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All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Ligand substituents modulate excited-state lifetime and energy-transfer reactivity in Cu( I ) photosensitizers supported by salicylaldimine and isocyanide ligands

The design of earth-abundant molecular photosensitizers with desirable photophysical properties and good excited-state reactivity is critical for sustainable photochemical applications. Herein, we report a new family of three-coordinate heteroleptic Cu(I) complexes supported by monoanionic salicylaldimine (N^O) chelating ligands and aryl isocyanides. By systematically tuning the steric bulk on each ligand, we establish clear structure–property relationships that govern the excited-state lifetimes and photocatalytic performance metrics of these complexes. Increasing steric congestion on the salicylaldimine ligand, which contributes to the HOMO, results in faster nonradiative decay and shortens excited-state lifetimes. In contrast, introducing steric bulk on the isocyanide ligand, where the LUMO is primarily localized, suppresses nonradiative decay, most likely by inhibiting excited-state geometric relaxation, thereby extending the lifetime up to 375 ns. These photophysical trends correlate directly with performance in triplet–triplet energy transfer (TTET) photocatalysis, where longer-lived complexes enable faster E/Z isomerization of trans-stilbene. This work demonstrates that remote steric modulation of ligand frameworks offers a simple yet powerful strategy for tuning the excited-state dynamics and catalytic properties of this new class of Cu(I) photosensitizers.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Welch Method and Bootstrapping Applied to Subcritical Gamma Noise

We measured the prompt neutron decay constant 𝛼 of the CROCUS zero-power reactor at the Swiss Federal Institute of Technology Lausanne using cross-power spectral density (CPSD) analysis of gamma-gamma correlations from two trans-stilbene organic scintillators positioned near the reactor core. We measured critical and subcritical states, with water levels ranging from 960 mm (critical) to 800 mm (𝜌=−1.4 $ subcritical). Our analysis used the Welch method, dividing signal segments for fast Fourier transform (FFT) frequency analysis and applying bootstrapping uncertainty quantification that uses Welch-defined segments. Results demonstrated a clear increase in the measured 𝛼 as reactor reactivity decreased, distinguishing critical from subcritical conditions. At the 960-mm critical level, 𝛼 was estimated at 155.9 ± 0.7 s −1 , and for the 800-mm subcritical level, 𝛼 increased significantly to 367.3 ± 6.9 s –1 . A linear regression of subcritical states yielded a critical estimate of 154.0 ± 3.1 s –1 , aligning with the static 𝛼 estimate at critical. The bootstrapping method produced normally distributed 𝛼 estimates, confirming data consistency. The gamma CPSD 𝛼 estimates clearly distinguish reactor states and improve monitoring of zero-power reactors. The future deployment of modular and microreactors as potential candidates for noise analysis is demonstrated in CROCUS, particularly zero-power mock-ups of new designs. The improvement of noise analysis in the subcritical domain from this work will support experimental data for reactor deployment and procedure.

CROCUS↗
DOE OSTI2023

Prompt Photofission Neutron Detection in Depleted Uranium

The detection of prompt photofission neutrons during active interrogation is a strong indication of the presence of special nuclear materials. However, the high-energy photons used for interrogation create a very challenging radiation environment for the detection of prompt fission signatures. These challenges include detector saturation and pulse pile-up. Additionally, there is an elevated neutron background that further challenges the detection of prompt fission neutrons. This background is produced because of (γ, Xn) photonuclear reactions in the surrounding high-Z materials. Here, we demonstrate the detection of prompt photofission neutrons in these challenging environments. Depleted uranium (DU) and lead targets are interrogated with bremsstrahlung photons produced by a 9-MV electron linear accelerator. Fast neutrons are detected with trans-stilbene organic detectors, and scintillation pulses are analyzed using a previously developed and demonstrated artificial neural network system. We observe a 5 times higher photoneutron count rate when the lead target is replaced with the DU target. Additionally, we observe a difference in the photoneutron light-output distributions of lead and DU. Here, this difference in the measured distributions is due to the difference in the photoneutron-energy spectra; DU photoneutrons are emitted with (γ, n) and watt-energy spectra, whereas lead photoneutrons are emitted with only the (γ, n) spectrum.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2021

