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DOE OSTI2021

Exploring the origins of the indentation size effect at submicron scales

Significance Downscaling material structure into ever-decreasing levels for modern technological advancements demands small-scale mechanical characterizations of materials, such as nanoindentation. Thus, a comprehensive understanding of indentation size effect (ISE) has a far-reaching impact, but such understanding remains incomplete at the submicron scale despite a decades-long quest since the 1980s. Here, we explored the origins of this effect experimentally by linking dislocation behavior evolution with nanoindentation mechanical data at various depths. Importantly, the dislocation behavior is found to be strongly depth dependent and gives rise to subgrain formation progressively. Aided by subgrain boundaries, the ISE mechanism transitions from dislocation source starvation to dislocation interaction as indentation depth increases. The critical mechanism transition elucidates the distinctive ISE behavior at the submicron scale.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Synergy of tensile strength and high cycle fatigue properties in a novel additively manufactured Al-Ni-Ti-Zr alloy with a heterogeneous microstructure

Alloy design strategies in additive manufacturing (AM) to achieve grain refinement and terminal eutectic solidification have been introduced to engineer Al alloys having microstructural hierarchy and heterogeneity. Such alloy design strategies enable crack-free builds with an expanded AM processing window and pushed the strength limit in Al alloys. However, fatigue performance of Al alloys made by AM is restricted by the presence of process induced defects and its stochasticity. In this work, tensile and high cycle fatigue (HCF) behavior of a novel Al-Ni-Ti-Zr alloy with a heterogeneous microstructure is studied in the as-built condition, supplemented by detailed microstructural and mechanical characterization. Excellent strength-ductility synergy of 342 MPa and 16% failure strain achieved in the alloy was associated with the microstructural attributes that pertain to the novel alloy. Additionally, the alloy showed excellent HCF performance with a fatigue endurance limit to ultimate tensile strength ratio of 0.29 in flexural fatigue mode. The study revealed the existence of multiple crack retardation mechanisms and favorable crack propagation pathways through the fine-grained regions which enabled good fatigue performance to the alloy. Further, a probabilistic model has been used to estimate the fatigue life of the alloy as a function of the stochastic microstructure by utilizing the statistical distribution of pores, solid-state inclusions, and grains in the AM Al alloy. Finally, the model parametric trends are consistent with the experimental observations.

36 MATERIALS SCIENCE↗

DOE OSTI2023

The characterization of wear-causing particles and silica sand in particular

Erodants and abradants are two types of wear-causing particles (WCP). Despite their effects on the severity and rate of wear, WCP are inadequately characterized in a surprising number of publications, especially those involving impingement erosion and three-body abrasion. That shortfall makes it difficult to correlate features of WCP with the details of worn surfaces, or to develop wear models that account for those features. It is argued that the documentation of WCP should go beyond simply reporting their composition and mean particle size. In late 1985, ASTM Committee G2 on Wear and Erosion established a task group on the characterization of WCP. At that time, image analysis was slower and less sophisticated than it is today. While that ASTM task group failed to produce a consensus standard, computerized particle characterization methods were developing in fields other than tribology, fields like geoscience, heavy sand mining, materials processing, and pharmaceuticals. A notable exception to this is ferrography, which is a widely-used diagnostic for lubricated tribosystems. In the context of dry wear, it is useful to identify which features of WCP would be beneficial to document, and to identify some techniques and scales of detail appropriate to particular tribosystems. In this paper, examples are presented for the morphological and mechanical characterization of silica sand grains, as prompted by a triboanalysis of the abrasive and erosive wear of biomass pre-processing equipment. The authors propose a minimum level of documentation for WCP, one that can enrich tribosystem analysis both in laboratory tests and field studies.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Experimental Assessment of Elastic Modulus vs. Relative Density for Stretch- and Bend-Dominated Lattices

This project was designed to study the possibility of using structural properties of lattices to replicate the material properties of certain hard to manufacture designs and use topology optimization to determine the lattice type and density required to mimic these properties. The integration of additively manufactured lattice structures with topology optimization highlights the need for well characterized mechanical properties and uncertainty analyses to insure these optimized structures respond as predicted. Stereolithographically printed octet and rhombic dodecahedron lattices were manufactured at 10%, 25% and 65% density by volume. As a separate task, yet integrated into this work, finite element analysis (FEA) was used to predict the printed lattice’s mechanical properties, which were then compared to our experimental results. After comparing FEA and experimentallymeasured elastic moduli, it was determined that the FEA provides highly reliable predictions for the modulus of these printed lattice structures. These lattices also exhibited greater tensile stiffness than that of the solid material demonstrating the flexibility that lattices provide to designing parts with designer structural properties. The accurate printing and reliable modeling of these lattices will enable topology optimization of complex parts from well-characterized rhombic dodecahedron and octet lattice structures of varying densities.

