The southern United States produces 90% of the nation’s cotton, and the Texas High Plains is the largest contiguous cotton producing region. Since 2011, glyphosate-resistant Palmer amaranth has complicated cotton production, and alternatives to glyphosate are needed. Integrating soil residual herbicides into a weed management program is a crucial step to control glyphosate resistant weeds before emergence. The recent development of p-hydroxyphenylpyruvate dioxygenase (HPPD)-resistant cotton by BASF Corporation may allow growers to use isoxaflutole in future weed management programs. In 2019 and 2020, field experiments were conducted in New Deal, Lubbock, and Halfway, Texas, to evaluate HPPD-resistant cotton response to isoxaflutole applied preemergence (PRE) or early postemergence (EPOST) and to determine the efficacy of isoxaflutole when used as part of a season-long weed management program. At the New Deal location, cotton response was observed following the EPOST application, but it never exceeded 10%. Cotton response was greatest following the PRE application in Lubbock in 2019 but did not exceed 14%. In 2020 in Lubbock, cotton was replanted due to severe weather. There was <1% cotton response following the PRE application, and maximum cotton response observed was 9% following EPOST and mid-postemergence (MPOST) applications. Cotton lint yields were not different from those of the nontreated, weed-free control at either location. In non-crop weed control studies in Halfway, all treatments controlled Palmer amaranth ≥94% 21 d after the EPOST application. Twenty-one days after the MPOST treatment, systems with isoxaflutole applied EPOST controlled Palmer amaranth by 88% to 93%, while systems with isoxaflutole PRE controlled Palmer amaranth by 94% to 98%. End-of-season Palmer amaranth control was lowest in the system without isoxaflutole (88%) and when isoxaflutole was used EPOST (88% to 91%). These studies suggest that the use of isoxaflutole in cotton weed management systems may improve season-long control of several troublesome weeds with no adverse effects on cotton yield and quality.

The effect of sample preparation on a pre-aged Al–Mg–Si–Cu alloy has been evaluated using atom probe tomography. Three methods of preparation were investigated: electropolishing (control), Ga+ focused ion beam (FIB) milling, and Xe+ plasma FIB (PFIB) milling. Ga+-based FIB preparation was shown to introduce significant amount of Ga contamination throughout the reconstructed sample (≈1.3 at%), while no Xe contamination was detected in the PFIB-prepared sample. Nevertheless, a significantly higher cluster density was observed in the Xe+ PFIB-prepared sample (≈25.0 × 1023 m−3) as compared to the traditionally produced electropolished sample (≈3.2 × 1023 m−3) and the Ga+ FIB sample (≈5.6 × 1023 m−3). Hence, the absence of the ion milling species does not necessarily mean an absence of specimen preparation defects. Specifically, the FIB and PFIB-prepared samples had more Si-rich clusters as compared to electropolished samples, which is indicative of vacancy stabilization via solute clustering.

Although recognized as one of the most significant cultural transformations in North America, the reintroduction of the horse to the continent after AD 1492 has been rarely addressed by archaeological science. A key contributing factor behind this limited study is the apparent absence of equine skeletal remains from early historic archaeological contexts. Here, we present a multidisciplinary analysis of a horse skeleton recovered in Lehi, Utah, originally attributed to the Pleistocene. Reanalysis of stratigraphic context and radiocarbon dating indicates a historic age for this horse (cal AD 1681–1939), linking it with Ute or other Indigenous groups, whereas osteological features demonstrate its use for mounted horseback riding—perhaps with a nonframe saddle. DNA analysis indicates that the animal was a female domestic horse, which was likely cared for as part of a breeding herd despite outliving its usefulness in transport. Finally, sequentially sampled stable carbon, oxygen, and strontium isotope values from tooth enamel (δ13C, δ18O, and 87Sr/86Sr) suggest that the horse was raised locally. These results show the utility of archaeological science as applied to horse remains in understanding Indigenous horse pastoralism, whereas consideration of the broader archaeological record suggests a pattern of misidentification of horse bones from early historic contexts.

We report the sputter deposition of Cu-7V and Cu-27V (at.%) alloy films in an attempt to yield a “clean” alloy to investigate nanocrystalline stability. Films grown in high vacuum chambers can mitigate processing contaminates which convolute the identification of nanocrystalline stability mechanism(s). The initial films were very clean with carbon and oxygen contents ranging between ~0.01 and 0.38 at.%. Annealing at 400 °C/1 h facilitated the clustering of vanadium at high-angle grain boundary triple junctions. At 800 °C/1 h annealing, the Cu-7V film lost its nanocrystalline grain sizes with the vanadium partitioned to the free surface; the Cu-27V retained its nanocrystalline grains with vanadium clusters in the matrix, but surface solute segregation was present. Though the initial alloy and vacuum annealing retained the low contamination levels sought, the high surface area-to-volume ratio of the film, coupled with high segregation tendencies, enabled this system to phase separate in such a manner that the stability mechanisms that were to be studied were lost at high temperatures. This illustrates obstacles in using thin films to address nanocrystalline stability.

