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DOE OSTI2020

Stimuli-responsive petroleum cement composite with giant expansion and enhanced mechanical properties

Shrinkage, as an inherent property of cement during the curing process, has been a concern in the oil & gas industry for centuries. Therefore, expansive cement has been studied for many decades, primarily through incorporation of expansive additives. Nevertheless, traditional expansive additives are not able to achieve the required expansive ratio or maintain a good mechanical property for the cement composite at extreme underground condition. Accordingly, a new generation of expansive additive, which not only has the required expansion, but also work at the downhole high temperature and high pressure environment, and maintain or even enhance the mechanical property, is highly desired. In this work, a high enthalpy storage shape memory polymer (SMP) as a new class of expansive additive is investigated. It is found that the cement composite achieves 1.4% circumferential expansion by only 6% by weight of SMP additives. The compressive strength and flexural strength are also enhanced at the same time, which is hardly achievable by other expansive additives with the same concertation. Good pumpability is also proved by rheological study. The mechanism controlling the enhanced properties is reveled through morphological study and element mapping analysis at the SMP/cement interface.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Loss circulation prevention in geothermal drilling by shape memory polymer

Geothermal formations are naturally fractured with large fracture openings and networks. This can often lead to frequent drilling fluid loss events which is a major contributor to the cost and non-productive time in geothermal drilling. Development of smarter technologies and methods to tackle problem lost circulation is vital for geothermal drilling cost reduction required for geothermal energy to be recognized as a competitive alternative energy source. Mitigation of this problem and other drilling problems such as stuck pipe can minimize overall project cost. In this report, a thermoset shape memory polymer that can be activated by formation natural heat was assessed to seal near wellbore fractures in geothermal wells. The performance of the shape memory polymer (SMP) was evaluated using artificial fractures created in aluminum discs and cylindrical granite cores. Rheology and particle size distribution were considered. A novel testing setup was built for this work, which allows testing of sealing efficiency under dynamic conditions at high temperature. Analysis showed that the SMP has efficiently succeeded in forming a strong plug inside the fractures and stopped fluid loss at high sealing pressure. This smart loss circulation material can expand within the fractures to reduces non-drilling time and strengthen the wellbore in high-temperature drilling operations.

58 GEOSCIENCES↗

DOE OSTI2024

Insights into Preceramic Polymer-Based Additive Manufacturing Inks via Rheological and Scattering Studies of Preceramic Polymer-Grafted Nanoparticles Suspended in Polycarbosilane

Preceramic polymers (PCPs) offer advantages in producing ceramics due to their processability and ability to tailor the final chemistry of the produced material. However, challenges such as volumetric shrinkage and mass loss during pyrolysis often result in polymer-derived ceramics containing pores and cracks. PCP-grafted ceramic nanoparticles (PCPGNPs) have been proposed and studied as a route to mitigate the shrinkage issues associated with neat PCPs. Prior studies on PCPGNPs have principally focused on the synthesis and characterization of neat materials. Dispersing PCPGNPs in commercial preceramic polymer is another attractive, but underexplored, route to control the rheological and char yield properties of PCP systems. In this work, a systematic rheological study of commercial PCP (SMP-877) and PCPGNP (silica with poly(1,1-dimethylpropylsilane) corona) mixtures was executed to develop design rules for the processing of such systems. A rheological study demonstrated the effect of increasing particle concentration on network formation with percolation occurring between 50 and 60 wt %. Samples above the percolation threshold exhibited higher viscosities and rapid shear thinning thus demonstrating their direct-write printability. X-ray photon correlation spectroscopy (XPCS) corroborated the rheology and showed two diffusive modes when the material was above percolation. Mixtures of PCPGNPs and SMP-877 had synergistically higher char yields upon thermal treatment and pyrolysis. XPCS and rheological measurements during thermal treatment identified thermal jamming of the polymer grafts as a key factor in improving the char yield. In conclusion, with the insights gained here, we expect these mixed systems to provide attractive feedstocks for polymer-derived ceramics, with proof-of-principal application as feedstocks for direct ink write (DIW) additive manufacturing.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Melting of spatially modulated phases at domain wall/surface junctions in antiferrodistortive multiferroics

