Compressive residual stresses in thin films can inhibit crack propagation under normal or sliding contact loading, with associated enhancement of the coating apparent toughness, load bearing capacity and wear resistance. This study investigates the influence of residual stress distributions on the thin film/substrate adhesion using a nanoindenter coupled with scanning electron microscope (SEM) investigations of indentation induced failure modes. Reactive and un-reactive magnetron sputtering with ion plating was used to coat a (100) silicon substrate with aluminum nitride (AlN) with and without an aluminum (Al) adhesion layer. The presence of an Al bond layer gives additional interfacial tensile stress because of the difference in thermal expansion coefficient. Additionally, a different magnitude of residual stresses in the AlN coating was achieved by changing the applied bias voltage onto the substrate. Wafer curvature method and incremental focused ion beam (FIB) milling, combined with high-resolution in situ scanning electron microscopy (SEM) imaging and full field strain analysis by digital image correlation (DIC), were used to measure the average and in-depth stress residual stress distribution in the produced coatings. The adhesion energy was then quantified by using a nanoindentation based model. Results demonstrate that the additional tensile residual stress in the aluminum adhesion layer decrease significantly the coating adhesion, even in presence of a higher compressive stress state in the AlN top-layer. Therefore, the coatings without Al-layer showed better adhesion because of a more homogeneous compressive residual stress in comparison with the coating having Al layer, even though both groups of coatings are produced under same bias voltage. Results are discussed, and some general suggestions are made on the correlation between coating/substrate property combination and the adhesion energy of multilayer stacks. The results suggested that Al bond-layer and inhomogeneous residual stresses affected the adhesion of AlN negatively to a substrate like silicon.

The pop-in effect in nanoindentation of metals represents a major collective dislocation phenome-non that displays sensitivity in the local surface microstructure and residual stresses. To under-stand the deformation mechanisms behind pop-ins in metals, large scale molecular dynamics simulations are carried out to investigate the pop-in behavior and indentation size effect in unde-formed and deformed Cu single crystals. Tensile loading, unloading and reloading simulations are performed to create a series of samples subjected to a broad range of tensile strains with/without pre-existing dislocations. The subsequent nanoindentation simulations are con-ducted to study the coupled effects of pre-strain, the presence of resulting dislocations and surface morphology, as well as indenter size effects on the mechanical response in indentation processes. Our work provides detailed insights into the deformation mechanisms and microstruc-ture-property relationships of nanoindentation in the presence of residual stresses and strains.

Urgent environmental challenges and emerging additive manufacturing (AM) technologies push research towards more performant and new materials. In the field of metallurgy, high entropy alloys (HEAs) have recently represented a topic of intense research because of their promising properties, such as high temperature strength and stability. Moreover, this class of multi-principal element alloys (MPEAs) have opened up researcher community to unexplored compositional spaces, making prosper literature of high-throughput methodologies and tools for rapidly screening large number of alloys. However, none of the methods has been aimed to design new MPEAs for AM process known as selective laser melting (SLM) so far. Here we conducted nanoindentation testing on single scan tracks of elemental powder blends and pre-alloyed powders after ball milling of AlTiCuNb and AlTiVNb. Results show that nanoindentation can represent an effective technique to gain information about phase evolution during laser scanning, contributing to accelerate the development of new MPEAs.

In this study, the effect of ZnO nanoparticles (Zn NPs) on the performance of epoxy resin composites was investigated. The new ZnO/epoxy resin composites were synthesized using halloysite nanotubes (HNT) and different types of ZnO nanoparticles (commercial ZnO and ZnO-ODTES). These ZnO nanoparticles were utilized for intending to enhance the interfacial bonding between the epoxy resin and the reinforcement. Various methods such as FTIR, TGA, DSC, TEM-EDX, and Nanoindentation analyses were used to prove that the ZnO nanoparticles can improve the properties of epoxy resin composites. The thermal properties of the epoxy resin composites were enhanced to a greater extent by the addition of ZnO NPS. DSC testing proved that the epoxy resin composites modified with ZnO NPS are more flexible and elastic than unmodified epoxy resin. It was seen that the epoxy resin modified with ZnO-ODTES shows a much improved hardness and penetration depth compared to the other samples. These findings can pave the way for the developing of ZnO-based marine coatings with improved properties.