36 MATERIALS SCIENCE↗

DOE OSTI2021

High-fidelity first principles nonadiabaticity: diabatization, analytic representation of global diabatic potential energy matrices, and quantum dynamics

We report nonadiabatic dynamics, which goes beyond the Born–Oppenheimer approximation, has increasingly been shown to play an important role in chemical processes, particularly those involving electronically excited states. Understanding multistate dynamics requires rigorous quantum characterization of both electronic and nuclear motion. However, such first principles treatments of multi-dimensional systems have so far been rather limited due to the lack of accurate coupled potential energy surfaces and difficulties associated with quantum dynamics. In this Perspective, we review recent advances in developing high-fidelity analytical diabatic potential energy matrices for quantum dynamical investigations of polyatomic uni- and bi-molecular nonadiabatic processes, by machine learning of high-level ab initio data. Special attention is paid to methods of diabatization, high fidelity construction of multi-state coupled potential energy surfaces and property surfaces, as well as quantum mechanical characterization of nonadiabatic nuclear dynamics. To illustrate the tremendous progress made by these new developments, several examples are discussed, in which direct comparison with quantum state resolved measurements led to either confirmation of the observation or sometimes reinterpretation of the experimental data. The insights gained in these prototypical systems greatly advance our understanding of nonadiabatic dynamics in chemical systems.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Uncertainty-Based Design: Finite Element and Explainable Machine Learning Modeling of Carbon–Carbon Composites for Ultra-High Temperature Solar Receivers

Design under uncertainty has significantly grown in research developments during the past decade. Additionally, machine learning (ML) and explainable ML (XML) have offered various opportunities to provide reliable predictable models. The current article investigates the use of finite element modeling (FEM), ML and XML predictions, and uncertain-based design of carbon-carbon (C-C) composites for use in ultra-high temperatures. A C-C composite concentrating solar power (CSP) as a microvascular receiver is considered as a case study. These C-C composites are fiber composites with directly integrated carbonized microchannels to form a lightweight, high-absorptivity material that includes an embedded microvascular network of channels. The topology of these microchannels is engineered to optimize heat transfer to a supercritical carbon dioxide (sCO2) heat transfer fluid. The mechanical characterization of C-C composites is highly challenging. Thus, designing every component made of C-C composites for ultra-high temperature applications needs an uncertainty-based analysis. As a part of a comprehensive project on the development of a novel carbonized microvascular C-C composite, this paper explores C-C composite sensitivity analysis, FEM, ML prediction, and XML analysis. The resulting composite can then be carbonized and coated with an oxidation-resistant coating to form a thermally efficient and mechanically robust C-C composite. An ANSYS 3-D-FE model was used to analyze the CSP’s stress/strain. To consider the variability in the mechanical and thermal properties of C-C composites, various mechanical properties are considered as the ANSYS FEM’s input. A synthetic dataset from 730 ANSYS runs was produced to feed into the ML and XML algorithms for uncertainty analysis and prediction. The ML and XML algorithms could accurately predict the CSP stresses/strains.

