Engineering topics

Allton, J. H.

Publications and source records attributed to Allton, J. H..

At least 37 records · Page 2

NASA NTRS2015

Enhanced Cleaning of Genesis Solar Wind Sample 61348 for Film Residue Removal

The Genesis mission returned to Earth on September 8, 2004, experiencing a nonnominal reentry. During the recovery of the collector materials from the capsule, many of the collector fragments were placed on the adhesive protion of post-it notes to prevent the fragments from moving during transport back to Johnson Space Center. This unknowingly provided an additional contaminate that would prove difficult to remove with the limited chemistries allowed in the Genesis Curation Laboratory. Generally when collector material samples are prepared for allocation to PIs, the samples are cleaned front side only with Ultra-Pure Water (UPW) via megasonic dispersion to the collector surface to remove crash debris and contamination. While this cleaning method works well on samples that were not placed on post-its during recovery, it has caused movement of the residue on the back of the sample to be deposited on the front in at least two examples. Therefore, samples placed on the adhesive portion on post-it note, require enhanced cleaning methods since post-it residue has proved resistant to UPW cleaning.

Allums, K. K.↗

NASA NTRS2015

Genesis Solar Wind Sample 61422: Experiment in Variation of Sequence of Cleaning Solvent for Removing Carbon-Bearing Contamination

The recovered Genesis collector fragments are heavily contaminated with crash-derived particulate debris. However, megasonic treatment with ultra-pure-water (UPW; resistivity (is) greater than18 meg-ohm-cm) removes essentially all particulate contamination greater than 5 microns in size [e.g.1] and is thus of considerable importance. Optical imaging of Si sample 60336 revealed the presence of a large C-rich particle after UPW treatment that was not present prior to UPW. Such handling contamination is occasionally observed, but such contaminants are normally easily removed by UPW cleaning. The 60336 particle was exceptional in that, surprisingly, it was not removed by additional UPW or by hot xylene or by aqua regia treatment. It was eventually removed by treatment with NH3-H2O2. Our best interpretation of the origin of the 60336 particle was that it was adhesive from the Post-It notes used to stabilize samples for transport from Utah after the hard landing. It is possible that the insoluble nature of the 60336 particle comes from interaction of the Post-It adhesive with UPW. An occasional bit of Post-It adhesive is not a major concern, but C particulate contamination also occurs from the heat shield of the Sample Return Capsule (SRC) and this is mixed with inorganic contamination from the SRC and the Utah landing site. If UPW exposure also produced an insoluble residue from SRC C, this would be a major problem in chemical treatments to produce clean surfaces for analysis. This paper reports experiments to test whether particulate contamination was removed more easily if UPW treatment was not used.

Allton, J. H.↗

NASA NTRS2015

Genesis Solar Wind Collector Cleaning Assessment: Update on 60336 Sample Case Study

To maximize the scientific return of Genesis Solar Wind return mission it is necessary to characterize and remove a crash-derived particle and thin film surface contamination. A small subset of Genesis mission collector fragments are being subjected to extensive study via various techniques. Here we present an update on the sample 60336, a Czochralski silicon (Si-CZ) based wafer from the bulk array (B/C). This sample has undergone multiple cleaning steps (see the table below): UPW spin wash, aggressive chemical cleanings (including aqua regia, hot xylene and RCA1), as well as optical and chemical (EDS, ToF-SIMS) imaging. Contamination appeared on the surface of 60336 after the initial 2007 UPW cleaning. Aqua regia and hot xylene treatment (8/13/2013) did little to remove contaminants. The sample was UPW cleaned for the third time and imaged (9/16/13). The UPW removed the dark stains that were visible on the sample. However, some features, like "the Flounder" (a large, 100 micron feature in Fig. 1b) appeared largely intact, resisting all previous cleaning efforts. These features were likely from mobilized adhesive, derived from the Post-It notes used to stabilize samples for transport from Utah after the hard landing. To remove this contamination, an RCA step 1 organic cleaning (RCA1) was employed. Although we are still uncertain on the nature of the Flounder and why it is resistant to UPW and aqua regia/hot xylene treatment, we have found RCA1 to be suitable for its removal. It is likely that the glue from sticky pads used during collector recovery may have been a source for resistant organic contamination [9]; however [8] shows that UPW reaction with crash-derived organic contamination does not make particle removal more difficult.

