Indentation Area Research Articles

Tomato Fruit Shape Analysis Using Morphometric and Morphology Attributes Implemented in Tomato Analyzer Software Program

Reliable analysis of plant traits depends on the accuracy of scoring the phenotype. We report here on the efficacy of two methods in the detection of quantitative trait loci (QTL) controlling fruit morphology in three segregating tomato (Solanum spp.) F2 populations using the software program, Tomato Analyzer. The first method uses fruit morphology attributes such as fruit shape index, blockiness, pear shape, indentation area, and angles of the fruit along the boundary. The second method uses morphometric points to quantify shape. The morphometric data were subjected to principle components analysis (PCA). QTL that control the fruit morphology attributes and the morphometric PCA were identified that revealed that the methods were comparable in that they resulted in nearly identical loci. Novel attributes were added to Tomato Analyzer that improved versatility of the program in measuring additional morphological features of fruit. We demonstrated that these novel attributes permitted identification of QTL controlling the traits.

Micro-fabrication techniques applied to aluminosilicate glass surfaces: Micro-indentation and wet etching process

Micro-indentation and HF etching were explored as micro-fabrication techniques applied to glass surfaces. The effects of the aluminosilicate glass composition and of the etching conditions on the etching rate were investigated. It was found that the etching rate increased with increasing the ratio of Al 2O 3 to SiO 2 in the aluminosilicate glass. Etching parameters , such as pH, concentration and temperature of HF acid , had effects on etching rate. However, the effects of these parameters were much smaller at indented area than at non-indented area. The results indicated that the etching rate difference between the two areas, which is one of the key factors in the micro-fabrication technique, could be controlled with these parameters. And the phenomena can be well explained in terms of etching and leaching mechanism of aluminosilicate glass.

Higher accuracy analysis of instrumented indentation data obtained with pointed indenters

We review current practice for describing force–displacement curves from pointed indenters, highlighting the consequences of the simplifications normally adopted. We derive two corrections, the ‘variable epsilon factor’ and the ‘radial displacement correction.’ These are especially important for highly elastic materials such as fused silica where the combined corrections can amount to 13% in the contact area, significantly increasing the accuracy of hardness and modulus results. In contrast, the so-called beta factor has minor importance. We compare our analytical results with finite element (FE) calculations and experimental results. Indenter area functions, obtained using the corrections, agree well with independent direct measurements by a traceably calibrated metrological atomic force microscope (AFM). Further formulae are derived to calculate the complete force–displacement curve of conical indenters and the indentation elastic and total energy. These formulae immediately identify a physical material limit above which a cone cannot generate plastic deformation; for a Berkovich indenter this is a hardness-to-modulus ratio of 0.18.

Effect of partial recovery of zinc surface at room temperature after basal plane indentation

The effect of partial recovery of zinc surface at room temperature after basal plane indentation was detected and studied with a scanning tunneling microscope. It was found that indentation depth recovery depending on time occurs in one stage and recovery of lateral sizes in two stages with different activation energies, which are less than that of bulk zinc self-diffusion. Possible mechanisms of surface self-diffusion of zinc atoms leading to surface crystal growth were discussed. It was shown that the dynamics of effects observed on the sample surface in the indentation area after 15-min annealing at 100°C is associated with emergence of thermally generated vacancies from the sample bulk.

Nanogroove formation by ion irradiation on indentation-modified amorphousSiO2

Ion beams are widely used for micro/nanostructure fabrication with unique features ofthe energetic processes. In this work, we present a self-assembled nanostructurefabrication by ion irradiation with a patterned strain/stress field. The patternedstrain/stress field is introduced by micro-Vickers indentation to amorphousSiO2 (load = 100 mN). Afterirradiation of 60 keV Cu− ions, nanogrooves (width from 150 to 250 nm) were created at the indentation edge. Under the ionirradiation of a constant ion flux, the nanogroove size linearly increased with ion fluence from2 × 1016 to1.2 × 1017 ions cm−2. Comparison of indented samples after irradiation and thermal annealing suggests that thenanogrooving originates from ion beam interactions with residual stress/strain byindentation and that a non-thermal effect results from the ion irradiation processes.Cross-sectional TEM analysis showed that the grooves extend over 200 nm below thesurface, implying that the groove growth is not caused by surface diffusion. It is concludedfrom the results that the grooving is due to irradiation-induced mass transportaccompanied by vacancy aggregation at the interface between the indented andnon-indented areas.