This paper describes a novel methodology of data management in materials characterisation, which has as starting point the creation and usage of Data Management Plan (DMP) for scientific data in the field of materials science and engineering, followed by the development and exploitation of ontologies for the harnessing of data created through experimental techniques. The case study that is discussed here is nanoindentation, a widely used method for the determination and/or modelling of mechanical properties on a small scale.The same methodology can be applicable to a large number of techniques that produce big amount of raw data, while at the same time it can be invaluable tool for big data analysis and for the creation of an open innovation environment, where data can be accessed freely and efficiently.Aspects covered include the taxonomy and curation of data, the creation of ontology and classification about characterization techniques, the harnessing of data in open innovation environments via database construction along with the retrieval of information via algorithms. The issues of harmonization and standardization of such novel approaches are also critically discussed.Finally, the possible implications for nanomaterial design and the potential industrial impact of the new approach are described and a critical outlook is given.

In this work, plastic deformation was locally introduced at room temperature by nanoindentation on a γ-TiAl based alloy. Comprehensive analyzes of microstructures were performed before and after deformation. In particular, the Burgers vectors, the line directions and the mechanical twinning systems were studied via accurate electron channeling contrast imaging. Accommodation of the deformation are reported and a scenario is proposed. All features help to explain the poor ductility of the TiAl based alloys at room temperature.

AFM nanoindentation showed variation in stiffness (Elastic modulus) due to heterogenous nature of the collagen fibres. The S values varied from 5 N/m to 11.11 n/m corresponding to an E change of 2.25 to 1.38 GPa. The variation in effective modulus (Eff) with respect to displacement indicated crossing the parabolic limit. A softening index n was proposed due to the heterogenous behaviour of the biomaterials

Hard coatings like Titanium diboride (TiB2) on silicon substrates are used for interconnects. micro-electro-mechanical devices and metallurgical protective coatings were analyzed based on shallow depths of nanoindentation penetration which involves a change in the nature of the contact from Hertzian to Pyramidal both in loading as well as unloading modes. Features like ductile fracture, linear unloading, and the creation of electrical conduction paths were analyzed. These high-precision features are influenced by the thickness and crystalline nature of the films and are significant for device fabrication.

Recent years witnessed progressive broadening of the practical use of 3D-printed aluminium alloy parts, in particular for specific aerospace applications where weight saving is of great importance. Selective laser melting (SLM) is an intrinsically multi-parametric fabrication technology that offers multiple means of controlling mechanical properties (elastic moduli, yield strength, ductility) through the control over grains size, shape, and orientation. Ultimately, this approach implies that structural elements can be purposefully fabricated to reinforce specific zones and directions where higher mechanical loads are anticipated by design. Targeted control over mechanical properties is achieved through the tuning of 3D-printing parameters and may even obviate the need of heat treatment or mechanical post-processing. Systematic studies of grain structure for different printing orientation with the help of EBSD techniques in combination with mechanical testing at different dimensional levels are the necessary first steps to implement this agenda. Samples of 3D-printable Al-Mg-Si RS-333 alloy were fabricated in 3 orientations with respect to the principal build direction and the fast laser beam scanning direction. Sample structure and proper-ties were investigated using a number of techniques, including EBSD, in situ SEM tensile testing, roughness measurements and nanoindentation. The as-printed samples we found to display strong variation in Young’s modulus values from nanoindentation (from 43 to 66 GPa) and tensile tests (from 54 to 75 GPa), yield stress and ultimate tensile strength (100…195 and 130…220 MPa) in different printing orientations, and almost constant hardness of about 0.8 GPa. A further preliminary study was conducted of the effect of surface finishing on the mechanical performance. Surface polishing appears to reduce Young’s modulus and yield strength, but improves ductility, whereas the influence of sand blasting is more controversial. The experimental results are dis-cussed in connection with the grain morphology and orientation.

