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DOE OSTI2021

Characterization results for the 2020 tank farm 2H and 3H evaporator overhead samples

The 2020 annual 2H and 3H Evaporator overhead samples were received at Savannah River National Laboratory (SRNL) on December 22, 2020. The delivered samples were analyzed for concentration of cesium-137 ( 137 Cs), strontium-90 (90 Sr) and iodine-129 ( 129 I) to validate compliance with the Effluent Treatment Project Waste Acceptance Criteria (ETP WAC, Rev. 7). The concentration of all three radionuclides, 137 Cs, 90 Sr, and 129 I, in the 2H Evaporator overhead sample were found to be less than the corresponding ETP WAC limits. Radiochemical analysis of the 3H Evaporator overhead sample indicated a 137 Cs content about an order of magnitude higher than the acceptable threshold value, and 90 Sr and 129 I concentrations within the acceptance limits.

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DOE OSTI2022

Characterization Results for the April 2022 Tank Farm 2H Evaporator Overhead Sample

On an annual basis, Savannah River Mission Completion (SRMC) provides 2H and 3H evaporator overhead samples to Savannah River National Lab (SRNL) to be analyzed per Section 5.2 of the Effluent Treatment Project (ETP) Waste Compliance Plan (WCP) and the Waste Acceptance Criteria (WAC). This report presents characterization results for the April 2022 2H evaporator overhead sample. The sample was clear and colorless with no visible solids. The results provide measurements for cesium-137 ( 137 Cs), strontium-90 ( 90 Sr), and iodine-129 ( 129 I) with the radionuclide concentration limits specified by the WAC.

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DOE OSTI2023

Characterization Results for the March 2023 Tank Farm 2H Evaporator Overhead Sample

On an annual basis, Savannah River Mission Completion (SRMC) provides 2H and 3H evaporator overhead samples to Savannah River National Lab (SRNL) to be analyzed per Section 5.2 of the Effluent Treatment Project (ETP) Waste Compliance Plan (WCP) and the Waste Acceptance Criteria (WAC). This report presents characterization results for the March 2023 2H evaporator overhead sample. The sample was clear and colorless with no visible solids. The results provide measurements for cesium-137 ( 137 Cs), strontium-90 ( 90 Sr), and iodine-129 ( 129 I) with the radionuclide concentration limits specified by the WAC.

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DOE OSTI2020

Iodine Speciation Basis and Gap Analysis for Hanford Tank Farm Inventory and during Processing

Pacific Northwest National Laboratory (PNNL) is providing baseline technical support to Washington River Protection Solutions (WRPS) for the One System River Protection Project (RPP) Integrated Flowsheet team. This report documents the evaluation of the technical bases available to support iodine speciation and distribution within Hanford wastes and subsequent waste streams generated during direct feed low-activity waste (DFLAW) pretreatment operations (specifically, waste retrievals and staging, and particle filtration and cesium decontamination using crystalline silicotitanate (CST) ion exchange [in the tank side cesium removal (TSCR) system]. The task performed a literature survey of information related to iodine species in environments analogous to Hanford tank waste and the subsequent waste streams to define a technical basis for the possible iodine speciation in Hanford waste. In doing so it can be determined how likely laboratory studies on iodine speciation in tank waste are to be universally relevant across the Hanford tanks. The task evaluated iodide and iodate as the primary species of interest with a focus on organo-iodine where appropriate.

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DOE OSTI2020

Status of SRNL Radiological Field Lysimeter Experiment (RadFLEx) – Year 7

The Radiological Field Lysimeter Experiment (RadFLEx) began in 2012 and is a collaboration between the Savannah River National Laboratory (SRNL) and Clemson University. The purpose of this facility is to study the long-term (2 to 20 years) fate and transport of radionuclides in the Savannah River Site (SRS) vadose zone under natural field and meteorological conditions. The unique facility houses 48 5-L cores filled with sediments amended with various radionuclide sources. The results from these studies have been applied to the development of geochemical models used to assess the risk posed by subsurface nuclear waste disposal, environmental remediation, and waste form development. This report describes the refurbishment of the exterior of the RadFLEx facility and the synthesis and deployment of six plutonium(Pu) sources, four neptunium (Np) sources and one radium (Ra) source. It is anticipated that these newly installed lysimeter cores will be studied for up to 10 years.

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DOE OSTI2023

Luminescent group 1A copper halides and uses thereof

High photoluminescence, high stability, inorganic perovskite compounds comprising an alkali metal selected from potassium (K), rubidium (Rb), and cesium (Cs); copper (Cu); and at least one halogen selected from chlorine (Cl), bromine (Br), and iodine (I). The perovskites may be free of lead (Pb). The inorganic perovskite compound may be used in an optoelectronic device. The optoelectronic device optionally contains a phosphor such as a blue-emitting phosphor. The inorganic perovskite compound may be used as an anti-counterfeiting nanotaggant applied on or within an object that susceptible to counterfeiting to enable confirmation of an authentic object.

