Mechanical heterogeneity characterization of coal materials based on nano-indentation experiments

To investigate the complex macro-mechanical properties of coal from a micro-mechanical perspective,we have conducted a series of micro-mechanical experiments on coal using a nano-indentation instrument.These experiments were conducted under both dynamic and static loading conditions,allowing us to gather the micro-mechanical parameters of coal for further analysis of its micro-mechanical heterogeneity using the box counting statistical method and the Weibull model.The research findings indicate that the load–displacement curves of the coal mass under the two different loading modes exhibit noticeable discreteness.This can be attributed to the stress concentration phenomenon caused by variations in the mechanical properties of the micro-units during the loading process of the coal mass.Consequently,there are significant fluctuations in the micro-mechanical parameters of the coal mass.Moreover,the mechanical heterogeneity of the coal at the nanoscale was confirmed based on the calculation results of the standard deviation coefficient and Weibull modulus of the coal body’s micromechanical parameters.These results reveal the influence of microstructural defects and minerals on the uniformity of the stress field distribution within the loaded coal body,as well as on the ductility characteristics of the micro-defect structure.Furthermore,there is a pronounced heterogeneity in the micromechanical parameters.Furthermore,we have established a relationship between the macro and micro elastic modulus of coal by applying the Mori-Tanaka homogenization method.This relationship holds great significance for revealing the micro-mechanical failure mechanism of coal.

Evaluation of microstructure and mechanical properties of Mg-xCe-0.5Zn alloys by nano-indentation

The microstructure and mechanical properties of Mg-xCe-0.5Zn （x=0.5, 1.5, 2.5, molar fraction, %） alloys were examined using a nano-indentation technique. The alloys were fabricated using a vacuum induction melting method under an argon atmosphere The microstruetures of Mg-xCe-0.5Zn alloys mainly consist ofa-Mg and eutectic Mg12Ce phase. The volume fraction and size of the eutectic Mgl2Ce phase increase with increasing Ce contents. Nano-indentation test results show that the indentation hardness and elastic modulus of the eutectic Mg12Ce phase are higher than those of the a-Mg matrix. In addition, the mean indentation hardness and elastic modulus of the Mg-xCe-0.5Zn alloys increase with the Ce addition amount increasing.

Effects of elastic-plastic properties of materials on residual indentation impressions in nano-indentation using sharp indenter

One of the primary features of nano-indentation technique is that the contact area induced by an indenter is indirectly measured by a relationship between the penetration depth and the known geometry of the indenter.However,this indirect measurement occasionally leads to inaccurate properties of the indented material.The objective of this study is to investigate the effects of E/σr and the strain hardening exponents n of materials on the behaviors of pile-up and sink-in in nano-indentation and to predict n values of materials from the residual indentation impressions.The relations between the residual indentation profile and n value of the indented material were identified by dimensional analysis.Also,they were numerically formulated using FE analysis of nano-indentation for 140 different combinations of elastic-plastic parameters such as E,σy and n.The parameters of hrp/hm,herp/hm,Rr/hm and HO&P/Hreal were introduced as various dimensionless parameters to represent and quantify the residual indentation profile after indentation.They were subsequently characterized as dimensionless functions using n and E/σr values.Finally,the validity of these functions was verified through 3D FE analysis of nano-indentation for Al 6061-T6 and AISI 1010 materials.

Analysis of Solvent Effect on Mechanical Properties of Poly(ether ether ketone) Using Nano-indentation

Poly（ether ether ketone） （PEEK） is a high-performance semi-crystalline thermoplastic polymer. Exposure of the polymeric surface to solvents can have a strong effect like softening/swelling of polymeric network or dissolution. In this study, nano-indentation analysis was performed to study the effect of acetone on the surface mechanical properties of PEEK using different exposure time. The experiments were performed with a constant loading rate （10 nrn/s） to a maximum indentation displacernent （1000 nrn）. A 30-second hold segrnent was included at the maximum load to account for any creep eft）ors followed by an unloading segrnent to 80% unloading. The indentation hardness and the elastic modulus were corn- puted as a continuous function of the penetration displacernent in the continuous stiffness mode （CSM） indentation. The experirnental data showed that the peak load decreased from -5.2 mN to -1.7 mN as exposure tirne in solvent environrnent increased from 0 to 18 days. The elastic modulus and the hardness of PEEK samples also displayed a decreasing trend as a function of exposure tirne in the solvent environrnent. Two empirical models were used to fit the experirnental data of hardness as a function of exposure tirne which showed a good agreernent with the experirnental values.

