Microindentation Hardness Testing Research Articles

Microhardness Variation with Indentation Depth for Body-Centered Cubic Steels Pertinent to Grain Size and Ferrite Content.

For a micro-indentation hardness test with non-destructivity, the Nix-Gao model is widely used to describe tested hardness or microhardness variation with an indentation depth induced by indentation size effect, in which tested hardness approaches the macrohardness when the indentation depth is large enough. Based on an analysis of hardness measurements on 10 body-centered cubic steels with diverse microstructure, this paper proposes an analytical relation between microhardness to macrohardness ratio and the indentation depth by explicitly linking characteristic indentation depth (a data-fitting parameter) to grain size and ferrite volume fraction using two different methods. In addition, the normal distribution theory is incorporated to consider the inevitable scatter of identical measurements resulting from material heterogeneity and machining/testing errors. Results show that the proposed model, with 96% reliability, can effectively predict microhardness variation with the indentation depth and its scatter.

Impact of Ultra-Flash Tempering Treatment on the Microstructure and Mechanical Properties of High-Strength Carbon Steel

A novel high-frequency induction technology was successfully developed to carry out ultra-flash tempering treatment (UFTT) of high-strength carbon steel (HS-CS) with a heating rate of 1000 °C/s. The as-received HS-CS is a fully martensitic structure with low toughness. UFTT strategy at various temperatures is proposed to produce a tempered martensitic lath structure with promoting carbide precipitates in this structure. Microstructure evolution during UFTT was characterized using secondary electron imaging and electron backscatter diffraction technique in a scanning electron microscope. Micro-indentation hardness tests were measured through the cross-section of the steel to analyze the impact extent of UFTT. The mechanical properties were measured by uniaxial tensile tests. The results revealed that UFTT at various temperatures (550-650 °C) significantly affected the microstructure and the mechanical strength of the steel. A fully tempered martensitic microstructure with various types of carbide precipitates was promoted. Although, the microhardness and tensile strength of flash-tempered steel decreased owing to the breakdown of lath and dislocation structure in the achieved microstructure by UFTT. Hence, it is expected that the promoted microstructure during UFTT in the tested steel will result in a superior strength-toughness synergy. Based on the achieved results, the UFTT technique provides an alternative route for the conventional processing to tailor the microstructure of microalloyed HS-CS, consequently, optimizing the mechanical performance. Meanwhile, Economically, it is a cost-effective route to manufacture advanced high-strength steel.

Influence of titanium particulate reinforcement on microstructural evolution and mechanical performance of AZ91 magnesium matrix surface composite developed through friction stir processing

ABSTRACT AZ91 Magnesium alloy is widely used in automobile components, bio-implants, mobile and computer parts, sporting goods, etc., owing to its low density, high strength to weight ratio, good machinability and biodegradable characteristics. However, it has moderate strength and poor ductility that hinders its engineering application. The incorporation of ceramic reinforcement in Mg alloys to form high-strength composites shows a major loss in its ductility. In this research work, friction stir processing (FSP) was used with two innovative tool designs to enhance mechanical and microstructural properties by employing titanium powders as reinforcement particles – metallic reinforcement possessing higher melting point, offering a solution to the issue. The tools were designed with stepped square profile, where in one design, the square steps were aligned with each other (S-type) and in the other design, the square edges were mis-aligned by 45˚ (D-type). Microstructural analysis was done using optical microscopy, scanning electron microscopy and X-ray diffraction. Mechanical properties, micro-indentation hardness test and compression test, were studied in detail. Results revealed that the FSP process performed with D-type tool yielded better results with more uniform distribution of Ti particles in the stir zone and grain refinement with refined recrystallised grains down to about 8 µm due to severe plastic deformation and dynamic recrystallisation. The compressive strength of the material processed using D-tool was found to be increased to 456 MPa. Ti particles established a proper interface with the matrix delaying the failure of the material, thereby improving the ductility of the material as well. The mechanisms leading to microstructural refinement and enhancement in mechanical performance are presented in detail.