Saparov, Bayram↗

DOE OSTI2020

Crystalline Aluminosilicates for Radionuclide Remediation

Crystalline aluminosilicates have a wide range of applications such as media for the capture and/or immobilization of radionuclides. Several different types of metal-exchanged zeolites have been successfully demonstrated as effective sorbents for gaseous, aqueous, or solid-state capture and immobilization of radionuclides including iodine [e.g., I2(g), CH3I(g)], xenon, krypton, radium (e.g., 226Ra and 228Ra), selenium (e.g., 79Se6+), technetium (e.g., 99TcO4-), strontium (e.g., 90Sr2+), cesium (e.g., 135Cs+, 137Cs+), mixed alkali halide streams (i.e., iodide and chloride salts), and actinides (e.g., U6+, Th4+). These zeolites include sodalite (SOD), mordenite (MOR or Z-type), faujasite (FAU), Linde type-A (LTA), cancrinite (CAN), gismondine (GIS), and heulandite (or clinoptilolite) (HEU). The structural building blocks of these seven materials vary from cages (e.g., a-cages, ß-cages, e-cages) to channels linking various cage types and these are mostly comprised of aluminosilicates. This chapter will delve into the crystallographic differences between these framework materials and provide a brief overview of literature data where these seven crystalline aluminosilicates have been utilized for the capture and/or immobilization of radionuclides. Metal-exchanged zeolites (e.g., MOR, FAU, LTA) have often been the source of study for gaseous capture of iodine where the more promising compositions include Ag-exchanged sorbents; these types of materials can be made in a variety of robust forms including berl saddles and extrudates. Sodalite can be used as an immobilization strategy for halide waste streams (e.g., Cl, I), including those from electrochemical reprocessing of used nuclear fuel, as well as TcO4–. Cancrinite has been demonstrated to enhance sorption capacity of sediments for several problematic ionic radionuclides including Cs+, SeO42–, and TcO4–. Actinides such as U6+ and Th4+ have been successfully captured from solutions using MOR, FAU, LTA, and HEU-type aluminosilicates. Finally, mixtures of aluminosilicates have been included in a set of zeolite materials that show promise as sorbents for 226Ra and 228Ra removal from mine waters.

zeolites, aluminosilicates, radionuclide remediati↗

DOE OSTI2020

Verification of Special Nuclear Material (SNM) using Active Well Coincidence Counter (AWCC) and a High Purity Germanium (HPGe) Detector

SNM verification can be accomplished via two methods i.e. destructive analysis (DA) or nondestructive analysis (NDA). The DA modes are much more accurate compared to NDA modes; nevertheless, the sample's physical integrity is destroyed in the process. Techniques such as ICP-MS, ID-ICP-MS, TI-MS are few examples of DA, where a bulk material is ground and mixed with a solution (some form of acid) to acquire a homogenous sample. In contrast, NDA modes utilize signals emitted by the sample such as gamma, neutrons, light, or heat to analyze samples under investigation. HPGe detectors are some of the most frequently used gamma detectors to assay SNM. However, in a high activity scenario it provides a large uncertainty and sometimes becomes unfeasible to measure low energy gamma rays. Meanwhile, neutron detectors are not affected by the gamma background, therefore they can be used in addition to the gamma detectors to verify total fissile mass ({sup 235}U + {sup 239}Pu) of SNM. The AWCC is one of the thermal neutron NDA systems developed at the Los Alamos National Laboratory (LANL). It consists of 42 {sup 3}He detectors to measure gross neutrons (singles), coincidence neutrons (doubles), higher order multiplicity counting (triples, quadruples, etc.). It can effectively operate in both active and passive neutron interrogation modes. It can utilize AmLi, AmBe, or {sup 252}Cf active interrogation neutron sources. It is used to verify declared fissile mass ({sup 235}U or {sup 239}Pu) present in SNM. Objectives: Calibrate HPGe and AWCC for lightly irradiated (with enough {sup 137}Cs gamma background) ∼93% enriched HEU fuels; Verify fissile mass ({sup 235}U +{sup 239}Pu) content using AWCC and HPGe; Model and benchmark AWCC in MCNP6. Neutron coincidence and multiplicity counting: Two or more neutrons are coincident if they are detected by the system within the specified gate window; In AWCC: Gate window is 128 μsec; Induced fission in fissile material such as {sup 235}U and {sup 239}Pu - emission of time correlated neutrons - Singles, Doubles, Triples, or Quadruples; No induced fission in non-fissile materials- no correlated neutrons - only singles. SNM can be verified with high accuracy and precision using gamma and neutron NDA instruments such as HPGe and AWCC. Interaction with thermal neutrons. Non-fissile atoms - do not emit correlated neutrons. Fissile atoms - emit correlated neutrons during induced fission events. The time correlated neutrons can be detected by using coincidence or multiplicity counters such as AWCC. Likewise, {sup 235}U produces 186 keV gamma peak that can be measured by a HPGe gamma detector. Counts under 186 keV gamma peak provide information about {sup 235}U content. Combining AWCC and HPGe results can provide better understanding of special nuclear material under investigation.

