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NASA NTRS2012

Curiosity: the Mars Science Laboratory Project

The Curiosity rover landed successfully in Gale Crater, Mars on August 5, 2012. This event was a dramatic high point in the decade long effort to design, build, test and fly the most sophisticated scientific vehicle ever sent to Mars. The real achievements of the mission have only just begun, however, as Curiosity is now searching for signs that Mars once possessed habitable environments. The Mars Science Laboratory Project has been one of the most ambitious and challenging planetary projects that NASA has undertaken. It started in the successful aftermath of the 2003 Mars Exploration Rover project and was designed to take significant steps forward in both engineering and scientific capabilities. This included a new landing system capable of emplacing a large mobile vehicle over a wide range of potential landing sites, advanced sample acquisition and handling capabilities that can retrieve samples from both rocks and soil, and a high reliability avionics suite that is designed to permit long duration surface operations. It also includes a set of ten sophisticated scientific instruments that will investigate both the geological context of the landing site plus analyze samples to understand the chemical & organic composition of rocks & soil found there. The Gale Crater site has been specifically selected as a promising location where ancient habitable environments may have existed and for which evidence may be preserved. Curiosity will spend a minimum of one Mars year (about two Earth years) looking for this evidence. This paper will report on the progress of the mission over the first few months of surface operations, plus look retrospectively at lessons learned during both the development and cruise operations phase of the mission..

project formulation↗

DOE OSTI2020

Sampling and Analysis Plan for Investigation of Undeclared Nuclear Activities - 20104

The nuclear-centered energy policy in South Korea is moving towards a nuclear-free era. It also facilitates an action or progress on the denuclearization of the Korean peninsula. The Nuclear Safety and Security Commission (NSSC) launched a new R and D project which attempts to verify nuclear activities via analyzing environmental samples. Environmental samples possibly contain significant radiological information relevant to past undeclared activities. In order to precisely verify them, it is essential to provide 1) the concrete information of target facilities, 2) appropriate methodologies and procedures, and 3) well-suited instrumentation and equipment corresponding to sample signatures. It is also important to provide scientific reliability or validity in any process such as sample collection, handling, transportation and laboratory analysis. Therefore, the information of nuclear facilities (fuel fabrication plant, graphite moderated reactor, reprocessing plant) in North Korea are reviewed in order to determine parameters for appropriate sampling methods representing a facility's characteristics. Secondly, a sampling procedure for radioactive elements is being developed based on international and domestic standards such as ASTM (American Society for Testing and Materials), KS (Korean industrial Standards), and International Atomic Energy Agency (IAEA) manuals. The procedure contains some specific information including sampling process, sampling tools, amount of sample, sample identification, and other related information. Developing the qualified national guidelines is most important since sampling and analyzing results can be used as evidences of nuclear activities. The guideline developed through this work will clearly define various methodologies such as document verification, sampling procedures, collection methods, sample storage criteria, chain of custody, and transportation conditions. The final objective of this work is to establish the infrastructure and regulatory framework for assessment of nuclear activities, and provide a national guideline for sampling and analysis. This will bring confidence in the results and play a critical role in complete denuclearization progress in South Korea. (authors)

98 NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL P↗

DOE OSTI2015

Improving public communication through environmental data transparency at Los Alamos National Laboratory - 15306