Neutron Imaging Using Organic Glass Scintillators

In this work, we develop of a compact neutron imaging system based on organic glass scintillator and silicon photomultiplier arrays. The recently developed organic glass scintillator has excellent neutron and gamma-ray detection efficiency and exhibits pulse shape discrimination capability that is nearly as good as current state-of-the-art materials such as trans-stilbene. We have cast and characterized 6 mm by 6 mm by 50 mm bars of organic glass in our laboratory. When coupled to a silicon photomultiplier array, these bars demonstrated better energy and timing resolution than the stilbene organic scintillator. Here, this performance makes organic glass an ideal material for a compact neutron imaging system, which must resolve neutron scatter events on a sub-nanosecond time scale. We have demonstrated neutron imaging with bars of organic glass scintillator coupled to arrays of silicon photomultipliers. Additional bars of organic glass will be implemented into the system to improve the efficiency and imaging performance. The resulting system will be demonstrated using 252 Cf and PuBe neutron sources in our laboratory. In addition, we will compare imaging performance to other compact neutron imaging systems that exist in literature.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2023

Multiplicity counting using organic scintillators to distinguish neutron sources: An advanced teaching laboratory

In this advanced instructional laboratory, students explore complex detection systems and nondestructive assay techniques used in the field of nuclear physics. After setting up and calibrating a neutron detection system, students carry out timing and energy deposition analyses of radiation signals. Through the timing of prompt fission neutron signals, multiplicity counting is used to carry out a special nuclear material (SNM) nondestructive assay. Our experimental setup is comprised of eight trans-stilbene organic scintillation detectors in a well-counter configuration, and measurements are taken on a spontaneous fission source as well as two (α,n) sources. By comparing each source's measured multiplicity distribution, the resulting measurements of the (α,n) sources can be distinguished from that of the spontaneous fission source. Such comparisons prevent the spoofing, i.e., intentional imitation, of a fission source by an (α,n) neutron source. This instructional laboratory is designed for nuclear engineering and physics students interested in organic scintillators, neutron sources, and nonproliferation radiation measurement techniques.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2024

Gamma-ray Spectroscopy in Low-Power Nuclear Research Reactors

Gamma-ray spectroscopy is an effective technique for radioactive material characterization, routine inventory verification, nuclear safeguards, health physics, and source search scenarios. Gamma-ray spectrometers typically cannot be operated in the immediate vicinity of nuclear reactors due to their high flux fields and their resulting inability to resolve individual pulses. Low-power reactor facilities offer the possibility to study reactor gamma-ray fields, a domain of experiments hitherto poorly explored. In this work, we present gamma-ray spectroscopy experiments performed with various detectors in two reactors: The EPFL zero-power research reactor CROCUS, and the neutron beam facility at the Ohio State University Research Reactor (OSURR). We employed inorganic scintillators (CeBr3), organic scintillators (trans-stilbene and organic glass), and high-purity germanium semiconductors (HPGe) to cover a range of typical—and new—instruments used in gamma-ray spectroscopy. The aim of this study is to provide a guideline for reactor users regarding detector performance, observed responses, and therefore available information in the reactor photon fields up to 2 MeV. The results indicate several future prospects, such as the online (at criticality) monitoring of fission products (like Xe, I, and La), dual-particle sensitive experiments, and code validation opportunities.

Pakari, Oskari V. (ORCID:0000000337048190)↗
DOE OSTI2021

Examination of New Theory for Neutron Multiplicity Counting of Non-Point-Like Sources of Special Nuclear Material

The purpose of a nondestructive assay is to accurately verify the declared mass of special nuclear material (SNM) samples in a limited amount of time. One measurement modality is neutron multiplicity counting (NMC), which relates time-correlated neutron detection rates to the mass of SNM present. Traditional theory assumes point-like sources, which can be ill-posed for kilogram-quantity, bulk samples. Recent theory was developed to improve NMC accuracy for non-point-like samples. This work preliminarily examines the theory with measured data. The OSCAR prototype (a 3-by-4 array of 5.08-cm-thick, 5.08-cm-diameter trans-stilbene organic scintillators) measures configurations of 29.41-49.00 kg of highly enriched uranium (93wt% 235 U). Adjusted factorial moments for the emitted neutron multiplicity distributions are used to account for the shape and type of SNM being measured.

252Cf↗
DOE OSTI2023

Examination of Digital-Delay Rossi-$\alpha$ for 252 Cf-Driven Highly Enriched Uranium Using Organic Scintillators

