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Extracting mechanical data of thin films on rigid substrates using nanoindentation is compromised by the mechanical properties of underlying substrates, which may falsify the obtained results. With ongoing miniaturization, the substrate influence becomes more pronounced. In this study we present an experimental approach to extract the true Youngs modulus of crystalline-amorphous multilayers by means of nanoindentation. We used 1 µm thick multilayers comprised of amorphous CuZr and nanocrystalline Cu. All films were deposited onto two rigid substrate types with Youngs moduli below and above the ones expected for the deposits (film-to-substrate hardness and elastic moduli ratios between 0.3 to 1.1 and 0.6 to 1.5, respectively). Linear extrapolation of indentation data to zero indentation depth allows to precisely determine the real films Youngs modulus. Same investigations were performed on monolithic Cu and CuZr films of same thickness. While the hardness values change with the variation of the bilayer thickness of the multilayer structures, the Youngs modulus is not affected by the interfaces.

Nanoindentation tests performed on nanocrystalline palladium films subjected to hydriding/dehydriding cycles demonstrate a significant softening when compared to the as-received material. The origin of this softening is unraveled by combining in situ TEM nanomechanical testing with automated crystal orientation mapping in TEM and high resolution TEM. The softening is attributed to the presence of a high density of stacking faults and of Shockley partial dislocations after hydrogen loading. The hydrogen induced defects affect the elementary plasticity mechanisms and the mechanical response by acting as preferential sites for twinning/detwinning during deformation. These results are analyzed and compared to previous experimental and simulation works in the literature. This study provides new insights into the effect of hydrogen on the atomistic deformation and cracking mechanisms as well as on the mechanical properties of nanocrystalline thin films and membranes.

A better understanding of the interfacial transition zone (ITZ) in biochar-augmented carbon-negative cementitious materials can facilitate their potential applications. This study illustrated the key chemical and mechanical features of such a region in Portland cement using backscattered electron microscopy-energy dispersive X-ray analysis (BSEM-EDX), nano-indentation, and X-ray computed tomography (X-CT). It was found that a significant ‘wall effect’ was identified at the side-edge of biochar, where the degree of hydration and the porosity significantly increased. The biochar was integrated into the hardened cement matrix via a layer of Ca-rich hydration products mainly composed of AFm phases, CH and C–S–H gels. Regarding the mechanical behaviour, the biochar showed a typical viscous-elastic (VE) deformation mode at the nano/micro scale, whereas the hardened cement was a typical plastic-elastic (PE) material. Therefore, the value of the hardness of biochar was not accurate under limited plastic deformation. The distinct differences in deformation resulted in the largest residual deformation (i.e., plasticity) of the hardened cement after indentation when compared to ITZ and biochar regions, whereas the ITZ maintained a lower value due to well connection with biochar. These microstructural characteristics partially explained the higher compressive strength of biochar-cement composites than previously expected.

TiO2 is an important oxide for property modifications in the conventional soda lime silicate glass family. It offers interesting optical and mechanical properties, for instance, by substituting heavy metals such as lead in consumer glasses. The compositional effects on the hardness, reduced elastic modulus and crack resistance as determined by indentation of chemically strengthened (CS) TiO2-doped soda lime silicate glass was studied in the current paper. The CS, which was performed by a K+ for Na+ ion exchange in a molten KNO3 salt bath at 450 °C for 15 h, yielded significant changes in the indentation mechanical properties. The hardness of the glass samples increased, and this was notably dependent on the SiO2, CaO and TiO2 content. The reduced elastic modulus was less affected by the CS but showed decrease for most samples. The crack resistance, an important property in many applications where glasses are subjected to contact damage, showed very different behaviors among the series. Only one of the series did significantly improve the crack resistance where low CaO content, high TiO2 content, high molar volume and increased elastic deformation favored an increased crack resistance., Funding: Forskningsrådet Formas 2018-00707, Tunnare och starkare glas för hållbar produktion och konsumtion

TiO2 is an important oxide for property modifications in the conventional soda lime silicate glass family. It offers interesting optical and mechanical properties, for instance, by substituting heavy metals such as lead in consumer glasses. The compositional effects on the hardness, reduced elastic modulus and crack resistance as determined by indentation of chemically strengthened (CS) TiO2-doped soda lime silicate glass was studied in the current paper. The CS, which was performed by a K+ for Na+ ion exchange in a molten KNO3 salt bath at 450 °C for 15 h, yielded significant changes in the indentation mechanical properties. The hardness of the glass samples increased, and this was notably dependent on the SiO2, CaO and TiO2 content. The reduced elastic modulus was less affected by the CS but showed decrease for most samples. The crack resistance, an important property in many applications where glasses are subjected to contact damage, showed very different behaviors among the series. Only one of the series did significantly improve the crack resistance where low CaO content, high TiO2 content, high molar volume and increased elastic deformation favored an increased crack resistance., Funding: Forskningsrådet Formas 2018-00707, Tunnare och starkare glas för hållbar produktion och konsumtion

The reinforcement function of shell ribs depends not only on their vaulted morphology but also on their microstructure. They are part of the outer layer which, in the case of the Pinna nobilis bivalve, is built from almost monocrystalline calcitic prisms, always oriented perpendicular to the growth surfaces. Originally, prisms and their c-axes follow the radii of rib curvature, becoming oblique to the shell thickness direction. Later, prisms bend to reach the nacre layer perpendicularly, but their c-axes retain the initial orientation. Calcite grains form nonrandom boundaries. Most often, three twin disorientations arise, with two of them observed for the first time. Nano-indentation and impact tests demonstrate that the oblique orientation of c-axes significantly improves the hardness and fracture toughness of prisms. Moreover, compression tests reveal that the rib area achieves a unique strength of 700 MPa. The detection of the specific microstructure formed to toughen the shell is novel.