Mechanism of the etching rate change of aluminosilicate glass in HF acid with micro-indentation

The etching rate of some kind of glass decreases with micro-indentation. This paper is concerned chiefly with the mechanism for aluminosilicate glass. The change of glass surface condition arising from the indentation and the etching has been examined with X-ray photoelectron spectroscopy (XPS). It was found that the leaching reaction observed through the HF acid etching at non-indented area was restricted at the indented area. The etching rate change should be attributed to the leaching mechanism.

Transmission electron microscopy studies and simulation of the indentation response of superelastic fullerenelike carbon nitride thin films

The highly elastic behavior of fullerenelike carbon nitride thin films on single crystal Si (001) substrates has been studied by nanoindentation. The films exhibit a microstructure of frequently bent and intersecting graphene sheets. Transmission electron microscopy of indented areas revealed no tendency to plastic deformation in the highly elastic and compliant film. Also, a unique deformation pattern in the Si substrate is observed, where a {111} facetted inverted pyramid of untransformed Si remained intact under the indenter with a retained CNx/Si(001) interface. Analytical approaches using the effective indenter method, supported by finite element methods, are employed to understand the nonlinear but fully elastic behavior of the coatings as well as to describe the critical parameters for the deformation and phase transformation of the Si substrate.

Fabrication of micro-structure on glass surface using micro-indentation and wet etching process

In order to improve the new micro-fabrication technology using micro-indentation and wet etching, in which the etching rate drastically decrease at the indented area and consequently micro-structure can be formed on the glass surface, the effect of the applying load on the etching rate change was investigated. The extent of the etching rate change was found to be almost constant irrespective of the amount of the applying load. Therefore, the height of the structure could be controlled simply by the etching depth as far as the densified portion remains beneath the glass surface. And some example micro-patterns were fabricated in this process. Various kinds of indentation methods were employed, including scanning a pointed tool under a load and wet abrasive blast. The patterns can be freely drawn by the use of numerical control (NC) machine. Mold pattern can be also applied, which enables drawing many lines simultaneously. In every method, the heights of the patterns were confirmed to be very uniform. This new type of the micro-fabrication method was referred to as “SMIL (Stress Masked Image Lithography)”.

On cracks and delaminations of thermal barrier coatings due to indentation testing: Experimental investigations

Rockwell indentation testing as a method of establishing the interfacial fracture toughness of thermal barrier coatings is investigated. To this end, indentation tests have been systematically performed on coatings with yttria-stabilized zirconia top coat deposited by electron beam physical vapor deposition. Specimens in “as-coated” condition and after heat treatment in air have been studied. Unexpectedly, indentation of the heat-treated samples resulted in smaller delaminations than the as-coated samples, suggesting an increase in fracture toughness for coatings subjected to elevated temperatures. Careful image analyses of the cross-section of the indented area show that the ceramic top coat undergoes a complex damage evolution during indentation that is altered by thermal treatment. The consequences of this are discussed and we note that care must be taken when evaluating fracture parameters for multilayered structures based on indentation testing.

Berkovich indentation-induced deformation behaviors of GaN thin films observed using cathodoluminescence and cross-sectional transmission electron microscopy

Presented in this study are the Berkovich nanoindentation-induced mechanical deformation mechanisms of metal-organic chemical-vapor deposition (MOCVD) derived GaN thin films, investigated by using the cathodoluminescence (CL) and the cross-sectional transmission electron microscopy (XTEM) techniques. The multiple “pop-in” events were observed in the load–displacement ( P– h) curves and appeared to occur randomly with increasing the indentation load. These instabilities are attributed to the dislocation nucleation and propagation. CL images of nanoindentation show a very well-defined rosette structures with the hexagonal system, and clearly display the distribution of deformation-induced extended defects/dislocations which affect CL emission. By using focused ion beam (FIB) milling to accurately position the cross-section of an indented area, XTEM results demonstrate that the major plastic deformation is taking place through the propagation of dislocations. The present observations are in support to the massive dislocations activities occurring underneath the indenter during the loading cycle. No evidence of either phase transformation or formation of micro-cracking was observed by using XTEM observations. We also discuss how these features correlate with Berkovich nanoindentation-induced defects/dislocations microstructures. Finally, this study has significant implications for the extent of contact-induced damage during fabrication of GaN-based optoelectronic devices.