Change in transition balance between durable tetragonal phase and stress-induced phase of cobalt surface-layered in Bi-2212 materials by semi-empirical mechanical models

This study has indicated the positive effect of sintering temperature on the mechanical durability, strength, critical stress, deformation degrees, durable tetragonal phase, failure and fracture by fatigue, and mechanical characteristic behavior to the applied test loads for the Co surface-layered Bi-2212 ceramic materials produced by the standard solid-state reaction method. The sintering mechanism has been used as the driving force for the penetration of cobalt ions in the Bi-2212 ceramic matrix. The microindentation hardness test measurements have been performed at the load intervals 0.245 N-2.940 N. The experimental findings have also been examined by the six different semi-empirical mechanical and indentation-induced cracking models. It has been found that all the mechanical performance parameters are improved considerably with increasing the diffusion sintering temperature up to 650 °C. On this basis, the Co surface-layered Bi-2212 sample produced at the sintering temperature of 650 °C has been observed to improve dramatically the mechanical durability and resistance to the applied test loads as a consequence of the formation of new force barrier regions, surface residual compressive stress regions, and slip systems in the Bi-2212 ceramic system. Similarly, the optimum sintering temperature has extensively enhanced the elastic recovery mechanism, critical stress values, and deformation degree levels, stored internal strain, and crack surface energy through the Bi-2212 ceramic materials. Accordingly, it has been noted that the best sample produced at 650 °C is more hardly broken than the other ceramics. Namely, the optimum sintering temperature has decreased the sensitivity to the applied test loads as a result of delaying the beginning of the plateau limit regions. On the other hand, all the mechanism has been found to reverse completely depending on the excess sintering temperature. Lastly, the indentation-induced cracking model has been found to exhibit the closest results to the original Vickers microhardness parameters in the plateau limit regions.

Interfacial behaviour and stress transfer mechanism of additively manufactured laser cladding sheet-covered steel plates

Laser cladding (LC), a metal additive manufacturing process, is employed to strengthen steel plate which has benefits over traditional steel structure retrofit approaches. In this study, the interfacial behaviour between the substrate and LC sheet of laser cladding sheet (LCS)-covered steel plates is investigated, through a series of mechanical tensile coupon tests by considering the effects of the scanning pattern and the thickness and length of the LC sheet. Double-shear pull tests, metallographic tests and microindentation hardness tests are also carried out to reveal the microstructure of the interfacial zone. It is observed from the macro and micro experimental results that the stresses in the LCS-covered plates in tension can be transferred effectively through the interface between the substrate and LC sheet, and perfect interfacial bonding behaviour with no slip could be assumed. A series of finite element (FE) analyses are further undertaken to calibrate such an assumption. Based on the fully bonded interface assumption, for convenient engineering application, a theoretical model is developed to describe the elastic stress/strain distributions of LCS-covered steel plates subject to tension, by following the equilibrium considerations and plane strain elastic theory. The theoretical model is validated by comparing its predictions with the experimental and FE analysis results. The proposed theoretical model would provide baseline solution for future elastic strain/stress analysis of the LCS-covered steel plates.

Evolution of dynamics of physico-chemical and mechanical properties of hydroxyapatite with fluorine addition and degradation stability of new matrices