Goreva, Y. S.↗

NASA NTRS2014

Development of Genesis Solar Wind Sample Cleanliness Assessment: Initial Report on Sample 60341 Optical Imagery and Elemental Mapping

Since 2005 the Genesis science team has experimented with techniques for removing the contaminant particles and films from the collection surface of the Genesis fragments. A subset of ~40 samples have been designated as "cleaning matrix" samples. These are small samples to which various cleaning approaches are applied and then cleanliness is assessed optically, by TRXRF, SEM, ToF-SIMS, XPS, ellipsometry or other means [1-9]. Most of these sam-ples remain available for allocation, with cleanliness assessment data. This assessment allows evaluation of various cleaning techniques and handling or analytical effects. Cleaning techniques investigated by the Genesis community include acid/base etching, acetate replica peels, ion beam, and CO2 snow jet cleaning [10-16]. JSC provides surface cleaning using UV ozone exposure and ultra-pure water (UPW) [17-20]. The UPW rinse is commonly used to clean samples for handling debris between processing by different researchers. Optical microscopic images of the sample taken before and after UPW cleaning show what has been added or removed during the cleaning process.

Gonzalez, C. P.↗

NASA NTRS2014

Genesis Solar Wind Collector Cleaning Assessment: 60366 Sample Case Study

In order to recognize, localize, characterize and remove particle and thin film surface contamination, a small subset of Genesis mission collector fragments are being subjected to extensive study via various techniques [1-5]. Here we present preliminary results for sample 60336, a Czochralski silicon (Si-CZ) based wafer from the bulk array (B/C).

Goreva, Y. S.↗

NASA NTRS2014

Cellulose Acetate Replica Cleaning Study of Genesis Non-Flight Sample 3CZ00327

The Genesis mission collected solar wind and brought it back to Earth in order to provide precise knowledge of solar isotopic and elemental compositions. The ions in the solar wind were stopped in the collectors at depths on the order of 10 to a few hundred nanometers. This shallow implantation layer is critical for scientific analysis of the composition of the solar wind and must be preserved throughout sample handling, cleaning, processing, distribution, preparation and analysis. We are working interactively with the community of scientists analyzing Genesis samples, using our unique laboratory facilities -- and, where needed, our unique cleaning techniques -- to significantly enhance the science return from the Genesis mission. This work is motivated by the need to understand the submicron contamination on the collectors in the Genesis payload as recovered from the crash site in the Utah desert, and -- perhaps more importantly -- how to remove it. That is, we are evaluating the effectiveness of the wet-chemical "cleaning" steps used by various investigators, to enable them to design improved methods of stripping terrestrial contamination from surfaces while still leaving the solar-wind signal intact.

Kuhlman, K. R.↗

NASA NTRS2014

Investigation of Backside Textures for Genesis Solar Wind Silicon Collectors

Genesis solar wind collectors were comprised of a suite of 15 types of ultrapure materials. The single crystal, pure silicon collectors were fabricated by two methods: float zone (FZ) and Czochralski (CZ). Because of slight differences in bulk purity and surface cleanliness among the fabrication processes and the specific vendor, it is desirable to know which variety of silicon and identity of vendor, so that appropriate reference materials can be used. The Czochralski method results in a bulk composition with slightly higher oxygen, for example. The CZ silicon array wafers that were Genesis-flown were purchased from MEMC Electronics. Most of the Genesis-flown FZ silicon was purchased from Unisil and cleaned by MEMC, although a few FZ wafers were acquired from International Wafer Service (IWS).