Accelerated irradiation studies in nuclear structural materials are essential for the roll-out of future GEN IV reactors. Over the operational lifetime of these systems, the associated embrittlement and hardening induced through neutron irradiation can be emulated through accelerator-based ion irradiation. While the complementarity of ion and neutron irradiation is evident, this thesis looks at the effects of the highly stratified damage profiles resulting from ion irradiation. Small scale experimental techniques, such as micro-tensile testing and nanoindentation, allow for the analysis of the shallow irradiation zones. A significant challenge to these techniques is the presence of gradient plasticity phenomena, that is most pronounced at these very shallow depths. Indenter size effects in nanoindentation can skew experimental results significantly. In addition, Hall-Petch type behaviour (grain size effects), along with strain rate sensitivity, will often affect the precision of micro-tensile test results. One of the major hypotheses underpinning the thesis is that ion-induced irradiation hardening is equivalent to Orowan-type strengthening. Suitable homogenisation techniques were adopted in light of the complementarity between the neutron and ion irradiation response. Validation of the hypotheses was through a systematic study of low and high dpa (displacements per atom) irradiation responses in a range of materials including austenitic stainless steel, single crystal nickel, duplex steel and a commercial aluminium alloy, with the aim of developing a synergetic and multiscale assessment framework. Kinetic Monte Carlo simulations of ion irradiation were used to inform a number of mesoscale and crystal plasticity finite element models and to better elucidate the gradient damage effects induced by ion irradiation. The multiscale simulations provided an accurate prediction of the hardness increase with a tractable pathway between the microscale testing and the mesoscal

A method for small-scale testing and imaging of freestanding, microtomed polymer films using a push-to-pull device is presented. Central to this method was the development of a sample preparation technique which utilized solvents at cryogenic temperatures to transfer and deposit delicate thin films onto the microfabricated push-to-pull devices. The preparation of focused ion beam (FIB)-milled tensile specimens enabled quantitative in situ TEM tensile testing, but artifacts associated with ion and electron beam irradiation motivated the development of a FIB-free specimen preparation method. The FIB-free method was enabled by the design and fabrication of oversized strain-locking push-to-pull devices. An adaptation for push-to-pull devices to be compatible with an instrumented nanoindenter expanded the testing capabilities to include in situ heating. These innovations provided quantitative mechanical testing, postmortem TEM imaging, and the ability to measure the glass transition temperature, via dynamic mechanical analysis, of freestanding polymer films. Results for each of these mentioned characterization methods are presented and discussed in terms of polymer nanomechanics. Graphic Abstract: [Figure not available: see fulltext.]

An important input parameter for numerical models that simulate cracking of the concrete cover due to reinforcement corrosion is the Elastic modulus of corrosion product (Ecp). Despite its relevance, Ecp is subject of significant variations according to the values reported in the literature, which vary from less than 100 MPa up to 360 GPa. Furthermore, Ecp values proposed in most of the present literature are representative of the corrosion product generated by anodic accelerated corrosion or extracted from the steel/concrete interface (SCI), which might differ from that formed in real corroding structures. Therefore, this study aims to investigate the Elastic modulus of naturally-generated corrosion product present at the SCI through nano-indentation conducted on six reinforced concrete polished sections. The polished sections were obtained from six 20-year-old reinforced concrete prisms cast with different cement type (CEM I, CEM II/B-V, CEM III/B, CEM V/A), same water/binder ratio (0.55) and which were previously exposed to NaCl solution wet/dry cycles. This study revealed that the range of Ecp did not considerably vary between corrosion products formed in different concrete mixes. However, corrosion product was microscopically found to consist of overlapping bands with different Ecp, varying for up to around 70 GPa between each other. Through Environmental Scanning-Electron Microscopy (ESEM) and Energy Dispersive Xray Spectrometry (EDS) analysis of the indented locations, it was found that Ecp is highly dependent on the presence of interfacial cracks and inversely proportional to the concentration of Si and Ca, representative for corrosion product mixed with the surrounding concrete. Furthermore, higher concentration of Fe leads to higher Ecp. Based on this study, an average range of values for Ecp between 80-100 GPa can be suggested for use in numerical models for corrosion induced cracking, regardless of cement type of the structure under investigation., Materials and Environment

The flexural strength of ultra-high performance concrete with basalt aggregates (UHPC-CA) strongly depends on the micromechanical property of CA, interfacial transition zone (ITZ) and matrix. However, the influence of micromechanical property on the rate-dependent flexural strength of UHPC-CA has not been well understood. Here, different initial micromechanical property distributions are produced by controlling the hydration development, and its influence on the rate-dependent flexural strength of UHPC-CA is investigated by a multi-scale analysis method. The results show that a more homogeneous micromechanical property of UHPC-CA results in a higher flexural strength, but a lower dynamic increase factor (DIF) of flexural strength. The lower DIF can mainly be attributed to the lower increasing rate of mesoscale fracture of CA. Moreover, based on a meso-mechanical model, it is revealed that higher fracture toughness ratios of ITZ/CA and ITZ/Matrix result in lower critical angles () of fractures of CA and matrix, consequently, higher mechanical contribution from CA and matrix.

An important input parameter for numerical models that simulate cracking of the concrete cover due to reinforcement corrosion is the Elastic modulus of corrosion product (Ecp). Despite its relevance, Ecp is subject of significant variations according to the values reported in the literature, which vary from less than 100 MPa up to 360 GPa. Furthermore, Ecp values proposed in most of the present literature are representative of the corrosion product generated by anodic accelerated corrosion or extracted from the steel/concrete interface (SCI), which might differ from that formed in real corroding structures. Therefore, this study aims to investigate the Elastic modulus of naturally-generated corrosion product present at the SCI through nano-indentation conducted on six reinforced concrete polished sections. The polished sections were obtained from six 20-year-old reinforced concrete prisms cast with different cement type (CEM I, CEM II/B-V, CEM III/B, CEM V/A), same water/binder ratio (0.55) and which were previously exposed to NaCl solution wet/dry cycles. This study revealed that the range of Ecp did not considerably vary between corrosion products formed in different concrete mixes. However, corrosion product was microscopically found to consist of overlapping bands with different Ecp, varying for up to around 70 GPa between each other. Through Environmental Scanning-Electron Microscopy (ESEM) and Energy Dispersive Xray Spectrometry (EDS) analysis of the indented locations, it was found that Ecp is highly dependent on the presence of interfacial cracks and inversely proportional to the concentration of Si and Ca, representative for corrosion product mixed with the surrounding concrete. Furthermore, higher concentration of Fe leads to higher Ecp. Based on this study, an average range of values for Ecp between 80-100 GPa can be suggested for use in numerical models for corrosion induced cracking, regardless of cement type of the structure under investigation.

