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At least 973 records · Page 54

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DOE OSTI2019

Challenge and Solution of Characterizing Glass Transition Temperature for Conjugated Polymers by Differential Scanning Calorimetry

Thermomechanical properties of polymers greatly depend on their glass transition temperature ( T g ). Differential scanning calorimetry (DSC) is commonly used to measure T g of polymers. Yet, many conjugated polymers (CPs), especially donor–acceptor CPs (D–A CPs), do not show a clear glass transition when measured by conventional DSC using simple heat and cool scan. In this work, we discuss the origin of the difficulty for measuring T g in such type of polymers. The changes in specific heat capacity (Δ c p ) at T g were accurately probed for a series of CPs by DSC. The results showed a significant decrease in Δ c p from flexible polymer (0.28 Jg -1 K -1 for polystyrene) to rigid CPs (10 -3 Jg -1 K -1 for a naphthalene diimide-based D–A CP). When a conjugation breaker unit (flexible unit) is added to the D–A CPs, we observed restoration of the Δ c p at T g by a factor of 10, confirming that backbone rigidity reduces the Δ c p . Additionally, an increase in the crystalline fraction of the CPs further reduces Δ c p . We conclude that the difficulties of determining T g for CPs using DSC are mainly due to rigid backbone and semicrystalline nature. We also demonstrate that physical aging can be used on DSC to help locate and confirm the glass transition for D-A CPs with weak transition signals.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Three-dimensional phenotyping of peach tree-crown architecture utilizing terrestrial laser scanning

Tree training systems for temperate fruit have been developed throughout history by pomologists to improve light interception, fruit yield, and fruit quality. These training systems direct crown and branch growth to specific configurations. Quantifying crown architecture could aid the selection of trees that require less pruning or that naturally excel in specific growing/training system conditions. Regarding peaches [Prunus persica (L.) Batsch], access tools such as branching indices have been developed to characterize tree-crown architecture. However, the required branching data (BD) to develop these indices are difficult to collect. Traditionally, BD have been collected manually, but this process is tedious, time-consuming, and prone to human error. These barriers can be circumnavigated by utilizing terrestrial laser scanning (TLS) to obtain a digital twin of the real tree. TLS generates three-dimensional (3D) point clouds of the tree crown, wherein every point contains 3D coordinates (x, y, z). To facilitate the use of these tools for peach, we selected 16 young peach trees scanned in 2021 and 2022. These 16 trees were then modeled and quantified using the open-source software TreeQSM. As a result, “in silico” branching and biometric data for the young peach trees were calculated to demonstrate the capabilities of TLS phenotyping of peach tree-crown architecture. The comparison and analysis of field measurements (in situ) and in silico BD, biometric data, and quantitative structural model branch uncertainty data were utilized to determine the reconstructive model’s reliability as a source substitute for field measurements. Mean average deviation when comparing young tree (YT) height was approx. 5.93%, with crown volume was approx. 13.26% across both 2021 and 2022. All point clouds of the YTs in 2022 showed residuals lower than 12 mm to cylinders fitted to all branches, and mean surface coverage greater than 40% for both the trunk and primary branching orders.

09 BIOMASS FUELS↗

DOE OSTI2024

Tip-Induced 3D Printing on the Nanoscale with Field Emission Scanning Probes

3D printing down to the nanoscale remains a significant challenge. In this paper, the study explores the use of scanning probes that emit low-energy electrons (<100 eV) coupled with the localized injection and electron-induced decomposition of precursor molecules, for the precise localized deposition of 3D nanostructures. The experiments are performed inside the chamber of a scanning electron microscope (SEM), enabling the use of the in-built gas injector system (GIS) with gaseous naphthalene precursor for carbon deposition, as well as immediate inspection of the deposits by SEM. Substrate materials are planar fused silica with thin conductive coatings and non-planar copper wedges. After investigation of the deposition process parameters, various 2D and 3D carbon deposits are grown. Vertical nanowires several microns in length with a diameter <100 nm are achieved and 3D deposits with a high degree of nanoscale branching are also obtained, presumably due to a charging effect. High aspect ratio carbon nanostructures such as those demonstrated here can be employed as miniaturized electrodes or field emitters. The tip-based approach presented thus paves the way toward 3D nanoscale printing of various materials and functional nanostructures.

