitor to monitor surface contamination (SC) in the payload bay. SC on the five sensors of the TQCM was analyzed by means of IR spectroscopy, scanning electron spectroscopy, and energy dispersive X-ray fluorescence. The amount of SC ranged from 1.4 micrograms/sq cm for the -Z sensor to 39.9 micrograms/sq cm for the +X sensor. The IR analysis showed strong CH2, CH3, and carbonyl absorption bands, indicative of ester and polyester compounds found in adhesives, plasticizers, and tape. The particulates (mostly ranging from 1 micron to 20 microns in size) were mainly composed of Mg, Al, Al2O3, and Si, and probably originated in the solid rocket firings.
One potential life-limiting mechanism in a Hall thruster is the erosion of the ceramic material comprising the discharge channel. This is especially true for missions that require long thrusting periods and can be problematic for lifetime qualification, especially when attempting to qualify a thruster by analysis rather than a test lasting the full duration of the mission. In addition to lifetime, several analytical and numerical models include electrode erosion as a mechanism contributing to enhanced transport properties. However, there is still a great deal of dispute over the importance of erosion to transport in Hall thrusters. The capability to perform an in-situ measurement of discharge channel erosion is useful in addressing both the lifetime and transport concerns. An in-situ measurement would allow for real-time data regarding the erosion rates at different operating points, providing a quick method for empirically anchoring any analysis geared towards lifetime qualification. Erosion rate data over a thruster s operating envelope would also be useful in the modeling of the detailed physics inside the discharge chamber. There are many different sensors and techniques that have been employed to quantify discharge channel erosion in Hall thrusters. Snapshots of the wear pattern can be obtained at regular shutdown intervals using laser profilometry. Many non-intrusive techniques of varying complexity and sensitivity have been employed to detect the time-varying presence of erosion products in the thruster plume. These include the use quartz crystal microbalances, emission spectroscopy, laser induced flourescence, and cavity ring-down spectroscopy. While these techniques can provide a very accurate picture of the level of eroded material in the thruster plume, it is more difficult to use them to determine the location from which the material was eroded. Furthermore, none of the methods cited provide a true in-situ measure of erosion at the channel surface while the thruster is in operation (i.e. none yield a continuous channel erosion measurement). A recent fundamental sensor development effort has led to a novel regression, erosion, and ablation sensor technology (REAST). The REAST sensor allows for measurement of real-time surface erosion rates at a discrete surface location. The sensor was tested using a linear Hall thruster geometry (see Fig. 1), which served as a means of producing plasma erosion of a ceramic discharge chamber. The mass flow rate, discharge voltage, and applied magnetic field strength could be varied, allowing for erosion measurements over a broad thruster operating envelope. Results are presented demonstrating the ability of the REAST sensor to capture not only the insulator erosion rates but also changes in these rates as a function of the discharge parameters.