Acrylonitrile butadiene styrene (ABS) and polycarbonate (PC) are considered a well-known class of engineering thermoplastics due to their efficient use in automotive, 3D printing, and elec-tronics. However, improvement in toughness, processability, and thermal stability is achieved by mixing together ABS and PC. The present study focuses on the understanding of surface mechanical characterization of acrylonitrile butadiene styrene (ABS) and polycarbonate (PC) blends using nano-indentation. Polymer blends sheets with three different proportions of ABS/PC (75:25, 50:50, and 25:75) were fabricated via melt-processing and thermal press. Fourier transform infrared (FTIR) spectroscopy was performed to analyze the intermolecular interactions between the blends’ compo-nents. To understand the surface mechanical properties of ABS and PC blends, a sufficient number of nano-indentation tests were performed at a constant loading rate to a maximum load of 100 mN. Creeping effects were observed at the end of loading and start of unloading section. Elastic modulus, indentation hardness, and creep values were measured as a function of penetration displacement in the quasi-continuous stiffness mode (QCSM) indentation. Load-displacement curves indicated an increase in the displacement with the increase in ABS contents while a decreasing trend was observed in the hardness and elastic modulus values as the ABS content was increased. We believe this study would provide an effective pathway for developing new polymer blends with enhanced mechanical performance., Aerospace Manufacturing Technologies

A method for small-scale testing and imaging of freestanding, microtomed polymer films using a push-to-pull device is presented. Central to this method was the development of a sample preparation technique which utilized solvents at cryogenic temperatures to transfer and deposit delicate thin films onto the microfabricated push-to-pull devices. The preparation of focused ion beam (FIB)-milled tensile specimens enabled quantitative in situ TEM tensile testing, but artifacts associated with ion and electron beam irradiation motivated the development of a FIB-free specimen preparation method. The FIB-free method was enabled by the design and fabrication of oversized strain-locking push-to-pull devices. An adaptation for push-to-pull devices to be compatible with an instrumented nanoindenter expanded the testing capabilities to include in situ heating. These innovations provided quantitative mechanical testing, postmortem TEM imaging, and the ability to measure the glass transition temperature, via dynamic mechanical analysis, of freestanding polymer films. Results for each of these mentioned characterization methods are presented and discussed in terms of polymer nanomechanics. Graphic Abstract: [Figure not available: see fulltext.]

The flexural strength of ultra-high performance concrete with basalt aggregates (UHPC-CA) strongly depends on the micromechanical property of CA, interfacial transition zone (ITZ) and matrix. However, the influence of micromechanical property on the rate-dependent flexural strength of UHPC-CA has not been well understood. Here, different initial micromechanical property distributions are produced by controlling the hydration development, and its influence on the rate-dependent flexural strength of UHPC-CA is investigated by a multi-scale analysis method. The results show that a more homogeneous micromechanical property of UHPC-CA results in a higher flexural strength, but a lower dynamic increase factor (DIF) of flexural strength. The lower DIF can mainly be attributed to the lower increasing rate of mesoscale fracture of CA. Moreover, based on a meso-mechanical model, it is revealed that higher fracture toughness ratios of ITZ/CA and ITZ/Matrix result in lower critical angles () of fractures of CA and matrix, consequently, higher mechanical contribution from CA and matrix.

An important input parameter for numerical models that simulate cracking of the concrete cover due to reinforcement corrosion is the Elastic modulus of corrosion product (Ecp). Despite its relevance, Ecp is subject of significant variations according to the values reported in the literature, which vary from less than 100 MPa up to 360 GPa. Furthermore, Ecp values proposed in most of the present literature are representative of the corrosion product generated by anodic accelerated corrosion or extracted from the steel/concrete interface (SCI), which might differ from that formed in real corroding structures. Therefore, this study aims to investigate the Elastic modulus of naturally-generated corrosion product present at the SCI through nano-indentation conducted on six reinforced concrete polished sections. The polished sections were obtained from six 20-year-old reinforced concrete prisms cast with different cement type (CEM I, CEM II/B-V, CEM III/B, CEM V/A), same water/binder ratio (0.55) and which were previously exposed to NaCl solution wet/dry cycles. This study revealed that the range of Ecp did not considerably vary between corrosion products formed in different concrete mixes. However, corrosion product was microscopically found to consist of overlapping bands with different Ecp, varying for up to around 70 GPa between each other. Through Environmental Scanning-Electron Microscopy (ESEM) and Energy Dispersive Xray Spectrometry (EDS) analysis of the indented locations, it was found that Ecp is highly dependent on the presence of interfacial cracks and inversely proportional to the concentration of Si and Ca, representative for corrosion product mixed with the surrounding concrete. Furthermore, higher concentration of Fe leads to higher Ecp. Based on this study, an average range of values for Ecp between 80-100 GPa can be suggested for use in numerical models for corrosion induced cracking, regardless of cement type of the structure under investigation., Materials and Environment

Acrylonitrile butadiene styrene (ABS) and polycarbonate (PC) are considered a well-known class of engineering thermoplastics due to their efficient use in automotive, 3D printing, and elec-tronics. However, improvement in toughness, processability, and thermal stability is achieved by mixing together ABS and PC. The present study focuses on the understanding of surface mechanical characterization of acrylonitrile butadiene styrene (ABS) and polycarbonate (PC) blends using nano-indentation. Polymer blends sheets with three different proportions of ABS/PC (75:25, 50:50, and 25:75) were fabricated via melt-processing and thermal press. Fourier transform infrared (FTIR) spectroscopy was performed to analyze the intermolecular interactions between the blends’ compo-nents. To understand the surface mechanical properties of ABS and PC blends, a sufficient number of nano-indentation tests were performed at a constant loading rate to a maximum load of 100 mN. Creeping effects were observed at the end of loading and start of unloading section. Elastic modulus, indentation hardness, and creep values were measured as a function of penetration displacement in the quasi-continuous stiffness mode (QCSM) indentation. Load-displacement curves indicated an increase in the displacement with the increase in ABS contents while a decreasing trend was observed in the hardness and elastic modulus values as the ABS content was increased. We believe this study would provide an effective pathway for developing new polymer blends with enhanced mechanical performance., Aerospace Manufacturing Technologies