Microwave plasma chemical vapor deposition (MPCVD) was used to diffuse boron into tantalum using plasma initiated from a feedgas mixture containing hydrogen and diborane. The role of substrate temperature and substrate bias in influencing surface chemical structure and hardness was investigated. X-ray diffraction shows that increased temperature results in increased TaB2 formation (relative to TaB) along with increased strain in the tantalum body-centered cubic lattice. Once the strained tantalum becomes locally supersaturated with boron, TaB and TaB2 precipitate. Additional boron remains in a solid solution within the tantalum. The combination of precipitation and solid solution hardening along with boron-induced lattice strain may help explain the 40 GPa average hardness measured by nanoindentation. Application of negative substrate bias did not further increase the hardness, possibly due to etching from increased ion bombardment. These results show that MPCVD is a viable method for synthesis of superhard borides based on plasma-assisted diffusion.

Isoconcentration surfaces are commonly used to delineate phases in atom probe datasets. These surfaces then provide the spatial and compositional reference for proximity histograms, the number density of particles, and the volume fraction of particles within a multiphase system. This paper discusses the influence of the isoconcentration surface selection value on these quantitative outputs, using a simple oxide dispersive strengthened alloy, Fe91Ni8Zr1, as the case system. Zirconium reacted with intrinsic oxygen impurities in a consolidated ball-milled powder to precipitate nanoscale zirconia particles. The zirconia particles were identified by varying the Zr-isoconcentration values as well as by the maximum separation data mining method. The associated outputs mentioned above are elaborated upon in reference to the variation in this Zr isosurface value. Considering the dataset as a whole, a 10.5 at.% Zr isosurface provided a compositional inflection point for Zr between the particles and matrix on the proximity histogram; however, this value was unable to delineate all of the secondary oxide particles identified using the maximum separation method. Consequently, variations in the number density and volume fraction were observed as the Zr isovalue was changed to capture these particles resulting in a loss of the compositional accuracy. This highlighted the need for particle-by-particle analysis.

Atom probe tomography (APT) of a nanocrystalline Cu–7 at.% V thin film annealed at 400°C for 1 h revealed chemical partitioning in the form of solute segregation. The vanadium precipitated along high angle grain boundaries and at triple junctions, determined by cross-correlative precession electron diffraction of the APT specimen. Upon field evaporation, the V2+/(V1+ + VH1+) ratio from the decomposed ions was ~3 within the matrix grains and ~16 within the vanadium precipitates. It was found that the VH1+ complex was prevalent in the matrix, with its presence explained in terms of hydrogen's ability to assist in field evaporation. The change in the V2+/(V1+ + VH1+) charge-state ratio (CSR) was studied as a function of base temperature (25–90 K), laser pulse energy (50–200 pJ), and grain orientation. The strongest influence on changing the CSR was with the varied pulse laser, which made the CSR between the precipitates and the matrix equivalent at the higher laser pulse energies. However, at these conditions, the precipitates began to coarsen. The collective results of the CSRs are discussed in terms of field strengths related to the chemical coordination.

Microstructure and phase evolution in magnetron sputtered nanocrystalline tungsten and tungsten alloy thin films are explored through in situ TEM annealing experiments at temperatures up to 1000 °C. Grain growth in unalloyed nanocrystalline tungsten transpires through a discontinuous process at temperatures up to 550 °C, which is coupled to an allotropic phase transformation of metastable β-tungsten with the A-15 cubic structure to stable body centered cubic (BCC) α-tungsten. Complete transformation to the BCC α-phase is accompanied by the convergence to a unimodal nanocrystalline structure at 650 °C, signaling a transition to continuous grain growth. Alloy films synthesized with compositions of W–20 at.% Ti and W–15 at.% Cr exhibit only the BCC α-phase in the as-deposited state, which indicate the addition of solute stabilizes the films against the formation of metastable β-tungsten. Thermal stability of the alloy films is significantly improved over their unalloyed counterpart up to 1000 °C, and grain coarsening occurs solely through a continuous growth process. The contrasting thermal stability between W–Ti and W–Cr is attributed to different grain boundary segregation states, thus demonstrating the critical role of grain boundary chemistry in the design of solute-stabilized nanocrystalline alloys.

In North America, terrestrial records of biodiversity and climate change that span Marine Oxygen Isotope Stage (MIS) 5 are rare. Where found, they provide insight into how the coupling of the ocean–atmosphere system is manifested in biotic and environmental records and how the biosphere responds to climate change. In 2010–2011, construction at Ziegler Reservoir near Snowmass Village, Colorado (USA) revealed a nearly continuous, lacustrine/wetland sedimentary sequence that preserved evidence of past plant communities between ~140 and 55 ka, including all of MIS 5. At an elevation of 2705 m, the Ziegler Reservoir fossil site also contained thousands of well-preserved bones of late Pleistocene megafauna, including mastodons, mammoths, ground sloths, horses, camels, deer, bison, black bear, coyotes, and bighorn sheep. In addition, the site contained more than 26,000 bones from at least 30 species of small animals including salamanders, otters, muskrats, minks, rabbits, beavers, frogs, lizards, snakes, fish, and birds. The combination of macro- and micro-vertebrates, invertebrates, terrestrial and aquatic plant macrofossils, a detailed pollen record, and a robust, directly dated stratigraphic framework shows that high-elevation ecosystems in the Rocky Mountains of Colorado are climatically sensitive and varied dramatically throughout MIS 5.

