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At least 73 records · Page 4

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DOE OSTI2024

Compositional Variation Tests on DuraMelter 100 with LAW Sub-Envelope C2 Feed in Support of the LAW Pilot Melter (Final Report)

One of the principal objectives of the DM100 melter tests was to demonstrate that the LAW Sub-Envelope C2 feeds with ± 15% variations in the amounts of waste simulant are suitable for large-scale tests on the LAW Pilot melter. The other principle objective for the DM100 tests was to determine the relative effects of sugar versus waste organics on glass redox state, NOx emissions, sulfur emissions, sulfur retention in the glass, secondary sulfate layer formation, and glass-melt foaming. Additional objectives included measurement of the feed rheological properties and collection of melter emissions data. Screening tests are conducted at the DM100 scale in order to identify and correct potential problems before testing at the larger scale LAW Pilot melter. Testing goals were met in that the results of the DM100 melter test resulted in selection of LAW Sub-Envelope C2 feed suitable for Pilot Melter testing.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2022

Coal polymer composites prepared by fused deposition modeling (FDM) 3D printing

Coal is a vital energy resource worldwide, but pollutants and greenhouse gases from its combustion cause environmental problems. To explore the non-combustion approach to use and valorize coal, anthracite and lignite were blended with polyamide 12 (PA 12) through FDM printing in this work and compared in the composites. By adding lignite, Young’s modulus improved with increasing loading to 50 wt% while tensile strength leveled off among the composites, compared to that of PA 12. By contrast, the addition of anthracite decreased the tensile performance at all loadings. Rheology tests and morphology analyses suggested that the interactions between fillers (anthracite and lignite) and PA 12 may cause differences in tensile properties. In addition, the printed lignite composites showed improved thermal conductivity (~ twofold), indicating lignite demonstrates the potential to build functional composites. This work provides a strategy to use lignite in composites by 3D printing for value-added products and reduces the demand for petroleum-based polymers. Overall, our approach diverts lignite from combustion processes and alleviates the negative impact of lignite use on the environment.

36 MATERIALS SCIENCE↗

NASA NTRS1987

Tribological properties of coal slurries

A pin-on-disk tribometer was used to study the tribological properties of methyl alcohol-coal slurries. Friction coefficients, steel pin wear rates and wear surface morphological studies were conducted on AISI 440C HT and M-50 bearing steels which were slid dry and in solutions of methyl alcohol, methyl alcohol-fine coal particles, and methyl alcohol-fine coal particles-flocking additive. The latter was an oil derived from coal and originally intended to be added to the coal slurry to improve the sedimentation and rheology properties. The results of this study indicated that the addition of the flocking additive to the coal slurry markedly improved the tribological properties, especially wear. In addition, the type of steel was found to be very important in determining the type of wear that took place. Cracks and pits were found on the M-50 steel pin wear surfaces that slid in the coal slurries while 440C HT steel pins showed none.

Fusaro, Robert L.↗

DOE OSTI2023

The Effects of Conditioning and Additives on the Viscosity Measurement of Cement Slurries

This study compares the rheological properties of several cement slurries of Class H, Class G, and two pozzolan-amended cement recipes. Viscosity measurements were taken on both preconditioned and unconditioned cement slurries. Tests were performed using a dual cylinder viscometer following the recommendations of the American Petroleum Institute (API). It was observed that the effect of conditioning on viscosity increased with the increase of particle size in the comparison of Class G to Class H cement. The addition of fly ash significantly changed how cement would react to conditioning. The unconditioned pozzolan-amended cement slurry’s viscosity decreased with the addition of fly ash, whereas the conditioned pozzolan-amended cement slurry increased with the addition of fly ash.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

Effect of ethoxylation and lauryl alcohol on the self-assembly of sodium laurylsulfate: Significant structural and rheological transformation