This multidisciplinary study examined sensitively the change in the dynamics of main mechanical performance, stability of crystal structure, crystallinity quality, strength, corrosion resistance, biocompatibility, resistance to structural degradation/separations and mechanical durability features of hydroxyapatite (HAp) biomedical materials based on the fluorine addition and degradation process to guide future medical and dental treatment studies. In the study, the fluorine ions were used to be the dental coating, filling and supporting material for biologically or synthetically produced bone minerals. The general characteristic properties were investigated by means of standard spectroscopic, structural and mechanical analysis methods including RAMAN, SEM-EDS, TEM, Vickers micro-indentation hardness and density measurements. A time dependent release test was performed to evaluate possible fluorine ion release after the degradation process. It was found that the fundamental characteristic properties of HAp biomedical materials are noted to improve with the increase in the fluoride level up to 2% due much more stabilization of HAp crystal system. The combination of RAMAN spectra and powder XRD analyzes indicates that 2% addition level affects positively the formation velocity of characteristic HAP phase. Besides, fluorine doped HAp materials all exhibited the main characteristic peaks after degradation process. This is attributed to the fact that the fluorine ions enabled the hydroxyapatite to enhance the structural quality and stability towards the corrosion environment. However, in case of excess dopant level of 3% the degradation rates were obtained to increase due to higher contribution rate and especially electrostatic interactions. As for the surface morphology examinations, 2% fluorine added HAp with the highest density of 3.0879 g/cm3 was determined to present the superior crystallinity quality (smallest grain size, best smooth surface, honeycomb pattern, regular shaped particles and densest particle distributions through the specimen surface). Conversely, the excess fluorine triggered to increase seriously degree of micro/macro porosity in the surface morphology and microscopic structural problems in the crystal system. Thus, the HAp doped with 3% was the most affected material from the degradation process. Additionally, the fluorine ion values read after the release process were quite far from the value that could cause toxic effects. Lastly, the optimum fluorine addition provides the positive effects on the highest durability, stiffness and mechanical fracture strength properties as a consequence of differentiation in the surface residual compressive stress regions (lattice strain fields), amplification sites and active operable slip systems in the matrix. Hence, the crack propagations prefer to proceed in the transcrystalline regions rather than the intergranular parts. Similarly, it was found that Vickers micro-indentation hardness tests showed that the microhardness parameters increased after the degradation process. All in all, the fluorine addition level of 2% was noted to be good choice to improve the fundamental characteristic properties of hydroxyapatite biomedical materials for heavy-duty musculoskeletal, orthopedic implant, biological and therapeutic applications in medicine and dentistry application fields.

Studying the strengthening mechanisms and mechanical properties of dissimilar laser-welded butt joints of medium-Mn stainless steel and automotive high-strength carbon steel

In this study, a post-weld heat treatment (PWHT) at a high temperature of 700 °C for 10 min was proposed to significantly improve the mechanical performance of dissimilar laser-welded butt joints between medium-manganese stainless steel (MMn-SS) and high-strength carbon steels (HS-CS) as base metals (BMs). Electron backscatter diffraction and transmission electron microscopy were employed to characterise the microstructures and study the deformation mechanisms in the paired metals of the dissimilar joints during PWHT and tensile straining. Micro-indentation hardness tests were performed to analyse the mechanical responses in the weld zones after PWHT. The results revealed that PWHT at 700 °C significantly affected the microstructure and mechanical strength of the BMs and their weldments. A fully tempered martensitic microstructure with recrystallised grain regions was formed in the fusion zones (FZs) of the weldments, which were processed at low and high specific point energies (SPEs) of 19, 25, and 30 J. BM HS-CS was significantly strengthened owing to the interphase precipitation hardening of vanadium carbide precipitates during the proposed PWHT. The strength-ductility balance of BM MMn-SS was improved by combining the martensitic transformation and mechanical twinning mechanisms. Although, the tensile strength of BM HS-CS increased from 500 to 630 MPa and that of the metal in the FZ decreased from 1100 to 800 MPa owing to PWHT. Hence, HS-CS is a weak metal for dissimilar joints, and joint failure was promoted in it.

Use of AFM topography images to determine microindentation hardness of cast tungsten carbide powders

Hardness is defined as the resistance of a material to localized plastic deformation. Owing to their non-destructive nature, static indentation hardness tests are widely used in industry. Hardness testing is particularly useful for the mechanical characterization of materials that cannot be tested otherwise, e.g. powdered materials. In this study, challenges related to Vickers microindentation hardness testing of hard brittle cast tungsten carbide (CTC) powders were extensively investigated. Test load was optimized to obtain sufficiently large crack-free indentations allowing for precise measurement of the diagonal lengths. The influence of the operator and imaging technique on the measured hardness value was evaluated. Topography of residual imprints was investigated using atomic force microscopy (AFM) and a systematic and operator bias-free method to locate the indentation vertexes was developed. Results suggested that measurement variability introduced by AFM scanning and post-processing was as low as 3.1% and 1.3% with respect to the mean hardness value, respectively. Since the variability due to the measuring system can be isolated, the homogeneity of powders can be reliably evaluated from the hardness measurements thus obtained.