Nano-indentation study on the(001) face of KDP crystal based on SPH method

In order to avoid the defects of mesh distortion when dealing with large deformation problems through using the finite element method, a mess-free simulation method--smooth particle hydrodynamics （SPH） has been introduced. The material constitutive model of KDP crystal has been established based on the elastic-plastic theory. Then the nano-indentation on the （001） face of KDP crystal has been carried out using SPH method. Simulation results show that the maximum equivalent stress and the maximum plastic strain concentrate on the area that located near the tip of the indenter during the loading process. The distribution shape of Von Mises stress is similar to concentric circles. During the unloading process, no obvious variation of plastic strain distribution exists. The maximum Von Mises stress is mainly located at the indentation and its edge at the end of the unloading process. The approximate direct proportion relationship between the maximum indentation depth and the depth of the maximum Von Mises stress distribution has been discovered when the maximum load is lower than 8 mN. In addition, the nano-indentation experiments on KDP crystal＇s （001） face have been carried out. Both the material parameters and the adjusted stress-strain curve have been verified. The hindering role of the affected layer has been found and analyzed.

Structural,mechanical and electronic properties of precipitates in Mg−Zn alloys

To accelerate the development and design of magnesium(Mg)alloys,the structural and mechanical properties of important precipitates in Mg−Zn alloys were studied by experiments and density functional theory.The nano-indentation tests revealed that the hardness of the precipitates initially increased and then decreased with increasing Zn content,and was significantly higher than that of pure Mg and Zn.The calculation results revealed that the precipitates stability initially increased and then decreased with increasing Zn concentration.The bulk moduli of the precipitates increased,whereas their shear and Young’s moduli initially increased and then decreased with increasing Zn content.The decreasing order of ductility for these compounds is MgZn_(2)>Mg_(21)Zn_(25)>Mg_(2)Zn_(11)>Mg_(4)Zn_(7).The surface profiles of the compounds revealed that they are obvious anisotropy.Both the degree of covalency and bond length of covalent bonds initially increased and then decreased with increasing Zn content.

Effect of laser remelting on microstructure and mechanical properties of CrMnFeCoNi high entropy alloy

Equiatomic CrMnFeCoNi high entropy alloy prepared by powder metallurgy was remelted by laser.The relative density and microstructure of fusion zone are evaluated.The nanoindentation tests are conducted to reveal the hardness difference of dendrite arms and interdendritic areas.Tensile tests are conducted to assess the mechanical properties of remelted HEA.After laser remelting,the number and morphology of voids changed significantly.Dendritic structure with face-centered cubic phase form in the fusion zone.Fe,Cr and Co are enriched in dendrite arm,while Mn and Ni are enriched in interdendritic area.Elements segregation led to a nanohardness difference between dendrite arm and interdendritic area.Local deformation occurs in interdendritic area during tensile tests and results in a fracture with directionality.

Nano-Mechanical Behavior and Nano-Tribological Properties of 316 Stainless Steel

The microstructure and nano-tribological properties of 316 austenitic stainless steel have been investigated by using the in situ nano-mechanical testing system Tribolndenter, in which six different normal forces were chosen to make a scratch and indentation. The results show that the contact depth of the indentation increases with the normal force and material is piled up on the edge of the indentation as plastic distortion. The stable nano-hardness and the reduced modulus of 316 austenitic stainless steel are approximately 6 GPa and 160 GPa, respectively. The friction coefficients of 316 stainless steel with conic-type diamond tip have a typical value of about 0.13, 0.15, 0.17, 0.19, 0.22 and 0.25 when the normal forces are kept at 500 μN, 1000 μN, 1500 μN, 2000 μN, 2500 μN and 3000 μN, revealing an increasing trend with the normal forces. The increase of the friction coefficient in the unloading segment may result from the adhesion force caused by the material piled up.