A method for measuring the mechanical parameters of viscoelastic polymers by nanoindentation technology was proposed and verified. Through the mechanical response of load-displacement curves at different loading rates, then creep compliances and relaxation modulus were fitted. Polyimide thin film was employed in this research and experiments for five different loading rates were conducted. The fitting load-displacement loading curves obtained by the inversion method were identical to the experimental curves at five different loading rates，confirming the validity of the method. Moreover, with the loading rates increased，the fitting curves were more consistent commensurately with the nanoindentation experiment. DMA experiments were tested, and the generalized Kelvin/ Maxwell model were used for fitting experiment data. Results from DMA tests generally agree well with data from nanoindentation method, thereby verifying the feasibility of the method. The Prony series obtained by the two methods were used to simulate the creep experiments, which further verified the method.

Due to the high temperature limitation associated with silicon, SiC, Si₃N₄, TiC, TiN, TiB₂, cBN, CNx, SiO₂, Al₂O₃ and novel multicomponent nanocomposites polymer derived ceramics (PDC) based thin films like Si-C-N, Ti-Si-B-C-N and Si-O-CN that are compatible with silicon and have a wider range of operation in ambient conditions are being investigated. Apart from small scale electro-mechanical devices like N/MEMS, sensors, areas like metallurgical protection, water purification, energy storage, bio medical implants and aerospace have been benefited. The cross-sectional study involving the role of oxygen and nitrogen dissolution at different interfacial configurations has been presented.

A series of Ti₄₀Zr₂₅Cu₉Ni₈Be₁₈)_100-xTM_x (x = 0, 1, 2, 3, 4 at.%, TM = Nb, Y) Bulk amorphous alloys were designed and prepared using the copper mold casting method. The microstructures, glass forming ability and mechanical properties of the alloys were investigated by means of X-ray diffractometry (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), differential scanning colorimetry (DSC), depth-sensitive nanoindentation and uniaxial compressive test. The Bulk amorphous alloys with different ductility were investigated by measuring their plastic deformation energy (PDE) of the first pop-in events during loading. The relationships between the PDE value, shear band formation and ductility in Bulk amorphous alloys have been investigated. The results show that the PDE value decreases by the Nb addition and promotes the generation of multiple shear bands easily, which increase the fracture strength and plasticity significantly. Substituting Nb with Y has exactly the reverse effect. A useful rule for preparing of Bulk amorphous alloys with high plasticity is herein proposed, whereby the chemical composition of the Bulk amorphous alloys can be tailored to possess a lower PDE value.

In-situ nanoindentation experiment has been widely adopted to characterize material behaviors of microelectronic devices. This work introduces the latest developments of nanoindentation experiment in characterizing nonlinear material properties of 3D integrated microelectronic devices with through-silicon-vias (TSVs). The elastic, plastic, and interfacial fracture behavior of the copper via and matrix-via interface have been characterized using small scale specimens prepared with focused-ion-beam (FIB) and nanoindentation experiment. A brittle interfacial fracture was found at the Cu/Si interface under mixed-mode loading with a phase angle ranging from 16.7 to 83.7 degrees. The mixed-mode fracture strengths were extracted using the linear elastic fracture mechanics (LEFM) analysis and a fracture criterion was obtained by fitting the extracted data with the power-law function. The vectorial interfacial strength and toughness were found to be independent with mode-mix.

Using nanoindentation under various strain rates, the mechanical properties of a selective laser melted (SLM) SKD61 at the 800 mm/s scan speed was investigated and compared to SLM H13. No obvious pile-up due to the ratio of the residual depth (h_f) and the maximum depth (h_max) being lower than 0.7 and no cracking were observed on any of the indenter surfaces. The nanoindentation strain-rate sensitivity (m) of SLM SKD61 was found to be 0.034, with hardness increasing from 8.65 GPa to 9.93 GPa as the strain rate increased between 0.002 s⁻¹ and 0.1 s⁻¹. At the same scan speed, the m value of SLM H13 (m = 0.028) was lower than that of SLM SKD61, indicating that the mechanical behavior of SLM SKD61 was more critically affected by the strain rate compared to SLM H13. SLM processing for SKD61therefore shows higher potential for advanced tool design than for H13.