Daghigh, Vahid (ORCID:0000000298941620)↗

DOE OSTI2026

Ionic-content-driven restructuring of spirobisindane ionene networks: implications for mechanics, self-healing, and gas transport

Polymers of intrinsic microporosity (PIMs) offer exceptional gas permeability but remain brittle and susceptible to physical aging, limiting their durability in separation applications. Here, we introduce a reconfigurable microporous polymer network that uniquely integrates permanent PIM microporosity with autonomous, intrinsic self-healing driven by imidazolium-based ionic motifs. Spirobisindane units generate the intrinsic free-volume architecture, while an imidazolium-containing polyamide ionene supplies dynamic ionic and hydrogen-bonding interactions that reorganize under mild activation. Incorporation of imidazolium-based ionic liquids further tunes cohesion, mobility, and densification, enabling the network to relax, re-associate, and retain microporosity without structural collapse. Through a comprehensive multiscale approach combining spectroscopy, scattering, thermal and mechanical characterization with all-atom molecular dynamics and density functional theory calculations, we elucidate how ionic content, as a single control parameter that reshapes free-volume distributions, modulates local coordination environments, and governs relaxation and healing kinetics. At intermediate ionic loadings, the networks achieve rapid, repeatable self-healing while maintaining CO$_2$ selectivity, demonstrating an optimal balance between segmental mobility and structural integrity. By establishing how hierarchical ionic interactions couple structure, dynamics, and transport in microporous ionene networks, this work provides generalizable design rules for adaptive soft-matter systems that require simultaneous mechanical resilience, reconfigurability, and selective gas transport.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Effect of the Segmental Structure of Thermoplastic Polyurethane (Hardness) on the Interfacial Adhesion of Textile-Grade Carbon Fiber Composites

In polymer composites, the fiber–matrix interface is primarily influenced by the surface treatment of the fibers and polymer morphology. Previous studies have investigated the effect of surface treatment of carbon fiber on the mechanical properties of the resulting composites. However, very few studies have explored the chemical structural modification of polymer effect on the fiber–matrix adhesion. In this work, the interfaces of soft thermoplastic polyurethane (S-TPU) and hard-segmented TPU (H-TPU) were investigated through surface, thermal, and mechanical characterization. A textile-grade carbon fiber (TCF) with 1% concentration of epoxy sizing (an emerging material for nonaerospace applications with 450 K filament tows) was used as a reinforcement to investigate the structure–property relationship at the interface. Atomic force microscopy results showed 39% higher surface roughness for S-TPU than for H-TPU. X-ray photoelectron spectroscopy results revealed a 550% increase in C=O content, which can provide multiple hydrogen bonding networks in H-TPU, and these C=O bonds can produce a strong chemical bond at the fiber–matrix interface. Additionally, dynamic mechanical analysis and differential scanning calorimetry results confirmed the presence of hydrogen bonding that enhances the cross-linked density by 232% in H-TPU compared to S-TPU. The improved mechanical properties of H-TPU composites, such as flexural, impact and tensile by 30, 50, and 130% compared to S-TPU composites, prove that the crystallinity and hydrogen bonding significantly increase the load bearing capacity due to the strong interface. The mechanical properties of TCF–TPU composites validate the formation of chemical bonds through a nucleophilic addition reaction at the interface and improve the bond strength of the composites. Thus, tailoring the polyurethane structure broadens the performance of segmented TPU in conjunction with TCF reinforcement, which has implications for cost-effective, high-strength composites.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Improvement of interfacial adhesion of unidirectional textile grade carbon fiber (TCF) with unsized, epoxy and urethane sizing reinforced in thermoset urethane composites

This work considers a unique wide tow (450k filaments) form of low-cost carbon fiber intended for non-aerospace applications. TCF is currently produced in epoxy and urethane sizing, and there is a need to understand its resulting composite properties. In this work, the interfacial adhesion of sized TCF reinforced in thermoset urethane (TSU) composites are examined through the surface, thermal and mechanical characterization techniques. Atomic force microscopy (AFM) results showed an increase in surface roughness for urethane (276%) and epoxy sized (78%) versus unsized TCF. XPS results showed 531% increase in O in epoxy sized TCF and 250% N content in urethane sized TCF compared to unsized TCF. The surface energy of epoxy and urethane sized TCF is enhanced by 78% and 96%, respectively compared to unsized TCF. The storage modulus showed improvement for urethane (23%) and epoxy (21%) sized than unsized TCF-TSU composites. The flexural, interlaminar shear strength (ILSS), and impact properties of urethane sized TCF increase by 24%, 50%, and 273%, respectively, than unsized TCF. The results demonstrate that the surface and thermal properties correlate with the mechanical properties of TCF-TSU composites and sizing enhances the wettability of the composites.