Gonzalez, C. P.↗

NASA NTRS2013

Reducing Organic Contamination in NASA JSC Astromaterial Curation Facility

Future robotic and human spaceflight missions to the Moon, Mars, asteroids and comets will require handling and storing astromaterial samples with minimal inorganic and organic contamination to preserve the scientific integrity of each sample. Much was learned from the rigorous attempts to minimize and monitor organic contamination during Apollo, but it was not adequate for current analytical requirements; thus [1]. OSIRIS-REx, Hayabusa-2, and future Mars sample return will require better protocols for reducing organic contamination. Future isolation con-tainment systems for astromaterials, possibly nitrogen enriched gloveboxes, must be able to reduce organic and inorganic cross-contamination. In 2012, a baseline study established the current state of organic cleanliness in gloveboxes used by NASA JSC astromaterials curation labs that could be used as a benchmark for future mission designs [2, 3]. After standard ultra-pure water (UPW) cleaning, the majority of organic contaminates found were hydrocarbons, plasticizers, silicones, and solvents. Hydro-carbons loads (> C7) ranged from 1.9 to 11.8 ng/cm2 for TD-GC-MS wafer exposure analyses and 5.0 to 19.5 ng/L for TD-GC-MS adsorbent tube exposure. Plasticizers included < 0.6 ng/cm2 of DBP, DEP, TXIB, and DIBP. Silicones included < 0.5 ng/cm2 of cyclo(Me2SiO)x (x = 6, 8, 9, 10) and siloxane. Solvents included < 1.0 ng/cm2 of 2-cyclohexen-1-one, 3,5,5-trimethyl- (Isopho-rone), N-formylpiperidine, and 2-(2-butoxyethoxy) ethanol. In addition, DBF, rubber/polymer additive was found at < 0.2 ng/cm2 and caprolactam, nylon-6 at < 0.6 ng/cm2. Reducing Organics: The Apollo program was the last sam-ple return mission to place high-level organic requirements and biological containment protocols on a curation facility. The high vacuum complex F-201 glovebox in the Lunar Receiving Labora-tory used ethyl alcohol (190 proof), 3:1 benzene/methanol (nano grade solution), and heat sterilization at 130degC for 48 hours to reduce organic contamination. In addition, both heat sterilization and peracetic acid sterilization were used in the atmospheric de-contamination (R) cabinets. Later, Lunar curation gloveboxes were degreased with a pressurized Freon 113 wash. Today, UPW has replaced Freon as the standard cleaning procedure, but does not have the degreasing solvency power of Freon. Future Cleaning Studies: Cleaning experiments are cur-rently being orchestrated to study how to degrease and reduce organics in a JSC curation glovebox lower than the established baseline. Several new chemicals in the industry have replaced traditional degreasing solvents such as Freon and others that are now federally restricted. However, these new suites of chemicals remain untested for lowering organics in curation gloveboxes. 3M's HFE-7100DL and DuPont's Vertrel XF are currently being tested as a replacement for Freon 113 as a degreaser at JSC cura-tion facilities. In addition, the use of UPW as a final rinse is be-ing tested, which presumably can maintain a lower total organic carbon load than the filtered purity of chemical solutions. References: [1] Allton J.H. et al. (2012) LPS XLIII, 2439; [2] Calaway M.

Calaway, M. J.↗

NASA NTRS2013

Cleaning Study of Genesis Sample 60487

The Genesis mission collected solar wind and brought it back to Earth in order to provide precise knowledge of solar isotopic and elemental compositions. The ions in the solar wind were stopped in the collectors at depths on the order of 10 to a few hundred nanometers. This shallow implantation layer is critical for scientific analysis of the composition of the solar wind and must be preserved throughout sample handling, cleaning, processing, distribution, preparation and analysis. Particles of Genesis wafers, brine from the Utah Testing Range and an organic film have deleterious effects on many of the high-resolution instruments that have been developed to analyze the implanted solar wind. We have conducted a correlative microscopic study of the efficacy of cleaning Genesis samples with megasonically activated ultrapure water and UV/ozone cleaning. Sample 60487, the study sample, is a piece of float-zone silicon from the B/C array approximately 4.995mm x 4.145 mm in size

Kuhlman, Kim R.↗

NASA NTRS2013

Application of CO2 Snow Jet Cleaning in Conjunction with Laboratory Based Total Reflection X-Ray Fluorescence

The Genesis mission was the first mission returning solar material to Earth since the Apollo program [1,2]. Unfortunately the return of the space craft on September 8, 2004 resulted in a crash landing, which shattered the samples into small fragments and exposed them to desert soil and other debris. Thus only small fragments of the original collectors are available, each having different degrees of surface contamination. Thorough surface cleaning is required to allow for subsequent analysis of solar wind material embedded within. An initial cleaning procedure was developed in coordination with Johnson Space Center which focused on removing larger sized particulates and a thin film organic contamination acquired during collection in space [3]. However, many of the samples have additional residues and more rigorous and/or innovative cleaning steps might be necessary. These cleaning steps must affect only the surface to avoid leaching and re-distribution of solar wind material from the bulk of the collectors. To aid in development and identification of the most appropriate cleaning procedures each sample has to be thoroughly inspected before and after each cleaning step. Laboratory based total reflection X-ray fluorescence (TXRF) spectrometry lends itself to this task as it is a non-destructive and surface sensitive analytical method permitting analysis of elements from aluminum onward present at and near the surface of a flat substrate [4]. The suitability of TXRF has been demonstrated for several Genesis solar wind samples before and after various cleaning methods including acid treatment, gas cluster ion beam, and CO2 snow jet [5 - 7]. The latter one is non-invasive and did show some promise on one sample [5]. To investigate the feasibility of CO2 snow jet cleaning further, several flown Genesis samples were selected to be characterized before and after CO2 snow application with sample 61052 being discussed below.