3D printing↗

DOE OSTI2023

A Platform for Atomic Fabrication and In Situ Synthesis in a Scanning Transmission Electron Microscope

Here, the engineering of quantum materials requires the development of tools able to address various synthesis and characterization challenges. These include the establishment and refinement of growth methods, material manipulation, and defect engineering. Atomic-scale modification will be a key enabling factor for engineering quantum materials where desired phenomena are critically determined by atomic structures. Successful use of scanning transmission electron microscopes (STEMs) for atomic scale material manipulation has opened the door for a transformed view of what can be accomplished using electron-beam-based strategies. However, serious obstacles exist on the pathway from possibility to practical reality. One such obstacle is the in situ delivery of atomized material in the STEM to the region of interest for further fabrication processes. Here, progress on this front is presented with a view toward performing synthesis (deposition and growth) processes in a scanning transmission electron microscope in combination with top-down control over the reaction region. An in situ thermal deposition platform is presented, tested, and deposition and growth processes are demonstrated. In particular, it is shown that isolated Sn atoms can be evaporated from a filament and caught on the nearby sample, demonstrating atomized material delivery. This platform is envisioned to facilitate real-time atomic resolution imaging of growth processes and open new pathways toward atomic fabrication.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Correlation of Processing and Structure in an Ethylene‐Glycol Side‐Chain Modified Polythiophene via Combined X‐Ray Scattering and 4D Scanning Transmission Electron Microscopy

The results of a combined grazing incidence wide-angle X-ray scattering (GIWAXS) and 4D scanning transmission microscopy (4D-STEM) analysis of the effects of thermal processing on poly(3[2-(2-methoxyethoxy)ethoxy]-methylthiophene-2,5-diyl) are reported, a conjugated semiconducting polymer used as the active layer in organic electrochemical transistor devices. GIWAXS provides a measure of overall crystallinity in the film, while 4D-STEM produces real-space maps of the morphology and orientation of individual crystallites along with their spatial extent and distribution. The sensitivity of the 4D-STEM detector allows for collection of electron diffraction patterns at each position in an image scan while limiting the imparted electron dose to below the damage threshold. In conclusion, the effects of heat treatment on the distribution and type of crystallites present in the films is determined.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Automatic Digitization and Orientation of Scanned Mesh Data for Floor Plan and 3D Model Generation

This paper describes a novel approach for generating accurate floor plans and 3D models of building interiors using scanned mesh data. Unlike previous methods, which begin with a high resolution point cloud from a laser range-finder, our approach begins with triangle mesh data, as from a Microsoft HoloLens. It generates two types of floor plans, a “pen-and-ink” style that preserves details and a drafting-style that reduces clutter. It processes the 3D model for use in applications by aligning it with coordinate axes, annotating important objects, dividing it into stories, and removing the ceiling. Its performance is evaluated on commercial and residential buildings, with experiments to assess quality and dimensional accuracy. Our approach demonstrates promising potential for automatic digitization and orientation of scanned mesh data, enabling floor plan and 3D model generation in various applications such as navigation, interior design, furniture placement, facilities management, building construction, and HVAC design.

Sharma, Ritesh↗

DOE OSTI2021

Perseverance’s Scanning Habitable Environments with Raman and Luminescence for Organics and Chemicals (SHERLOC) Investigation

