Nanoindentation Technique Research Articles

Characterizing nano-indentation and microstructural properties of mine tailings-based geopolymers

The mining industry's extraction processes produce vast amounts of waste, including mine tailings (MT), traditionally stored in large ponds, causing significant environmental harm due to a lack of effective recycling methods. This research explores the potential of converting MT into a resource i.e., precursors in geopolymer synthesis. By analyzing the physicochemical and mineralogical properties of MT, the study formulates four geopolymer composites, substituting up to 30 wt% MT for fly ash. The composites' mechanical and microstructural properties show a contribution of MT in the stability of the matrix. Compressive strength of 59 MPa when incorporating 30 wt% MT, along with water absorption, microstructural analysis, and environmental impact assessments, support the hypothesis that the matrix is improved. Nano-indentation techniques further evaluated the nanomechanical properties, such as Young's modulus and fracture toughness. The findings reveal that geopolymers with 30 wt% MT exhibits up to 130 % increased strength. This research highlights the potential for innovative, eco-friendly solutions in waste management and material production, contributing to sustainable mining practices and advancing the field of geopolymer technology.

Comparison of the mechanical properties of Mo films by different nanoindentation techniques

Nanocrystalline Mo films were prepared by magnetron sputtering. Indentation size effect (ISE) on hardness (H) was both studied by constant strain rate method (CSR) and continuous stiffness method (CSM). Inverse ISE appears and H from CSR is higher than that from CSM. Significant dislocation motion barrier effect of increased grain boundary (GB) induces strengthening. Each step of CSM promotes the generation of heterogeneous GBs and enhances GB-emitting dislocations ability, leading to softening.

Deposition of nanocomposite carbon-based thin films doped with copper and fluorine

This paper is focused on plasma-enhanced chemical vapor deposition (PECVD) of novel carbon-based thin films. Unique thin films were deposited from a mixture of methane, hydrogen, and a precursor containing fluorine and copper: (hfac)copperVTMS (hfac = hexafluoroacetylacetonato and VTMS = vinyltrimethylsilane). Using the (hfac)copperVTMS precursor in PECVD deposition results in the advantageous chemical composition of carbon-based thin films while maintaining sufficient mechanical properties. Furthermore, with optimized plasma parameters, the films deposited on the substrate exhibit a nanocomposite structure. This nanostructured surface can increase the surface area, which is beneficial for various applications, including antibacterial and antiviral properties. The radiofrequency glow discharge at low pressure (≈70Pa) and power P=25W and P=250W was used for deposition. Deposited thin films were analyzed using X-ray photoelectron spectroscopy, water contact angle measurement, atomic force microscopy, and nanoindentation techniques. Despite the doping of carbon-based thin films with soft copper, the prepared films exhibited sufficient mechanical properties, which are crucial for the future implementation of this deposition process.

Surface modification of superduplex stainless steel with C and N: Microstructural and nanomechanical insights

In this study, the effect of thermochemical processes, such as nitriding and carburizing, on the microstructural evolution of superdúplex stainless steel is presented. The objective is to find a correlation between the microstructure and the mechanical properties of the constitutive phases of this stainless steel (i.e., austenite and ferrite) and analyze the diffusion elements influence on the precipitation of secondary phases, such as sigma (σ), chi (χ), nitrides, and carbides. Hardness (H) and elastic modulus (E) maps were obtained by using a high-speed nanoindentation technique. H and E values for the individual phases were determined through the application of Gaussian Mixture Model statistical analysis. Assessments of the mechanical properties of the different phases were achieved by overlaying field emission-scanning electron microscopy micrographs. An excellent correlation between microstructure and small-scale mechanical properties was attained. Secondary phases have been detected and nanoindentation statistics have proven their influence on the mechanical properties.