Fatty alcohols are added to the surfactant solutions to modify foaming and lubrication properties, while the degree of ethoxylation is increased to improve mildness to the skin. However, it is envisioned that both parameters are capable of manipulating rheological and morphological properties. Therefore, an efficient control over the carbon chain length, amount of fatty alcohol and degree of ethoxylation could modify the surfactant self-assembly in an unprecedented way. The present work is focused on understanding the structural transformation, intermolecular interactions and rheological properties of the colloidal systems containing various amounts of lauryl alcohol (LA), and surfactant with varying degrees of ethoxylation. Additionally, combined small-angle neutron scattering (SANS), nuclear magnetic resonance (NMR) spectroscopy, rheological and morphological studies were performed to elucidate these properties. The results reveal that an increase in LA content increases the system viscosity ultimately forming a gel, and drives the assembly pattern of the surfactant from ellipsoidal micellar to lamellar via a vesicular and vesicular/lamellar mixed intermediates. Conversely, higher degrees of ethoxylation delay the onset of morphological transformation and gel formation. The interplay between hydrophobic and polar interactions coupled with hydrogen bonding interactions drive the overall rheological and morphological transformations. Therefore, fine-tuning residual chemicals can offer a novel tool for optimization of the product formulation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2026

Can classical DEM simultaneously capture compressibility and flowability of milled biomass?

Accurate prediction of the rheological behavior of biomass is essential for the design and operation of hoppers, feeders, and storage systems in biorefineries. This study examines whether the classical, coarse-grained discrete element method (DEM) formulation can simultaneously reproduce the compressibility and flowability of milled herbaceous biomass, using Miscanthus × giganteus as a representative material. The model represents particles as rigid spheres interacting through Hertz-Mindlin elastic-frictional contacts augmented with an area-dependent cohesion term. Laboratory cyclic compression and wedge-shaped hopper discharge experiments were used as calibration benchmarks. Although the model can independently reproduce each behavior by appropriately tuning particle Young's modulus E and cohesion energy density k, an extensive parametric investigation comprising more than 600 simulations reveals that the optimal parameter regions for compression and hopper flow are distinct and non-overlapping in (E, k) space. Surrogate surface analysis further shows that the corresponding objective-function valleys exhibit similar trends but are approximately parallel and spatially offset, precluding a unified calibration within the explored domain. Sensitivity analysis indicates that compressibility is governed predominantly by stiffness and cohesion, whereas the slope of the mass flow rate-opening relation in hopper discharge is primarily controlled by tangential friction. Extensions incorporating particle size distribution and clumped-sphere representations do not eliminate the incompatibility. These results systematically reveal, for the first time, the structural limitation of simplified DEM formulations in representing biomass rheological behavior, underscoring the necessity for models incorporating additional physical mechanisms, such as particle deformability or enhanced interlocking, to achieve unified predictive capability for biomass handling behavior.

09 BIOMASS FUELS↗

DOE OSTI2022

Relaxation Dynamics and Ion Conduction of Poly(Ethylene Carbonate/Ethylene Oxide) Copolymer-Based Electrolytes

Poly(ethylene carbonate/ethylene oxide) P(EC/EO) copolymer was synthesized from EC monomer as a new matrix component of solid polymer electrolytes (SPEs), and the correlation between polymer dynamics and ionic conductivity in the P(EC/EO)-based SPEs at various lithium salt weight fractions (w Li ) was investigated by dielectric spectroscopy, rheology, and molecular dynamics (MD) simulations. With the addition of lithium salt, the molecular motions at various scales (i.e., from local to segmental and global motion scales) were found to change as follows: (i) the local motion of P(EC/EO) was slightly accelerated, and at w Li ≥ 0.22, it was separated into two relaxation modes, one faster and the other slower than that of P(EC/EO), (ii) the segmental motion of P(EC/EO) became significantly slower with the addition of lithium salt, and (iii) the global terminal relaxation became slightly slower with the increase of w Li . Thus, the motion of P(EC/EO) at various scales in SPEs changed with different trends with increasing lithium salt. It was also found that the temperature dependence of the ionic conductivity was described by a Vogel–Fulcher–Tammann-type function, which was correlated with the segmental motion, as is known in other SPE systems. Furthermore, from MD simulations, lithium ions are coordinated with the EC units more likely and with a closer distance than EO units in P(EC/EO), and the coordination number of oxygens around one lithium ion was estimated as 6–7 at the distance of 0.30 nm. Here, these results suggest that the coordination structure of the oxygens around the lithium ion is slightly disrupted due to the presence of EC units compared to the chelating structure of pure PEO electrolytes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Thixotropic polysiloxane pastes for additive manufacturing