The slip systems in ZrB2 flexural tested at 1000 °C and 1500 °C have been quantified. The dislocations in both samples were long and straight with a dislocation density of approximately 1013 m−2. The structure of the dislocations as well as the low density is in agreement with a ceramic that is hard and brittle and dislocation nucleation and motion is restricted. The low temperature slip systems were found to include c-prismatic slip— ${1 \mathord{\left/ {\vphantom {1 3}} \right. \kern-\nulldelimiterspace} 3}\left[ {0001} \right]\left( {\bar 1010} \right)$ —and a-pyramidal slip— ${1 \mathord{\left/ {\vphantom {1 3}} \right. \kern-\nulldelimiterspace} 3}\left[ {11\bar 20} \right]\left( {\bar 1101} \right)$ whereas the elevated temperature sample revealed a-basal slip— ${1 \mathord{\left/ {\vphantom {1 3}} \right. \kern-\nulldelimiterspace} 3}\left[ {11\bar 20} \right]\left( {0001} \right)$ . Density functional theory Generalized Stacking Fault Energy curves for perfect slip were calculated and agreed well with geometric considerations for slip, including interplanar spacing and planar packing. Though basal slip has the lowest fault energy, the presence of the other dislocation types is suggestive that the activation barrier is not a hindrance for the temperatures studied and is likely activated to increase the number of plastic degrees of freedom.

A series of (HfN)1−x(TaN)x, ceramics with x representing the starting powder blend compositions of 0.0, 18.8, 28.1, and 46.7 at.%, have been fabricated by vacuum plasma spraying. During the plasma spraying, the mixture lost approximately 25 at.% nitrogen facilitating the precipitation of metallic and metal-rich nitride phases. These specimens underwent static air oxidation exposure up to 1700 °C. In general, it was found that the addition of tantalum nitrides to the hafnium nitrides resulted in poorer oxidation behavior. However, the 18.8 at.% specimen deviated from this trend and had the lowest observed mass change. This specimen formed a dark-colored oxide scale, indexed as Hf6Ta2O17, which acted as a passivation layer. Within the scale, hafnium oxynitride phases were observed. A transformation pathway in forming these rhombohedral oxynitride phases is proposed by the filling in of oxygen in the light element interstitial locations of the rhombohedral ε-Hf3N2 and ζ-Hf4N3 structures.

The material characterization toolbox has recently experienced a number of parallel revolutionary advances, foreshadowing a time in the near future when material scientists can quantify material structure evolution across spatial and temporal space simultaneously. This will provide insight to reaction dynamics in four-dimensions, spanning multiple orders of magnitude in both temporal and spatial space. This study presents the authors’ viewpoint on the material characterization field, reviewing its recent past, evaluating its present capabilities, and proposing directions for its future development. Electron microscopy; atom probe tomography; x-ray, neutron and electron tomography; serial sectioning tomography; and diffraction-based analysis methods are reviewed, and opportunities for their future development are highlighted. Advances in surface probe microscopy have been reviewed recently and, therefore, are not included [D.A. Bonnell et al.: Rev. Modern Phys. in Review]. In this study particular attention is paid to studies that have pioneered the synergetic use of multiple techniques to provide complementary views of a single structure or process; several of these studies represent the state-of-the-art in characterization and suggest a trajectory for the continued development of the field. Based on this review, a set of grand challenges for characterization science is identified, including suggestions for instrumentation advances, scientific problems in microstructure analysis, and complex structure evolution problems involving material damage. The future of microstructural characterization is proposed to be one not only where individual techniques are pushed to their limits, but where the community devises strategies of technique synergy to address complex multiscale problems in materials science and engineering.

Eight FePt thin film specimens of various thicknesses, compositions, and order parameters have been analyzed to determine the robustness and fidelity of multislice simulations in determining the chemical order parameter via electron diffraction (ED). The shape of the simulated curves depends significantly on the orientation and thickness of the specimen. The ED results are compared to kinematical scattering order parameters, from the same films, acquired from synchrotron X-ray diffraction (XRD). For the specimens analyzed with convergent beam electron diffraction conditions, the order parameter closely matched the order parameter as determined by the XRD methodology. However, the specimens analyzed by selected area electron diffraction conditions did not show good agreement. This has been attributed to substrate effects that hindered the ability to accurately quantify the intensity values of the superlattice and fundamental reflections.