New elucidating into the microstructural evolution mechanisms and micromechanical properties of C4AF and gypsum synergistic hydration

Increasing the C4AF content significantly enhances the sulfate and impact resistance of Portland cement-based materials. However, the research on the microstructural evolution mechanisms and micromechanical properties of the binary synergistic hydration products of C4AF and gypsum is not yet sufficiently deep. This study employed thermodynamic simulations, phase structure characterization, and nanoindentation techniques to investigate the microstructure evolution of gypsum-assisted C4AF hydration. Results indicated that the final hydration product of C4AF, C3(A,F)H6, formed through the stacking of lamellar OH-AFm phases. The addition of gypsum altered the formation pathway of C3(A,F)H6, causing it to precipitate directly from an amorphous iron-aluminum gel, which resulted in smaller particles with higher crystallinity. Gypsum also filled pores in the hydration products, thereby positively influenced their micromechanical properties.

Atomic force microscopy-based nanoindentation technique for characterizing the transverse and shear moduli of flax fibers

Experimentally evaluating the elastic properties of flax fibers is challenging due to their complex hierarchical structure, and a standard test procedure for measuring their transverse and shear moduli is currently not reported in the literature. Hence, this study presents an atomic force microscopy (AFM) based nanoindentation technique to evaluate the transverse and shear moduli of flax fiber. A high-precision focused ion beam (FIB)-milling process was used to fabricate a flat surface for indentation along the longitudinal fiber cross-section of the fiber and transverse fiber cross-section by polishing the unidirectional (UD) lamina in order to evaluate the indentation modulus. Further, Swanson's numerical contour approach was adopted to evaluate the elastic properties of the fiber from the measured indentation modulus. The accuracy of the experimentally obtained fiber properties is verified by using it in a micromechanics model for predicting the elastic properties of the UD lamina and comparing it with experimental results reported in the literature.

EFFECT OF PHENOL FORMALDEHYDE RESIN IMPREGNATION ON NANODYNAMIC VISCOELASTICITY OF PINUS MASSONIANA LAMB IN WET STATE

We evaluated the effects of phenol formaldehyde (PF) resin modification on Masson pine (Pinus massoniana Lamb.) wood cell wall in wet states. The penetration degree of PF resin into wood cell was determined using confocal laser scanning microscopy (CLSM). The micromechanical properties of PF-modified wood cell walls in wet state were analyzed by quasi-static nanoindentation and dynamic modulus mapping techniques. Results showed that the PF resin significantly affected the static viscoelasticity and nanodynamic viscoelasticity of wood cell walls in oven-dried and wet states. The cell-wall mechanics increased at a PF resin concentration due to the increased bulking effects, such as decreased crystallinity of cellulose. Furthermore, the microfibrillar angle (MFA) of cell walls was lower than that of the control wood cell wall. The cell-wall mechanics of PF resin-modified sample decreased small than control sample in wet states.

Effects of coarse aggregate size on thickness and micro-properties of ITZ and the mechanical properties of concrete

This research delves into the impact of coarse aggregate particle size on the mechanical properties of concrete. Nano-indentation and scanning electron microscope (SEM) techniques were applied to characterize the micro-properties and thickness the Interfacial Transition Zone (ITZ). The effect of coarse aggregate size on concrete's compressive strength (σc) and elastic modulus (E) and the relationship between the micro properties of the ITZ and the macro properties of concrete were discussed. In addition, Griffith's microcrack theory was adopted to explain related mechanisms. The relationship between the microscopic properties of the ITZ and the macroscopic properties of concrete was discussed. The results show that, in concrete with a low water cement-ratio w/c (0.3), thickness of ITZ increased with the coarse aggregate size and concrete properties decreased. While, in concrete with a higher w/c (0.4), there exists an optimum coarse aggregate size for the lowest thickness of ITZ and highest strength. Taking the ITZ as the initial crack in concrete failure, concrete properties can be linked to ITZ thickness from Griffith's microcrack theory.