The Los Alamos National Laboratory (LANL) environmental data span a wide range of media, including air, soil, sediment, water, foodstuff, and biota as well as over 1000 analytes and time periods extending over 4 decades, resulting in over 14 million records to manage and analyze. At a time of budget cuts and rapid social and technological change, the public, regulatory and compliance agencies, and stakeholders demand accelerated data delivery and efficiency, information sharing, and transparency in the dissemination and handling of samples collected in and around LANL. Meeting these requirements, while constraining the associated costs can be challenging; however, LANL has achieved this by adopting a cloud-based database called the Environmental Information Management (EIM) system and its public database counterpart, IntellusNM (Intellus) (www.intellusnm.com). To be consistent with federal initiatives to move government computing into cloud-based services, LANL chose to partner with an existing cloud-based vendor, Locus Technologies, to implement a software-as-a-service model. As an additional cost-saving measure, local regulatory and compliance agencies collaborated with LANL to incorporate their data into EIM and Intellus database. By adopting a single platform cloud-based solution to replace 12 different pre-existing environmental data systems, LANL has streamlined environmental data processes, resulting in over $15 million cost savings through 2015. EIM, LANL's internal cloud database, provides a cradle-to-grave process for data handling. EIM supports LANL's entire data process from detailed sample planning, mobile data collection using iOS mobile devices, to automated bottle labeling, generation of chain of custody, analytical lab electronic data deliverable upload, auto data validation, sample tracking, and custom regulatory and compliance reports. EIM has functionality to assess data in various ways such as the ability to design new formatted reports, a free-form structured query language tool of the entire database, exceedance reports, calculation engine, charting, trends, and statistics. EIM also has interactive geographic information system layers and analyte concentration color contour mapping capabilities. Additionally, and of greater importance to LANL, EIM supports the ability for third-party landowners to review data before release to the public, thus ensuring transparency and confidence in LANL's stewardship of human health and the environment. Intellus, the database counterpart of EIM, is the publicly available view of the entire LANL database and requires no data feeds or transformations. Intellus allows user-friendly access to LANL's environmental data as it is collected, providing the public, scientists, remediation teams, regulators, and stakeholders within hours of receipt. Full transparency in giving the public access to environmental data information provides LANL's overall solution to environmental data management for the public. By making the data easy to obtain, search, and query for interested stakeholders, the system enables confidence in LANL's stewardship of the environment. Working together identifies key topics of improvements, develop strategies and help support innovation and substantial advances within LANL's environmental data management system. (authors)

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2019

Solving Operational Challenges with INL's Integrated Waste Treatment Unit (IWTU) - 19003

In 2005, the THOR steam reforming fluidized-bed reactor technology was selected by the U.S. Department of Energy for treatment of sodium-bearing waste at the INL. The initial commissioning was typical, until June of 2012 when an over-pressurization event resulted in a significant release of solids. Recovery and subsequent testing systematically dealt with challenges associated with operation of three primary vessels: the denitration and mineralization reformer, the process gas filter, and the carbon reduction reformer. Additional challenges with the following ancillary systems surfaced during testing: the auger/grinder, sample system, and the approach to decontamination of the process vessels prior to outages. The major operational challenges covered fluidization issues, premature refractory failure, high-temperature gaseous filter element blinding, cementitious material formation in solids handling equipment, sampling reliability, and vessel decontamination. The purpose of this paper is to share the lessons learned during the extended commissioning of the Integrated Waste Treatment Unit. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

NASA NTRSDate not supplied

Hydrogen Peroxide as a Method for Bioburden Reduction in Facilities with Strict Materials Requirements.

The cleanrooms used to curate NASA’s Astromaterials samples are carefully monitored for particulate and inorganic contamination. The clean labs also have a very limited set of acceptable materials and cleaning agents to further minimize the potential for contamination. Labs are cleaned primarily with isopropyl alcohol. Astromaterials samples are handled with tools made of stainless steel (304 or 316), Teflon, or aluminum alloy (6061). Although our current collections are not particularly susceptible to biological alteration or organic contamination, this will not be the case for new collections from the OSIRIS-REx mission, Hayabusa2, and from Mars Sample Return. Therefore, it is necessary to develop and test methods to reduce the bioburden in astromaterials cleanrooms without introducing unwanted contaminants. We will report on the results of three case studies where 7.5 wt% hydrogen peroxide was prepared from a stock solution of ultrapure 30 wt% hydrogen peroxide (JT Baker) using curation-grade ultrapure water. We followed CDC (Center for Disease Control) guidelines for using hydrogen peroxide as a high level disinfectant. This solution was used to clean a glovebox prior to processing Apollo samples, as well as surfaces in the Antarctic meteorite processing lab and Stardust lab after facilities monitoring indicated an unwanted increase in bioburden. In all three instances, the culturable bioburden was significantly reduced after a 30 min. exposure to the 7.5% hydrogen peroxide solution without a corresponding increase in inorganic or organic contamination. We observed 77 to 100% reductions in the bioburden recovery rate. In one case study, we also performed amplicon DNA sequencing on samples collected from the surfaces before and after cleaning. We observed a significant change in microbial community composition after peroxide cleaning. These results suggest that routine cleaning with hydrogen peroxide could be an effective way to control bioburden in astromaterials cleanrooms and other facilities with strict contamination control requirements.

