Simultaneous data of the quasi-static compaction and electrical conductivity of porous, binary powder mixtures have been collected as a function of bulk density. The powder mixtures consist of a metal conductor, either titanium or iron, an insulator, and pores filled with ambient air. The data show a dependency of the conductivity in terms of relative bulk density and metal volume fraction on conductor type and conductor particle characteristics of size and shape. Finite element models using particle domains generated by discrete element method are used to simulate the bulk conductivity near its threshold while the general effective media equation is used to model the conductivity across the compression regime.
This Laboratory Directed Research and Development project developed and applied closely coupled experimental and computational tools to investigate powder compaction across multiple length scales. The primary motivation for this work is to provide connections between powder feedstock characteristics, processing conditions, and powder pellet properties in the context of powder-based energetic components manufacturing. We have focused our efforts on multicrystalline cellulose, a molecular crystalline surrogate material that is mechanically similar to several energetic materials of interest, but provides several advantages for fundamental investigations. We report extensive experimental characterization ranging in length scale from nanometers to macroscopic, bulk behavior. Experiments included nanoindentation of well-controlled, micron-scale pillar geometries milled into the surface of individual particles, single-particle crushing experiments, in-situ optical and computed tomography imaging of the compaction of multiple particles in different geometries, and bulk powder compaction. In order to capture the large plastic deformation and fracture of particles in computational models, we have advanced two distinct meshfree Lagrangian simulation techniques: 1.) bonded particle methods, which extend existing discrete element method capabilities in the Sandia-developed , open-source LAMMPS code to capture particle deformation and fracture and 2.) extensions of peridynamics for application to mesoscale powder compaction, including a novel material model that includes plasticity and creep. We have demonstrated both methods for simulations of single-particle crushing as well as mesoscale multi-particle compaction, with favorable comparisons to experimental data. We have used small-scale, mechanical characterization data to inform material models, and in-situ imaging of mesoscale particle structures to provide initial conditions for simulations. Both mesostructure porosity characteristics and overall stress-strain behavior were found to be in good agreement between simulations and experiments. We have thus demonstrated a novel multi-scale, closely coupled experimental and computational approach to the study of powder compaction. This enables a wide range of possible investigations into feedstock-process-structure relationships in powder-based materials, with immediate applications in energetic component manufacturing, as well as other particle-based components and processes.
It has long been observed that oxidation processes in metals tend to follow a parabolic rate law associated with the growth of a surface oxide layer. Here we observe that for certain titanium powders, the expected parabolic law (∝ t1/2) is recovered, yet for others, the exponent differs significantly. One explanation for this non-parabolic, anomalous diffusion arises from fractal geometry. Theo retical considerations indicate that the time response of diffusion-limited processes in an object closely follow a power-law in time (tn) with n=(E−D)/2, where E is the object's Euclidean dimension and D is its boundary's Hausdorff dimension. Non-integer, (fractal) values of D will result in n≠1/2. Finite element simulations of several canonical fractal objects were performed to verify the application of this theory; the results matched the theory well. Two different types of titanium powder were tested in isothermal thermogravimetric tests under dilute oxygen. Time-dependent mass uptake data were fit with power-law forms and the associated exponents were used to determine an equivalent fractal dimension. One Ti powder type has an implied surface dimension of ca. 2.3 to 2.5, suggesting fractal geometry may be operative. The other has a dimension near 2.0, indicating it behaves like traditional material.
We have used a modified version of the Sandia Instrumented Thermal Ignition (SITI) experiment to develop a pressure-dependent, five-step ignition model for a plastic bonded explosive (PBX 9501) consisting of 95 wt% octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazoncine (HMX), 2.5 wt% Estane® 5703 (a polyurethane thermoplastic), and 2.5 wt% of a nitroplasticizer (NP): BDNPA/F, a 50/50 wt% eutectic mixture bis(2,2-dinitropropyl)-acetal (BDNPA) and bis(2,2-dinitropropyl)-formal (BDNPF). The five steps include desorption of water, decomposition of the NP to form NO2, reaction of the NO2 with Estane® and HMX, and decomposition of HMX. The model was fit using our experiments and successfully validated with experiments from five other laboratories with scales ranging from about 2 g to more than 2.5 kg of PBX. Our experimental variables included density, confinement, free gas volume, and temperature. We measured internal temperatures, confinement pressure, and ignition time. In some of our experiments, we used a borescope to visually observe the decomposing PBX. Our observations included the endothermic β–δ phase change of the HMX, a small exothermic temperature excursion in low-density unconfined experiments, and runaway ignition. We hypothesize that the temperature excursion in these low density experiments was associated with the NP decomposing exothermically within the PBX sample. This reactant-limited temperature excursion was not observed with our thermocouples in the high-density experiments. For these experiments, we believe the binder diffused to the edges of our high density samples and decomposed next to the highly conductive wall as confirmed by our borescope images.