Effects of Heat Treatment on Microstructure and Mechanical Properties of AlSi10Mg Fabricated by Selective Laser Melting Process

AlSi10Mg is the most widely additively manufactured and commercialized aluminum alloy and has been used in this study to analyze the effect of heat treatment on its microstructure and mechanical properties. Although research indicates AlSi10Mg parts produced by selective laser melting have characteristically very fine microstructures, there is a need for more intensive study to comprehend the effect of heat treatment on the mechanical properties of this alloy by analyzing its microstructure. In this study, AlSi10Mg specimens heat-treated at varying temperatures were analyzed by optical and electron microscopes. Micro-indentation hardness and tensile tests were performed to evaluate mechanical properties while considering the specimen build orientation. Observation shows that it is nearly impossible to completely dissolve the evolved second phase silicon-rich particles, which may have significant effects on the mechanical characteristics. Electron microscopy images show the evolution of iron-rich particles in the Al matrix, which may have a significant influence on the mechanical properties of the alloy.

Synthesis, microstructure and indentation Vickers hardness for (Y3Fe5O12)x/Cu0.5Tl0.5Ba2Ca2Cu3O10-δ composites

High-performance and low-cost composites are engineers’ dream for technological applications. To fulfill the material for an engineering application, it is important to understand the mechanical properties of the material. The primary goal of this research is to investigate the impact of nano-sized Yttrium iron garnet (Y3Fe5O12) addition on the microstructure and mechanical properties of the polycrystalline Cu0.5Tl0.5Ba2Ca2Cu3O10-δ (CuTl-1223) superconductor. Co-precipitation and solid-state reaction methods were utilized to prepare Y3Fe5O12 nanoparticles and Cu0.5Tl0.5Ba2Ca2Cu3O10-δ superconductor, respectively. (Y3Fe5O12)x/Cu0.5Tl0.5Ba2Ca2Cu3O10-δ nanoparticle/superconductor composites were formed by adding small contents of Y3Fe5O12 (x = 0.00, 0.02, 0.04, 0.06, 0.08, and 0.10 wt%) to the CuTl-1223 matrix. The volume fraction percentage of the main phase, CuTl-1223, was increased from 87.9 to 91.4% as x was adjusted from 0.00 to 0.04 wt%. The unit cell parameters (a and c) remained unchanged following the addition of Y3Fe5O12 nanoparticles to the host CuTl-1223. The porosity percentage (P %) was decreased from 39.1 to 29.4% as x was increased from 0.00 to 0.10 wt%. Thus, the addition of Y3Fe5O12 nanoparticles has the ability to reduce weak links and voids among the CuTl-1223 superconducting grains. The grain morphology for the prepared composites was identified through scanning electron microscopy. The different elemental compositions were detected by energy-dispersive X-ray measurements. Vickers microindentation hardness test was employed to study the mechanical strength of the prepared composites. Analysis and modelling of Vickers hardness (Hv) versus test load (F) were done through various models. Meyer’s empirical law showed that all the prepared composites follow normal indentation size effect behaviour. Hays and Kendall model clarified that the applied test load was sufficient to produce both elastic and plastic deformation for the investigated samples. The elastic/plastic deformation model indicated that the prepared samples contain an elastic relaxation portion that recovers after withdrawing the test load. The proportional sample resistance and modified proportional sample resistance models confirmed the HK model findings. Moreover, the HK model was found to be the most suitable model for describing the microhardness results of the prepared samples. Furthermore, the elastic modulus (E), yield strength (Y), fracture toughness (K) and brittleness index (B) for the prepared composites were calculated as function of Y3Fe5O12 addition.

Biodegradable Thermoplastic Starch/Polycaprolactone Blends with Co-Continuous Morphology Suitable for Local Release of Antibiotics.

We report a reproducible preparation and characterization of highly homogeneous thermoplastic starch/pol(ε-caprolactone) blends (TPS/PCL) with a minimal thermomechanical degradation and co-continuous morphology. These materials would be suitable for biomedical applications, specifically for the local release of antibiotics (ATB) from the TPS phase. The TPS/PCL blends were prepared in the whole concentration range. In agreement with theoretical predictions based on component viscosities, the co-continuous morphology was found for TPS/PCL blends with a composition of 70/30 wt.%. The minimal thermomechanical degradation of the blends was achieved by an optimization of the processing conditions and by keeping processing temperatures as low as possible, because higher temperatures might damage ATB in the final application. The blends’ homogeneity was verified by scanning electron microscopy. The co-continuous morphology was confirmed by submicron-computed tomography. The mechanical performance of the blends was characterized in both microscale (by an instrumented microindentation hardness testing; MHI) and macroscale (by dynamic thermomechanical analysis; DMTA). The elastic moduli of TPS increased ca four times in the TPS/PCL (70/30) blend. The correlations between elastic moduli measured by MHI and DMTA were very strong, which implied that, in the future studies, it would be possible to use just micromechanical testing that does not require large specimens.