Enhanced nanoparticle formation by indentation and annealing on 2 MeV Cu ion-implanted SiO 2

Enhancement of surface plasmon resonance (SPR) in optical absorption has been found on Cu ion-implanted SiO 2 substrate modified by micro-indentation and post-annealing. Micro-indentation effects on surface plasmon resonance (SPR) in optical absorption have been studied to control nanoparticle formation in Cu ion-implanted SiO 2 substrate. The SiO 2 was firstly implanted with 2 MeV Cu 2+ ions at an ion flux of 4 μA/cm 2, up to a fluence of 6 × 10 16 ions/cm 2. After the ion implantation, dot-array patterns of micro-indents were made by a micro-Vickers hardness tester, and followed by annealing at 600 °C in vacuum for 1 h. The optical absorption spectra of the indented region and the non-indented flat region were measured and compared with each other. After post-annealing at 600 °C, the indented area showed higher absorbance of SPR at 2.2 eV than that of the flat region annealed under the same annealing conditions. The TEM study shows larger and denser Cu precipitates inside the indentation than those in the flat area. The results indicate that the defects produced by indentation enhance the atomic migration in the plastic zone during thermal relaxation process, resulting in promoting the enhanced precipitation of Cu nanoparticles.

Cathodoluminescence and Cross-sectional Transmission Electron Microscopy Studies for Deformation Behaviors of GaN Thin Films Under Berkovich Nanoindentation

In this study, details of Berkovich nanoindentation-induced mechanical deformation mechanisms of metal-organic chemical-vapor deposition-derived GaN thin films have been systematic investigated with the aid of the cathodoluminescence (CL) and the cross-sectional transmission electron microscopy (XTEM) techniques. The multiple “pop-in” events were observed in the load-displacement (P–h) curve and appeared to occur randomly by increasing the indentation load. These instabilities are attributed to the dislocation nucleation and propagation. The CL images of nanoindentation show very well-defined rosette structures with the hexagonal system and, clearly display the distribution of deformation-induced extended defects/dislocations which affect CL emission. By using focused ion beam milling to accurately position the cross-section of an indented area, XTEM results demonstrate that the major plastic deformation is taking place through the propagation of dislocations. The present observations are in support to the massive dislocations activities occurring underneath the indenter during the loading cycle. No evidence of either phase transformation or formation of micro-cracking was observed by means of scanning electron microscopy and XTEM observations. We also discuss how these features correlate with Berkovich nanoindentation produced defects/dislocations structures.

Flexural strength, fatigue life, and stress‐induced phase transformation study of Y‐TZP dental ceramic

Yttria partially-stabilized zirconia polycrystalline (Y-TZP) has been the subject of extensive research because of its high strength and toughness. The aim of this study was to evaluate the biaxial flexural strength, fatigue life, and to investigate in more detail on single cycle specimens, the pressure-induced phase transformation of a Y-TZP dental ceramic using Raman microspectroscopy. Thirty standardized discs (15 x 1.2 mm(2)) were used to examine the biaxial flexural strength (ISO 6872 standard) using a Dartec HC10 Servohydraulic testing machine (Zwick Ltd., UK). The specimens were also submitted to Vickers hardness (on polished and as-received surfaces within the same specimen) and dynamic fatigue test. The initial bulk phases were examined via X-ray diffraction and the local phase transformations that occurred in the zirconia induced by the various Vickers indentation loads (20-50 kg) were examined via Raman microspectroscopy on single cycle specimens. The fracture surface after biaxial flexural testing was also examined via Raman spectroscopy. The Cercon specimens tested had flexural strength and Weibull modulus (m) of approximately 823.3 (+/-114.7) MPa and 8.3, respectively. As-received surfaces (1378.7 +/- 51.8 Hv) had slightly higher hardness value compared with polished surfaces (1354.33 +/- 50.9 Hv); however, two-way analysis of variance showed no significant difference in hardness values between polished and as-received surfaces (P > 0.05). Additionally, the specimens survived to 5 x 10(5) cycles when using a load of 70% of the mean biaxial flexural strength or lower. Raman microspectroscopy showed transformation of tetragonal to cubic and monoclinic phases within the indentation area. The fraction of monoclinic phase showed only limited variation with load or distance from the center to indentation edge. The level of cubic phase, however, was greatest at the indentation center. Transformation to cubic phase was observed on the lower surfaces (tension side) of fractured specimens. It was also observed near the specimen center exposed upon fracture. In the latter region an increase in monoclinic phase was additionally observed. Further work will be carried out using Raman microspectroscopy to assess the effect of fatigue on phase transformations. The zirconia based ceramic has mechanical properties that may allow it to withstand the loading found in posterior areas. Transformation toughening was found when high loads impacted on the surface of zirconia. However it should be born in mind that this work was not carried out on veneered specimens, which exhibit different failure modes.