Sandstone-concrete interface transition zone (ITZ) damage and debonding micromechanisms under freeze-thaw

The sufficient bond between concrete and rock is an important prerequisite to ensure the effect of shotcrete support. However, in cold regions engineering protection system, the bond condition of rock and concrete surface is easily affected by freeze-thaw cycles, resulting in interface damage, debonding and even supporting failure. Understanding the micromechanisms of the damage and debonding of the rock-concrete interface is essential for improving the interface protection.Therefore, the micromorphology, micromechanical properties, and microdebonding evolution of the sandstone-concrete interface transition zone(ITZ) under varying freeze-thaw cycles(0, 5, 10, 15, 20) were studied using scanning electron microscope, stereoscopic microscope, and nano-indentation. Furthermore, the distribution range and evolution process of ITZ affected by freeze-thaw cycles were defined. Major findings of this study are as follows:(1) The microdamage evolution law of the ITZ under increasing freeze-thaw cycles is clarified, and the relationship between the number of cracks in the ITZ and freeze-thaw cycles is established;(2) As the number of freeze-thaw cycles increases, the ITZ's micromechanical strength decreases, and its development width tends to increase;(3) The damage and debonding evolution mechanisms of sandstone-concrete ITZ under freeze-thaw cycles is revealed, and its micromechanical evolution model induced by freeze-thaw cycles is proposed.

Characterization of the Diamond-like Carbon Based Functionally Gradient Film

Diamond-like carbon coatings have been used as solid lubricating coatings in vacuum technology for their good physical and chemical properties. In this paper, the hybrid technique of unbalanced magnetron sputtering and plasma immersion ion implantation (Plll) was adopted to fabricate diamond-like carbon-based functionally gradient film, N/TiN/Ti(N,C)/DLC, on the 304 stainless steel substrate. The film was characterized by using Raman spectroscopy and glancing X-ray diffraction (GXRD), and the topography and surface roughness of the film was observed using AFM. The mechanical properties of the film were evaluated by nano-indentation. The results showed that the surface roughness of the film was approximately 0.732 nm. The hardness and elastic modulus, fracture toughness and interfacial fracture toughness of N/TiN/Ti(N,C)/DLC functionally gradient film were about 19.84 GPa, 190.03 GPa, 3.75 MRa.m1/2 and 5.68 MPa.m1/2, respectively. Compared with that of DLC monolayer and C/TiC/DLC multilayer, this DLC gradient film has better qualities as a solid lubricating coating.

Load Dependence of Nanohardness in Nitrogen Ion Implanted Ti6Al4V Alloy and Fractal Characterization

Three different nitrogen ion doses were implanted into a Ti6A14V alloy to improve its mechanical surface properties for the application of artificial joints. The titanium nitride phase and nitrogen element distribution profile were characterized with X-ray photoelectron spectroscopy （XPS）. Nano-indentation tests were carried out on the surface of the Ti6A14V alloy and implanted samples on a large scale of applied loads. The XPS analysis results indicate that nitrogen diffuses into the titanium alloy and forms a hard TiN layer on the Ti6A14V alloy. The nanohardness results reveal that nitrogen ion implantation effectively enhances the surface hardness of Ti6A14V. In addition, the nanohardness clearly reveals load dependence over a large segment of the applied loads. Thus a concept of nanohardness fractal dimension is first proposed and the dual fractal model can effectively describe nonlinear deformation in indentation areas on the Ti6A14V surface. The fractal dimension shows a decreased trend in two regions of applied loads, indicating a decrease of the self-similarity complexity in surface indentation owing to an increase in nanohardness after nitrogen ion implantation.

Microstructure and mechanical properties of as-cast(CuNi)100-xCox medium-entropy alloys

Microstructure and mechanical properties of non-equiatomic(CuNi)_(100-x)Co_(x)(x=15,20,25 and 30,at.%)medium-entropy alloys(MEAs)prepared by vacuum arc-melting were investigated.Results show that all the as-cast MEAs exhibit dual face-centered cubic(fcc)solid-solution phases with identical lattice constant,showing typical dendrite structure consisting of(Ni,Co)-rich phase in dendrites and Cu-rich phase in inter-dendrites.The positive enthalpy of mixing among Cu and Ni-Co elements is responsible for the segregation of Cu.With the increase of Co content,the volume fraction of(Ni,Co)-rich phase increases while the Cu-rich phase decreases,resulting in an increment of yield strength and a decrement of elongation for the(CuNi)_(100-x)Co_(x) MEAs.Nano-indentation test results show a great difference of microhardness between the two fcc phases of the MEAs.The measured microhardness value of the(Ni,Co)-rich phase is almost twofold as compared to that of the Cu-rich phase in all the(CuNi)_(100-x)Co_(x) MEAs.During the deformation of the MEAs,the Cu-rich phase bears the main plastic strain,whereas the(Ni,Co)-rich phase provides more pronounced strengthening.