Shelf-stable, rapid crosslinking, “all-in-one” pastes useful as “inks” in additive manufacturing are provided. These pastes exhibit desirable rheological flow properties and crosslinking upon exposure to UV light. The pastes are based on vinylsilyl-functionalized, completely amorphous, linear terpolysiloxanes containing predominantly dimethylsiloxy-repeat units with small amounts of diphenylsiloxy-, methylphenylsiloxy-, diethylsiloxy-, and/or methyltrifluoroalkylsiloxy-crystallization disruptors. The base polymers are preferably compounded with a trimethylsilylated-hydrophobic silica filler, thixotropic flow agent, hydrosilyl-functionalized oligomeric crosslinker, and a catalytic system comprising platinum(II) acetylacetonate or trimethyl(methylcyclopentadienyl)-platinum(IV), and diethyl azodicarboxylate.

Messman, Jamie Michael↗

DOE OSTI2023

Thixotropic polysiloxane pastes for additive manufacturing

Messman, Jamie Michael↗

DOE OSTI2024

Thixotropic polysiloxane pastes for additive manufacturing

Shelf-stable, rapid crosslinking, “all-in-one” pastes useful as “inks” in additive manufacturing are provided. These pastes exhibit desirable rheological flow properties and crosslinking upon exposure to UV light. The pastes are based on vinylsilyl-functionalized, completely amorphous, linear terpolysiloxanes containing predominantly dimethylsiloxy- repeat units with small amounts of diphenylsiloxy-, methylphenylsiloxy-, diethylsiloxy-, and/or methyltrifluoroalkylsiloxy- crystallization disruptors. The base polymers are preferably compounded with a trimethylsilylated-hydrophobic silica filler, thixotropic flow agent, hydrosilyl-functionalized oligomeric crosslinker, and a catalytic system comprising platinum (II) acetylacetonate or trimethyl(methylcyclopentadienyl)-platinum (IV), and diethyl azodicarboxylate.

Messman, Jamie Michael↗

DOE OSTI2024

Additive Manufacturing of Dissolvable Mandrels

ORNL collaborated with Mitsubishi Chemical America to investigate different grades of vinyl alcohol co-polymers as a potential feedstock material for large-scale material extrusion additive manufacturing (AM). Dissolvable polymers and can find potential applications in AM tooling for complex, hollow, and trapped composite structures without the need for specialized molds and tools. This CRADA Phase I work involved analysis of three different developmental grades of vinyl alcohol co-polymers for thermal and rheological properties, followed by print trials on the Big Area Additive Manufacturing (BAAM) system using these materials. Finally, printed part properties, including mechanical and thermal performance, as well as dissolvability were evaluated. The properties and performance evaluated in this phase of the project have provided guidelines to further develop these vinyl alcohol co-polymers to enable large-scale printing at high deposition rates and obtain parts that satisfy high temperature molds and dies requirements.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Recyclability of additively manufactured bio-based composites

As the flexibility, efficiency, and application space of additive manufacturing continues to grow, many have begun to investigate more sustainable feedstocks as well as options for the end of life of additively manufactured parts. This study examines the effects of mechanical recycling on additively manufactured parts from bio-based feedstock. Here, articles were printed on the Big Area Additive Manufacturing (BAAM) system at the Oak Ridge National Laboratory using poly (lactic acid)/wood flour (PLA/WF) pellets. These parts were shredded and granulated, and the granulate was fed directly back into the BAAM system for re-printing, skipping the costly and energy-intensive steps of extrusion and pelletization. The chemical, mechanical, thermal, and rheological changes to PLA/WF before and after recycling were investigated. Additionally, the energy savings from directly printing granulate on the BAAM system without extrusion and pelletization is reported. It is shown that PLA/WF is an excellent candidate for recycling of large format additively manufactured parts, and value of these parts can be reclaimed while saving cost and energy through mechanical recycling.