Effect of fly ash and nano Silica on the formation and evolution of Calcium Silicate Hydrate in Portland Cement during hydration process

Recently, the trend of replacing cement with mineral admixtures in concrete has witnessed increasing interest in the construction industry due to the reduction in embodied energy and CO2 emissions. However, the addition of these admixtures in Portland Cement (PC) affected the formation as well as the structure of the hydration product Calcium-Silicate-Hydrate (C-S-H), which is reflected in the mechanical and durability properties of cement concrete. In the present study, nano-silica (NS) and a mixture of fly ash (FA) and NS were replaced into PC (PC + 0.5 % NS, PC + 1 % NS, PC + 0.5 % NS + 20 % FA and PC + 1 % NS + 40 % FA) to systematically study the formation and structural evolution of hydration products, namely C-S-H, at atomic and micro-scales at the early stage of hydration (3 days) and a later stage of hydration (90 days). The formation and structure of C-S-H were analyzed to correlate the microstructure development by using XRD, Rietveld technique, FESEM, TEM, FTIR and nano-scale mechanical properties by employing the nanoindentation techniques. Atomic Pair Distribution Function (PDF) is used to understand the effect of admixtures on the C-S-H structure from atomic point of view. PDF shows the structural modification of C-S-H such as different polyhedral, separation of intralayer/interlayer, pair/bond length, coordination number of atoms corresponding to the addition of additives with hydration age. Also, porosity measurements show increasing or decreasing porosity during hydration with additives. It is observed that the contribution of low-density C-S-H (LD C-S-H) is greater than that of high-density C-S-H (HD C-S-H) in the beginning days, whereas HD C-S-H more than LD C-S-H in the latter days of hydration. The elastic modulus increased from 15.44 GPa to 19.82 GPa and the hardness decreased from 0.41 GPa to 0.35 GPa of LD C-S-H in early days, whereas elastic modulus decreased from 34.84 GPa to 29.33 GPa and the hardness increased from 0.75 GPa to 0.83 GPa of HD C-S-H in the latter stage due to addition of additives. However, both increased for LD C-S-H and HD C-S-H for each corresponding mixture during hydration. The present study reported the formation and microstructural modifications of C-S-H and the correlation with nano-mechanical properties due to addition of nano or micro-sized admixtures (nano silica and fly ash) in the cement system. This correlation helps to develop low-energy cement composites by tailoring cement systems with desired properties.

Silica infiltration as a strategy to overcome zirconia degradation

The excellent clinical performance of yttria-partially stabilized zirconias (Y-SZs) makes them promising materials for indirect restorations. However, the Y-SZ phase stability is a concern, and infiltrating Y-SZs with a silica nanofilm may delay their degradation processes. In this study, we analyzed stabilities of silica-infiltrated zirconia surfaces after exposure to artificial aging (AA).Four zirconia materials with different translucencies (n = 40) were used, including low translucency 3 mol% Y-SZ (3Y-LT, Ceramill ZI, Amann Girrbach); high translucency 4 mol% Y-SZ (4Y-HT, Ceramill Zolid); and two high translucency 5 mol% Y-SZs (5Y-HT, Lava Esthetic, 3M and 5Y-SHT, Ceramill Zolid, FX white). Sintered specimens were exposed to 40 cycles of silica (SiO2) through room temperature atomic layer deposition (RT-ALD) using tetramethoxysilane (TMOS) and ammonium hydroxide (NH4OH). AA was applied for 15 h in an autoclave (134°C, 2 bar pressure). Stabilities of zirconia-silica surfaces were characterized in terms of hardness and Young's modulus using nanoindentation techniques and crystalline contents using x-ray diffraction (XRD) analyses. Silica deposition was also characterized by X-ray photoelectron spectroscopy (XPS).There was a significant effect of the interaction of materials and surface treatments on the hardness and Young's modulus values of zirconia-silica surfaces (p < 0.001). Silica deposition on zirconia surfaces improved the material resistance to degradation by AA.

Exploring W-EUROFER brazed joints: S/TEM and nanoindentation analysis following post-brazing tempering treatment