An important input parameter for numerical models that simulate cracking of the concrete cover due to reinforcement corrosion is the Elastic modulus of corrosion product (Ecp). Despite its relevance, Ecp is subject of significant variations according to the values reported in the literature, which vary from less than 100 MPa up to 360 GPa. Furthermore, Ecp values proposed in most of the present literature are representative of the corrosion product generated by anodic accelerated corrosion or extracted from the steel/concrete interface (SCI), which might differ from that formed in real corroding structures. Therefore, this study aims to investigate the Elastic modulus of naturally-generated corrosion product present at the SCI through nano-indentation conducted on six reinforced concrete polished sections. The polished sections were obtained from six 20-year-old reinforced concrete prisms cast with different cement type (CEM I, CEM II/B-V, CEM III/B, CEM V/A), same water/binder ratio (0.55) and which were previously exposed to NaCl solution wet/dry cycles. This study revealed that the range of Ecp did not considerably vary between corrosion products formed in different concrete mixes. However, corrosion product was microscopically found to consist of overlapping bands with different Ecp, varying for up to around 70 GPa between each other. Through Environmental Scanning-Electron Microscopy (ESEM) and Energy Dispersive Xray Spectrometry (EDS) analysis of the indented locations, it was found that Ecp is highly dependent on the presence of interfacial cracks and inversely proportional to the concentration of Si and Ca, representative for corrosion product mixed with the surrounding concrete. Furthermore, higher concentration of Fe leads to higher Ecp. Based on this study, an average range of values for Ecp between 80-100 GPa can be suggested for use in numerical models for corrosion induced cracking, regardless of cement type of the structure under investigation.

Thin films on PEEK have been designing by magnetron sputtering, using bias voltages ranging from −31 to −157 V. The X-ray diffraction and EDX show how the amorphous films resulting have an elemental composition very close to the stoichiometry TiSi. The AFM and SEM performed on top and cross-section, respectively, of film reveal a smooth and uniform surface, free of pores and cracks, and a compact microstructure. The evaluation of the resolved shear stress, yield strength, hardness, scratch resistance, and fracture toughness show how these values increase in the TiSi/PEEK system as the bias voltage increase. The development of these hard and tough thin films has enabled the fracture toughness achieved by the TiSi/PEEK system increase when a bias voltage equal to or higher than −108 V is used during the deposition process. For these bias conditions, the compressive residual stresses generated are large enough to prevent crack nucleation. The increase of the crack resistance gives as a result that K reaches values above 32 MPa*m. This value is much greater than those values corresponding to the classic ceramic coatings, such as AlO (4.6 MPa*m) and ZrO (7.6 MPa*m).

Cross-linking is a process in which polymer chains are associated through chemical bonds. The cross-linking level can be adjusted by the irradiation dosage and often by means of a cross-linking booster. The polymer additional cross-linking influences the surface nano and micro layers in the way comparable to metals during the thermal and chemical-thermal treatments. Polybutylene terephthalate (PBT) can be found in a group of structural polymers, which are often used in industry, especially in automotive. Applying the technology of electron radiation induces a creation of 3D network structure, which improves the local mechanical properties. These were later measured by a depth sensing indentation (DSI) test. This state of the art method is based on immediate detection of indentation depth in relation to applied force. The creation of 3D network caused an increase in nano-mechanical properties values, such as indentation hardness and indentation modulus, in comparison to the virgin material. The indentation hardness rose by 80%, while the indentation modulus elevated by 62%. The selected structural materials, e.g. PBT, were modified by the electron irradiation in a positive way and as such could be moved to a group of high performance materials. © Czech Technical University in Prague, 2020.

This study describes the effect of electron radiation on the nano-mechanical properties of surface layers of selected polyamide (PA) types. Electron radiation initiates the cross-linking of macromolecules in the polyamide structure, leading to the creation of a 3Dnetworkwhich fundamentally changes the properties of the tested polymers. Selected types of polyamide (PA 6, PA 66 and PA 9T) were exposed to various intensities of electron radiation (33 kGy, 66 kGy, 99 kGy, 132 kGy, 165 kGy and 198 kGy). The cross-linked polyamides' surface properties were measured by means of the modern nano-indentation technique (Depth Sensing Indentation; DSI), which operates on the principle of the immediate detection of indenter penetration depth in dependence on the applied load. The evaluation was preformed using the Oliver-Pharrmethod. The effect of electron radiation on the tested polyamides manifested itself in the creation of a 3D network, which led to an increase of surface layer properties, such as indentation hardness, elastic modulus, creep and temperature resistance, by up to 93%. The increase of temperature and mechanical properties substantially broadens the field of application of these materials in technical practice, especially when higher temperature resistance is required. The positive changes to the nano-mechanical properties as well as mechanical and temperature capabilities instigated by the cross-linking process were confirmed by the gel volume test. These measurements lay the foundation for a detailed study of this topic, as well as for a more effective means of modifying chosen properties of technical polyamide products by radiation. © 2020 by the authors.

In this paper, the compressive stress of pristine and coated vertically-aligned (VA) multi-walled (MW) carbon nanotube (CNT) pillars were investigated using flat-punch nano-indentation. VA-MWCNT pillars of various diameters (30–150 µm) grown by low-pressure chemical vapor deposition on silicon wafer. A conformal brittle coating of niobium-titanium-nitride with high superconductivity temperature was deposited on the VA-MWCNT pillars using atomic layer deposition. The coating together with the pillars could form a superconductive vertical interconnect. The indentation tests showed foam-like behavior of pristine CNTs and ceramic-like fracture of conformal coated CNTs. The compressive strength and the elastic modulus for pristine CNTs could be divided into three regimes of linear elastic, oscillatory plateau, and exponential densification. The elastic modulus of pristine CNTs increased for a smaller pillar diameter. The response of the coated VA-MWCNTs depended on the diffusion depth of the coating in the pillar and their elastic modulus increased with pillar diameter due to the higher sidewall area. Tuning the material properties by conformal coating on various diameter pillars enhanced the mechanical performance and the vertical interconnect access (via) reliability. The results could be useful for quantum computing applications that require high-density superconducting vertical interconnects and reliable operation at reduced temperatures., Electronic Components, Technology and Materials