A physical understanding of the nature of spatially modulated phases (SMPs) in rare-earth-doped antiferrodistortive (AFD) multiferroics and how they behave close to surfaces and interfaces is lacking. Here the emergence of the antiferroelectric (AFE), ferroelectric (FE), or ferrielectric (AFE-FE) spatial modulation in the vicinity of the morphotropic phase transition in La x Bi 1 – x Fe O 3 ( x ~ 0.2 ) is explored on the atomic level using high-resolution scanning transmission electron microscopy (HRSTEM). The suppression, or “melting,” of the AFE-type SMP in the vicinity of the AFD twin wall/surface junction is revealed by HRSTEM in La 0.22 Bi 0.78 Fe O 3 films and explained by the hybrid approach combining Landau-Ginzburg-Devonshire (LGD) phenomenology and the semimicroscopic four-sublattice model (FSM). The LGD-FSM approach reduces the problem of AFE (or AFE-FE) SMP emergence and stability to the thermodynamic analysis of the free-energy functional with AFE, FE, and AFD long-range order parameters and two master parameters: the FE-AFE coupling strength between four neighboring A sites and the nonstoichiometry factor, which are proportional to the variations of La concentration in La x Bi 1 – x Fe O 3 films. Finally, we establish that the surface-induced melting of SMPs and the associated broadening of AFE AFD domain walls minimize the film free energy under certain conditions imposed on the master parameters and gradient energy below the critical value. The observed behavior provides insight into the origin of SMPs in AFD multiferroics.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2022

Synthesis and Characterization of Silicon Carbide Ceramic Composites with CeO 2 Powder

This study pioneers the fabrication and characterization of silicon carbide (SiC) containing cerium dioxide (CeO 2 ). CeO 2 powder was tested as a surrogate for actinide oxide waste forms such as uranium dioxide (UO 2 ) and plutonium dioxide (PuO 2 ). Several syntheses were evaluated with varying amounts of preceramic polymer (SMP-10 resin) and CeO 2 containing either SiC fiber, carbon fiber, or no fibers. Scanning electron microscopy (SEM) was used to characterize morphology and compositional differences, and energy-dispersive x-ray spectroscopy (EDS) was used to provide semiquantitative elemental analysis. In addition, each sample was characterized by density, powder x-ray diffraction (pXRD), and Raman spectroscopy. Samples containing nearly more than four times CeO 2 powder than SMP-10 resin by mass had the best properties. This research establishes a unique synthesis for SiC containing high concentrations of CeO 2 powder to illustrate how it may be managed as a potential waste form.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2025

Develop a new integrated macro→micro←nano (MMN) multiscale modeling framework to optimize high strength aluminum alloys and processes for vehicle light-weighting

Bending tests provide a means to study plane strain fracture performance of 6000 series aluminum alloys. Metrics from bending tests have been correlated with self-pierce riveting (SPR) performance of a high strength AA6111 automotive aluminum alloy in previous works. Using the ORNL HPC resources, this project developed an innovative macro→micro←nano (MMN) multiscale microstructure-based finite element (FE) code to further understanding of the relationship between microstructure and fracture properties of high-strength 6000-series alloys. This work started with microstructural characterization in both mesoscale and nanoscale and bending performance characterization of AA6111 HS2-T6 alloy at Ford, the MMN framework was applied to this alloy to simulate 3-point VDA bending. From the results of the macro-modeling of 3-point VDA bending, the critical region of fracture was identified, and the region geometry was used to construct the micro-model. The fracture criterion of micron-scale precipitates and aluminum matrix which contains submicron and nano particles (AL-SMP-NP) in the micro-model was calibrated and validated by comparing simulated and measured bending results. With the AL-SMP-NP fracture strain obtained, the fracture strain of Al-matrix containing nano particles (ALNP) will similarly be determined by a submicron scale-model using an edge-constrained FE modeling approach developed by Hu et al. With the ALNP fracture strain obtained, the fracture strain of Al-matrix containing no particles will similarly be determined by a nano scale-model using an edge-constrained FE modeling approach. After the MMN framework is built and fracture criterion calibrated, nano-model FE simulations with virtual microstructures was performed to obtain a reduced order model (ROM) of the fracture criterion of the ALNP as a function of volume fraction, size, and distribution of the nanoparticle. This nano→submicron→micro modeling part allows exploration of the influence of different material nanostructures from different process conditions on the bending properties within the multiscale bending simulation framework and the ROM of material bendability as a function of nanoparticle size and shape was established. This obtained reduced order model (ROM) could help guide the design and selection of materials to improve existing SPR process models that could replace trial-and-error rivet/die selection and help to design new rivet/die combinations capable of robustly joining new higher strength 6000 5 series alloys in automotive body structures. This would enable lightweighting of Ford vehicles leading to greater fuel efficiency and reduce manufacturing time and energy.