A B Regberg↗

NASA NTRSDate not supplied

Hydrogen Peroxide as a Method for Bioburden Reduction in Facilities with Strict Materials Requirements

A B Regberg↗

DOE OSTI2020

Design of a Biomass Scale Cubical Triaxial Tester

The bioenergy industry is dependent on predictable and reliable feedstock handling equipment. High profile failures in the industry demonstrate the need for better modeling tools for feedstock handling, specifically tools which can model the bulk flow of biomass feedstock materials in handling equipment such as hoppers or screw conveyors. Measurement of bulk material flow characteristics is a critical component to inform modeling tools. Following examples in the soils and pharmaceuticals industries, a Cubical Triaxial Tester (CTT) was selected as a critical component to study relationships between applied stress on a bulk sample and the resulting strain on the bulk material. In cooperation with The Pennsylvania State University, Forest Concepts designed a CTT specifically to measure bulk biomass flowability characteristics. Several mechanical design constraints were identified to ensure proper scaling and repeatability. Major design constraints included sample chamber size versus particle length, volumetric strain sensing accuracy, independent axial pressure control, and sample chamber handling. This report explains how major design constraints were determined.

09 BIOMASS FUELS↗

DOE OSTI2012

Small-Scale Testing of Plutonium(IV) Oxalate Precipitation and Calcination to Plutonium Oxide to Support the MOX Feed Mission

The H-Canyon facility will be used to dissolve Pu metal for subsequent purification and conversion to plutonium dioxide (PuO 2 ) using Phase II of HB-Line. To support the new mission, SRNL conducted a series of experiments to produce calcined plutonium (Pu) oxide and measure the physical properties and water adsorption of that material. This data will help define the process operating conditions and material handling steps for HB-Line. An anion exchange column experiment produced 1.4 L of a purified 52.6 g/L Pu solution. Over the next nine weeks, seven Pu(IV) oxalate precipitations were performed using the same stock Pu solution, with precipitator feed acidities ranging from 0.77 M to 3.0 M nitric acid and digestion times ranging from 5 to 30 minutes. Analysis of precipitator filtrate solutions showed Pu losses below 1% for all precipitations. The four larger precipitation batches matched the target oxalic acid addition time of 44 minutes within 4 minutes. The three smaller precipitation batches focused on evaluation of digestion time and the oxalic acid addition step ranged from 25-34 minutes because of pump limitations in the low flow range. Following the precipitations, 22 calcinations were performed in the range of 610 – 690 °C, with the largest number of samples calcined at either 650 or 635 °C. Characterization of the resulting PuO 2 batches showed specific surface areas in the range of 5-14 m 2 /g, with 16 of the 22 samples in the range of 5-10 m 2 /g. For samples analyzed with typical handling (exposed to ambient air for 15-45 minutes with relative humidities of 20-55%), the moisture content as measured by Mass Spectrometry ranged from 0.15 to 0.45 wt % and the total mass loss at 1000 °C, as measured by TGA, ranged from 0.21 to 0.58 wt %. For the samples calcined between 635 and 650 °C, the moisture content without extended exposure ranged from 0.20 to 0.38 wt %, and the TGA mass loss ranged from 0.26 to 0.46 wt %. Of these latter samples, the samples calcined at 650 °C generally had lower specific surface areas and lower moisture contents than the samples calcined at 635 °C, which matches expectations from the literature. Taken together, the TGA-MS results for samples handled at nominally 20-50% RH, without extended exposure, indicate that the Pu(IV) oxalate precipitation process followed by calcination at 635-650 °C appears capable of producing PuO 2 with moisture content < 0.5 wt % as required by the 3013 Standard. Exposures of PuO 2 samples to ambient air for 3 or more hours generally showed modest mass gains that were primarily gains in moisture content. These results point to the need for a better understanding of the moisture absorption of PuO 2 and serve as a warning that extended exposure times, particularly above the 50% RH level observed in this study will make the production of PuO 2 with less than 0.5 wt % moisture more challenging. Samples analyzed in this study generally contained approximately 2 monolayer equivalents of moisture. In this study, the bulk of the moisture released from samples below 300 °C, as did a significant portion of the CO 2 . Samples in this study consistently released a minor amount of NO in the 40-300 °C range, but no samples released CO or SO 2 . TGA-MS results also showed that MS moisture content accounted for 80±8% of the total mass loss at 1000 °C measured by the TGA. The PuO 2 samples produced had particles sizes that typically ranged from 0.2 – 88 μm, with the mean particle size ranging from 6.4 – 9.3 μm. The carbon content of ten different calcination batches ranged from 190-480 μg C/g Pu, with an average value of 290 μg C/g Pu.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRSDate not supplied