Tempering treatments are essential for restoring the hardness and microstructure of EUROFER steel when W-EUROFER joints are formed at temperatures exceeding the steel's austenitization point (890 °C). This post-brazing heat treatment can, however, alter the microstructure and thereby affect the mechanical properties. This study explores the microstructural and nanomechanical effects in the brazed area of W-EUROFER joints following this heat treatment, utilizing copper as an intermediate filler material. Using Scanning Transmission Electron Microscopy (STEM) with Energy Dispersive Spectroscopy (EDS) on FIB lamellae and nanoindentation techniques we examined the stability and phase characteristics of the post-tempered microstructure in two lamellae that covers the whole phases of the braze microstructure.The tempering process enhances copper diffusion and the growth of copper precipitates without significantly altering the joint's overall microstructure. Despite the general stress-relief effects of tempering, which typically lower mechanical properties, the diffusion phases formed during brazing maintained high hardness and modulus, indicative of a complex, element-rich composition. A reduction in mechanical properties was observed in the iron-rich phase near the W-braze interface and the EUROFER base material, aligning with the purpose of the heat treatment. However, the copper braze and tungsten base material largely retained their stability and resilience to thermal treatments.This research provides vital insights into the behavior of these material systems under thermal processing, highlighting the necessity of optimizing heat treatment parameters to preserve joint integrity in high-performance applications such as nuclear fusion reactors. The findings contribute significantly to the development of durable and reliable materials for fusion energy, emphasizing the importance of controlled tempering processes to enhance material properties.

Investigating microstructure dynamics and strain rate sensitivity in gradient nanostructured AISI 304 L stainless steel: TEM and nanoindentation insights

In recent years, gradient nanostructured (GNS) materials have gained significant attention due to their superior strength-ductility balance and enhanced functional properties compared to their coarse-grained counterparts. This research examines the microstructure evolution and nanomechanical responses of GNS AISI 304 L austenitic stainless steel using transmission electron microscopy (TEM) and nanoindentation techniques. Through surface mechanical attrition treatment (SMAT), a gradient nanostructured layer with ultrafine grains (∼15 nm) and nanoscale martensite (up to ∼40 %) within the austenite matrix has been successfully created on the steel’s surface. This treated surface exhibits a hardness of ∼6.7 GPa, nearly double the original value. The GNS layer demonstrates single-step (γ → α’) and two-step (γ → ε → α’) martensitic transformations, deformation twinning (γ -twin), a decrease in the density of deformation bands, compressive residual stress, lattice strain, and martensite content, along with an increase in grain size. Strain rate sensitivity (SRS) increases with austenitic grain size and inversely correlates with martensite proportion as depth increases in the GNS layer. A significant amount of ultrafine martensite is primarily responsible for the limited SRS in the topmost layer.

Micro-mechanical properties of Song Dynasty tilestones based on nanoindentation tests and homogenization approach

Song Dynasty tilestones are one type of ancient Chinese building materials. Studying their mechanical properties is of great significance for the design and development of restoration materials. It is a challenge to sample and perform traditional tests (ϕ50mm × 100mm) for the tilestone cultural relics. In this work, a combination of nanoindentation techniques and the homogenization calculation method based on the Mori–Tanaka model were used to determine the mechanical parameters of Song Dynasty tilestones. The study process involved several steps: (1) Using X-ray diffraction and scanning electron microscopy to examine the surface morphology and mineral composition of the tilestones. (2) Determining the mechanical parameters (i.e., the elastic modulus, hardness and fracture toughness) through nanoindentation tests. (3) Upgrading mechanical parameters from micro to meso-scale using the Mori–Tanaka model and comparing these with uniaxial compression test results. The result shows that the red tilestones and green tilestone are mainly composed of quartz, feldspar and mica. The average elastic modulus of the red tilestones and the green tilestones are 29.47 GPa and 30.21 GPa, respectively. Compared with the parameter result obtained by upscaling, the deviation rates of the red tilestones and green tilestones are 10.3% and 9.6%, respectively, which proves that the test method is reliable. The nanoindentation test and homogenization approach in this work provide the robust theoretical and practical basis for evaluating the mechanical strength of Song Dynasty tilestones.