42 ENGINEERING↗

DOE OSTI2021

Exfoliation of surfactant swollen layered MWW zeolites into two-dimensional zeolite nanosheets using telechelic liquid polybutadiene

We report two-dimensional (2D) zeolites have the potential to enhance mass transport by reducing diffusion lengths and thus find applications in catalysis and separation. High aspect ratio 2D zeolite nanosheets are required for fabrication of thin, high-flux zeolite membranes. Preparation of 2D zeolite nanosheets can be achieved by exfoliation of layered zeolite precursors, which usually requires multiple steps including swelling with cationic surfactants, exfoliation by applying a mechanical force such as shearing or sonication, purification and removal of the surfactants. The exfoliation of surfactant swollen layered zeolite precursors has been studied using molten polystyrene and telechelic liquid polybutadiene, but still requires extensive shearing force. Recently, a novel one-step exfoliation method has been developed for nonswollen MWW zeolite precursors using tetrabutylammonium hydroxide (TBAOH) solution. In this work, we study the exfoliation of surfactant swollen MWW layered precursors (with and without aluminum) in commercially available liquid hydroxyl-terminated polybutadiene (HTPB) with the aim to provide fundamental understanding of the interaction between the liquid polybutadiene and the surfactant swollen layered zeolite precursors. It was found that surfactant swollen ITQ-1, (ITQ-1(S)), a pure silica layered precursor with MWW framework after being swollen with a cationic surfactant, can be exfoliated in liquid HTPB at room temperature without applying any additional shearing force. The aluminum containing surfactant swollen MWW precursors can be also exfoliated in HTPB at room temperature, but require additional shearing forces. The exfoliation process was monitored using rheology experiments and studied by tuning the composition of the zeolite precursors. The interaction between the layered zeolite precursor and the hydroxyl group of the liquid polybutadiene allows the polymer to intercalate the precursor and exfoliate it into nanosheets. The presence of framework aluminum and the nature of the organic structure directing agents (OSDAs) are key parameters affecting the exfoliation process. Framework Al is unfavorable for the exfoliation possibly due to the surface charges introduced by the aluminum. Bulky OSDA, trimethyladamantammonium (TMAda + ), in the interlayer spacing may facilitate the exfoliation.

2D nanosheets↗

DOE OSTI2024

Porous Polymer Structures with Tunable Mechanical Properties Using a Water Emulsion Ink

Recently, the manufacturing of porous polydimethylsiloxane (PDMS) with engineered porosity has gained considerable interest due to its tunable material properties and diverse applications. An innovative approach to control the porosity of PDMS is to use transient liquid phase water to improve its mechanical properties, which has been explored in this work. Adjusting the ratios of deionized water to the PDMS precursor during blending and subsequent curing processes allows for controlled porosity, yielding water emulsion foam with tailored properties. The PDMS-to-water weight ratios were engineered ranging from 100:0 to 10:90, with the 65:35 specimen exhibiting the best mechanical properties with a Young’s Modulus of 1.17 MPa, energy absorption of 0.33 MPa, and compressive strength of 3.50 MPa. This led to a porous sample exhibiting a 31.46% increase in the modulus of elasticity over a bulk PDMS sample. Dowsil SE 1700 was then added, improving the storage capabilities of the precursor. The optimal storage temperature was probed, with -60 °C resulting in great pore stability throughout a three-week duration. The possibility of using these water emulsion foams for paste extrusion additive manufacturing (AM) was also analyzed by implementing a rheological modifier, fumed silica. Fumed silica’s impact on viscosity was examined, revealing that 9 wt% of silica demonstrates optimal rheological behaviors for AM, bearing a viscosity of 10,290 Pa·s while demonstrating shear-thinning and thixotropic behavior. This study suggests that water can be used as pore-formers for PDMS in conjunction with AM to produce engineered materials and structures for aerospace, medical, and defense industries as sensors, microfluidic devices, and lightweight structures.