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DOE OSTI2026

Photophysical Properties and Phase Behavior of Ultrawide Photovoltaic Bandgap Cesium–Lead-Based Triple Halide Perovskites

Metal halide perovskite films in the top cell of triple-junction tandems require bandgaps around 2.0 eV to achieve current matching, assuming that the middle absorbing layer is the commonly used FAPbI 3 composition and the bottom cell has a bandgap around 1.1 eV. Unfortunately, mixed organic/inorganic metal halide perovskites that have the necessary Br content to reach a bandgap of 2.0 eV segregate into iodine-rich and bromine-rich phases under illumination, limiting their obtainable voltage. Previous reports have shown improved photostability using either Cs-based inorganic compositions or Cl incorporation on the X-site. Here, we investigate the inorganic triple halide compositional space CsPb(I 1–x–y Br y Cl x ) 3 where bandgaps near 2.0 eV are expected based on the knowledge that CsPbI2Br has a bandgap of 1.90 eV. Incorporation of Cl occurs readily for x ≤ 0.07–0.10 within perovskites with a Br content of 0.3 ≤ y ≤ 0.42. When x >0.1, X-ray diffraction and photoluminescence (PL) measurements indicate that multiple compositional phases form. We hypothesize that the variable sizes of the three halide ions are not supported within the rigid Cs lattice, resulting in the formation of multiple compositional phases. The photoluminescence quantum yield of the single-phase compositional space–CsPb(I 1–x–y Br y Cl x ) 3 where x ≤ 0.07was typically 0.001–0.004%, most likely as a result of a high defect density, including mobile iodine species. PL light-soaking measurements of many perovskite compositions with bandgaps in the range of 1.89–2.05 eV demonstrate that phase segregation occurs when initial bandgaps are above 1.95 eV regardless of halide content: indicating further iodide oxidation and corresponding migration under illumination. The conclusion is that further compositional or additive engineering is necessary for the development of inorganic triple halide compositions that accomplish the elusive goal of fabricating high-quality and photostable 2.0 eV films for use in multijunction tandems.

Electrical conductivity↗

DOE OSTI2020

Iodine (I) Expulsion at Photoirradiated Mixed Halide Perovskite Interface. Should I Stay or Should I Go?

Visible light irradiation of the mixed halide perovskite film in contact with a solvent (dichloromethane, DCM) in which the film otherwise is stable, leads to selective expulsion of iodide (I) from the film with concurrent shift in the band edge to lower wavelengths. Here we have now employed mixed halide perovskites to uncover the influence of A-site cation (Methyl ammonium, MA and Cesium, Cs) on the mobility of iodide ions under photoirradiation. In the absence of solvent contact, the mixed halide perovskite films undergo photoinduced segregation with a rate constant that decreases with increasing Cs content. Interestingly, the iodide expulsion rate in DCM is strongly dependent on the rate of photoinduced segregation. At Cs atomic concentrations higher than 50%, the films become stable as the iodide expulsion is largely suppressed. The role of A-site cation in dictating the mobility of halide ions is discussed.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

DOE OSTI2020

Mechanisms of mechanochemical synthesis of cesium lead halides: pathways toward stabilization of α-CsPbI 3

Cesium lead iodide with cubic perovskite structure (α-CsPbI 3 ) is gaining significant interest in photovoltaic applications due to its excellent absorbance of the visible solar light and other attractive optoelectronic properties. However, the synthesis of stable α-CsPbI 3 poses a significant challenge. Mechanochemical synthesis is emerging as a suitable method for the preparation of cesium lead halides. This work investigates the ball milling-induced synthesis of cesium lead halides perovskite phase using halide mixing or doping approaches. The synthesis in the CsI + PbI 2 , CsBr + PbBr 2 , CsBr + PbI 2 , and CsI + PbI 2 + NdI 3 mixtures and halide exchange reactions in the CsPbBr 3 + 3KI and CsBr + PbBr 2 + 3KI systems are investigated to elucidate the mechanism of this process. Then, CsPb(I 1–x Br x ) 3 and CsPb( 1–y )Nd y I 3 materials with different x and y ratios are prepared, and their stability is probed in the air using light absorption spectroscopy. These results suggest that Nd doping is more efficient in the stabilization of the perovskite structure than partial replacement of iodine with bromine. Microstructure observations reveal the existence of two different product formation mechanisms depending on the mechanical properties of reactants. The results reveal that the milling temperature has a significant impact on the reaction kinetics. Here, the produced particles nucleate and grow at the reactant interface and retard the synthesis reaction by creating a diffusion barrier. Extended milling reduces the product particle size and creates fresh contact between reactants, thus facilitating reaction completion.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Vitrification of Hanford Tank Wastes for Condensate Recycle and Feed Composition Changeover Testing