Nano-indentation, a depth sensing technique, is a useful and exciting tool to investigate the surface mechanical properties of a wide range of materials, particularly polymers. Knowledge of the influence of experimental conditions employed during nano-indentation on the resultant nano-mechanical response is very important for the successful design of engineering components with appropriate surface properties. In this work, nano-indentation experiments were carried out by selecting various values of frequency, amplitude, contact depth, strain rate, holding time, and peak load. The results showed a significant effect of amplitude, frequency, and strain rate on the hardness and modulus of the considered polymer, ultrahigh molecular weight polyethylene (UHMWPE). Load-displacement curves showed a shift towards the lower indentation depths along with an increase in peak load by increasing the indentation amplitude or strain rate. The results also revealed the strong dependence of hardness and modulus on the holding time. The experimental data of creep depth as a function of holding time was successfully fitted with a logarithmic creep model (R2 ≥ 0.98). In order to remove the creeping effect and the nose problem, recommended holding times were proposed for the investigated polymer as a function of different applied loads., Aerospace Manufacturing Technologies, Rivers, Ports, Waterways and Dredging Engineering

This study's goal was to describe the influence of a wide range of ionizing beta radiation upon the changes in surface layer mechanical properties and structural modifications of selected types of polymer. Radiation crosslinking is a process whereby the impingement of high-energy electrons adjusts test sample structures, thus enhancing the useful properties of the material, e.g., hardness, wear-resistance, and creep, in order that they may function properly during their technical use. The selected polymers tested were polyolefin polymers like polyethylene (Low-density polyethylene LDPE, High-density polyethylene HDPE). These samples underwent exposure to electron radiation of differing dosages (33, 66, 99, 132, 165, and 198 kGy). After the crosslinking process, the samples underwent testing of the nano-mechanical properties of their surface layers. This was done by means of a state-of-the-art indentation technique, i.e., depth-sensing indentation (DSI), which detects the immediate change in the indentation depth associated with the applied force. Indeed, the results indicated that the optimal radiation dosage increased the mechanical properties by up to 57%; however, the beneficial levels of radiation varied with each material. Furthermore, these modifications faced examination from the structural perspective. For this purpose, a gel test, Raman spectroscopy, and crystalline portion determination by X-ray all confirmed the assumed trends. © 2020 by the authors.

Nano-indentation, a depth sensing technique, is a useful and exciting tool to investigate the surface mechanical properties of a wide range of materials, particularly polymers. Knowledge of the influence of experimental conditions employed during nano-indentation on the resultant nano-mechanical response is very important for the successful design of engineering components with appropriate surface properties. In this work, nano-indentation experiments were carried out by selecting various values of frequency, amplitude, contact depth, strain rate, holding time, and peak load. The results showed a significant effect of amplitude, frequency, and strain rate on the hardness and modulus of the considered polymer, ultrahigh molecular weight polyethylene (UHMWPE). Load-displacement curves showed a shift towards the lower indentation depths along with an increase in peak load by increasing the indentation amplitude or strain rate. The results also revealed the strong dependence of hardness and modulus on the holding time. The experimental data of creep depth as a function of holding time was successfully fitted with a logarithmic creep model (R2 ≥ 0.98). In order to remove the creeping effect and the nose problem, recommended holding times were proposed for the investigated polymer as a function of different applied loads., Aerospace Manufacturing Technologies, Rivers, Ports, Waterways and Dredging Engineering

In this paper, the compressive stress of pristine and coated vertically-aligned (VA) multi-walled (MW) carbon nanotube (CNT) pillars were investigated using flat-punch nano-indentation. VA-MWCNT pillars of various diameters (30–150 µm) grown by low-pressure chemical vapor deposition on silicon wafer. A conformal brittle coating of niobium-titanium-nitride with high superconductivity temperature was deposited on the VA-MWCNT pillars using atomic layer deposition. The coating together with the pillars could form a superconductive vertical interconnect. The indentation tests showed foam-like behavior of pristine CNTs and ceramic-like fracture of conformal coated CNTs. The compressive strength and the elastic modulus for pristine CNTs could be divided into three regimes of linear elastic, oscillatory plateau, and exponential densification. The elastic modulus of pristine CNTs increased for a smaller pillar diameter. The response of the coated VA-MWCNTs depended on the diffusion depth of the coating in the pillar and their elastic modulus increased with pillar diameter due to the higher sidewall area. Tuning the material properties by conformal coating on various diameter pillars enhanced the mechanical performance and the vertical interconnect access (via) reliability. The results could be useful for quantum computing applications that require high-density superconducting vertical interconnects and reliable operation at reduced temperatures., Electronic Components, Technology and Materials

Cross-linking is a process in which polymer chains are associated through chemical bonds. The cross-linking level can be adjusted by the irradiation dosage and often by means of a cross-linking booster. The polymer additional cross-linking influences the surface nano and micro layers in the way comparable to metals during the thermal and chemical-thermal treatments. Polybutylene terephthalate (PBT) can be found in a group of structural polymers, which are often used in industry, especially in automotive. Applying the technology of electron radiation induces a creation of 3D network structure, which improves the local mechanical properties. These were later measured by a depth sensing indentation (DSI) test. This state of the art method is based on immediate detection of indentation depth in relation to applied force. The creation of 3D network caused an increase in nano-mechanical properties values, such as indentation hardness and indentation modulus, in comparison to the virgin material. The indentation hardness rose by 80%, while the indentation modulus elevated by 62%. The selected structural materials, e.g. PBT, were modified by the electron irradiation in a positive way and as such could be moved to a group of high performance materials. © Czech Technical University in Prague, 2020.

This study's goal was to describe the influence of a wide range of ionizing beta radiation upon the changes in surface layer mechanical properties and structural modifications of selected types of polymer. Radiation crosslinking is a process whereby the impingement of high-energy electrons adjusts test sample structures, thus enhancing the useful properties of the material, e.g., hardness, wear-resistance, and creep, in order that they may function properly during their technical use. The selected polymers tested were polyolefin polymers like polyethylene (Low-density polyethylene LDPE, High-density polyethylene HDPE). These samples underwent exposure to electron radiation of differing dosages (33, 66, 99, 132, 165, and 198 kGy). After the crosslinking process, the samples underwent testing of the nano-mechanical properties of their surface layers. This was done by means of a state-of-the-art indentation technique, i.e., depth-sensing indentation (DSI), which detects the immediate change in the indentation depth associated with the applied force. Indeed, the results indicated that the optimal radiation dosage increased the mechanical properties by up to 57%; however, the beneficial levels of radiation varied with each material. Furthermore, these modifications faced examination from the structural perspective. For this purpose, a gel test, Raman spectroscopy, and crystalline portion determination by X-ray all confirmed the assumed trends. © 2020 by the authors.