36 MATERIALS SCIENCE↗

DOE OSTI2025

B‐Staging and Crosslinking of Polycarbosilane at Room Temperature: Cure Mechanism and Properties

The viscosity of polycarbosilane (PCS) polymers is not advantageous for free forming. Various fillers and heat are used to obtain a formable paste. Due to the low yield stress, structures and preforms tend to slump or resin will flow out, especially during the curing of the polymer. B-staging of PCS allows for a more stable structure from room temperature until the full cure of the allyl groups occurs with heat. Additionally, hydrosilation is an effective means of crosslinking at room temperature and controlling viscosity. A network structure was formed in SMP-10 using silane and a vinyl-based crosslinker to bridge each polymer chain. Pt addition catalysts were added to enhance the increase in viscosity to make a lightly crosslinked gel to aid in thickening and forming and to improve the ceramic yield at 1000°C. In conclusion, this enables several options for controlling rheology and improving the properties of preceramic polymers to avoid slumping during curing.

inorganic polymers↗

DOE OSTI2022

Influence of Thermal Treatment on Preceramic Polymer Grafted Nanoparticle Network Formation: Implications for Thermal Protection Systems and Aerospace Propulsion Components

Preceramic polymer grafted nanoparticles (PCP GNPs) offer potential advantages in the production of polymer-derived ceramic composites compared to neat preceramic polymers (PCPs), such as reduced thermal shrinkage and increased char yield. In comparison to traditional composites (particles + free polymer), PCPs avoid issues of compatibility, agglomeration, and phase separation during processing and provide routes to control nanoparticle arrangement. Prior literature has established that the conversion efficiency of PCPs and PCP GNPs to ceramics and ceramic composites is linked to the thermal pretreatment of these precursor polymers (e.g., curing). In this paper, we investigate the material transformations that occur when exposing PCP GNPs to a low-temperature thermal treatment (≤250 °C) prior to pyrolysis. The PCP GNPs explored in this study possessed silica nanoparticle cores but were distinct in their PCP coronas, having poly(1,1-dimethylpropylsilane) (allyl-GNP)- or poly(1,1-dimethylbenzylethylsilane) (styryl-GNP)-grafted polymers. After undergoing low-temperature thermal treatment, these PCP GNPs exhibited increased char yield at 800 °C; however, unlike commercial PCPs (e.g., allylhydridopolycarbosilane (SMP-10)), obvious cross-linkable sites are not present in the PCP corona structure. Differential scanning calorimetry, oscillatory rheology, and X-ray photon correlation spectroscopy were utilized to elucidate the thermally induced material changes in the allyl- and styryl-GNPs. Thermally induced changes to the structure and behavior of the PCP GNPs were determined to be linked to the chemical structure of the grafted polycarbosilane chains. Styryl-GNPs experienced a curing event between 180 and 250 °C, effecting the formation of a network, which contributed to char yield improvement (at 800 °C). The nanoscale dynamics of this material also shows a transition from diffuse behavior to ballistic behavior because of the cross-linking event. Conversely, the allyl-GNPs did not exhibit a curing event under heat treatment but did show an increase in thermally induced physical cross-linking. The allyl-GNP physical network is stronger after the first cycle of thermal treatment, and it is considered that this contributed to the improvement in char yield post thermal treatment. The advancements in the understanding of the cross-linking behavior of these hybrid materials are expected to advance the application of these materials to turbine engine, advanced friction, and heat-shielding components.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Vortex phases and glassy dynamics in the highly anisotropic superconductor HgBa 2 CuO 4+δ

We present an extensive study of vortex dynamics in a high-quality single crystal of HgBa 2 CuO 4+ δ , a highly anisotropic superconductor that is a model system for studying the effects of anisotropy. From magnetization M measurements over a wide range of temperatures T and fields H , we construct a detailed vortex phase diagram. We find that the temperature-dependent vortex penetration field H p ( T ), second magnetization peak H smp ( T ), and irreversibility field H irr ( T ) all decay exponentially at low temperatures and exhibit an abrupt change in behavior at high temperatures T / T c >~0.5. By measuring the rates of thermally activated vortex motion (creep) S ( T , H ) = | d ln M ( T , H )/ d ln t |, we reveal glassy behavior involving collective creep of bundles of 2D pancake vortices as well as temperature- and time-tuned crossovers from elastic (collective) dynamics to plastic flow. Based on the creep results, we show that the second magnetization peak coincides with the elastic-to-plastic crossover at low T , yet the mechanism changes at higher temperatures.