The Scanning Habitable Environments with Raman and Luminescence for Organics and Chemicals (SHERLOC) is a robotic arm-mounted instrument on NASA’s Perseverance rover. SHERLOC has two primary boresights. The Spectroscopy boresight generates spatially resolved chemical maps using fluorescence and Raman spectroscopy coupled to microscopic images (10.1 μm/pixel). The second boresight is a Wide Angle Topographic Sensor for Operations and eNgineering (WATSON); a copy of the Mars Science Laboratory (MSL) Mars Hand Lens Imager (MAHLI) that obtains color images from microscopic scales (~13 μm/pixel) to infinity. SHERLOC Spectroscopy focuses a 40 μs pulsed deep UV neon-copper laser (248.6 nm), to a ~100 μm spot on a target at a working distance of ~48 mm. Fluorescence emissions from organics, and Raman scattered photons from organics and minerals, are spectrally resolved with a single diffractive grating spectrograph with a spectral range of 250 to ~370 nm. Because the fluorescence and Raman regions are naturally separated with deep UV excitation (<250 nm), the Raman region ~ 800 – 4000 cm -1 (250 to 273 nm) and the fluorescence region (274 to ~370 nm) are acquired simultaneously without time gating or additional mechanisms. SHERLOC science begins by using an Autofocus Context Imager (ACI) to obtain target focus and acquire 10.1 μm/pixel greyscale images. Chemical maps of organic and mineral signatures are acquired by the orchestration of an internal scanning mirror that moves the focused laser spot across discrete points on the target surface where spectra are captured on the spectrometer detector. ACI images and chemical maps (< 100 μm/mapping pixel) will enable the first Mars in situ view of the spatial distribution and interaction between organics, minerals, and chemicals important to the assessment of potential biogenicity (containing CHNOPS). Single robotic arm placement chemical maps can cover areas up to 7x7 mm in area and, with the < 10 min acquisition time per map, larger mosaics are possible with arm movements. This microscopic view of the organic geochemistry of a target at the Perseverance field site, when combined with the other instruments, such as Mastcam-Z, PIXL, and SuperCam, will enable unprecedented analysis of geological materials for both scientific research and determination of which samples to collect and cache for Mars sample return.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2019

Prevalence and variability in reporting of clinically actionable incidental findings on attenuation-correction CT scans in a veteran population

Background: Myocardial perfusion imaging (MPI) often employs attenuation-correction computed tomography (CTAC) to reduce attenuation artifacts and improve specificity. While there is no specific guideline on how they should be reported, incidental noncardiac findings identified on these scans may be clinically significant. The prevalence of these findings in veterans is not currently known. In addition, variability in reporting these findings may depend on the interpreting physician’s specialty. Methods: To guide future decision-making, CTACs in veterans referred for MPI were prospectively evaluated in a quality-control project for a set of prespecified actionable incidental findings by cardiologists and a radiologist. Results: On the 771 scans performed over eight months, 285 incidental noncardiac findings were identified by the interpreting cardiologists and 378 were identified by the interpreting radiologist. Pulmonary nodules were the most common occurring in 20% of studies read by the radiologist. Interreader agreements between cardiologists and the radiologist were poor for pulmonary nodules ≥ 10 mm and hiatal hernias; fair for pulmonary nodules < 10 mm, extracardiac masses, and aortic aneurysms; and moderate for pleural plaques. Conclusion: Incidental noncardiac findings on CTACs are common in our veteran population. Overall interobserver agreement in identifying these findings between cardiologists and radiologists is fair. Specific guidelines are needed on how CTACs should be read and reported.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

DOE OSTI2022

Mapping structural heterogeneity at the nanoscale with scanning nano-structure electron microscopy (SNEM)

Here, in this work, we explore the use of scanning electron diffraction (also known as 4D-STEM) coupled with electron atomic pair distribution function analysis (ePDF) to understand the local order (structure and chemistry) as a function of position in a complex multicomponent system, a hot rolled, Ni-encapsulated, Zr 65 Cu 17.5 Ni 10 Al 7.5 bulk metallic glass (BMG), with a spatial resolution of 3 nm. We show that it is possible to gain insight into the chemistry and chemical clustering/ordering tendency in different regions of the sample, including in the vicinity of nano-scale crystallites that are identified from virtual dark field images and in heavily deformed regions at the edge of the BMG. In addition to simpler analysis, unsupervised machine learning was used to extract partial PDFs from the material, modeled as a quasi-binary alloy, and map them in space. These maps allowed key insights not only into the local average composition, as validated by EELS, but also a unique insight into chemical short-range ordering tendencies in different regions of the sample during formation. The experiments are straightforward and rapid and, unlike spectroscopic measurements, don’t require energy filters on the instrument. We spatially map different quantities of interest (QoI’s), defined as scalars that can be computed directly from positions and widths of ePDF peaks or parameters refined from fits to the patterns. We developed a flexible and rapid data reduction and analysis software framework that allows experimenters to rapidly explore images of the sample on the basis of different QoI’s. The power and flexibility of this approach are explored and described in detail. Because of the fact that we are getting spatially resolved images of the nanoscale structure obtained from ePDFs we call this approach scanning nano-structure electron microscopy (SNEM), and we believe that it will be powerful and useful extension of current 4D-STEM methods.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Influence of scan pattern and geometry on the microstructure and soft-magnetic performance of additively manufactured Fe-Si