This study describes the effect of electron radiation on the nano-mechanical properties of surface layers of selected polyamide (PA) types. Electron radiation initiates the cross-linking of macromolecules in the polyamide structure, leading to the creation of a 3Dnetworkwhich fundamentally changes the properties of the tested polymers. Selected types of polyamide (PA 6, PA 66 and PA 9T) were exposed to various intensities of electron radiation (33 kGy, 66 kGy, 99 kGy, 132 kGy, 165 kGy and 198 kGy). The cross-linked polyamides' surface properties were measured by means of the modern nano-indentation technique (Depth Sensing Indentation; DSI), which operates on the principle of the immediate detection of indenter penetration depth in dependence on the applied load. The evaluation was preformed using the Oliver-Pharrmethod. The effect of electron radiation on the tested polyamides manifested itself in the creation of a 3D network, which led to an increase of surface layer properties, such as indentation hardness, elastic modulus, creep and temperature resistance, by up to 93%. The increase of temperature and mechanical properties substantially broadens the field of application of these materials in technical practice, especially when higher temperature resistance is required. The positive changes to the nano-mechanical properties as well as mechanical and temperature capabilities instigated by the cross-linking process were confirmed by the gel volume test. These measurements lay the foundation for a detailed study of this topic, as well as for a more effective means of modifying chosen properties of technical polyamide products by radiation. © 2020 by the authors.

This contribution explores different strategies to electrically contact vertical pillars with diameters less than 100 nm. Two process strategies have been defined, the first based on Atomic Force Microscope (AFM) indentation and the second based on planarization and reactive ion etching (RIE). We have demonstrated that both proposals provide suitable contacts. The results help to conclude that the most feasible strategy to be implementable is the one using planarization and reactive ion etching since it is more suitable for parallel and/or high-volume manufacturing processing.

The formation and temporal evolution of the modulated structure in a lamellar gamma-based Ti-45Al-8.5Nb alloy have been investigated by transmission electron microscopy (TEM) in combination with first-principles theory in this work. The results show that the Nb-rich O phase as a constituent of the modulated structure is thermodynamically stable below 650 degrees C in the alpha(2) lamellae. The morphology of the O phase variants changes from thin plate-like shape with a low volume fraction at initial annealing to rectangle/square shape with a high volume fraction after a prolonged annealing, and the retransformed alpha(2), named as alpha(2-II) hereafter, emerges at intersections of the variants with two orthogonal habit planes due to their elastic interactions. The partitioning coefficient of Nb between the O phase and alpha(2) is about 2 at 600 degrees C. The diffusion coefficient of Nb derived from growth kinetics of the O phase is about (1.3 +/- 0.2) x 10(-22) m(2)s(-1) in the alpha(2) lamellae. Significant precipitation hardening effect of the O phase has been revealed for the alpha(2) lamellae and gamma/(alpha(2)+O) lamellar microstructure, which is supposed to be attributed to refining the alpha(2) lamellae associated with elastic strain energy from the alpha(2) -> O phase transformation and introducing the interface between the modulated lamella and adjacent gamma phase. (C) 2018 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

The formation and temporal evolution of the modulated structure in a lamellar gamma-based Ti-45Al-8.5Nb alloy have been investigated by transmission electron microscopy (TEM) in combination with first-principles theory in this work. The results show that the Nb-rich O phase as a constituent of the modulated structure is thermodynamically stable below 650 degrees C in the alpha(2) lamellae. The morphology of the O phase variants changes from thin plate-like shape with a low volume fraction at initial annealing to rectangle/square shape with a high volume fraction after a prolonged annealing, and the retransformed alpha(2), named as alpha(2-II) hereafter, emerges at intersections of the variants with two orthogonal habit planes due to their elastic interactions. The partitioning coefficient of Nb between the O phase and alpha(2) is about 2 at 600 degrees C. The diffusion coefficient of Nb derived from growth kinetics of the O phase is about (1.3 +/- 0.2) x 10(-22) m(2)s(-1) in the alpha(2) lamellae. Significant precipitation hardening effect of the O phase has been revealed for the alpha(2) lamellae and gamma/(alpha(2)+O) lamellar microstructure, which is supposed to be attributed to refining the alpha(2) lamellae associated with elastic strain energy from the alpha(2) -> O phase transformation and introducing the interface between the modulated lamella and adjacent gamma phase. All rights reserved., QC 20190401

In this work, the nano-indentation of plasma-exposed tungsten is simulated at room temperature and elevated temperature (300–700 K) by the recently developed crystal plasticity finite element model. A nonlinear function is applied to characterize the depth profile of plasma-induced dislocation density in the sub-surface region. The model parameters are calibrated by comparing the simulated results with corresponding experimental data at 300 K for both the force-depth and hardness-depth relationships. Furthermore, the mechanical responses of plasma-exposed tungsten are predicted at 500 K and 700 K in order to characterize the plasma effect at the fusion-relevant operational temperature. The dominant results and conclusions are that: (1) The heterogeneously distributed dislocations in the sub-surface region induced by the plasma exposure are responsible for the increase of hardness at 300 K. (2) The plasma-induced microstructural modification does not yield to considerable increase of hardness at operational temperature. (3) The expansion of the plastic zone in the sub-surface region is, to some extent, limited by the presence of plasma-induced dislocations. Whereas, the increase of temperature can effectively reduce this limitation.