Design and micro mechanical properties of nano-SiO_2 strengthened composite coatings towards remanufacturing

Nano-SiO2 particles strengthened Ni-based composite coating was designed and prepared on steel substrate. The structures and nanoparticle content of the nano-SiO2/Ni composite coating were determined by SEM, EDS and TEM; and the micro mechanical properties were tested by nano-indentation technique. The results show that 56% of particles in the solution are dispersed in size of less than 100nm, the content of nanoparticles co-deposited in the coating doubles and structure of the coating is more compact and uniform than that of Ni coating. Nano-SiO2/Ni coating exhibits excellent micro mechanical properties, and the nanohardness and elastic modulus are 7.81GPa and 198GPa, respectively, which are attributed to finer crystal strengthening, dispersion strengthening and high-density dislocation strengthening of nano-SiO2 particles to the composite coatings.

Development and characterization of hot dip aluminide coated stainless steel 316L

Stainless steel(SS)grade 316L is used for orthopedic implants due to its biocompatibility;yet the effort should be done to minimize the carcinogenic and inflammatory effects related to SS 316L implants.In this research,aluminide coating of Al–Si alloy on SS 316L is characterized by using optical microscopy,energy dispersive spectroscopy(EDS),nano-indentation and corrosion testing technique.Hot dip aluminizing process is used to coat the SS 316L specimens at 765°C for 2 min immersion time.Half of the specimens are also diffusion treated in a Muffle furnace at 550°C for 4 h to produce diffused specimens of SS 316L.Microstructural examination shows the formation of flat coating/substrate interface due to Si addition.EDS analysis confirms the formation of complex intermetallic at the coating/substrate interface which finally results in increasing the hardness and corrosion resistance properties of coating.

Determinationofelasticmodulus of claystone:Nano-/micro-indentation andmeso-compression tests used to investigate impact of alkaline fluid propagation over 18 years

Micro-mechanical properties of a claystone were tested after undergoing alkaline perturbation on site(Tournemire,CD borehole)for 18 years.In a saturated context and outside the excavation disturbed zone(EDZ),the claystone exhibits a 11.6-mm black rim at the cement/paste interface,which shows a different mechanical behaviour from the rest of the claystone.Three sets of measurements of elastic modulus were performed using:(i)nano-indentation tests with a constant indentation depth of 2 mm,(ii)microindentation tests with a constant indentation depth of 20 mm,and(iii)meso-compression tests with a constant displacement of 200 mm.The increase of the modulus of deformability in the black rim is between 15 GPa and 20 GPa according to the scale.Moreover,an overall decrease of the modulus of deformability from the smallest to the largest scale is observed in each zone.In view of the mineralogy and petrographic observations,higher values of modulus of deformability in the black rim are related to carbonate content and its distribution.Precipitation of cementitious carbonates as inclusions and very thin partings leads to hardening of the claystone.

Intratree Variation in Viscoelastic Properties of Cell Walls of Masson Pine (Pinus Massoniana Lamb)

In this study,Pinus massoniana Lamb at different heights,across the annual rings,and between earlywood and latewood was measured by X-ray diffraction and the chemical composition was analyzed by chemical treatment.Results indicated that the microfibril angle(MFA)decreased and the chemical composition changed little with the increase in height from 1 m to 9 m.In the radial direction,the MFA decreased and the chemical composition changed little with an increase in annual rings.The cellulose content of latewood was higher than that of early-wood.The viscoelastic changes of wood cell walls at different heights,across the annual rings by the method of quasi-static nanoindentation and dynamic modulus mapping techniques.Results indicated that the wood cell walls’elastic modulus increased,and the creep rate and creep compliance decreased with the increase in height;The elastic modulus and hardness increased with the annual rings.The cell walls’storage modulus increased and the loss modulus gradually decreased with an increase in height;the storage modulus gradually increased and the loss modulus decreased with the annual rings.