Pro-oxidant activity of biocompatible catechin stabilizer during photooxidation of polyolefins

Polymer plaques made of high-density polyethylene (HDPE) or cycloolefin copolymer (COC) were stabilized with natural phenolic stabilizer (+)-catechin (CAT) and aged using accelerated weathering technique (WOM; accelerated photooxidation). The efficiency of the phenolic stabilizer was compared with a well-established hindered amine stabilizer (HAS) Tinuvin®770 (Tin770). In pursuit of the stabilization and identification of short-living radicals generated in the process of photooxidation of the polymers, a spin trapping agent 2,4,6-tri-tert-butylnitrosobenzene (TTBNB) was added to selected samples. Profiles of oxidation products and crystallinity inside the HDPE plaques were determined by IR microspectroscopy, oxidation products in COC copolymers were identified using ATR spectroscopy, concentration profiles of radicals generated inside polymer plaques during WOM exposure were determined by ESRI, the changes of local mechanical properties at the surface of polymer plaques were characterized using microindentation hardness testing (MHI), and the surface morphology changes were studied by light and/or scanning electron microscopy. All methods are in accordance with the conclusion that the natural phenolic stabilizer CAT exhibited pro-oxidant activity during accelerated photooxidation of both polymers, i.e. higher concentration of oxidation products, bigger changes of local mechanical properties and/or more microcracks on the exposed surfaces in comparison with non-stabilized systems and systems stabilized with Tin770.

Effect of annealing ambient conditions on crack formation mechanisms of bulk Bi-2212 ceramic systems

ABSTRACT This study paves way to examine the influence of different annealing conditions (temperature range of 830-850°C and duration intervals 24-48 h) on the fundamental mechanical performance and characteristic quantities of polycrystalline Bi2.1Sr2.0Ca1.1Cu2.0Oy (Bi-2212) superconducting ceramics by means of Vickers microindentation hardness tests at the various indentation test loads (0.245 N≤F≤2.940 N) and some available theoretical approaches. The annealing ambient plays an important role on the operable slip systems and crystal quality. The bulk Bi-2212 superconducting compound prepared at 840 °C and 24 h is found to be the least sensitive to the applied test load due to less structural problems, voids, cracks and stress raisers in the crystal system. Conversely, the excess annealing ambient complicates remarkably the control of crack growth size and velocity. Thus, relatively lower load can lead to the formation of crack and acceleration of crack rate up to the critical size and terminal velocity. The samples exhibit the typical indentation size effect (ISE) behavior as a result of predominant character of elastic recovery mechanism. As for the theoretical examination in the saturation limit regions, the indentation-induced cracking (IIC) model wins the comparison as it provides the most accurate results to the experimental findings.

A novel investigation into edge effect reduction of 4340 steel spur gear during induction hardening process

Induction hardening, a promising approach for selective hardening of metal parts, is widely used for surface hardening, where a hard surface is required alongside a tough core. Regarding the complexity of this process, parts’ geometry deeply affects the temperature distribution and hardness profile accordingly. In this study, two magnetic flux concentrators are introduced to our induction machine set in order to control the magnetic flux and consequently hardness profile (case depth) of spur gears. The performance of magnetic flux concentrators is examined by the effect of machine parameters on the case depth and the edge effect of AISI 4340 steel-made spur gear. Design of experiments based on Taguchi method is primarily used to optimize the number of experimental trials. Then, the hardness profiles of heat-treated gears at the tip and root of gears are measured by microindentation hardness tests. The results are analyzed using analysis of variance (ANOVA) and response surface methodology (RSM) to determine the main effect of process parameters, also the best combination of process parameters that maximizes the case depth and minimizes the undesirable feature of edge effect. Finally, the predicted case depth models versus process parameters are developed based on linear regression method. To this end, four predictive models of case depth at tip and root in the edge plane and middle plane of spur gears are generated. Results imply that maximum case depth with minimum edge effect at root and tip is achieved by setting up the highest machine power, longest heating time, and minimum axial gap between concentrators and the spur gear. This study provides a good exploration of case depth in presence of magnetic flux concentrators under various process parameters and gives a reliable guideline towards edge effect during induction hardening process.