36 MATERIALS SCIENCE↗

DOE OSTI2020

The effect of loading direction on the fracture behaviors of cortical bone at a dynamic loading rate

Here, the dynamic cracking processes in porcine cortical bone were visualized in real-time using the high-speed synchrotron X-ray phase-contrast imaging (PCI) technique in three osteon orientations: in-plane transverse, out-of-plane transverse and in-plane longitudinal. The dynamic flexural loading applied on the pre-notched bone specimens was introduced by a modified Kolsky compression bar. High-speed X-ray images of the entire loading events were documented with a high-speed camera. Three-dimensional X-ray micro-computed tomography was conducted to examine the intact microstructures and obtain the basic material properties of the bone material used for mechanical characterizations. The onset location, where crack initiated, and the subsequent direction, along which the incipient crack propagated, were measured quantitatively using the high-speed X-ray images and the latter was found dependent on the osteon direction significantly. The crack propagation velocities were dependent on crack extension over the entire crack path significantly for all the three directions while the initial velocity for in-plane longitudinal direction was lower than the other two directions. Straight-through crack paths were observed for in-plane longitudinal specimens while the cracks were deflected and twisted in the in-plane transverse direction. For out-of-plane transverse direction, the cracks follow paths with tortuosity fall in between the other two directions, showing a mixed mode of fractures of the former two extreme cases. The toughening mechanisms, visualized by the high-speed X-ray images, and the corresponding fracture toughness, evaluated in terms of fracture initiation toughness and crack growth resistance curve (R-curve), were also found significantly different among the three osteon directions, suggesting an overall transition from brittle to ductile-like fracture behaviors at the dynamic displacement rate (5.4 m/s) as the osteon orientation varies from in-plane longitudinal to out-of-plane transverse, and to in-plane transverse eventually.

42 ENGINEERING↗

DOE OSTI2021

Responses of the Plant Cell Wall to Sub-Zero Temperatures: A Brief Update

Our general understanding of plant responses to sub-zero temperatures focuses on mechanisms that mitigate stress to the plasma membrane. The plant cell wall receives comparatively less attention, and questions surrounding its role in mitigating freezing injury remain unresolved. Despite recent molecular discoveries that provide insight into acclimation responses, the goal of reducing freezing injury in herbaceous and woody crops remains elusive. This is likely due to the complexity associated with adaptations to low temperatures. Understanding how leaf cell walls of herbaceous annuals promote tissue tolerance to ice does not necessarily lead to understanding how meristematic tissues are protected from freezing by tissue-level barriers formed by cell walls in overwintering tree buds. In this mini-review, we provide an overview of biological ice nucleation and explain how plants control the spatiotemporal location of ice formation. We discuss how sugars and pectin side chains alleviate adhesive injury that develops at sub-zero temperatures between the matrix polysaccharides and ice. The importance of site-specific cell-wall elasticity to promote tissue expansion for ice accommodation and control of porosity to impede ice growth and promote supercooling will be presented. How specific cold-induced proteins modify plant cell walls to mitigate freezing injury will also be discussed. The opinions presented in this report emphasize the importance of a plant’s developmental physiology when characterizing mechanisms of freezing survival.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2026

High Temperature High Vacuum Mechanical Property Assessment of Zirconium Nuclear Fuel Cladding

This report presents the mechanical characterization of a specific Zry-4 cladding batch serving as the foundation for a diverse range of fuel performance research at Oak Ridge National Laboratory (ORNL). This effort supports research needs for the U.S. Department of Energy (DOE), particularly regarding evaluating accident tolerant fuel (ATF) cladding coating concepts, expanding understanding of cladding response to loss-of-coolant accidents (LOCA) transients, refining post-critical heat flux (CHF) limits (t@T), and upcoming irradiation campaigns. The central objective was to define the baseline performance of the substrate Zircaloy-4 (Zry-4) material leveraged across ORNL Advanced Fuel Campaign (AFC) efforts through controlled high-temperature vacuum tensile testing. This work begins to address gaps in existing models where implementation based on nominal heat-treatment labels, such as stress relief annealed (SRA), often fail to capture the interplay of recovery, recrystallization, and grain growth. To quantify this, data was benchmarked against the Pacific Northwest National Laboratory (PNNL) stress strain model to determine where this material falls in comparison to assumed values for materials in the same heat treatment regime. Analysis of the tensile data revealed that this specific SRA batch exhibits a transitional microstructural state best described by an effective cold-work (CW) parameter of 0.09, diverging from the previous estimation of 0.5 for SRA materials. Additionally, comparative testing of Cr coated specimens demonstrated no distinct difference in axial strength relative to the bare substrate. This suggests that the strengthening benefits of Cr coatings observed in burst scenarios are driven by residual stress mechanisms acting solely in the hoop direction.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2025