Schmeling, M.↗

NASA NTRS2013

Ultra Pure Water Cleaning Baseline Study on NASA JSC Astromaterial Curation Gloveboxes

Future sample return missions will require strict protocols and procedures for reducing inorganic and organic contamination in isolation containment systems. In 2012, a baseline study was orchestrated to establish the current state of organic cleanliness in gloveboxes used by NASA JSC astromaterials curation labs [1, 2]. As part of this in-depth organic study, the current curatorial technical support procedure (TSP) 23 was used for cleaning the gloveboxes with ultra pure water (UPW) [3-5]. Particle counts and identification were obtained that could be used as a benchmark for future mission designs that require glovebox decontamination. The UPW baseline study demonstrates that TSP 23 works well for gloveboxes that have been thoroughly degreased. However, TSP 23 could be augmented to provide even better glovebox decontamination. JSC 03243 could be used as a starting point for further investigating optimal cleaning techniques and procedures. DuPont Vertrel XF or other chemical substitutes to replace Freon- 113, mechanical scrubbing, and newer technology could be used to enhance glovebox cleanliness in addition to high purity UPW final rinsing. Future sample return missions will significantly benefit from further cleaning studies to reduce inorganic and organic contamination.

Calaway, Michael J.↗

NASA NTRS2013

Organic Contamination Baseline Study on NASA JSC Astromaterial Curation Gloveboxes

Future planned sample return missions to carbon-rich asteroids and Mars in the next two decades will require strict handling and curation protocols as well as new procedures for reducing organic contamination. After the Apollo program, astromaterial collections have mainly been concerned with inorganic contamination [1-4]. However, future isolation containment systems for astromaterials, possibly nitrogen enriched gloveboxes, must be able to reduce organic and inorganic cross-contamination. In 2012, a baseline study was orchestrated to establish the current state of organic cleanliness in gloveboxes used by NASA JSC astromaterials curation labs that could be used as a benchmark for future mission designs.

Calaway, Michael J.↗

NASA NTRS2013

Examples of Optical Assessment of Surface Cleanliness of Genesis Samples

Optical microscope assessment of Genesis solar wind collector surfaces is a coordinated part of the effort to obtain an assessed clean subset of flown wafer material for the scientific community. Microscopic survey is typically done at 50X magnification at selected approximately 1 square millimeter areas on the fragment surface. This survey is performed each time a principle investigator (PI) returns a sample to JSC for documentation as part of the established cleaning plan. The cleaning plan encompasses sample handling and analysis by Genesis science team members, and optical survey is done at each step in the process. Sample surface cleaning is performed at JSC (ultrapure water [1] and UV ozone cleaning [2]) and experimentally by other science team members (acid etch [3], acetate replica peels [4], CO2 snow [5], etc.). The documentation of each cleaning method can potentially be assessed with optical observation utilizing Image Pro Plus software [6]. Differences in particle counts can be studied and discussed within analysis groups. Approximately 25 samples have been identified as part of the cleaning matrix effort to date.

Rodriquez, Melissa C.↗

NASA NTRS2013

Laser Subdivision of the Genesis Concentrator Target Sample 60000

The Genesis Allocation Committee received a request for ~ 1 square centimeter of the diamond-like-carbon (DLC) concentrator target for the analysis of solar wind nitrogen isotopes. The target consists of a single crystal float zone (FZ) silicon substrate having a thickness on the order of 550 micrometers with a 1.5-3.0 micrometer-thick coating of DLC on the exposed surface. The solar wind is implanted shallowly in the front side DLC. The original target was a circular quadrant with a radius of 3.1 cm; however, the piece did not survive intact when the spacecraft suffered an anomalous landing upon returning to Earth on September 8, 2004. An estimated 75% of the DLC target was recovered in at least 18 fragments. The largest fragment, Genesis sample 60000, has been designated for this allocation and is the first sample to be subdivided using our laser scribing system Laser subdivision has associated risks including thermal diffusion of the implant if heating occurs and unintended breakage during cleavage. A careful detailed study and considerable subdividing practice using non-flight FZ diamond on silicon, DOS, wafers has considerably reduced the risk of unplanned breakage during the cleaving process. In addition, backside scribing reduces the risk of possible thermal excursions affecting the implanted solar wind, implanted shallowly in the front side DLC.