36 MATERIALS SCIENCE↗

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

Linking thermoset ink rheology to the stability of 3D-printed structures

Thermoset polymer composites show promise for additive manufacturing (AM) applications to address some of the limitations of the more widely used thermoplastic feedstock materials. Thermosets offer attractive mechanical properties while providing excellent interlayer bonding, high thermal and chemical stability, and reduced energy consumption as a result of deposition at room temperature. However, since thermoset resins rely on a crosslinking reaction to solidify, rather than quickly cooling like thermoplastics, viscoelastic properties must be relied upon to maintain deposited shape after deposition until crosslinking can occur. This fact has not impeded development and characterization of new thermoset feedstocks on the small scale, but recent efforts to increase scale of thermoset printing have highlighted issues with structural stability under self-weight. This study addresses issues of self-weight by investigating the mechanisms that cause collapse of tall, thin printed walls. Using nanoclay- and fumed silica-filled epoxy feedstocks, this work compares the collapse height for printed walls to stability models based on yielding and buckling mechanics. Inputs for these models – shear yield stress and storage modulus – were taken directly from parallel plate rheometry measurements. Model predictions were found to be in good agreement with experimental results, where both yielding and buckling behavior were observed, provided the rheological properties after a shear excursion were used as inputs. This work establishes a direct link between basic rheological properties of the feedstock, geometry of the printed object, and achievable height. Overall, the results presented highlight the importance of understanding recovery behavior in thermoset feedstocks and provide valuable guidance on the development of more effective direct-ink writing feedstock materials.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Linear viscoelastic measurements of commerical therapy putties for design and intuition

This dataset complements the publication Mapping Linear Viscoelasticity for Design and Tactile Intuition (Corman & Ewoldt, 2019). It contains rigorous shear rheometry measurements for six commercial silicone putties, including creep recovery, SAOS, LAOS, and stress relaxation. Additional, unpublished data was generated as part of a graduate rheology course taught by Randy Ewoldt at University of Illinois Urbana-Champaign. Together, these datasets provide a comprehensive example of linear viscoelasticity of a commercial material. The collection is intended both as a pedagogical resource for developing physical intuition in linear viscoelasticity and as a reference dataset for data interpretation, model fitting, and comparative rheological analysis.

C. Marsh, Maxwell↗

DOE OSTI2024

Use of Lignin-Based Admixture as Water Reducer (WRA) for Tailoring the Rheological Properties of Mortars for 3D-Printing

Efforts towards decarbonizing construction materials and industrial processes related to cement and concrete can be aided via multifaceted approaches that target alternative admixtures as well as precision control of fabrication. Chemical admixtures for water reduction have played a crucial role in the development of advanced mortar and concrete mixtures. Newer biomass processing techniques developed for aviation fuel production from corn stover biomass produce a highly reactive lignin byproduct that is suitable for chemical modifications to mimic the properties of commonly used polycarboxylate ethers (PCEs) with a smaller carbon footprint. These lignin-based plasticizers developed at NREL can be used in place of petrochemical-derived superplasticizers to tailor the rheological properties of cement-based systems for applications such as additive manufacturing while reducing the carbon intensity of the concrete mix. Lignosulfonates derived from paper pulping were historically used as water reducers only to be displaced with the rise of PCEs. The present study examines the use of a NREL produced lignin-based water reducing admixture (WRA), in cement pastes and mortar mixtures for 3D-printing at small- (mm) scale. The experimental program consisted of different formulations of oxidized lignin-based WRAs added in variable dosages to cement pastes with a fixed water-to-cement ratio. The objective is to achieve an appropriate workability, extrudability and buildability of mortar mixtures to produce 3D-printed specimens. The rheological characterization was performed to compare the initial yield stress and viscosity of the different mixtures with lignin-based admixture with respect to conventional PCE superplasticizers. The rheological characterization shows that the proposed material act as an effective water-reducer in cement systems, affecting the yield stress, plastic viscosity, and structuration rate of the mixtures evaluated. On the other hand, the effect on early hydration process of the cement pastes containing lignin-based admixtures is comparable to conventional superplasticizers.

3D-printing↗