Atomistic simulations on adhesive contact of single crystal Cu and wear behavior of Cu-Zn alloy

Atomistic simulations are carried out to investigate the nano-indentation of single crystal Cu and the sliding of the Cu-Zn alloy.As the contact zone is extended due to adhesive interaction between the contact atoms,the contact area on a nanoscale is redefined.A comparison of contact area and contact force between molecular dynamics(MD)and contact theory based on Greenwood-Williamson(GW)model is made.Lower roughness causes the adhesive interaction to weaken,showing the better consistency between the calculated results by MD and those from the theoretical model.The simulations of the sliding show that the substrate wear decreases with the mol%of Zn increasing,due to the fact that the diffusion movements of Zn atoms in substrate are blocked during the sliding because of the hexagonal close packed(hcp)structure of Zn.

Scratching by pad asperities in copper electrochemical-mechanical polishing

Low dielectric constant materials/Cu interconnects integration technology provides the direction as well as the challenges in the fabrication of integrated circuits(IC) wafers during copper electrochemical-mechanical polishing(ECMP). These challenges arise primarily from the mechanical fragility of such dielectrics, in which the undesirable scratches are prone to produce. To mitigate this problem, a new model is proposed to predict the initiation of scratching based on the mechanical properties of passive layer and copper substrate. In order to deduce the ratio of the passive layer yield strength to the substrate yield strength and the layer thickness, the limit analysis solution of surface scratch under Berkovich indenter is used to analyze the nano-scratch experimental measurements. The modulus of the passive layer can be calculated by the nano-indentation test combined with the FEM simulation. It is found that the film modulus is about 30% of the substrate modulus. Various regimes of scratching are delineated by FEM modeling and the results are verified by experimental data.

Measurement of the Energy Absorbed during Nanoscale Deformation of Human Peritubular and Intertubular Dentin

Mineralized tissues are usually constructed of nanosized materials with ordered hierarchical structures. The main reason for their high load-bearing ability is the multi-scale hierarchy. It is important to have a method for measuring the energy absorbed during the nanoscale deformation of mineralized tissues. The objective of this study was to use a combination of nanoindentation and elastic-plastic mechanics techniques to measure the damage resistance of peritubular and intertubular dentin, based on the energy consumed in the plastic deformation regime and the volume created by the indents. The control materials were soda-lime glass, gold, and poly-methyl methacrylate (PMMA). Plastic deformation energy was calculated from the plastic part of load-displacement curves. The mean values of peritubular dentin and intertubular dentin were 3.8 × 109, and 5.2 × 109 J/m3, respectively, compared to glass, PMMA, and gold which were 3.3 × 107, 1.3 × 109, and 3.1 × 109 J/m3, respectively. This method can be applied to study the resistance of mineralized tissues or organic/inorganic hybrid materials to deformation at the nanoscale.

Exploring the Effect of Plasticity on the Phase Imaging of TM-AFM Through Molecular Dynamics Simulations

In the tapping-mode atomic force microscope(TM-AFM),the probe tip continuously taps the sample surface,which may cause plastic deformation of the sample and result in energy dissipation.The energy dissipation of the probe is closely related to the scanned phase image.To quantify the energy dissipation due to plastic indentations of the sample,this study utilized a combination of molecular dynamics(MD)simulations and experiments on single-crystal copper samples,including multiple nano-indentation tests.The energy dissipation of the probe due to the plastic deformation of the sample was calculated by integrating the hysteresis curve of the indentation depth versus the force applied to the indenter.The simulation results are in good agreement with the experimental ones.Both sets of results have demonstrated that the plastic energy dissipation decreases as the number of indentations increases,and eventually the energy of the probe tends to stabilize.This equilibrium energy dissipation is associated with other dissipation mechanisms.Furthermore,it was observed that,after hundreds of taps,the dissipated energy of plastic deformation could be ignored,implying that the scanned image may not reflect the plasticity information of the sample after multiple taps of the probe on the sample surface for scanning.