Nano-indentation is an interesting tool for analyzing nano-scale mechanical properties. The analysis of nano-mechanical properties as a function of experimental conditions is very critical for designing engineering components. In this study, nano-indentation experiments were performed by considering different values of amplitude (1, 5, 10 nm), frequency (11.2, 22.5, 45 Hz), strain rate (0.02, 0.05, 0.1, 0.2, 1 s −1 ), peak load (10, 30, 100 mN) and hold time (1, 3, 5, 10, 20, 50, 100 sec) to analyze their effect on the mechanical properties of LDPE. The results showed that the effect of amplitude and frequency on the nano-mechanical properties of LDPE were negligible. Load-displacement curves displayed a shift towards higher indentation depths along with a decrease in peak load from 20.6 to 14.8 mN by having a decrease in strain rate from 1 to 0.02 s −1 . Elastic modulus and hardness values exhibited a decrease with an increase in hold time. Logarithmic creep model was used to fit the experimental data of creep as a function of holding time which showed good agreement (r 2 ≥ 0.97) with the experimental values. Recommended holding times are also suggested to eliminate the creep and nose problem in order to achieve high accuracy in measurements., Hydraulic Engineering, Rivers, Ports, Waterways and Dredging Engineering

Carbon fibre reinforced polymer composite has been widely used in structural component due to lower and not well studied because of the extre modulus was measured by nano-scale indentation tests, which were performed on fabricated flat surfaces, using both atomic force microscopy and nano-indentation. The surface damage induced by the high energy ion beam was also assessed., Conference code: 165341; Export Date: 8 September 2021; Conference Paper; Correspondence Address: Asp, L.; Industrial and Materials Science, Sweden; email: leif.asp@chalmers.se; Funding details: Horizon 2020, 738085; Funding details: Energimyndigheten; Funding details: FA9550-17-1-0338; Funding details: Svenska Forskningsrådet Formas, 46598-1; Funding details: VINNOVA; Funding text 1: This work was funded by USAF office of scientific research (Award no.: FA9550-17-1-0338), and EU Horizon 2020 under Grant Agreement Number 738085. FL and LA acknowledge support from LIGHTer, a program financed within Strategic Innovation Areas, a mutual venture between VINNOVA, the Swedish Energy Agency, and Formas. FL also acknowledges funding from the Swedish Energy Agency (project nr. 46598-1).

Nano-indentation is an interesting tool for analyzing nano-scale mechanical properties. The analysis of nano-mechanical properties as a function of experimental conditions is very critical for designing engineering components. In this study, nano-indentation experiments were performed by considering different values of amplitude (1, 5, 10 nm), frequency (11.2, 22.5, 45 Hz), strain rate (0.02, 0.05, 0.1, 0.2, 1 s −1 ), peak load (10, 30, 100 mN) and hold time (1, 3, 5, 10, 20, 50, 100 sec) to analyze their effect on the mechanical properties of LDPE. The results showed that the effect of amplitude and frequency on the nano-mechanical properties of LDPE were negligible. Load-displacement curves displayed a shift towards higher indentation depths along with a decrease in peak load from 20.6 to 14.8 mN by having a decrease in strain rate from 1 to 0.02 s −1 . Elastic modulus and hardness values exhibited a decrease with an increase in hold time. Logarithmic creep model was used to fit the experimental data of creep as a function of holding time which showed good agreement (r 2 ≥ 0.97) with the experimental values. Recommended holding times are also suggested to eliminate the creep and nose problem in order to achieve high accuracy in measurements., Hydraulic Engineering, Rivers, Ports, Waterways and Dredging Engineering

The aim of this work was to evaluate the nano-mechanical properties of glass ionomer materials, the ion concentrations at the surfaces in relation to the storage media and the pH environments using a scanning electron microscope with an energy-dispersive spectrometer (SEM/EDX). the glass-ionomer-based materials, Fuji Triage (FT), Fuji VIII (FVIII). Fuji IX GP (FIX), were analyzed. The sample comprised 45 cured cement disks. Five specimens of each tested material were placed in 3 storage solutions (saline, acidic solution with pH of 5.5, NaF solution with 0.05 % of fluoride). Nano-indentations were performed with a force up to 30 mN, penetration depths of 2500-2700 nm for 1 d and 21 d after setting. The EDX evaluation was carried out for each experimental disk, identifying the ions: O, Al, Sr, Si, F,Na, P, Ca. The level of significance was placed at p lt 0.05.The highest fluoride proportion at the specimen surface was recorded in the FT material. FT also exhibited the lowest fluoride ions content when stored in low-pH environments compared with the other tested materials (p lt 0.05). The surface hardness of the tested materials decreased from 1.377 GPa (in saline) to 0.03 GPa (in acid). The Young's modulus varied from 14.35 GPa to 0.112 GPa, depending on the material type (Fuji VIII>Fuji IX>FT) (p lt 0.001) and the storage media (p lt 0.001). Both the mechanical and cariostatic surface properties of commercially available glass ionomer materials are affected by the storage media.

Electrodeposition of Al–W alloy films with high W contents has been carried out using 1-ethyl-3-methylimidazolium chloride (EMIC)–aluminum chloride (AlCl₃) ionic liquids containing tungsten(II) chloride (W₆Cl₁₂). Although the corrosion resistance and hardness of the alloy films are expected to be improved with an increase in the W content, dense films with W contents higher than ∼12 at% have not been obtained by electrodeposition to date. This study has demonstrated that electrodeposition using a EMIC-AlCl₃-W₆Cl₁₂ bath with a lower AlCl₃/EMIC molar ratio can yield Al–W alloys with higher W contents. The maximum W content of the alloys electrodeposited using the EMIC–1.5AlCl₃ bath reached 19.4 at%. The alloy films with up to ∼18 at% W were dense and smooth, whereas those with >∼18 at% W exhibited increased surface roughness. The hardness and Young’s modulus of the dense and smooth 17.7 at% W film were determined by nano-indentation. The hardness of this film was confirmed to be higher than those of the Al–W alloy films previously obtained from the EMIC–2AlCl₃ baths.

This article deals with the influence of electron beam radiation on nano-mechanical properties and the structure of polyamide 11. Crosslinking of polymers is a process, during which macromolecular chains start to connect to each other and the spatial network creates in the structure. During the action of the ionizing radiation two actions can occur: crosslinking and scission of macromolecules – degradation. Both these processes run parallel. Using the crosslinking technology the standard and construction polymer can obtain the more “expensive” high-tech polymeric materials properties and thus replace these materials in many applications. Tested material was irradiated by different doses of beta radiation (33, 66 and 99 kGy). The nano-mechanical properties were measured using DSI method, which fluently records the change of the indentation in time. From this dependence it is possible to determine nano-mechanical properties such as indentation hardness, indentation modulus etc. During results consideration it is obvious that irradiation acts on each polymer differently, but always when the optimal dose was found, nano-mechanical properties increased up to 34 %. The changes of nano-mechanical properties were confirmed by structural measurement when the change of hardness and modulus corresponded to gel content. © 2018, North Atlantic University Union. All rights reserved.