Rapid Nucleic Acid Isolation Method and Fluid Handling Devices Overview

Sample preparation is a common bottleneck in genetic analysis. Tools that reduce time and effort are of value in a laboratory setting. There is a need for a genetic analysis/detection system that is not only mobile, ruggedized, easy-to-use but also provides an enclosed fluid handling that diminishes the risks of Ribonucleic acid (RNA) contamination and degradation during processing. NASA has developed a novel assay methodology and suite of devices to isolate nucleic acids and prepare samples for real-time (quantitative) polymerase chain reaction (PCR) analysis that solves the problem of contamination and degradation because of the advanced microfluidics which provides better fluid handling. The assay employs an aqueous-based non-alcohol method that yields robust RNA quality. The suite of ready-to-use devices provide pre-loaded reagents in liquid and lyophilized formats to enable rapid, cost effective, and portable manual operation in the laboratory or remote field environments.

Travis Boone↗

DOE OSTI2011

Examination of core samples from the Mount Elbert Gas Hydrate Stratigraphic Test Well, Alaska North Slope: Effects of retrieval and preservation

Collecting and preserving undamaged core samples containing gas hydrates from depth is difficult because of the pressure and temperature changes encountered upon retrieval. Hydrate-bearing core samples were collected at the BPXA-DOE-USGS Mount Elbert Gas Hydrate Stratigraphic Test Well in February 2007. Coring was performed while using a custom oil-based drilling mud, and the cores were retrieved by a wireline. The samples were characterized and subsampled at the surface under ambient winter arctic conditions. Samples thought to be hydrate bearing were preserved either by immersion in liquid nitrogen (LN), or by storage under methane pressure at ambient arctic conditions, and later depressurized and immersed in LN. Eleven core samples from hydrate-bearing zones were scanned using x-ray computed tomography to examine core structure and homogeneity. Features observed include radial fractures, spalling-type fractures, and reduced density near the periphery. These features were induced during sample collection, handling, and preservation. Isotopic analysis of the methane from hydrate in an initially LN-preserved core and a pressure-preserved core indicate that secondary hydrate formation occurred throughout the pressurized core, whereas none occurred in the LN-preserved core, however no hydrate was found near the periphery of the LN-preserved core. To replicate some aspects of the preservation methods, natural and laboratory-made saturated porous media samples were frozen in a variety of ways, with radial fractures observed in some LN-frozen sands, and needle-like ice crystals forming in slowly frozen clay-rich sediments. Suggestions for hydrate-bearing core preservation are presented.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2016

Characterization of Fresh Nuclear Fuel using Time-Of-Flight Neutrons

Neutrons offer excellent characterization capabilities for nuclear fuels and can provide non-destructive insight on micro structure, chemistry and crystallographic phase. Measurements are possible at reactors or pulsed sources, but the inherent energy resolution implicit at pulsed sources offers unique opportunities. Recent advances in 2D neutron detection enabled new capabilities of material characterization using neutron imaging and tomography for nuclear materials. Moreover, time-of-flight (TOF) neutron measurements can enable isotope specific tomography by deriving isotope densities from transmission spectra exhibiting neutron resonances, which are recorded for each pixel. Tomographic algorithms allow 3D reconstructions of the spatial distribution of isotopes, density and features in typical fuel pellet samples. The ability to select radiographs for different energies allows characterizing samples which are opaque for thermal neutrons, such as enriched fuels or fuels containing plutonium, by selecting epi-thermal neutron energies and by knowledge of the total neutron cross sections of the constituents, isotopic enrichment levels can be determined. Nuclear cross sections are typically not calculated directly and databases such as the Evaluated Nuclear Data File (ENDF) database provide this information with cross sections determined by standardized experimental measurements, such as neutron transmission measurements for individual isotopes. Utilizing the information in the ENDF database, the 'inverse' problem can be solved by assuming cross section parameters to be known parameters and areal densities can be determined. This work presents recent advances at the Los Alamos Neutron Science Center (LANSCE) facility at Los Alamos National Laboratory (LANL), which provides the infrastructure to handle radioactive samples, in the development of fuel characterization with TOF neutrons. Examples include recent work on prototype accident tolerant nuclear fuels (ATF). The potential application of these techniques for nondestructive examination of irradiated fuel is under consideration. Non-destructive access to materials features for specimens embedded in containers, particularly for hazardous samples, such as a radioactive nuclear fuel, is indispensable to characterize and ultimately license new fuel forms. Energy-resolve neutron imaging is a new tool for this research field. The results reported here present a new imaging technique, setting a milestone in the capabilities of measuring non-destructively absolute quantities of physical properties. The enabling physics behind this new technique are nuclear resonances. We have demonstrated how absolute areal densities can be extracted from radiographs utilizing pulsed neutron sources. This technique provides information that is otherwise difficult and costly to obtain. In the case of nuclear fuels, the results from energy-dispersive neutron imaging may guide destructive examination of irradiated fuel. This summery does not describe recent analysis, which is ongoing. Particularly, the implementation of calibration standards has improved the determination of enrichment levels without additional calibration. The analysis of the samples was performed with full tomographic reconstructions for isotope specific data and presents a first approach in absolute isotope specific 3D reconstruction. This work was predominantly funded by and received substantial support from the Fuel Cycle R and D program at Los Alamos National Laboratory. (authors)