The influence of geometry and scan pattern on the microstructure evolution and magnetic performance of additively manufactured Fe-3Si components was investigated. To reduce eddy current losses, novel geometries were designed and built and the microstructure and properties of these samples were characterized. The laser scan pattern was shown to strongly influence both the as-built grain structure and strength of the crystallographic texture, resulting in measurable changes in the as-built magnetic performance. In thin wall samples, heat treatment resulted in an increase in the maximum relative magnetic permeability and decrease in power losses in most samples, consistent with grain growth. However, decreases in the spacing between thin walls to increase the stacking factor of the cross-section was shown to result in unwanted electrical shorting between walls and an increase in eddy current losses. Compared to simple parallel plate construction and a mesh structure, a novel cross-section design based on the Hilbert space filling curve was found to produce the lowest power losses. The mechanisms behind these results were explored using a combination of heat conduction and electromagnetic simulations, providing a route for future component and process optimization.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Spot-Scanning Proton Radiation Therapy for Pediatric Chordoma and Chondrosarcoma: Clinical Outcome of 26 Patients Treated at Paul Scherrer Institute

Purpose: To evaluate the clinical results of fractionated spot-scanning proton radiation therapy (PT) in 26 pediatric patients treated at Paul Scherrer Institute for chordoma (CH) or chondrosarcoma (CS) of the skull base or axial skeleton. Methods and Materials: Between June 2000 and June 2010, 19 CH and 7 CS patients with tumors originating from the skull base (17) and the axial skeleton (9) were treated with PT. Mean age at the time of PT was 13.2 years. The mean prescribed dose was 74 Gy (relative biological effectiveness [RBE]) for CH and 66 Gy (RBE) for CS, at a dose of 1.8-2.0 Gy (RBE) per fraction. Results: Mean follow-up was 46 months. Actuarial 5-year local control (LC) rates were 81% for CH and 80% for CS. Actuarial 5-year overall survival (OS) was 89% for CH and 75% for CS. Two CH patients had local failures: one is alive with evidence of disease, while the other patient succumbed to local recurrence in the surgical pathway. One CS patient died of local progression of the disease. No high-grade late toxicities were observed. Conclusions: Spot-scanning PT for pediatric CH and CS patients resulted in excellent clinical outcomes with acceptable rates of late toxicity. Longer follow-up time and larger cohort are needed to fully assess tumor control and late effects of treatment.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

DOE OSTI2014

Four-Dimensional Patient Dose Reconstruction for Scanned Ion Beam Therapy of Moving Liver Tumors

Purpose: Estimation of the actual delivered 4-dimensional (4D) dose in treatments of patients with mobile hepatocellular cancer with scanned carbon ion beam therapy. Methods and Materials: Six patients were treated with 4 fractions to a total relative biological effectiveness (RBE)–weighted dose of 40 Gy (RBE) using a single field. Respiratory motion was addressed by dedicated margins and abdominal compression (5 patients) or gating (1 patient). 4D treatment dose reconstructions based on the treatment records and the measured motion monitoring data were performed for the single-fraction dose and a total of 17 fractions. To assess the impact of uncertainties in the temporal correlation between motion trajectory and beam delivery sequence, 3 dose distributions for varying temporal correlation were calculated per fraction. For 3 patients, the total treatment dose was formed from the fractional distributions using all possible combinations. Clinical target volume (CTV) coverage was analyzed using the volumes receiving at least 95% (V{sub 95}) and 107% (V{sub 107}) of the planned doses. Results: 4D dose reconstruction based on daily measured data is possible in a clinical setting. V{sub 95} and V{sub 107} values for the single fractions ranged between 72% and 100%, and 0% and 32%, respectively. The estimated total treatment dose to the CTV exhibited improved and more robust dose coverage (mean V{sub 95} > 87%, SD < 3%) and overdose (mean V{sub 107} < 4%, SD < 3%) with respect to the single-fraction dose for all analyzed patients. Conclusions: A considerable impact of interplay effects on the single-fraction CTV dose was found for most of the analyzed patients. However, due to the fractionated treatment, dose heterogeneities were substantially reduced for the total treatment dose. 4D treatment dose reconstruction for scanned ion beam therapy is technically feasible and may evolve into a valuable tool for dose assessment.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