Lauer, Howard V., Jr.↗

NASA NTRS2012

Toward Lower Organic Environments in Astromaterial Sample Curation for Diverse Collections

Great interest was taken during the frenzied pace of the Apollo lunar sample return to achieve and monitor organic cleanliness. Yet, the first mission resulted in higher organic contamination to samples than desired. But improvements were accomplished by Apollo 12 [1]. Quarantine complicated the goal of achieving organic cleanliness by requiring negative pressure glovebox containment environments, proximity of animal, plant and microbial organic sources, and use of organic sterilants in protocols. A special low organic laboratory was set up at University of California Berkeley (UCB) to cleanly subdivide a subset of samples [2, 3, 4]. Nevertheless, the basic approach of handling rocks and regolith inside of a positive pressure stainless steel glovebox and restrict-ing the tool and container materials allowed in the gloveboxes was established by the last Apollo sample re-turn. In the last 40 years, the collections have grown to encompass Antarctic meteorites, Cosmic Dust, Genesis solar wind, Stardust comet grains and Hayabusa asteroid grains. Each of these collections have unique curation requirements for organic contamination monitor-ing and control. Here is described some changes allowed by improved technology or driven by changes in environmental regulations and economy, concluding with comments on organic witness wafers. Future sample return missions (OSIRIS-Rex; Mars; comets) will require extremely low levels of organic contamination in spacecraft collection and thus similarly low levels in curation. JSC Curation is undertaking a program to document organic baseline levels in current operations and devise ways to reduce those levels.

Allton, J. H.↗

NASA NTRS2012

Using Image Pro Plus Software to Develop Particle Mapping on Genesis Solar Wind Collector Surfaces

The continued success of the Genesis mission science team in analyzing solar wind collector array samples is partially based on close collaboration of the JSC curation team with science team members who develop cleaning techniques and those who assess elemental cleanliness at the levels of detection. The goal of this collaboration is to develop a reservoir of solar wind collectors of known cleanliness to be available to investigators. The heart and driving force behind this effort is Genesis mission PI Don Burnett. While JSC contributes characterization, safe clean storage, and benign collector cleaning with ultrapure water (UPW) and UV ozone, Burnett has coordinated more exotic and rigorous cleaning which is contributed by science team members. He also coordinates cleanliness assessment requiring expertise and instruments not available in curation, such as XPS, TRXRF [1,2] and synchrotron TRXRF. JSC participates by optically documenting the particle distributions as cleaning steps progress. Thus, optical document supplements SEM imaging and analysis, and elemental assessment by TRXRF.

Rodriquez, Melissa C.↗

NASA NTRS2011

Higher Magnification Imaging of the Polished Aluminum Collector Returned from the Genesis Mission

The polished aluminum collector (previously referred to as the polished aluminum kidney) was intended for noble gas analysis for the Gene-sis mission. The aluminum collector, fabricated from alloy 6061T, was polished for flight with alumina, then diamond paste. Final cleaning was performed by soak-ing and rinsing with hexane, then isopropanol, and last-ly megasonically energized ultrapure water prior to installation. It was mounted inside the collector canister on the thermal shield at JSC in 2000. The polished aluminum collector was not surveyed microscopically prior to flight.

Rodriquez, Melissa C.↗

NASA NTRS2011

Nuts and Bolts - Techniques for Genesis Sample Curation

The Genesis curation staff at NASA Johnson Space Center provides samples and data for analysis to the scientific community, following allocation approval by the Genesis Oversight Committee, a sub-committee of CAPTEM (Curation Analysis Planning Team for Extraterrestrial Materials). We are often asked by investigators within the scientific community how we choose samples to best fit the requirements of the request. Here we will demonstrate our techniques for characterizing samples and satisfying allocation requests. Even with a systematic approach, every allocation is unique. We are also providing updated status of the cataloging and characterization of solar wind collectors as of January 2011. The collection consists of 3721 inventoried samples consisting of a single fragment, or multiple fragments containerized or pressed between post-it notes, jars or vials of various sizes.

Burkett, Patti J.↗