36 MATERIALS SCIENCE↗

DOE OSTI2025

An accurate measurement of the spectral resolution of the JWST Near Infrared Spectrograph

The spectral resolution (R ≡ λ/Δλ) of spectroscopic data is crucial information for accurate kinematic measurements. In this letter we present a robust measurement of the spectral resolution of the JWST Near Infrared Spectrograph (NIRSpec) in fixed slit (FS) and integral field spectroscopy (IFS) modes. Due to the similarity of the utilized slit dimension in the FS mode to that of the shutters in the multi-object spectroscopy (MOS) mode, our resolution measurements in the FS mode can also be used for the MOS mode in principle. We modeled H and He lines of the planetary nebula SMP LMC 58 using a Gaussian line spread function (LSF) to estimate the wavelength-dependent resolution for multiple disperser and filter combinations. We corrected for the intrinsic width of the planetary nebula’s H and He lines due to its expansion velocity by measuring it from a higher-resolution X-shooter spectrum. We find that NIRSpec’s in-flight spectral resolutions exceed the pre-launch estimates provided in the JWST User Documentation by 11–53% in the FS mode and by 1–24% in the IFS mode across the covered wavelengths. We recover the expected trend that the resolution increases with the wavelength within a configuration. The robust and accurate LSFs presented in this letter will enable high-accuracy kinematic measurements using NIRSpec for applications in cosmology and galaxy evolution.

methods: data analysis↗

DOE OSTI2025

An in vitro BRAF activation assay elucidates molecular mechanisms driving disassembly of the autoinhibited BRAF state

The RAF kinases (ARAF, BRAF, and CRAF) are essential components of the RAS-ERK signaling pathway, which controls vital cellular processes and is frequently dysregulated in human disease. Notably, mutations that alter BRAF function are prominent drivers of human cancer and certain RASopathy disorders, making BRAF an important target for therapeutic intervention. Despite extensive research, several aspects of BRAF regulation remain unclear. In this study, we developed an in vitro BRAF activation assay using purified autoinhibited BRAF:14-3-3 2 :MEK complexes. Our results show that fully processed, active-state KRAS alone can promote dimer-dependent BRAF activation. Moreover, we found that phosphatidylserine (PS)-containing liposomes synergized with KRAS to promote BRAF activation, achieving activity levels comparable to those observed with BRAF proteins that constitutively dimerize. In contrast, the SMP phosphatase complex had only a minimal effect on BRAF catalytic activity in this system but mediated the dephosphorylation of the negative regulatory pS365 14-3-3 binding site in a manner that was accelerated by the presence of KRAS alone or KRAS and 30% PS liposomes. Finally, we show that inhibitors blocking the BRAF RBD:KRAS interaction were able to suppress the in vitro activation of BRAF, underscoring the critical role of RAS binding in initiating the disassembly of the BRAF autoinhibited state. Thus, this assay provides valuable insights into the steps required for BRAF activation and can serve as an effective screening tool for identifying compounds that may inhibit this process and have therapeutic potential.

BRAF↗

DOE OSTI2024

Impact of temperature and concentration on flow behaviour of reconstituted lactose and protein–rich dairy powders

To help with designing the drying process, this study investigated the flow behaviour of lactose and protein-rich reconstituted dairy powders at 25°C and 50°C. Lactose-rich samples, 50% dried whey (DW) and 60% whey protein concentrate (WPC35) did not follow the Herschel–Bulkley model because of presence of lactose crystals. Reconstituted 50% skim milk powder (SMP) and protein-rich dairy powders exhibited shear-thinning behaviour (n < 0.3). With increasing concentration, whey protein concentrate/isolate (WPC80/WPI) and micellar casein concentrate high-solid dispersions exhibited more shear-thinning behaviour (n < 0.4). Furthermore, understanding shear-thinning behaviour of lactose-rich and protein-rich reconstituted dairy powders will provide basis for optimising drying parameters.

36 MATERIALS SCIENCE↗

DOE OSTI2023

What is needed for BISCO to work in a dipole insert for 20 tesla hybrid accelerator magnets

Developing HTS dipole inserts producing fields larger than 5 T within 15 T Nb3Sn outserts is necessary to generate 20 T or higher fields for future high energy colliders. Dipole inserts based on the cos-theta coil geometry with various stress management concepts and Bi2212 super-conducting strand and cable are being developed at Fermilab both within and beyond the U.S. national effort. On paper, the potential reach for the maximum magnetic field in existing or planned Nb3Sn outserts is close to 20 T, thanks to the progress realized in Bi2212 wires’ critical current density. To achieve the Bi2212 potential in accelerator magnets, however, a number of technological challenges still have to be faced. These for instance include the need to design billets that are adequate for Rutherford cabling; developing insulation processes and materials that prevent leaks, which reduce transport current and increase the risk of shorts; control and limit Bi2212 coils’ stresses and strains; reconsider the Split Melt Process (SMP) to lower costs and simplify the processing. This paper reviews Bi2212 conductor properties and coil technolo-gies, and proposes new ideas to face the challenges that Bi2212 still presents as an accelerator magnet conductor.