Neutron noise techniques constitute several analysis methods applicable to non-destructive assay. One technique is the Rossi-α method to calculate the prompt neutron decay constant (α) or its inverse, the prompt neutron period (1/α), for assemblies of fissionable material. This work evaluates a high-data-throughput measurement at the National Criticality Experiments Research Center (NCERC) with organic scintillators measuring a subcritical assembly of highly enriched uranium (HEU) metal (93% 235 U). The assembly comprises hemi shells stacked together to form fully closed shells and is driven by a Cf source at the center. The assembly is a total of 59.85 kg HEU and a k eff of 0.99, according to MCNP6.2 KCODE simulations. Measurements were acquired with a three-by-four array of 5.08-cm-diameter by 5.08-cm-length trans-stilbene crystals 166 cm from the assembly center. Two types of coincident binning methods are used to build the Rossi-α distribution of coincident neutron detections: A) type 1 binning, also known as any-and-all forward time differences, and B) type 1 binning with a digital-delay technique that is analogous to Orndoff’s use of delay cabling in early Rossi-alpha measurements. Method B) disregards same-detector coincidences and once all nearest time coincidences are collected between all detectors after a trigger, a time delay of 0.75 µs is implemented. The measured prompt neutron decay constants for both techniques are calculated from single exponential fits and the two methods are compared. Method A) shows an apparent timing discontinuity near 500 ns time differences. This timing discontinuity interferes with the fitting method used to calculate the prompt neutron decay constant. Method B) mitigates the artificial timing discontinuity and removes the disagreement of the fit. Future work will model the time-dependent detector response to discern why this timing discontinuity occurs, discern how Method B) reduces the amplitude of this timing discontinuity, and apply this method to critical assembly measurements to ultimately confirm the recommendation to use Method B) for high-data-throughput measurements.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2023

Future of the MUSiC Experiment Data

The Measurements of Uranium Subcritical and Critical (MUSiC) experiment was a highly enriched uranium (HEU) experiment performed at the National Criticality Experiments Research Center (NCERC) executed between December 2020 and April 2021. The experiment intended to measure criticality and reactor kinetics parameters in a bare HEU system. The experiment concurrently measured radiation signatures from the system while utilizing different neutron source types. This was an attempt to benchmark both detectors and analysis techniques against one another for identical measurements. The experiment consisted of the Rocky Flats HEU hemi-shells constructed into ten configurations spanning between deeply subcritical (about 14 kgs) to supercritical (about 60 kgs). Two of the ten configurations were supercritical and the other eight were subcritical. The two supercritical configurations, often referred to as the critical configurations, were documented into an International Criticality Safety Benchmark Evaluation Project (ICSBEP) benchmark evaluation and submitted to the technical review group (TRG). The subcritical configurations of the MUSiC experiment were examined using three different detection systems. The systems include: the NoMAD He-3 neutron detector which consists of 15 He-3 tubes surrounded by a polyethylene matrix, a liquid scintillator system called the Rossi-α Measurement Rapid Organic Discriminating Detector (RAM-RODD), and a trans-stilbene organic scintillator array (OSCAR) provided by the University of Michigan. The NoMAD and RAM-RODD data are planned to be evaluated in two separate ICSBEP evaluations utilizing neutron noise methods such as Feynman Variance-to-Mean, Rossi-α and the pulsed neutron source method. Each of the subcritical configurations were examined using three different source types including: a Cf-252 source in the center, with only the intrinsic neutron source in the HEU, and with an external D-T neutron generator.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2021

An Artificial Neural Network System for Photon-Based Active Interrogation Applications

Active interrogation (AI) is a promising technique to detect shielded special nuclear materials (SNMs). At the University of Michigan, we are developing a photon-based AI system that uses bremsstrahlung radiation from an electron linear accelerator (linac) as an ionizing source and stilbene organic scintillating detectors for neutron detection. Stilbene scintillators are sensitive to fast neutrons and photons and have excellent pulse shape discrimination (PSD) capabilities. The traditional charge integration (CI) method commonly used for PSD analysis eliminates piled-up pulses and relies on a particle discrimination line to separate neutrons and photons. The presence of the intense photon flux during AI creates a significant number of piled-up events in the stilbene scintillator, thereby posing a great challenge to the traditional CI method. Identifying true single neutron pulses becomes challenging due to the presence of a pile-up cloud and overlapping neutron, photon and pile-up clouds in the PSD analysis. To mitigate the effect of pulse pile up and identify true single neutron pulses from stilbene scintillators, an artificial neural network (ANN) system is developed. The developed ANN system identifies single neutron pulses and neutron-photon combinations from piled-up events. The results obtained from a 252Cf measurement in the presence of the intense photon flux show that the developed ANN system outperforms the traditional CI method. Since many piled-up events lie above the particle discrimination line, they get misclassified as neutrons by the traditional CI method resulting in 25% overestimation of the net neutron count rate during the linac pulse. The overall net neutron count rate (single and restored neutrons) during the linac pulse, estimated by the ANN system is 60% of the ground truth. Energy spectroscopy of the ANN attributed single neutron pulses further provides evidence on the detection of prompt fission neutrons from the 252Cf fission source.

42 ENGINEERING↗