During the vitrification of Hanford Site nuclear waste at the Waste Treatment and Immobilization Plant (WTP), which is a part of the safe and efficient retrieval, treatment, and disposal mission of the U.S. Department of Energy Office of River Protection, the offgas condensate generated from the waste-to-glass conversion is currently planned to be concentrated by evaporation in the Effluent Management Facility (EMF). This concentrated condensate can then be recycled back to the incoming waste and vitrified. To test the recycle process, an apparatus was designed and built to mimic the EMF evaporator and was then used to concentrate a volume of condensate produced during the vitrification of a sample of Hanford tank 241-AP-107 (referred to herein as AP-107) waste in a continuous laboratory-scale melter (CLSM). The concentrated condensate was added to an additional sample of AP-107 waste, to mimic one round of the recycle process, and the combined solution was vitrified, producing a second round of recycle condensate. In the current study, the EMF test apparatus was used to concentrate the second-round recycle condensate under evaporation conditions (at 45 °C and 1.4 psia) designed to emulate EMF operation. The condensate was successfully concentrated by a factor of ~10 while retaining over 95 % of the technetium-99 ( 99 Tc), Cs, and I inventories in the concentrate. Another portion of AP-107 waste was retrieved by Washington River Protection Solutions, LLC (WRPS) and transferred to Pacific Northwest National Laboratory (PNNL), where it was pretreated and then combined with the second-round recycle AP-107 condensate concentrate and glass-forming chemicals (GFCs) to form the two-time recycle AP-107 melter feed, approximating a second round to the recycling action to be performed at the WTP. A portion of AP-105 waste was also retrieved by WRPS and provided to PNNL for pretreatment and combining with GFCs to form AP-105 melter feed. The two-time recycle AP-107 and AP-105 melter feeds were processed consecutively in the CLSM. The CLSM run proceeded for 13.63 hours, producing 9.70 kg of glass for an average glass production rate of 1464 kg m 2 d -1 during the two-time recycle AP-107 feed charging and 1568 kg m 2 d -1 during the AP-105 feed charging. The rate during AP-107 charging was essentially equivalent to the rate when processing no-recycle AP-107 feed and lower than that achieved when processing one-time recycle AP-107 feed. However, all rates were within the potential range of variability when processing melter feeds with similar composition in the CLSM. Likewise, the rate during AP-105 charging was higher than the previous rate processing AP-105, but within the potential CLSM range. The cold-cap characteristics changed from the typically thin AP-107 cold cap to a foamy-edged cold cap as previously seen with AP-105 shortly after transitioning to the AP-105 melter feed. The glass produced during the CLSM run was within 10 % of its target composition for the primary glass components. The CaO and Li 2 O targets varied by more than 1 wt% between the two-time recycle AP-107 and AP-105 glass targets and it took about 2 turnovers of the CLSM glass inventory to reach a relative chemical steady state in the glass for CaO and Li 2 O after the melter feed inputs were switched. The 99 Tc and total cesium content in the melter feeds were maintained at concentrations expected to be experienced at the WTP. During the CLSM run, while processing the two-time recycle AP-107 melter feed at a relative chemical steady state, the 99 Tc/Cs ratio was 10, and 34% of 99 Tc and 74% of Cs were retained in the glass. These values were higher than those measured in the CLSM run with one-time recycle AP-107 melter feed. After the transition to processing the AP-105 melter feed, when the production reached a relative chemical steady state, the 99 Tc/Cs ratio was 77 while 44% of 99 Tc was retained in the glass. The C's retention during this time frame reached 200% due to the excess C's in the glass after the target content decreased to 15% of its initial level in the two-time recycle AP-107 melter feed to the lower target in the Ap-105 melter feed. While iodine was below inductively coupled plasma mass spectrometry analytical reporting limits in the melter feed and glass samples, it was detected in quantities above the analytical reporting limits in the liquid and filter samples collected from the CLSM offgas treatment system. The behavior of iodine in the CLSM offgas treatment system followed a similar pattern to those of 99 Tc and Cs.

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