Morphological Heterogeneity Impact of Film Solid-State Cathode on Utilization and Fracture Dynamics

Structural heterogeneity in solid-state batteries can impact material utilization and fracture mechanisms. Crystallographically oriented lithium cobalt oxide film cathodes serve as a model electrode system for exploring how void distribution contributes to stress relief and build up during cycling. Real- and reciprocal-space operando and ex situ synchrotron based experiments are utilized to understand structural changes across multiple length scales contribute to stress generation and fracture. Nanotomography uncovers a depth-dependent porosity variation in the pristine electrode and highlights preferential fracture in regions of lower porosity during delithiation. Energy-dispersive X-ray diffraction and 3D X-ray absorption near-edge spectroscopy (XANES) reveal the underutilization of cathode material in these regions. 3D XANES also confirms preferential delithiation near the sub-grain boundaries. Chemo-mechanical modeling coupled with site-specific mechanical characterization demonstrate how stress accumulation in dense regions of the electrode leads to fracture and underutilization of active material. In conclusion, our findings reveal the importance of materials design to alleviate stress in small-volume changing cathodes.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Coupling Thermal-Hydraulics with Reactor Pressure Vessel Fracture Models

Because of the importance of maintaining the integrity of the reactor pressure vessel (RPV) in light-water reactors, significant effort has been devoted over the last several decades to understand the potential failure mechanisms, characterize how material properties evolve due to environmental conditions, and develop tools to assess the probability of fracture in aged RPVs during potential transient events. One important aspect of this problem that has not yet been fully addressed is the effects of nonuniform cooling on the RPV inner wall due to the way low-temperature water injected into the primary coolant system is distributed within the RPV during potential loss-of-coolant accident transients. Colder temperatures are expected in the regions near the inlets, causing a “cold-plume” effect. Rapid cooling of the RPV wall increases the likelihood of fracture initiation, and localized cooling due to cold-plume effects could potentially exacerbate this problem. The Grizzly code can perform a three-dimensional simulation of the RPV thermomechanical response as well as the probabilistic assessment of fracture for a population of pre-existing flaws, which is necessary to account for spatial variations in coolant temperature. This report documents a first effort to couple Grizzly RPV fracture models with computational fluid dynamics models performed using the Cardinal code, which allows for a realistic representation of the temperature distribution. This report demonstrates this coupling approach on two test cases: a simplified proof-of-concept scenario and a realistic small-break loss-of-coolant accident scenario. In both cases, the effects of the spatially varying temperature are evident; although, because the small-break loss-of-coolant accident scenario was far from challenging the RPV’s margins, it is still inconclusive how important cold-plume effects are in realistic accident scenarios. However, this effort represents an important step toward performing realistic analyses to determine to what extent spatially nonuniform cooling might affect RPV integrity under more aggressive accident scenarios.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2021

Integrating Emerging Polymer Chemistries for the Advancement of Recyclable, Biodegradable, and Biocompatible Electronics

Abstract Through advances in molecular design, understanding of processing parameters, and development of non‐traditional device fabrication techniques, the field of wearable and implantable skin‐inspired devices is rapidly growing interest in the consumer market. Like previous technological advances, economic growth and efficiency is anticipated, as these devices will enable an augmented level of interaction between humans and the environment. However, the parallel growing electronic waste that is yet to be addressed has already left an adverse impact on the environment and human health. Looking forward, it is imperative to develop both human‐ and environmentally‐friendly electronics, which are contingent on emerging recyclable, biodegradable, and biocompatible polymer technologies. This review provides definitions for recyclable, biodegradable, and biocompatible polymers based on reported literature, an overview of the analytical techniques used to characterize mechanical and chemical property changes, and standard policies for real‐life applications. Then, various strategies in designing the next‐generation of polymers to be recyclable, biodegradable, or biocompatible with enhanced functionalities relative to traditional or commercial polymers are discussed. Finally, electronics that exhibit an element of recyclability, biodegradability, or biocompatibility with new molecular design are highlighted with the anticipation of integrating emerging polymer chemistries into future electronic devices.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Borehole breakout modeling in arkose and granite rocks