43 PARTICLE ACCELERATORS↗

DOE OSTI2024

Venado acceptance: results and tips [Slides]

Nvidia compiler support is not available through cray-mpich/compiler wrapper interface. Adjust CMAKE files to use the correct COMPILER_ID in conditionals and explicit variables to package flags. Use pinned host memory in cray-libsci_acc and cublasXt calls. Set a large blockDim for cublasXt calls. Try MPS and/or explicit numactl binding if performance is lackluster. Use CRAY_MALLOPT_OFF=1 if unexpected OOM errors appear using cce. Use MPICH_SMP_SINGLE_COPY_MODE=CMA for xpmem issues. Use MPICH_OPT_THREAD_SYNC=0 for MPI_THREAD issues. Poor CUDA-aware MPI performance remains an issue.

97 MATHEMATICS AND COMPUTING↗

DOE OSTI2025

Geophysical measurements of a demolition at NRF

On May 31 st , 2025, at approximately 14:40:00 UTC, the former Submarine First Westinghouse (SW1) structure housing a large crane was demolished at the Naval Reactors Facility (NRF) located within the perimeter of the Idaho National Laboratory (INL). Several targeted explosives were used to facilitate this demolition. The INL Seismic Monitoring Program (SMP) installed four temporary seismic instrument suites around the site of the demolition in order to monitor ground motion including measuring peak ground acceleration (PGA), peak ground velocity (PGV), and to calculate peak ground displacement (PGD). The demolition produced three types of waves: body waves, surface waves, and acoustic waves. The acoustic wave represents the largest signal received. The PGA, measured on the eastern component of the instrument located approximately 95m away from the demolition site, was 0.187g. The PGV measured was 0.0004 m/s, and the PGD was approximately 0.000006m. Rayleigh waves incident on an instrument located at the Advanced Test Reactor, about 7.6km away, were used to estimate a magnitude of 0.3 at the ATR, representing a yield of energy equivalent to approximately 3 grams of TNT.

58 - GEOSCIENCES↗

DOE OSTI2020

Controlled thermal coefficient product system and method

A controlled thermal coefficient product manufacturing system and method is disclosed. The disclosed product relates to the manufacture of metallic material product (MMP) having a thermal expansion coefficient (TEC) in a predetermined range. The disclosed system and method provides for a first material deformation (FMD) of the MMP that comprises at least some of a first material phase (FMP) wherein the FMP comprises martensite randomly oriented and a first thermal expansion coefficient (FTC). In response to the FMD at least some of the FMP is oriented in at least one predetermined orientation. Subsequent to deformation, the MMP comprises a second thermal expansion coefficient (STC) that is within a predetermined range and wherein the thermal expansion of the MMP is in at least one predetermined direction. The MMP may be comprised of a second material phase (SMP) that may or may not transform to the FMP in response to the FMD.

Monroe, James Alan↗

DOE OSTI2023

Controlled thermal coefficient product system and method

Monroe, James Alan↗

DOE OSTI2025

Search for rare decays of the Z and Higgs bosons to a J / ψ or ψ(2S) meson and a photon in proton-proton collisions at s = 13 TeV

A search is presented for rare decays of the Z and Higgs bosons to a photon and a J∕ψ or a ψ(2S) meson, with the charmonium state subsequentially decaying to a pair of muons. The data set corresponds to an integrated luminosity of 123 fb −1 of proton-proton collisions at a center-of-mass energy of 13TeV collected with the CMS detector at the LHC. No evidence for branching fractions of these rare decay channels larger than predicted in the standard model is observed. Upper limits at 95% confidence level are set: $\mathcal{B}$(H → J∕ψγ ) < 2.6 × 10 −4 , $\mathcal{B}$(H → ψ(2S)γ ) < 9.9 × 10 −4 , $\mathcal{B}$(Z → J∕ψγ ) < 0.6 × 10 −6 , and $\mathcal{B}$(Z → ψ(2S)γ ) < 1.3 × 10 −6 . The ratio of the Higgs boson coupling modifiers 𝜅 c ∕𝜅 γ is constrained to be in the interval (−157, +199) at 95% confidence level. Assuming 𝜅 γ = 1, this interval becomes (−166, +208).

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