A CoCrFeNiNb0.65 eutectic high-entropy alloys (EHEAs) prepared by arc melting were irradiated with a 100 keV He+ ion beam. Swelling, helium bubbles and mechanical response induced by irradiation were evaluated. When the ion fluence reached 1.0×1018 ions/cm2, the irradiation-induced swelling occurred on the sample surface, and as the ion fluence increasing, the swelling became increasingly severe and the surface of Nb-rich phase appeared peeling and shedding. Meanwhile, along the boundaries of matrix and Nb-rich phase there was a neat line of helium bubbles. The size of these helium bubbles decreased with distance from the center of the helium bubble layer. This result indicated that the phase boundaries were favorable sites for the nucleation and gathering of helium bubbles. Nanoindentaion results indicated that hardening and softening induced by He+ ion irradiation occurred in various ion fluences. At ion fluence of 5.0×1017 ions/cm2, the CoCrFeNiNb0.65 EHEAs exhibited an obvious hardening behavior, which can be explained by dislocation-dominated hardening effect. When the ion fluence reached 1.0×1018 ions/cm2 and 2.0×1018 ions/cm2, the hardening effect decreased probably due to the helium bubble aggregation and growth, as well as helium bubbles induced noncompact structures. The results of this study provide insights into the effect of helium bubbles on mechanical evolution and pave the way for designing EHEAs suitable for the nuclear industry.

We present a high-throughput nanoindentation study of in-situ bending effects on incipient plastic deformation behavior of polycrystalline and single-crystalline pure aluminum and pure copper at ultra-nano depths (<200nm). We find that hardness displays a statistically inverse dependence on in-plane stress for indentation depths smaller than 10nm, and the dependence disappears for larger indentation depths. In addition, plastic noise in the nanoindentation force and displacement displays statistically robust noise features, independently of applied stresses. Our experimental results suggest the existence of a regime in FCC crystals where ultra-nano hardness is sensitive to residual applied stresses, but plasticity pop-in noise is insensitive to it.

At room temperature, the indentation morphologies of crystalline copper with different grain size including nanocrystalline (NC), ultrafine-grained (UFG) and coarse-grained (CG) copper were studied by nanoindentation at the strain rate of 0.04/s without holding time at indentation depth of 2000 nm. As the grain size increasing, the height of the pile-up around the residual indentation increases and then has a slightly decrease in the CG Cu, While the area of the pile-up increases constantly. Our analysis has revealed that the dislocation motion and GB activities in the NC Cu, some cross- and multiple-slips dislocation insides the larger grain in the UFG Cu, and forest dislocations from the intragranular Frank-Read sources in the CG Cu, would directly induce these distinct pile-up effect.

Nanoindentation load-depth (P-h) plots is the basis for determination of mechanical properties of the samples and is especially vital for thin coatings deposited on substrates of various mechanical makeup from amorphous-brittle (borosilicate glass) to Silicon (having different crystallographic texture) to ductile substrates like stainless steel as well other aspects like indenter tip shape. The elastic-plastic response by simulated P-h plots as per modified empirical relations have been presented. The outcomes of this computational studies enlighten the database on the P-h plots for various coating/substrate systems and shall aid in the analysis of experimental P-h plots obtained,

In this work, the ternary titanium, copper and silver (Ti-Cu-Ag) system is investigated as a potential candidate for the production of mechanically robust biomedical thin films. The coatings are produced by physical vapor deposition-magnetron sputtering (MS-PVD). The composite thin films are deposited on a silicon (100) substrate. The ratio between Ti and Cu was approximately kept one, with the variation of the Ag content between 10 and 35 at.%, while the power on the targets is changed during each deposition to get the desired Ag content. Thin film characterization is performed by x-ray diffraction (XRD), nanoindentation (modulus and hardness) and Atomic force microscopy to determine the surface topography. The residual stresses are measured by focused ion beam and digital image correlation method (FIB-DIC). The produced Ti-Cu-Ag thin films appear to be smooth, uniformly thick and exhibit amorphous structure for the Ag contents lower than 25 at.%, with a transition to partially crystalline structure for higher Ag concentrations. The Ti-Cu control film shows higher values of 124.5 GPa and 7.85 GPa for modulus and hardness respectively. There is a clear trend of continuous decrease in the modulus and hardness with the increase of Ag content, as lowest value of 105.5 GPa and 6 GPa for 35 at.% Ag containing thin films. In particular, a transition from the compressive (-36.5 MPa) to tensile residual stresses between 229 MPa and 288 MPa are observed with an increasing Ag content. The obtained results suggest that the Ag concentration should not exceed 25 at.%, in order to avoid an excessive reduction of the modulus and hardness with maintaining (at the same time) the potential for an increase of the antibacterial properties. In summary, Ti-Cu-Ag thin films shows characteristic mechanical properties that can be used to improve the properties of biomedical implants such as Ti-alloys and stainless steel.