Macro-, Micro- and Nanomechanical Characterization of Crosslinked Polymers with Very Broad Range of Mechanical Properties.

This work is focused on the comparison of macro-, micro- and nanomechanical properties of a series of eleven highly homogeneous and chemically very similar polymer networks, consisting of diglycidyl ether of bisphenol A cured with diamine terminated polypropylene oxide. The main objective was to correlate the mechanical properties at multiple length scales, while using very well-defined polymeric materials. By means of synthesis parameters, the glass transition temperature (Tg) of the polymer networks was deliberately varied in a broad range and, as a result, the samples changed their mechanical behavior from very hard and stiff (elastic moduli 4 GPa), through semi-hard and ductile, to very soft and elastic (elastic moduli 0.006 GPa). The mechanical properties were characterized in macroscale (dynamic mechanical analysis; DMA), microscale (quasi-static microindentation hardness testing; MHI) and nanoscale (quasi-static and dynamic nanoindentation hardness testing; NHI). The stiffness-related properties (i.e., storage moduli, indentation moduli and indentation hardness at all length scales) showed strong and statistically significant mutual correlations (all Pearson′s correlation coefficients r > 0.9 and corresponding p-values < 0.001). Moreover, the relations among the stiffness-related properties were approximately linear, in agreement with the theoretical prediction. The viscosity-related properties (i.e., loss moduli, damping factors, indentation creep and elastic work of indentation at all length scales) reflected the stiff-ductile-elastic transitions. The fact that the macro-, micro- and nanomechanical properties exhibited the same trends and similar values indicated that not only dynamic, but also quasi-static indentation can be employed as an alternative to well-established DMA characterization of polymer networks.

Comparison of macro-, micro- and nanomechanical properties of clinically-relevant UHMWPE formulations

We characterized a set of eleven clinically relevant formulations of UHMWPE for total joint replacements. Although their molecular and supermolecular structure were quite similar as evidenced by IR, DSC and SAXS measurements, there were slight differences in their crystallinity (DSC crystallinity ranging from 52 to 61%), which were connected with processing conditions, such as the total radiation dose, thermal treatment and/or addition of biocompatible stabilizers. Mechanical properties were assessed at all length scales, using macroscale compression testing, non-instrumented and instrumented microindentation hardness testing (at loading forces ~500 mN), and nanoindentation hardness testing measured at both higher and lower loading (~4 mN and ~0.6 mN, respectively). In agreement with theoretical predictions, we found linear correlations between UHMWPE crystallinity and its stiffness-related properties (elastic moduli, yield stress, and hardness) at all length scales (macro-, micro- and nanoscale). Detailed statistical evaluation of our dataset showed that the accuracy and precision of the applied methods decreased in the following order: non-instrumented microindentation ≥ instrumented microindentation ≥ macromechanical properties ≥ nanoindentation measured at higher loading forces ≫ nanoindentation measured at lower loading forces. The results confirm that microindentation and nanoindentation at sufficiently high loading forces are reliable methods, suitable for UHMWPE characterization.

A novel method of identifying porosity during laser welding of galvanized steels using microhardness pattern matrix

Galvanized steel welded joints are susceptible to porosities since their protective zinc layer may be evaporated and trapped during welding. In this study, a novel approach of identifying voids and porosities is developed by performing a pattern matrix of micro-indentation hardness tests in the cross-section of welds. The hardness grid is then visualized by 3D contour plots to identify the form and position of porosities. This method is investigated on laser-welded galvanized steel plates with reinforcement in which low hardness measurements in the welding area present voids, porosities, and unexpected gaps between joining and reinforcing plates.