Static Indentation Response of H30 Foam ‐ an Experimental and Computational Study

This article presents an approach for assessing the damage resistance of H30 rigid foam subjected to local static loading. The main goal of the experimental part of this paper is to obtain the loaddisplacement response of foam beam specimens under static indentation by steel cylindrical indentors for both loading (indentation) and unloading stages. The instant residual dent magnitude is also measured in the testing. The nonlinear character of the mechanical behavior and the formation of a residual dent (after unloading) are attributed to local crushing of the foam in the zone directly under the indentation area. A visual inspection of a lateral surface of the foam specimens after indentation tests revealed that the local damage underneath the indentor consists of crushed and highly compacted foam, while the rest of the specimen is almost undeformed. A two‐dimensional numerical model is developed to simulate the static indentation response using the ABAQUS computer code. No overall bending of the foam specimens is assumed. The finite element modeling procedure takes into account both physical and geometrical non‐linearities. In order to simulate the plastic part of the response, the model employs the *CRUSHABLE FOAM and *CRUSHABLE FOAM HARDENING options. The modeling procedure is capable of analyzing indentation as well as unloading of foam beam specimens. Thus, the instant residual dent can be predicted. Results generated by this model exhibit good correlation with indentation tests data, thus substantiating its validity.

Controlled electrostatic methodology for imaging indentations in documents

The electrostatic process for imaging indentations on documents using the ESDA device is investigated under controlled experimental settings. An in-house modified commercial xerographic developer housing is used to control the uniformity and volume of toner deposition, allowing for reproducible image development. Along with this novel development tool, an electrostatic voltmeter and fixed environmental conditions facilitate an optimization process. Sample documents are preconditioned in a humidity cabinet with microprocessor control, and the significant benefit of humidification above 70% RH on image quality is verified. Improving on the subjective methods of previous studies, image quality analysis is carried out in an objective and reproducible manner using the PIAS-II. For the seven commercial paper types tested, the optimum ESDA operating point is found to be at an electric potential near −400 V at the Mylar surface; however, for most paper types, the optimum operating regime is found to be quite broad, spanning relatively small electric potentials between −200 and −550 V. At −400 V, the film right above an indented area generally carries a voltage which is 30–50 V less negative than the non-indented background. In contrast with Seward's findings [G.H. Seward, Model for electrostatic imaging of forensic evidence via discharge through Mylar–paper path, J. Appl. Phys. 83 (3) (1998) 1450–1456; G.H. Seward, Practical implications of the charge transport model for electrostatic detection apparatus (ESDA), J. Forensic Sci. 44 (4) (1999) 832–836], a period of charge decay before image development is not required when operating in this optimal regime. A brief investigation of the role played by paper-to-paper friction during the indentation process is conducted using our optimized development method.