The existence of a deep borehole in the Earth’s crust disturbs the local stresses and creates a stress concentration that may result in breakout and damage to the borehole. Maintaining wellbore integrity mitigates environmental impacts such as groundwater contamination, gas leakage to the atmosphere, and fluid spills and seepage at the surface. In this paper, the stability of deep boreholes (5 km) is examined by laboratory experiments and numerical models in the context of nuclear waste disposal in Israel. Two rock types in southern Israel are considered: the crystalline basement (granite) and the Zenifim Formation (arkose). A series of room-temperature triaxial rock deformation experiments were conducted at different confining pressures. This mechanical characterization was then used to parameterize the elastic properties and damage behavior of the rocks. This facilitated modeling the stability of the deep boreholes by two different formulations of damage rheology: a dynamic-oriented formulation used to model deformation immediately after the creation of the open hole and a quasi-static formulation used to model longer stress corrosion regime. The calibrated modeling results indicate greater stability with Zenifim arkose than the crystalline granite for deep borehole conditions despite the granite having a greater triaxial compressive strength. Dissipation associated with dilation and porous compaction in the arkose during deformation plays a significant stabilizing role in the borehole compared to crystalline rocks. These results suggest that common strength-based borehole stability assessment may lead to inaccurate predictions. Three-dimensional modeling of bottom-hole stress conditions and the effects of transient borehole geometry show conventional two-dimensional analysis may not be conservative when predicting borehole damage.

58 GEOSCIENCES↗

DOE OSTI2024

Manufacturing Oxide Dispersion Strengthened (ODS) steel plate via cold spray and friction stir processing

Oxide dispersion strengthened (ODS) steels, traditionally fabricated by ball milling and conventional powder metallurgy techniques to achieve bulk form, followed by intricate rolling and thermal treatment steps to achieve plate or sheet form. Here, we present a novel processing route that combines cold spray (CS) with friction stir processing (FSP) to manufacture ODS steel plate directly from gas atomization reaction synthesis (GARS)-prepared powder, thus no rolling steps involved. Microstructural and mechanical characterizations were performed to assess the quality and properties of the resulting ODS steel plate. Our findings demonstrate that the slightly porous CS deposited layer was fully consolidated after FSP, yielding a fully dense ODS steel plate that exhibited a favorable tradeoff between strength and ductility upon extraction from the substrate. Furthermore, through microstructural analysis, we revealed the presence of an appreciable density (∼10 22 /m 3 ) of nano-sized oxide particles, with the majority being smaller than 5 nm via the combined CS + FSP fabrication route. This work serves as a first proof-of-concept demonstration of the manufacturing approach described herein, offering a possible alternative route for producing ODS steel plates.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Nanoscale Examination of Chemical and Enzymatic Degradation of Plant Cell Walls

Lignocellulosic materials present the largest source of biomass for biotechnology and green energy. This study aimed at better understanding the cell wall disintegration mechanisms relevant for the biochemical conversion of biomass to carbohydrates. Herein, we examined nanoscale changes in cell wall structure and composition upon industrially relevant chemical and enzymatic treatments to achieve the desired level of breakdown. One treatment involved hydrogen peroxide and acetic acid to remove lignin. Another modification used the cellulase enzyme for cell wall degradation. Band excitation contact resonance atomic force microscopy was used to visualize and mechanically characterize cell wall layers. After cellulase treatments, we detected microcracks across the cell wall. Wet-chemical, Fourier-transform infrared and Raman spectroscopic analyses confirmed the removal of lignin and extractives through acid bleaching, while the enzymatic treatment minimally affected the biopolymer composition. Delignification resulted in cell wall delamination and reduced stiffness. In conclusion, X-ray diffraction revealed changes in cellulose structure and crystallinity.

Soini, Steven A. [Florida Atlantic Univ., Boca Rat↗