Evaluation of plasma process-induced mechanical property change in SiN films using a cyclic nanoindentation technique

Evaluation of plasma process-induced mechanical property change in SiN films using a cyclic nanoindentation technique

HARDENING BEHAVIOR OF NUCLEAR STRUCTURAL MATERIALS UNDER ION IRRADIATION

The evaluation of irradiation hardening and embrittlement is critically important for the development of next generation nuclear structural materials tolerant to neutron irradiation. This review summarizes research progress on experimental observations aimed at elucidating the mechanisms of radiation induced hardening in ion irradiated materials, focusing on the correlation between irradiation effects and mechanical property changes. We present the basic information for the application of ion irradiation and nanoindentation techniques to characterize the mechanical properties of nuclear structural materials. The effects of irradiation on advanced structural materials, including oxide dispersion strengthened (ODS) austenitic steels, ferritic martensitic steels, and high entropy alloys, are analyzed. The dependence of hardening parameters on the irradiation dose and their relationship with microstructural evolution are examined. Findings indicate that these advanced alloys exhibit reduced susceptibility to irradiation induced hardening compared to conventional austenitic stainless steels.

Increase in elastic and hardness anisotropy of titanium with oxygen uptake due to high temperature oxidation: A multimodal framework using high speed nanoindentation mapping

Titanium and its alloys combine an important mechanical anisotropy and a high capacity to dissolve oxygen. The detailed evolution of the elastic compliance of titanium as a function of its oxygen content is only partially known, despite its importance in structural applications. Here, high speed nanoindentation mapping (HSNM) was conducted on a grade 2 commercially pure titanium (CP-Ti) to probe elastic and hardness anisotropy as well as property evolution as a function of the oxygen content within Ti using pre-oxidized specimens. The oxygen concentration investigated ranged from 600 ppm to 20% atomic. Pre-oxidation of the CP-Ti was performed at 700 °C for 100 h under air to create a gradient of oxygen content within the metal, denoted oxygen-rich layer (ORL). Local oxygen content was quantified using microprobe analyses (EPMA) and crystal orientation using electron backscattered diffraction (EBSD). Reduced modulus and hardness maps were obtained on the pre-oxidized sample within the ORL and far from the ORL using large but highly resolved nanoindentation technique in continuous stiffness measurement (CSM) mode. Data merging techniques were used on this multi-modal dataset to statistically link local mechanical properties to chemical and crystal orientation information. Oxygen insertion in the Ti lattice was found to significantly increase the hardness and elastic moduli of titanium and was correlated to orientation of the c-axis of the α-Ti as a function of the nanoindentation loading direction. Using the Vlassak and Nix theory, it was possible to identify the evolution of the Cij terms of the stiffness matrix as a function of the oxygen content up to 20% at. in O.

Effect of MWCNTs-OH on the mechanical properties of cement composites: From macro to micro perspective

This study is focused on elucidating the role and mechanism of hydroxyl-functionalized multi-walled carbon nanotubes (MWCNTs-OH) as a reinforcement material in cement-based composites. The dispersion of MWCNTs-OH within the cement composites was first assessed using Raman spectroscopy. Subsequently, SEM, FT-IR, TGA, XRD, and nano-indentation techniques were employed to investigate the structural transformation and phase changes occurring in the cement matrix upon incorporating MWCNTs-OH. The results reveal that MWCNTs-OH can significantly improve the macro-mechanical properties of cement composites by their capacity for pulling out, pore-filling, inducing multi-cracking, and promoting hydration. From a micro-perspective, observations of the micro-morphology demonstrate that MWCNTs-OH reinforces cement composites through crack-bridging and pull-out effects. Regarding the hydrated calcium silicate (C-S-H), the addition of MWCNTs-OH has a negligible impact on the ratio of low-density C-S-H (LD-CSH) to high-density C-S-H (HD-CSH). Moreover, the results obtained from FT-IR and XRD tests provide evidence that the bonding between MWCNTs-OH and the cement matrix is predominantly governed by physical interactions.