Monitoring of Morphology and Properties During Preparation of PCL/PLA Microfibrillar Composites With Organophilic Montmorillonite

Biodegradable microfibrillar composites PCL/PLA/C15, where PCL is poly(e-caprolactone), PLA is poly(lactic acid) and C15 is organophilic montmorillonite, have been prepared. Microindentation hardness testing was employed in monitoring the gradual improvement of PCL stiffness due to PLA addition, C15 addition, flow-induced orientation, and changing crystallinity throughout the whole preparation process. Neat PCL after extrusion and injection molding was quite soft, but the stiffness of the material increased after melt-blending with 20 wt.% of PLA, after the addition of 2 wt.% of C15, and after the preparation of the final microfibrillar composite. The indentation modulus and indentation hardness of all intermediate products and the final PCL/PLA/C15 microfibrillar composite were associated not only with the composition and morphology but also with the crystallinity of both components. The modulus of the final PCL/PLA/C15 composite was almost two times higher in comparison with the original PCL matrix.

Mechanical Resistance in Decapod Claw Denticles: Contribution of Structure and Composition

The decapod crustacean exoskeleton is a multi-layered structure composed of chitin-protein fibers embedded with calcium salts. Decapod claws display tooth-like denticles, which come into direct contact with predators and prey. They are subjected to more regular and intense mechanical stress than other parts of the exoskeleton and therefore must be especially resistant to wear and abrasion. Here, we characterized denticle properties in five decapod species. Dactyls from three brachyuran crabs (Cancer borealis, Callinectes sapidus, and Chionoecetes opilio) and two anomuran crabs (Paralomis birsteini and Paralithodes camtschaticus) were sectioned normal to the contact surface of the denticle, revealing the interior of the denticle and the bulk endocuticle in which it is embedded. Microhardness, micro- and ultrastructure, and elemental composition were assessed along a transect running the width of the cuticle using microindentation hardness testing, optical and scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDS), respectively. In all species tested, hardness was dramatically higher—up to ten times—in the denticle than in the bulk endocuticle. Likewise, in all species there was an increase in packing density of mineralized chitin-protein fibers, a decrease in width of the pore canals that run through the cuticle, and a decrease in phosphorous content from endocuticle to denticle. The changes in hardness across the cuticle, and the relationship between hardness, calcium, and magnesium content, however, varied among species. Although mechanical resistance of the denticles was exceptionally high in all species, the basis for resistance appears to differ among species. Statement of SignificanceUnderstanding the diverse mechanisms by which animals attain exceptionally high mechanical resistance may enable development of novel, biologically inspired materials. Decapod crustacean claws, and particularly the tooth-like denticles that these claws display, are of interest in this regard, as they must be especially resistant to wear. We assessed mechanical, elemental, and structural properties of the claw cuticle in five decapod species. Without exception, microhardness was dramatically higher in the denticle than in the bulk endocuticle. Multivariant statistical analyses, however, showed that the relationships among microhardness, elemental content, and structural variables differed among species. Such patterns likely result from strong evolutionary pressure on feeding and defensive structures and a trade-off between mechanical properties and energetic cost of exoskeleton formation.

Effect of Hydrogen Electrosorption on Mechanical and Electronic Properties of Pd80Rh20 Alloy.

The interaction of hydrogen with Pt-group metals and alloys is at the center of research in the fields of electrochemistry, electrocatalysis, hydrogen technologies and fuel cells developed under the Hydrogen Economy. In this work, the material under study was Pd80Rh20 alloy (50 μm foil) subjected to hydrogen electrosorption at potentials corresponding to formation of α, α-β and β phase in 0.1 M H2SO4 at 25 °C. The total amount of hydrogen adsorbed at the surface and absorbed in octahedral interstitial positions of fcc Pd80Rh20 alloy, was determined from the oxidation charges. The H/(Pd+Rh) was 0.002, 0.4 and 0.8 for α, α-β, and β Pd80Rh20H, respectively. Microindentation hardness testing and nanoindentation showed weakening of mechanical properties of the Pd80Rh20 alloy after hydrogen electrosorption due to internal stresses. Decrease of work function with increasing amount of hydrogen absorbed occurred due to the surface roughness changes and the presence of electropositive hydrogen atoms absorbed in the crystal lattice responsible for the dipole interaction. The detailed mechanism of hydrogen absorption/diffusion in the Pd80Rh20 alloy structure is discussed. The obtained results give a new insight into the relationship between the amount of absorbed hydrogen and mechanical and electronic properties of the Pd80Rh20 alloy at the micro- and nanoscale.