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2019

Intercomparison of the Radio-Chronometric Ages of Plutonium-Certified Reference Materials with Distinct Isotopic Compositions

In this article, an intercomparison of the radio-chronometric ages of four distinct plutonium-certified reference materials varying in chemical form, isotopic composition, and period of production are presented. The cross-comparison of the different 234 U/ 238 Pu, 235 U/ 239 Pu, 236 U/ 240 Pu, and 241 Am/ 241 Pu model purification ages obtained at four independent analytical facilities covering a range of laboratory environments from bulk sample processing to clean facilities dedicated to nuclear forensic investigation of environmental samples enables a true assessment of the state-of-practice in “age dating capabilities” for nuclear materials. The analytical techniques evaluated used modern mass spectrometer instrumentation including thermal ionization mass spectrometers and inductively coupled plasma mass spectrometers for isotopic abundance measurements. Both multicollector and single collector instruments were utilized to generate the data presented here. Consensus values established in this study make it possible to use these isotopic standards as quality control standards for radio-chronometry applications. Results highlight the need for plutonium isotopic standards that are certified for 234 U/ 238 Pu, 235 U/ 239 Pu, 236 U/ 240 Pu, and 241 Am/ 241 Pu model purification ages as well as other multigenerational radio-chronometers such as 237 Np/ 241 Pu. Due to the capabilities of modern analytical instrumentation, analytical laboratories that focus on trace level analyses can obtain model ages with marginally larger uncertainties than laboratories that handle bulk samples. Lastly, when isotope ratio measurement techniques like thermal ionization mass spectrometry and inductively coupled plasma mass spectrometry with comparable precision are utilized, model purification ages with similar uncertainties are obtained.

36 MATERIALS SCIENCE↗

DOE OSTI2018

System Integration for Remote Systems at DOE Hanford Nuclear Site - 18712

The deployment of remotely operated technology that functions in environments too hazardous for worker entry are often needed at the Hanford Site to perform functions like infrastructure inspection; decommissioning and decontamination; characterization; environmental sampling; and nuclear waste sampling, mobilization, and retrieval. The development and production of Hanford remote systems typically requires the integration of robotic components and sensor technologies that have been engineered or adapted to meet function and performance requirements. Pacific Northwest National Laboratory has led the engineering and integration of robotic and sensor/manipulator technology for several remote system deployments at Hanford and for national security sponsors. This paper describes the system integration process for ensuring that the mechanical, electrical, and software aspects of each component are successfully brought together to produce a remote system that meets function and performance requirements under extreme environments and limited-access operational demands. A brief summary of previous and current remote system projects is also provided. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

NASA NTRS2012

Rotary Percussive Sample Acquisition Tool (SAT): Hardware Development and Testing

In support of a potential Mars Sample Return (MSR) mission an Integrated Mars Sample Acquisition and Handling (IMSAH) architecture has been proposed to provide a means for Rover-based end-to-end sample capture and caching. A key enabling feature of the architecture is the use of a low mass sample Acquisition Tool (SAT) that is capable of drilling and capturing rock cores directly within a sample tube in order to maintain sample integrity and prevent contamination across the sample chain. As such, this paper will describe the development and testing of a low mass rotary percussive SAT that has been shown to provide a means for core generation, fracture, and capture.