DOE OSTI2015

Reducing Dose Uncertainty for Spot-Scanning Proton Beam Therapy of Moving Tumors by Optimizing the Spot Delivery Sequence

Purpose: To develop and validate a novel delivery strategy for reducing the respiratory motion–induced dose uncertainty of spot-scanning proton therapy. Methods and Materials: The spot delivery sequence was optimized to reduce dose uncertainty. The effectiveness of the delivery sequence optimization was evaluated using measurements and patient simulation. One hundred ninety-one 2-dimensional measurements using different delivery sequences of a single-layer uniform pattern were obtained with a detector array on a 1-dimensional moving platform. Intensity modulated proton therapy plans were generated for 10 lung cancer patients, and dose uncertainties for different delivery sequences were evaluated by simulation. Results: Without delivery sequence optimization, the maximum absolute dose error can be up to 97.2% in a single measurement, whereas the optimized delivery sequence results in a maximum absolute dose error of ≤11.8%. In patient simulation, the optimized delivery sequence reduces the mean of fractional maximum absolute dose error compared with the regular delivery sequence by 3.3% to 10.6% (32.5-68.0% relative reduction) for different patients. Conclusions: Optimizing the delivery sequence can reduce dose uncertainty due to respiratory motion in spot-scanning proton therapy, assuming the 4-dimensional CT is a true representation of the patients' breathing patterns.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

DOE OSTI2017

Prompt Gamma Imaging for In Vivo Range Verification of Pencil Beam Scanning Proton Therapy

Purpose: To report the first clinical results and value assessment of prompt gamma imaging for in vivo proton range verification in pencil beam scanning mode. Methods and Materials: A stand-alone, trolley-mounted, prototype prompt gamma camera utilizing a knife-edge slit collimator design was used to record the prompt gamma signal emitted along the proton tracks during delivery of proton therapy for a brain cancer patient. The recorded prompt gamma depth detection profiles of individual pencil beam spots were compared with the expected profiles simulated from the treatment plan. Results: In 6 treatment fractions recorded over 3 weeks, the mean (± standard deviation) range shifts aggregated over all spots in 9 energy layers were −0.8 ± 1.3 mm for the lateral field, 1.7 ± 0.7 mm for the right-superior-oblique field, and −0.4 ± 0.9 mm for the vertex field. Conclusions: This study demonstrates the feasibility and illustrates the distinctive benefits of prompt gamma imaging in pencil beam scanning treatment mode. Accuracy in range verification was found in this first clinical case to be better than the range uncertainty margin applied in the treatment plan. These first results lay the foundation for additional work toward tighter integration of the system for in vivo proton range verification and quantification of range uncertainties.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

DOE OSTI2017

Development of first ever scanning probe microscopy capabilities for plutonium

Scanning probe microscopy capabilities have been developed for plutonium and its derivative compounds. Specifically, a scanning tunneling microscope and an atomic force microscope housed in an ultra-high vacuum system and an inert atmosphere glove box, respectively, were prepared for the introduction of small non-dispersible δ-Pu coupons. Experimental details, procedures, and preliminary imaging of δ-Pu coupons are presented to demonstrate the functionality of these new capabilities. In conclusion, these first of a kind capabilities for plutonium represent a significant step forward in the ability to characterize and understand plutonium surfaces with high spatial resolution.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2014