Using the ratio: maximum load over unload stiffness squared, Pm/Su², on the evaluation of machine stiffness and area function of blunt indenters on depth-sensing indentation equipment

Depth sensing indentation study was conducted in a Fischerscope H100V machine, equipped with a Vickers indenter with a tip roundness of approximately 1330 nm. Tests were carried out on soda-lime glass, fused silica, sapphire, aluminum (1100 alloy), high alloyed steel, titanium and copper. The widely used iterative method of Oliver and Pharr was unsuccessful in the attempts to analyze machine compliance and indenter area function. Therefore, an alternative procedure was adopted. The alternative procedure is based on the ratio between maximum load and unload stiffness squared, Pm/Su². It was found that this procedure, which is not iterative, gives good results. A careful study of the Pm/Su² ratio, lead us to conclude that the Fischercope machine has a low compliance which depends on the sample mounting. This low compliance in conjunction with the recent discovery of the dependence of beta factor on the tip roundness/maximum depth ratio, which appears in the relation between contact stiffness and contact area, explains why the iterative method does not converge. However, variations in beta and machine compliance produces deviation on the hardness and elastic modulus lower that 6% with respect to expected values for the materials and the machine studied in this work.

Probing elastic modulus and depth of bottom-supported inclusions in model tissues using piezoelectric cantilevers

We have experimentally investigated the depth sensitivity limit of a piezoelectric cantilever tissue elastic modulus sensor and simultaneously determined the elastic modulus and the depth of a tumor directly. Using model tissues consisting of bottom-supported modeling clay inclusions of various depths in a gelatin matrix, we empirically determined that the depth sensitivity limit of a piezoelectric cantilever sensor was twice the linear dimension of the indentation area (or the cantilever width). Knowing the depth sensitivity limit of the individual cantilever sensor as input and treating a model tissue that has the gelatin matrix on top and the modeling clay inclusion at the bottom as two springs in series, we showed that the elastic moduli and depths of the hard inclusions could be simultaneously determined with the elastic modulus profiles measured by two cantilevers with different widths as input.

Structural heterogeneity of pharmaceutical compacts probed by micro-indentation

Indentation has been used for several decades to conveniently assess the hardness and modulus of various compacts. However, this measurement is dependent on the size of the indentation area from a few nanometers to several millimeters, which is determined by the maximum indentation force (MIF). Micro-indentation often loses its ability to give an accurate representation of the hardness due to its relatively small micron-size indentation area compared with the dimensions of the structural inhomogeneity of compacts. This study used a different approach to micro-indentation by examining whether this method can probe the inhomogeneity of compacts with varying MIF. Two typical pharmaceutical excipients, one brittle and one ductile, were used as model compacts. The representative hardness and modulus values were available when the MIF was >1000 mN. Changes in the standard deviation of the indentation hardness reflected the structural inhomogeneity of the compacts, which was found to increase with decreasing MIF to below 800 mN in the case of the microcrystalline cellulose compacts. The information on the structural inhomogeneity obtained by micro-indentation appears to be consistent with the observations from microscopy investigations. Anisotropy and other related structural information could be readily obtained by probing the two different surfaces of compacts with changing MIF, one parallel and the other perpendicular to the compaction pressure direction.

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

Abstract Three different nitrogen ion doses were implanted into a Ti6Al4V 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 Ti6Al4V 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 Ti6Al4V alloy. The nanohardness results reveal that nitrogen ion implantation effectively enhances the surface hardness of Ti6Al4V. 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 Ti6Al4V 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.

Berkovich nanoindentation and deformation mechanisms in GaN thin films

The deformation mechanisms of GaN thin films obtained by metal-organic chemical vapor deposition (MOCVD) method were studied using nanoindentation with a Berkovich diamond indenter, micro-Raman spectroscopy and the cross-sectional transmission electron microscopy (XTEM) techniques. Due to the sharpness of the tip of Berkovich indenter, the nanoindentation-induced deformation behaviors can be investigated at relatively lower load and, hence, may cover wider range of deformation-related phenomena over the same loading range. The load–displacement curves show the multiple “pop-ins” during nanoindentation loading. No evidence of nanoindentation-induced phase transformation and cracking patterns were found up to the maximum load of 300 mN, as revealed from the micro-Raman spectra and the scanning electron microscopy (SEM) observations within the mechanically deformed regions. In addition, XTEM observation performed near the cross-section of the indented area revealed that the primary deformation mechanism in GaN thin film is via propagation of dislocations on both basal and pyramidal planes. The continuous stiffness measurement (CSM) technique was used to determine the hardness and Young's modulus of GaN thin films. In addition, analysis of the load–displacement data reveals that the values of hardness and Young's modulus of GaN thin films are 19 ± 1 and 286 ± 25 GPa, respectively.