Integrated Mars Sample Acquisition and Handling (I↗

DOE OSTI2017

Advances in containment methods and plutonium recovery strategies that led to the structural characterization of plutonium(IV) tetrachloride tris-diphenylsulfoxide, PuCl 4 (OSPh 2 ) 3

In an attempt to further advance the understanding of plutonium coordination chemistry, we report a robust method for recycling and obtaining plutonium aqueous stock solutions that can be used as a convenient starting material in plutonium synthesis. This approach was used to prepare and characterize plutonium(IV) tetrachloride tris-diphenylsulfoxide, PuCl 4 (OSPh 2 ) 3 , by single crystal X-ray diffraction. The PuCl 4 (OSPh 2 ) 3 compound represents a rare example of a 7-coordinate plutonium(IV) complex. Structural characterization of PuCl 4 (OSPh 2 ) 3 by X-ray diffraction utilized a new containment method for radioactive crystals. The procedure makes use of epoxy, polyimide loops, and a polyester sheath to provide a robust method for safely containing and easily handling radioactive samples. Lastly, the described procedure is more user friendly than traditional containment methods that employ fragile quartz capillary tubes. Additionally, moving to polyester, instead of quartz, lowers the background scattering from the heavier silicon atoms.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

DOE OSTI2021

Pushing the limits of high-resolution polymer microscopy using antioxidants

High-resolution transmission electron microscopy (HRTEM) has been transformative to the field of polymer science, enabling the direct imaging of molecular structures. Although some materials have remarkable stability under electron beams, most HRTEM studies are limited by the electron dose the sample can handle. Beam damage of conjugated polymers is not yet fully understood, but it has been suggested that the diffusion of secondary reacting species may play a role. As such, we examine the effect of the addition of antioxidants to a series of solution-processable conjugated polymers as an approach to mitigating beam damage. Characterizing the effects of beam damage by calculating critical dose D c values from the decay of electron diffraction peaks shows that beam damage of conjugated polymers in the TEM can be minimized by using antioxidants at room temperature, even if the antioxidant does not alter or incorporate into polymer crystals. As a consequence, the addition of antioxidants pushes the resolution limit of polymer microscopy, enabling imaging of a 3.6Å lattice spacing in poly[(5,6-difluoro-2,1,3-benzothiadiazol-4,7-diyl)-alt-(3,3"-di(2-octyldodecyl)-2,2';5',2";5",2"-quaterthiophene-5,5"-diyl)] (PffBT4T-2OD).

36 MATERIALS SCIENCE↗

DOE OSTI2019

Quantitative infrared spectroscopy of environmentally sensitive and rough materials

Fourier transform infrared (FTIR) spectroscopy is a widely used characterization technique for studying chemical compositions and lightmatter interactions in the infrared range. However, it remains challenging to use conventional FTIR equipment to characterize materials that are environmentally sensitive and/or have rough surfaces due to their dynamic response to external stimuli (e.g., humidity) and light scattering from the sample surface. Here, we describe an approach enabling quantitative infrared spectroscopy measurements of these challenging samples, including transmittance, reflectance, and emissivity. We designed and 3D-printed a miniaturized environmental chamber that can be directly inserted into the sample holder of a conventional integrating sphere to perform total transmission and reflection measurements in controlled environments. Moreover, a calibration method was developed to exclude light scattering from rough surfaces of the sample and the distortion created by infrared windows. To illustrate the potential application of this method, we have performed quantitative infrared measurements, both specular and diffusive, on a sapphire standard reference with a specular surface, as well as a textile sample that has a rough surface and is dynamically responsive to changes in humidity. The calibrated results measured with the equipped chamber match those measured without the IR windows, demonstrating the viability of our environmental chamber and the proposed calibration method. This quantitative infrared spectroscopy measurement technique may help advance fields such as metasurfaces and adaptive textiles, where samples are often rough, dynamically responsive, and/or environmentally sensitive.

3D printing↗

DOE OSTI2019

Structure and Photophysics of Indigoids for Singlet Fission: Cibalackrot

Here, we report an investigation of structure and photophysics of thin layers of cibalackrot, a sturdy dye derived from indigo by double annulation at the central double bond. Evaporated layers contain up to three phases, two crystalline and one amorphous. Relative amounts of all three have been determined by a combination of X-ray diffraction and FT-IR reflectance spectroscopy. Initially, excited singlet state rapidly produces a high yield of a transient intermediate whose spectral properties are compatible with charge-transfer nature. This intermediate more slowly converts to a significant yield of triplet, which, however, does not exceed 100% and may well be produced by intersystem crossing rather than singlet fission. The yields were determined by transient absorption spectroscopy and corrected for effects of partial sample alignment by a simple generally applicable procedure. Formation of excimers was also observed. Here, in order to obtain guidance for improving molecular packing by a minor structural modification, calculations by a simplified frontier orbital method were used to find all local maxima of singlet fission rate as a function of geometry of a molecular pair. The method was tested at 48 maxima by comparison with the ab initio Frenkel-Davydov exciton model.

14 SOLAR ENERGY↗