Atomistic insight of deformation mechanisms and mechanical characteristics of nano-scale silver (100) using nanoindentation

This work aims to utilize the widely adopted nanoindentation technique to explore the deformation behavior and mechanical characteristics of nanocrystalline silver (Ag) materials. Molecular Dynamics simulations were conducted to understand the material behavior at the nanometer scale. In this simulation, the effect of indentation velocity and indentation depth on defect formation and hardness during nanoindentation of Ag specimens was analyzed and discussed in detail. The results show that the deformation behavior of the Ag specimen was affected by different indentation velocities. These phenomena were confirmed by analyzing the load-displacement curve, which indicates elastic deformation by the appearance of a linear load-displacement at low indentation velocities. In contrast, plastic deformation was found by the presence of intensified serration in the load-displacement relationship at higher indentation velocities. In these cases, the hardness showed little variation when the indenter velocity was increased from 5 m/s to 10 m/s, whereas a significant increase in hardness was observed when the indentation velocity was further increased to 20 m/s. Importantly, the progression of load-displacement curves during nanoindentation demonstrates the occurrence of minor and major load drops, corresponding to an increase in indentation depth from 0.5 nm to 2 nm respectively. These findings were elucidated through dislocation extraction analysis (DXA), which revealed that a minor load drop at low indentation depths is attributed to the nucleation of an amorphous structure, while a major load drop at higher indentation depths is associated with the expansion of dislocation nucleation. Consequently, the hardness increased significantly as the indentation depth increased. This research, provides insight into atomistic investigation and offers guidelines for designing materials with excellent mechanical properties using nanoindentation.

Effect of hydrogen on the microstructural evolution and local mechanical properties of 430 ferritic stainless steel at high-temperature conditions

The present study investigated the impact of hydrogen on the microstructural evolution and mechanical properties of 430 ferritic stainless steel at high-temperature conditions. Hydrogen trap sites were analyzed at high temperatures using thermal desorption spectrometry through high-temperature hydrogen atmosphere charging and electrolytic hydrogen charging. The microstructural evolution was characterized using scanning electron microscopy and electron backscatter diffraction. The nanoindentation technique was employed to analyze the local mechanical properties of ferrite matrix, grain boundaries, and M23C6/matrix interfaces. Hydrogen trap sites in 430 ferritic stainless steel included ferrite crystal lattice, grain boundaries, intragranular dislocations, and M23C6/matrix interfaces where hydrogen could not intrude at room temperature. At high temperatures, hydrogen caused a decrease in grain size. Furthermore, at high temperatures, hydrogen altered the crystal orientation and texture of the ferrite matrix. There was an increase in the number of ferrite grains with (001) and (101) orientation increase and the formation of a new α-fiber texture. Hydrogen inhibited the triggering of the slip system in body centered cubic crystal lattice and induced an increase in dislocation density and internal stress. While hydrogen at high temperatures had a minimal impact on the matrix strength limit, it reduced the strength limit of the near grain boundaries and (Fe, Cr)23C6 precipitates. The influence of hydrogen on the microstructural evolution and mechanical properties of 430 ferritic stainless steel could be elucidated by the mechanisms of hydrogen enhanced decohesion, hydrogen-enhanced localized plasticity, and hydrogen enhanced specific crystal plane rotation suggested in the present study.

Combining fast scanning chip calorimetry and nanoindentation: Young's modulus and hardness of poly (l-lactic acid) containing α′- and α-crystals

Fast scanning chip calorimetry (FSC) allows subjecting polymer melts to well-defined vitrification, crystal nucleation, and crystal growth pathways and, therefore, precise control of morphologies, from fully amorphous glassy states to semicrystalline structures containing perfect crystals. Due to the required use of nanogram-sized samples, needed to achieve high cooling rates, their mechanical properties, in order to establish structure-property relations, are difficult to assess. In this work, indentation modulus and indentation hardness of FSC samples are successfully determined on example of semicrystalline poly (ʟ-lactic acid) (PLLA) containing spherulitically grown disorder α′- or rather perfect α-crystals, with the correctness of the applied preparation and analyses routes confirmed by nanoindentation measurements on milligram-sized samples prepared through hotstage microscopy, and by applying both static single-step and quasi-continuous stiffness measurements. Modulus and hardness data are consistent with prior analyses of bulk samples, confirming that semicrystalline PLLA containing α-crystals exhibits around 10–20 % higher values of these properties compared to PLLA containing α′-crystals, related to the different molecular-chain packing in the crystal lattice. This work demonstrates that combination of FSC and nanoindentation techniques is an effective tool for determining mechanical properties of samples solidified at specific thermal pathways which otherwise cannot be realized.