Intergrowth structure of α-phase in β-type TmAlB{sub 4} compound studied by high-angle annular detector dark-field scanning transmission electron microscopy

Nanostructure of a ThMoB{sub 4}-type (β-type) TmAlB{sub 4} compound, in which YCrB{sub 4}-type (α-type) domains are locally intergrown, is studied by high-angle annular detector dark-field scanning transmission electron microscopy (HAADF-STEM). Z-contrast images by HAADF-STEM directly represent the arrangements of Tm atoms located at centers of heptagonal atomic columns of B atoms as bright dots, and give us detailed information of intergrowth of type domains in the matrix of the β-type phase, which coherently occurs. Structural and bonding analyses for β-TmAlB{sub 4} point out the closeness in atomic interactions and energy of the α- and β-type structures which support the easy formation of such nanostructure intergrowths. From combination between HAADF-STEM and electronic structure calculation, a detailed local crystal structure with intrinsic building defects is effectively revealed. - Graphical abstract: Nanostructure of a ThMoB{sub 4}-type (β-type) TmAlB{sub 4} compound, in which YCrB{sub 4}-type (α-type) domains are locally intergrown, is studied by high-angle annular detector dark-field scanning transmission electron microscopy (HAADF-STEM). Z-contrast images by HAADF-STEM directly represent arrangements of Tm atoms located at centers of heptagonal atomic columns of B atoms as bright dots, and give us detailed information of the characteristic intergrowth structure of type domains in the matrix of the β-type phase. - Highlights: • HAADF-STEM images directly represent arrangements of Tm atoms as bright dots. • The α-type planar domains coherently intergrown in the β-type matrix. • Bright strips appear at overlapped regions of Tm hexagons along interfaces between α- and β-type domains.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2018

Characterization of dislocation microstructures in cyclically deformed [001] copper single crystals using high voltage scanning transmission electron microscopy

Highlights: • High voltage scanning transmission electron microscopy is adopted. • Dislocation structure strongly depends on given plastic strain amplitude. • Evolution of dislocation structure from vein-like to labyrinth is revealed. - Abstract: Low-cycle fatigue tests of copper single crystals with the [001] stress axis were performed at room temperature under constant plastic shear strain amplitudes between γ{sub pl} = 3.5 × 10{sup − 4} and 1.0 × 10{sup − 2}. Characteristic dislocation structures, which are highly dependent on a given plastic strain amplitude, were observed by high voltage scanning transmission electron microscopy. A vein-like dislocation structure, having a parallelepiped shape with two longitudinal (100) and (001) sides, was periodically formed along the [010] direction at around γ{sub pl} = 1.0 × 10{sup − 3}. Labyrinth structure with the (100) and (001) dislocation walls was then gradually developed with increasing plastic strain amplitude.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Scan strategies in EBM-printed IN718 and the physics of bulk 3D microstructure development

Three-dimensional (3D) characterization provides opportunities for understanding processing-structure relationships in additively manufactured (AM) materials. Bulk samples of Inconel 718 were fabricated via electron beam melting (EBM) in order to study microstructural development as a function of energy input and beam scan strategy. TriBeam tomography of bulk Inconel 718 microstructures built under steady-state growth conditions reveals the sensitivity of microstructure formation and evolution to machine process parameters. Here, samples manufactured using a narrow range of energy input per unit build area result in varied grain morphologies and crystallographic textures. Using TRUCHAS, a thermal simulation software, the thermal history of bulk scan strategies was predicted, and combined with a calibrated microstructure-processing map to accurately predict bulk grain morphologies. The solidification parameters and the 3D measured nucleation density are used to predict the transition between columnar and equiaxed grain morphologies, providing a process map to guide AM parameter choices to locally control as-printed microstructure. A two-dimensional metric for characterizing bulk grain morphology was also found to agree well with predictions from the process map calibrated by 3D data. Combined with 3D tomography and thermal modelling, the physics of structure development were understood at a new level of detail with respect to the competing processes of grain nucleation and epitaxial growth.

36 MATERIALS SCIENCE↗