Enhancement of mechanical properties by using TiN/TiCN/TiC multilayer thin films deposited on commercially pure cast Titanium (CP-Ti), Ti6Al4V and silicon (Si) substrates via magnetron sputtering technique was investigated in this study. The structural, chemical and mechanical properties of the coatings were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), nanoindentation and scratch test. Results of the XRD analysis showed reflections corresponded to FCC (1 1 1) cubic and polycrystalline structure for TiN/TiCN/TiC films. XPS analysis revealed formation of titanium nitride, titanium carbonitride and titanium carbide in the coatings. According to SEM images, the coatings demonstrated dense cross-sectional morphology and columnar structure as well as good adhesion to the substrate with a thickness of 1.77 μm deposited on silicon (1 0 0). Scratch and nanoindentation test results showed the best mechanical behavior for the coated Ti6Al4V substrate material with the 19.96 GPa hardness and 25 N critical load values, because of its higher hardness and toughness of substrate in compared to Cp-Ti substrate.

Enhancement of mechanical properties by using TiN/TiCN/TiC multilayer thin films deposited on commercially pure cast Titanium (CP-Ti), Ti6Al4V and silicon (Si) substrates via magnetron sputtering technique was investigated in this study. The structural, chemical and mechanical properties of the coatings were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), nanoindentation and scratch test. Results of the XRD analysis showed reflections corresponded to FCC (1 1 1) cubic and polycrystalline structure for TiN/TiCN/TiC films. XPS analysis revealed formation of titanium nitride, titanium carbonitride and titanium carbide in the coatings. According to SEM images, the coatings demonstrated dense cross-sectional morphology and columnar structure as well as good adhesion to the substrate with a thickness of 1.77 μm deposited on silicon (1 0 0). Scratch and nanoindentation test results showed the best mechanical behavior for the coated Ti6Al4V substrate material with the 19.96 GPa hardness and 25 N critical load values, because of its higher hardness and toughness of substrate in compared to Cp-Ti substrate.

An oxidation resistant coating on cemented tungsten carbides is characterised in this work. Cemented tungsten carbides (cWCs) are routinely used in mining and manufacturing but are also candidate materials for compact radiation shielding in fusion power generation. In both environments, cWCs will suffer significant degradation due to oxidation at relatively low temperatures. In a recent study, a Si-deposition coating method was demonstrated to improve the oxidation resistance of cWCs by up to a factor of 1,000. This work focusses on the growth kinetics, phase composition, and mechanical properties of these coatings. By combining quantitative X-ray diffraction, electron microscopy and nanoindentation, we show that the coating layer has a 20 % higher hardness than the substrate, which was explained on the basis of a previously-unknown presence of a fine distribution of very hard SiC laths. To interpret the coating stability, a coating growth map is developed. The map shows the structure is stable under a broad range of processing temperatures and composite compositions, demonstrating the potential application of these coatings in a variety of nuclear shielding cWCs.

In this study various samples were fabricated by increasing the amount of CNT from 0% to 5%. The bulk mechanical properties of the samples were measured using DMA. Alternatively, the local mechanical properties were assessed using nanoindentation technique. There is a clear trend that the behavior of the material is dependent of carbon fillers before, during and after percolation threshold. The bulk mechanical properties were reduced after the percolation threshold due to CNT agglomeration. Then the samples were exposed to acid solution for one week and one month. Regardless the amount of CNT in the matrix, there is always a gradient of properties from the skin to the core of the sample. There is a net reduction of in physical properties. However, the level of degradation was a dependent of the amount of CNT in the host polymer. At higher concentration the CNTs behave as a barrier. However due to the formation of porosity around the CNT agglomerates, the acid diffusion encounters preferential path ways. . Both techniques lead to the same observation..