This article deals with the influence of electron beam radiation on nano-mechanical properties and the structure of polyamide 11. Crosslinking of polymers is a process, during which macromolecular chains start to connect to each other and the spatial network creates in the structure. During the action of the ionizing radiation two actions can occur: crosslinking and scission of macromolecules – degradation. Both these processes run parallel. Using the crosslinking technology the standard and construction polymer can obtain the more “expensive” high-tech polymeric materials properties and thus replace these materials in many applications. Tested material was irradiated by different doses of beta radiation (33, 66 and 99 kGy). The nano-mechanical properties were measured using DSI method, which fluently records the change of the indentation in time. From this dependence it is possible to determine nano-mechanical properties such as indentation hardness, indentation modulus etc. During results consideration it is obvious that irradiation acts on each polymer differently, but always when the optimal dose was found, nano-mechanical properties increased up to 34 %. The changes of nano-mechanical properties were confirmed by structural measurement when the change of hardness and modulus corresponded to gel content. © 2018, North Atlantic University Union. All rights reserved.

Little is known today about the mechanical properties of the graphite nodules, despite the key influence these particles have on the performance of ductile cast irons. To address this issue, nano-indentation tests were performed on the cross-section of a nodule whose sub-surface morphology was characterized via 3D computed tomography. From the recorded load vs. penetration curves, the spatial variation of the maximum indenter penetration hmax and of the reduced Young's modulus E* was determined. It was observed that the pattern of hmax presents features which, statistically, cannot be explained with the experimental error. Conversely, they can be justified by a model which takes into account the geometrical interaction between the indenter and the local orientation of the graphite platelets forming the nodule. To the authors’ best knowledge, this result constitutes the first direct proof of a clear link between internal structure and mechanical properties of the nodules. The existence of a non-negligible mechanical anisotropy implies that the calculated mean value of E* can only be seen as indicative of a sort of “averaged” elastic stiffness. Caution should then be used when assessing the elastic response of the entire nodule just on the basis of this parameter, as complex anisotropic effects associated with the non-random orientation of the graphite platelets can be foreseen.

Al–W alloy films with various W contents up to ~ 12 at.% were prepared by electrodeposition using 1-ethyl-3-methylimidazolium chloride (EMIC)–AlCl₃ ionic liquids with different concentrations of W precursor, W₆Cl₁₂. The hardness (H) and Young's modulus (E) of the films were examined by nano-indentation. The films were composed of a single-phase fcc Al super-saturated solid solution, an amorphous phase, or both, depending on the W content and the deposition conditions. The H value increased with increasing W content up to 9.8 at.% and then decreased slightly with further increases in the W content up to 12.4 at.%. A similar trend was observed in the E value with increasing W content, but the decrease in E value at 12.4 at.% W was more significant than that in H value. The changes in the H and E values are discussed from the viewpoints of the grain size and the constituent phases. The 9.8–12.4 at.% W films, which had relatively high H values and H/E ratios, are expected to have a higher resistance to mechanical damage than Al films.

A comparison is made between the mechanical properties of the ultra-high-strength steel KNDS4 of fastener grade 14.9 and of conventional, high-strength steels 34Cr4 of fastener grade 12.9 and 33B2 of grade 10.9. The results show that the ratio of the yield strength at elevated temperatures to the yield strength at room temperature is higher for the ultra-high-strength steel than for both conventional highstrength steels, especially at 500°C. Moreover, the results show a trend in which the nano-indentation creep rate is lower as the strength of the steels is higher. The improved mechanical properties of the KNDS4 steel compared to the conventional high-strength steels are related to the smaller size of the alloy carbides in the KNDS4 steel. Furthermore, the effect of an alternative (industrial) heat-treatment on the evolution of the microstructure and hardness of the KNDS4 steel was investigated. Changing the industrial heat treatment can increase the hardness of KNDS4 by about 8%, since more alloy carbides can nucleate and grow. However, the standard industrial heat treatment results in a refinement of the martensite microstructure (grain size), which might be more beneficial for the toughness of the steel. Independent of the heat treatment, the mechanical performance of KNDS4 fasteners at elevated temperature and the low nano-indentation creep rates are two strong indicators that fasteners made from KNDS4 steel might be used at higher service temperatures than traditional high strength fasteners., OLD Metals Processing, Microstructures and Properties, Steel & Composite Structures, (OLD) MSE-1

Radiation crosslinking of filled PBT is a well-recognized modification of improving basic material characteristics. Radiation, which penetrated through specimens and reacted with the cross-linking agent, gradually formed cross-linking (3D net), first in the surface layer and then in the total volume, which resulted in considerable changes in specimen behaviour. The specimens of 30% glass fiber filled PBT were made by injection moulding technology and irradiated by doses of beta radiation (0, 33, 66 and 99 kGy). The change of nano-mechanical properties is greatly manifested mainly in the surface layer of the modified PBT where a significant growth of nano-mechanical values can be observed. Indentation modulus increased from 1.1 to 1.8 GPa (increasing about 64%) and indentation hardness increased from 56 to 85 MPa (increasing about 52%).The results of the measurements showed considerable increase in nano-mechanical properties (indentation hardness, indentation elastic modulus, indentation creep) when beta radiation are used. © 2016, MM publishing Ltd. All rights reserved.

The influence of high doses of beta radiation on the changes in the structure and selected properties (mechanical and thermal) polymers were proved. Using high doses of beta radiation for low density polyethylene (LDPE) and its influence on the changes of mechanical properties of surface layer has not been studied in detail so far. The specimens of low density polyethylene (LDPE) were made by injection moulding technology and irradiated by high doses of beta radiation (0, 132, 165 and 198 kGy). The changes in the microstructure and micromechanical properties of surface layer were evaluated using FTIR, WAXS and instrumented nanohardness test. The results of the measurements showed considerable increase in mechanical properties (indentation hardness, indentation elastic modulus) when the high doses of beta radiation are used. © 2016, MM publishing Ltd. All rights reserved.

When skeletonized remains are found it becomes a police task to determine to identify the body and establish the cause of death. It assists investigators if the Post-Mortem Interval (PMI) can be established. Hitherto no reliable qualitative method of estimating the PMI has been found. A quantitative method has yet to be developed. This paper shows that IR spectroscopy and Raman microscopy have the potential to form the basis of a quantitative method.